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SDMS Document 115568 FINAL REMEDIAL INVESTIGATION REPORT Virgin Island Chemical Site St. Croix, U.S. Virgin Islands VOLUME in APPENDIX H '.''Si- Prepared By: McLaren/Hart, Inc. 25 Independence Boulevard Warren, NJ 07059 Prepared For: Berlex Laboratories, Inc. 15049 San Pablo Avenue P.O. Box 4099 Richmond, CA 94804 and Pharmacia & Upjohn 7171 Portage Road Kalamazoo, MI 49001 f3iS Vv, February 2000 SGjpN^i ' IT^Tpgy ' TP^HN9L@€Y ' §@l-yT!@N§ 3 04 2 63 m FINAL REMEDIAL INVESTIGATION REPORT Virgin Island Chemical Site St. Croix, U.S. Virgin Islands VOLUME i n APPENDIX H Prepared By: McLaren/Hart, Inc. 25 Independence Boulevard Warren, NJ 07059 Prepared For: Berlex Laboratories, Inc. 15049 San Pablo Avenue P.O. Box 4099 Richmond, CA 94804 and Pharmacia & Upjohn 7171 Portage Road Kalamazoo, MI 49001 February 2000 3 0 4 2 6 4 f m m 304265 APPENDIX H QA/QC SUMMARY PACKAGES AND CHECKLISTS # 304266 SDG No. 97129 TOCy MetalSy and Inorganic Checklist 304267 ^2A A, QA/QC Review of Alkalinity Data for Pace Analytical SDG# 97129 October 30, 1997 Holding Times: Samples were analyzed within holding times. Initial and Continuing Calibration Verification: Data not applicable. Blanks: The method blank reported alkalinity as not detected. Spike Sample Recovery: Data not applicable. Duplicates: Data not provided in this SDG. Laboratory Control Sample: Alkalinity (102%) had a percent recovery within control limits (80- 120%) for the soil LCS. G:\STAFF\DANNE\Island\978129.ALK.wpd 304268 QA/QC Review of Total Organic Carbon (TOC) Data for Pace Analytical SDG# 97129 October 30, 1997 Holding Times: Samples were analyzed within holding times. Initial and Continuing Calibration Verification: All percent recoveries were within control limits (85-115%). Blanks: The method blank reported TOC as not detected. Spike Sample Recovery: TOC (83%) had a percent recovery within control limits (75-125%i) for the spike sample. Duplicates: TOC (4%) had a relative percent difference below the allowable maximum (20%) for the duplicate sample. Laboratory Control Sample: TOC (106%) had a percent recovery within control limits (80-120%)) for the soil LCS. G:\STAFF\DANNE\Island\9 78129.TOC.wpd 304269 SD&: 97/21 Evaluation of Metals Data for the Contrac± Laboratory Program (CLP) based on SOW. 3/90 (SOP R e v i s i o n XT) ?7>RZD EY: .'.1 t /— • - ' ^ i _ .—- • - ^ • - '» DATE: ' • ^ ^ - ? s Hahi: Sr.eirii, (?aaliT/ Assurance Qiemisr. Tcxic and kazardous Waste Section ; "•FT.avZD BY: •.;: <-.AA Kevin K'Jbxk, Qiief Tcxic arid Hazardous Waste Section ?ri3VED EY Robert Runyon, thiKf Monitoring K^anagerent Branch DATE: DATE: -'. '^ -f-A^— 304270 STATiTARD OPERATING TPPOCEDJEE Evsduation of Metals Data for the Date: Jan. 1992 Contract laboratory Program Nccnber: HW-2 Revision: 11 Socpe This procedure is applicable to inorganic data obtained frcrn uontractor laboratories vorking for Hazardous Waste Site Contract laboratory Program (CLP) . The data validation is based upcn analytical and quality assurance requirements specified in Statement of Work (SOW) 3/90 . Responsibilities - Data reviewers vill ccrplete the following tasks as assigned by t:he Data Review Coordinator: For 2 total rgview: 1 Data Assessment - "Total Rgviev-lnorcTanies" Chec3clist Ar»pendix (A.H. ^ e reviewer rrwiist answer every question on the checklist. iL ta Assessnient - Data Asses^mpnt KeLrrative (Apoepr^W A.2) Ihe answer on the checklist musr ratch the action in the narrative (appendix A.2) and on Form I's. Do not use pencil to write the narrative. .2 Ccntraot Non-Cenoliance - EH3 Report (Appendix A.3) lhis report is to be cxxpleted only when a serious contract violation is encc-..ir.t.ered, cr upon the request of the Data Validation Task Monitor, or Technical Project Officer (T?0). Foruard 5 copies: one each for internal files, appropriate Regional TPO, Sample Management Office (SMO) and last two addresses of Ilailing List for Data Reviewers (Appendix A.4). In other cases, all contract violations should be appended to the end of the Data Assessment Narrative (Sec. A.2.2). .4 CLP Data Ti^ssessment Burrr^-ry Fo-rwi .1 Appendix A.5 Fill in the total njmber of analytes einalyzed by different cinalyses and the nurber of analyties rejected or flagged as estiratad due to corresponding CTjaliry control criteria. Place an "X" in boxes where analyses were not performed, or criteria do not apply. .2 Appendix A.6 Cata reviewer is also required to fill out Inorganic Regioral Data Assessment form (/appendix A.7) provided by EPA Headquarters. Codes listed on the form ^ ^ 1 1 1 be used tjo describe the Data Assessment SuiTcrar\'. 304271 STWiT^PD OFraATING iWXlIUPE .le: Evaluation of Metzals Data for the Contract Laboratory Program Date: Jan. 1992 Nvacber: HW-2 Revision: 11 1.5 Data Reviev Log; It is iHniiiiHnded that each data reviewer sivxild maintain a log of the reviews caipleted to include: a. date of start of case reviev; b. date of ccnpleticn of case review c. site d. case number e. ccntract laboratory f. number of samples g. matrix h. hours worked i. reviewer's initials Telephone Record Log - the data reviewer should enter the bare facts of inquiry', before initiating any phone conversation with CLP laboratory. After the case review has been caipleted, rail white copy of Telephone Record Log to the laboratory and pink copy to SMO. File yellow copy in tihe Telephone Reooru Log folder, and attach a xerox copy of the Telephone Record Log to the ccrpleted Data Assessment Narrative (Appendix A.2). 1.7 Forw?Lrded Paperwork ..7-1 Upon completion of review, the following are to be .forwarded to the Regional Sarple Control Center (RSCC) located in the Surveillance and Monitoring Branch: a. data package ccrpleted data cissessment checklist (Appendix A. 1,original) £:-:o Ccntract Ccnpiiance Screening (CCS) Record cf Ccmm"JL-vication (copy) CL? Reanalysis Request/Approval Record (original + 3 copies) Appendix A.6 (original). b. c. d. e. f. '.2 Foruard 2 copies of completed Eat:a Assessment Narrative (Appendix A.2) along with 2. copies of the Inorganic Data Assessment Form (Appendix A. 6) and Telephone Record Log , if any,: one each for appropriate Regional TPO, and the other one to EPA EMSL office in Las Vegas. The addresses of TPOs and EPA office in Las Vegas are given in Appendix A-4. 3 Filed Paperwork - Upon ccsrpleticn of review, the following are t a be filed within K:-3 files: a. Two copies of completed Data Assessment Narrative (Appendix A.2) each carr,'ing — Appendix A. 6. b. Telephone Record Log (ccpy) c. SI'D Report (copy Appendix A-3) d. CLP Reanalysis Request/Approval Record (copy) 304272 STANDARD OFS^ATDG FHXnURE Le: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Rsvisicn: 11 Data Cocpleteness Each data package is checked by a Regional Sanple Control Coordinator (RSSC) for completeness. A data package is ^le^csTmeH to be corpletfi when all the deliverables required iinder the contract are present. If a data package is incctiplete, the RSSC would call the laboratory for missing document(s). If the laboratory does not respond within a week, SMO and HMB coordinator of Ragicn H vill be notified. Re-iecrlon of Data - All values determined to be unacceptable on the Inorganic Analysis Data Sheet (Form I) must be lined over with a red pencil. As soon as any reviev; criteria causes data to be rejected, that data can be eliminated frcn any further reviev or consideration. • Acceptance Criteria - In order that reviews be consistent among reviewers, acceptance criteria as stated in Appendix A.l (pages 4-25) should be used. Additional guidance 'can be found in the National Inorganic Functional Guidelines of October 1, 1989. EM3 Contract Ccrsliance Sgreeniixr (CCS^ - This is intended to aid reviewer in locating any problems, both corrected and uncorrected. However, the validation should be carried out e-ven if CCS is not present. Resubrdttals received frcn laboratory in response to CCS .'rust be used by the reviewer. Request for Reanalysis - Data reviewers must note all items of contract non-compliance v.lthm Data Assessment Narrative. If holding tires and sample storage times have not been exceeded, TPD ray request reanalysis if items of non-ccrpliance are critical to data assessment. Requests are to be made on "CLP Re-Ar^alysis Request/Approval Record". Record of Ccrramication - Provided by the Regionad Sample Control Center (RSCC) to indicate which data packages have been received and are ready to be reviewed. Rounding off r/jmbers - The data reviewer will follow the standard practice. 304273 STANDARD OPERATOJC FKXEDRE E^'aluation of Metals Data for the Contract laboratory Program Appe-ndix A.l: Data Assessment - Contract Carpi iance (Total Review) Date: Jan. 1992 Nunber: HW-2 Revision: 11 1 Contract Cccpliance Screer-iria Report- (CCS) - Present? ACTION: If no, ccntact RSCC. 2 Reoord of Ccctminication (frcrn R90C) - Present? ACTION: If no, request from RSCC. 2 Trip Report - Present and ccrplete? ACTION: If no, contact RSCC for t r i p report. ^ ^ m p l e Traffic Report - Present? Legible? ACTION: If no, request from Regional Sample Control Center (RSCC). Ccr/er Paoe - Present? Is cc/er page properly filled in and signed by the lab manager or the manager's designee? ACTION: If no, prepare Telephone Record Log, "and contact laboratory. Do numbers of samples correspond to numbers on Record of Ccr7r.^J.cation? Do sarple numbers on cover page agree with sample numbers on: (a) Traffic Report Sheet? ' c - > 0CJT (b) Form I ' s ? ON: If no for any of the above, ccntact RSCC for clarification. iES. m IIZA C ] [ ] [ ] [ ] [ ] _ X _ A _ X [J^] _ X _ _ ^ [ ] J i 304274 STANI^iRD OFIRATING PROCEDURE .le: Evaluation of Metals Data for the Contract Laboratory Program Appendix A.l: Data Assesanent - Ccntract Ccmpliance (Total Review) Date: Jan. 1992 Nunber: HW-2 Revision: 11 rom I to rx I^ BQ. liZA .6-1 Are all the Form I through Form IX labeled with: Laboratory name? Case/SAS number? EPA sample No.? SDG No.? Contract No.? Correct units? Matrix? ACTION: If no for any of the above, note under Contract Problem/Non-Ccrpl iance section of the "Data Assessment Naurrative". .C.2 Do any ccmputation/transcription errors exceed 10% of reported values on Forms I-ZX for: (NGTE: Check all forms against raw data.) (a) a l l analytes analyzed by ICP? (b) a l l analytes analyzed by GFAA? (c) a l l analytes analyzed by AA Flame? (d) Mercury? (e) Cyanide? ACTION: If yes, prepare Telephone Log, contact — laboratory for corrected data eind correct errors with red pencil and initial. [ ] [JI] [JU [.:L] ^ y. t») r 1 r 1 r t i t > i ^ ^ K 1^ ^ 304275 STANDARD OPERATHC HRDCEDURE e: Ev'aluation of Jtetals Data for the Date: Jan. 1992 Contract Laboratory Program Nunber: HW-2 Appendix A.l: Data Assessment - Contract Pevisicn: 11 Compiiance (Total Review) — ^ _ ^ ^ .7 Raw cata .7.1 Digestion Log* for flame AA/ICP (Form XIU) present? f ^ 1 Digestion Log for furnace AA Form XTIT present? [ ] X. Distillation Log for mercury Form X H I present? [ Y- 1 Distillation Log for cyanides Form XIII present? f X> 1 Are pH values (pH<2 for all metals, pH>12 for cyanide) present? [ ] X^ *Wei(^ts, dilutions and volumes used to obtain values. ^ ^ Percent solids calculation present for soils/sediments? [_J—} Are p' -ation dat:es present on sample preparation logs sheets? .7.2 Keas-^_:._-it read out record present? ICP Flame AA Furnace AA Mercury • Cyanides ,.7.3 Are a l l raw data to support a l l sample analyses and QC operations present? Legible? Properly Labeled? ACTION: If no for any of the above questions — in sections A.1.7.1 through A.1.7.3, write Telephone Record Log and contact laboratory for resubtiuttals. r"^i [ j ^ ] [ ] [ 3 [ • ^ ] [ X J f_i^3 [JL] r X i X Y:' 304276 STANDARD OPERATING PROCEDURE Evaluation of hfetals for the Contract Date: Jan. 1992 Laboratory Program Number: HW-2 Appendix A.l: Dat:a Assessment - Ccntract Revision: 11 Compliance (Total Review) YES m H ^ Holding Tirv^q - (aqueous and soil sasples ) (Examine saitple traffic reports and digestdcn/distillat:icn logs.) Mercury analysis (28 days) exceeded? f X l Cyanide distillation (14 days). . . . . exceeded? f ^ 1 Other Metals analysis (6 months).... exceeded? f ^ 1 HTIE: Prepare a list cf all saitples and analytes for which holding times have been exceeded. Specify the number of days from date of collection to the date of preparation (frtm raw data). Attach to checklist. ACTION: If yes, reject (red-line) values less than Instrument Detection Limit (IDL) and flag as estimated (J) the values above IDL even though sample(s) vas preserved properly. Is pH of aqueous sanples for: Metals Analysis >2? [ ] Cyanides Analysis <12? [. Action: If yes, flag the associatied metals and cyanides data as estimated. Form I (Final Data) Are all Form I's present and ccrplete? r X l ACTION: If no, prepare telephone record log and contact laboratory for suixiittal. Are correct units (ug/1 for waters and mg/kg for soils) indicated on Form I's? [_^] Are soil sample resultis for each peurameter corrected for .^ percent solids? [ Xl Are all "less than IDL" \alues properly coded with "U"? [ X l T 304277 STANDARD OPERATING FRDCEDCIRE tie: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Nunber: HW-2 Appe.ndix A.l: Data Assessment - Cut-;tract Revision: 11 Coitpliance (Total Review) ^^ m H2K Are the correct concentration cualif iers used with final data? * f Y ^ ftCTICM; If no for any of the above, prepare Telephone Record Log, and ccntact laboratory for corrected data. 1.9.3 Are EPA sample H s and corresponding laboratory sample ID * s the same as on the Cover Page, Form I's and in the raw data? [ X^l Was a brief physical description of samples given . , on Form I's? [_X] Was the dilution of any sample diluted beyond the requirements of the contract noted on Form I or Form xrv? f Nv.1 ACTION: If no for arsy of the above, rx3te under Contract-Prcbl em/Non-Oorpl iance of the"Data Assessment Narrative". Calibration Is record of at least 2 point calibration present for IC? analysis? ^ A^ Is record of 5 point calibration present for ^ Hg analysis? f /\1 Is record of 4 point calibration present for: Flame AA? [ ] Vf, Furnace AA? [ ] X Cyanides? [ X l Is one calibration standard at the CRDL level for all AA (except Hg) and cyanides analyses? [ X 1 ACTION: If no for any of the above, writze in the Contract Proble.m/Non-Ccrpliance section of the "Cata Assessment Narrative". 304278 STANDARD OPERATING PROCEDURE :le: Ev'aluation of Itetals Data for the Contract Laboratory Program Appendix A.l: Data Assessment - Ccntract Compliance (Total Review) Date: Jan. 1992 Nunber: HW-2 Revision: 11 ,10.2 Is correlaticn coefficient less than 0.995 for: Mercury Analysis? _ cyanide Aralysis? _ Atxtnic Absorption Analysis? _ ACTION: If yes, flag the associated data as estimated. NCTE: The data validator shall calculate the correlation coefficient using concerrtraticns of the standards and the corresponding instrument response ( e.g. absorbance, peak area, peak height, etc.). 1.10.3 IS£ ACTION: In the instance v^ere less than 4 stiandards are measured in absorbance (or peak area, peak hei(^t,etc.) mode, are the remaining standards anadyzed in concentration mode immediatiely after calibration within ilO% of the true values? [ ] If no, flag th& associated datia as estimated if standards are not within +10% of true values. Do not flag the data as estimated in linear range indicated by good recovery of standard(s). m [ ] Elh X Form II A (Initial and ContinuinQ Calibration Verification)- Present and complete for every metal and cyanide? Present and ccrplete for AA and ICP when both are used f cr the same analyte? ACTION: If no for any of the above, prepare Telephone Reoord Log and contact laboratory. L1.2 Circle on each Form IIA all percent recoveries that are outiside the contract windows. Are all calibration standards (initial and continuing) — vithin control limits: Metals- 90-110%R? Hg - 80-120%R? cyanides- 85-115%R? [JI] [ ] [ ] [JL] [X] _ JI X 304279 STAJIDARD OPERATING PROCEDURE "^Valuation of Ifetals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 Ccnpliance (Total Review) • '• ^ ^ N7A" ACnCM: Flag as estimated (J) all positive data (not flagged with a "U") analyzed between a calibraticffi standard with %R between 75-89% (65-79% for Hg; 70-84% for CN) or 111-125% (121-135% for Hg; 115-130% .for CN) neoovery and nearest good calibration standard. Quzdify results <IDL as estimated (UJ) if the ICV or OC7 %R is 75-89% (CN, 70-84% ; HG, 65-79%). Reject (red-line) as imaooeptable data if recovery of the ICV or CCV is outside the range 75-125% (O^, 70-130%; Jig, 65-135%). (j^ialify five samples on either side of verification standard out of control limits. L1.3 Was continuing calibration performed every 10 sanples v, or every 2 hours? [__i] Was ICV for cyanides distilled? f X ] ^cnON: If no for any of the above, write in the Contract-Prcblem/Non-Ccrpliance section of the "Data Assessment Narrative". ,12 Form II B (CRDL Standards for AA and ICP) - .12-1 Was a C3^L standard (CRA) analyzed after initial y , calibration for all AA metals (except Hg)? [ ,Xl Was a mid-range calib. verification standard distilled and analyzed for cyanide analysis? [ ] >^ Was a 2XCRDL ( or 2xIDL when IDI>CRDL) analyzed (CRI) for each ICP run? * f J\] (Note: CRI for AL,Ba,Ca,Fe,Mg,Na,or K is not required.) ACTION: If no for any of the above, flag as estimated all data falling within the affected ranges. The affected ranges are: AA Ansilysis - **True Value + CRDL ICP Aralysis - **True Value + 2CRDL CN Analysis - **True Value + 0.5 x True Value. U) o lO 00 o rje value of CRA, CRI or nid-range standard. Substitute IDL for CRDL when IDL > CRDL. •pute the ccnce-ntration of the missing mid-range standard from the calibration range. STANEftRD OPSVOriNG PROCEDURE :tle: Evaluation of Metals Data for the Contract Laboratory Program Appendix A.l: Data Assessment - Ccntract Ccnpiiance (Total Review) Date: Jan. 1992 Nonber: HW-2 Revisicn: 11 ,12.2 Was CRI analyzed after ICV/ICB and before the final OCV/CCB, and twice every eit^t hours of ICP run? AgnON; If no, write in Contract Problem/Nan-CoBpliance Section of the "Data Assesanent Narrative". .12.3 Circle on each Form H E all the percent reooveries that are outside the acceptance windows. Are CRA and CRI standards within cantrol limits: Metals 80 - 120%R? Is mid-range standard within control limilLs: YES [Ji] [ ] cyanide 80 - 120%R? [ ] ACTION: Flag as estimated cdl sample results within the affected range if the recovery of the standard is between 50-79%; flag only positive data within the affected range if the recovery is between 121-150%; reject all data within the affected range if the recovery is less than 50%; reject only positive data within the affected range if the recovery is greater than 150%. Qualify 50% of the samples on either side of CRI standard outside the control limits. Note; Flag or reject the final results only when sample raw data aure within the affected ranges and the CRDL standards are outside the acceptance windows. m N/A X ,13 Form III (Initial and Continuing Calibration Blan)C3) ,13.1 Present ax>d caiplete? For both AA and ICP when both are used for the same analyte? Was an initial calibration blank analyzed? ~" Was a continuing calibration blank analyzed after every 10 sar:ples or every 2 hours (which ever is more frequent)? [-A] [ ] [ALi _ > ^ 304281 STANIARD OPERATING FRCXZEDURE Evaluation of hfetais Data for the Date: Jan. 1992 Contract Laboratory Program Nunber: HW-2 Appendix A.l: Data Assessnent - Ccntract Revisicn: 11 Coiplianoe (Total Review) jEs. m N/A JCTTOJ: If no, prepare Tel^ahcne Record Log, ccntact laboratory and write in the Contract-Problems/ Non-Ccrplianoe section of the "Data Assessment Narrative". .13.2 Circle on each Form III all calibratzicn blank values that are above C3^DL (or 2 x IDL vAien IDL > C3^DL). Are cdl calibration blanks (when IDLcCRDL) less than or equal to the Contract Required Detecticn Limits (CRDLs)? r X ] Are all calibration blanks less than two times ^ Instrument Detection Limit (v*ien IDLX3^DL)? [ ] _ K ACTION: If no for any of the above, flag as estimated (J) positive sample results when raw sample value is less than or equcd to calibration blank value anadyzed between calibration blank with value over CRDL (or 2xIDL) and nearest good calibration blank. Flag five samples on either side of the calibration blank outside the cantrol limits. 14 FORM III (Preparation Blank) - (Note: The preparation blcink for mercury is the same as the calibration blank.) .l-;.l Was one prep, blank analyzed for: each Sample Delivery Group (SDG)? r \ 1 each batch of digested sanples? r "Xl each matrix type? r X 1 both AA and ICP when both are used for ^^ the same analyte? [ ] X ACTION: If no for any of the above, flag as estimated (J) all the associated positive data <10 X IDLs for which prep, blank - was not analyzed. NOTE: If only one blank was analyzed for more than 20 samples, then first 20 samples analyzed do not have to be flagged as estimated (J). 304282 STANDARD OPERAUNG PROCEDURE E'.'aluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Nonber: HW-2 Appendix A.l: Data Assessnent - Contract Revisicn: 11 cixpliance (Total Review) — — ^^ _ ^2A~~ i. 14.2 Is concentraticn of prep, blank valvje greater than the CRDL when TPT, is less than or equal to CRDL? f X l If yes, is the concentraticn of the sanple with the least ccncentrated analyte less than 10 ti-m^ -^ the prep.blank? [ ] X- ACTT^: If yes, reject (red-line) all associated data greater than CRDL concentration but less than ten times the prep, blank value. 1.14.3 Is co-ncentraticn of prep, blank value (Form III) less than rwD times IDL, when IDL is greater than CRDL? [ ] X ACTTCN: If no, reject (red-line) all positive sample results when sample raw data are less than 10 times the prep, blank value. 1 Is concentration of prep, blank below the negative CRDL? [ X. 1 ACTIGN; If yes, reject (red-line) all associated sample results less than lOxCRDL. Form IV (ICP Lnterference Check R^Trrpie) L Present and ccnplete? f Y1 (NDTE: Not required for furnace AA, flame AA, mercury, cyanide and Ca, Mg, K and Na.) Was ICS analyzed at beginning and end of run w (or at least trwice every 8 hours)? [ Xl ACTION: If no, flag as estimated (J) all the samples for wtuch AL, Ca, Fe, or Mg is higher than in ICS. .15.2 Circle all values on each Form IV that are more than ± 20% of true or established mean value. Are all Interference Check Sample results inside , the control limits (± 20%)? [ ] X If no, is concentration of Al, Ca, Fe, or Mg Icwer than the respective concentration in ICS? [ ] X 304283 STANEftRD 0I5RATING IWXEDURE -.le: Evaluation of Metals Dat:a for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Appendix A . l : Data Assessment - Ccntract Revision: 11 cirrpliance (Itital Review) ^ m m ,ACTir»: If no. flag as est.iTmted (J) those positive results for vhich ICS reocTvery is betareen 121-150%; flag all sample results as estimated if ICS recovery falls vithin 50-79%; reject (red-line) those sarple results for vhich ICS reoovery is less than 50%; if ICS reacvery is above 150%, reject positive results only (not flagged with a "U"). :. 15 Form V A (gpiked Sample RBooverv - Pre-Digestion/Pre-Distillation)- ( Note: Not required for Ca, Mg, K, and Na (both matrices), Al, and Fe (soil only.) .,1£-1 Present and ccrplete for: each SDG? f X l each matrix type? f X ] eac±i cone, range (i.e. low, med., high)? F X"^ For both AA and ICP when both arc i:sad for , tihe same aralyte? [ ] > ACTION; If no for any of the above, flag as estimated (J) all the positive data less than four times the spiking levels specified in sew for which spiked sanple was not analyzed. NCTTE: If one spiked sample was analyzed for more than 20 samples, then first 20 sanples cinalyzed do not have to be flagged as estimated (J). ,1£.2 Was field blank used for spiked sanple? r X l JCTTQN: If yes, flag all positive data less than 4 X spike added as estimated (J) for vhicdi field blank was used as spiked sairple. 16.3 Circle on each Form VA all spike recoveries that are outside control limits (75% to 125%). | Q "" Are all recoveries within control limits? [ ] X ' '^ If no, is sample concentiration greater than or equal to four times spike concentration? [ ] X^ 00 STANCARD OPERATING PROCEDURE le: Evaluation of Metals Data for the Contract Laboratory Program Appendix A.l: Data Assessnent - Ccntract Ccrnpliance (Total Review) Date: Jan. 1992 Number: HW-2 Revision: 11 XSS. ACTTCN; If yes, disregard spike recoveries for analytes whose ccnoentraticns are greater than or equsd to four times spike edded. If no, circle those analytes cn Form V for vhich sanple ccnoentratian is less than four times the ^ i k e concentration. Are results outside the cantrol limits (75-125%) flagged with "N" cn Form I's and Form VA? t^] 16.4 ACTION: If no, write in the Contract - Problem/Non - Ccnpiiance section of "Data Assessment Narrative". Agueous Are any spike recoveries: (a) less than 30%? (b) between 30-74%? (c) between 126-150%? (d) greater than 150%? If less than 30%, reject all associated aqueous data; if between 30-74%, flag all associated aqueous data as estiratad (J); if between 126-150%, flag as estimated (J) all associated aqueous data not flagged with a "U"; if greater than 150%, reject (red-line) all associated aqueous data not fla;^ed with a "U". ?JCTION: m [ ] [ ] [ ] [ ] N/A 1.16.5 Soil/Sedi.mfint Are any spike recoveries: (a) less than 10%? (b) between 10-74%? (c) between 126-200%? (d) greater than 200%? _ [^] _X. [ ] 1. [_] 304285 STANDARD OPERATD*: HQZEDURE ^tie: D/aluation of Ifetals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Afpendix A.l: Data Assessment - Ccntract Revision: 11 Compiiance (Total Review) ^^ "^ "HZT" AcncM: If less than 10%, reject all Aco^-ia^-gri data; if between 10-74%, flag a l l associated data as estimated; if between 126-200%, flag as estimated all associated data was net flagged with a n r ; if greater than 200%, reject all associated data not flagged with a "U". 1.17 Form VI (Lab Duplicates) " 1.17.1 Present and caiplete for: each SDG? [_XJ each matrix type? [ALJ each concentration range (i.e. low, med., hi^)? f ^C ) . both AA and ICP when both aure used for the same analyte? [ ] ^ ACTION: If no for any the above, flag as estimated (J) all the data >CRDL* for which duplicate sanple was not analyzed. Note: 1. If one duplicate sanple was analyzed for more than 20 sanples, then first 20 samples do not have to be flagged as estimated. 2. If percent solids for soil sanple and its duplicate differ by mere than 1%, prepare a Form VI for each duplicate pair, report concentrations in ug/L on wet weight basis and calculate RPD or Difference for each analyte- 1.17.2 Was field blank used for duplicate analysis? f jSl ACTION: If yes, flag all data >CRDL* as estimated (J) for vhich field blank was used as duplicate. 1.17-3 Are all values within control limits (RPD 20% or difference < iCRDL) ? [ ] If no, are all results outside the control limits flagged with an * on Form I's and VI? [_il] ACTION: If no, write in the Contract - Problems/Non- Ccrpliance section of "Data Assessment Narrative". * Substirute IDL for CRDL when IDL > CRDL. X. 304286 STANTARD OPERATING PROCEDURE .e: Evaluation of Hetals Data for the Contract Laboratory Program Appendix A.l: Data Assessment - Ccntract cijipliance (Ittal Review) Date: Jan. 1992 Hunter: HW-2 Revisicn: 11 ICTE: 1. RPD is not calculable for an analyte of the sample - diplicate pair viien both values are less than IDL. 2. If the result of lab duplicate aralyzed by GFAA is rejectable due to coefficient of correlation of MSA, analytical spike recovery, or duplicate injections criteria, do not apply precision criteria to TOP^-J^TR anedyzed by GFAA. .17.4 Agueous Circle on each Form VI all values that are: RPD > 50%, or Difference > C333L* Is any RPD greater than 50% where sanple and duplicate are both greater than or equal to 5 times *CRDL? Is any difference** between sanple and duplicate greater than «CRDL where sample and/or duplicate is less than 5 times *CRDL? ACTION: If yes, flag the associated data as estimated. Soil/SediriPnt Circle on each Form VI cdl values that are: RPD > 100%, or Difference > 2 x CRDL* Is any RPD (where sanple and duplicate are both greater than or equal to 5 times *CRDL) : > 100%? Is any •*differe.ooe between sample and duplicate (where sample and/or duplicate is less than 5x*CRDL) ; > 2x*CRDL? YES m Bih [ ] _ [ ^ ] _ [2L] S'ubstitute IDL for CRDL v^en IDL > CRDL. '-se absolute values of samole and duplicate to calculate the difference. 304287 STAND?JRD OPERATING HOTTTIRE Evaluation of Metals Data for the Date: Jan. 1992 Contract laboratory Program Number: HW-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 Compliance (Total Review) YES NO N/A ACTION; If yes, flag the in'=>qnriatpri data as estimated. .18 yield Explicates .13.1 Were field duplicates analyzed? [ ] X ACTION; If yes, prepare a Form VI for each agueous field duplicate pair. Prepare a Form VI for each soil duplicate pair, if percent solids for sample and its duplicate differ by more than 1%; report conoentraticns of soils in ug/1 cn wet weic^t basis and calculate RPDs or Difference for each ainalyte. NOTE: 1. Do not calculate RPD'when both values are less than IDL. 2. Flag all associated data only for field dLplicate pair. .IB.2 Agueous Circle all values on self prepared Form VI for field d'uplicates that are: RPD > 50%, or Difference > CRDL* Is any RPD greater th^an 50% where sample and duplicate are both greater than or equal to 5 time$ *CRDL? [ ] X Is any **differe.nce between sample and duplicate greater than *CRDL where sanple and/or duplicate is less than 5 times *CRDL? [ ] 2;^ ACTION: If yes, flag the associated data as estimated. * S'ubstit'Ute IDL for CRDL when IDL > CRDL. "** Use absolute values of sample and duplicate to calculate the difference. 304288 STANDARD DISRATING PRDdUIRE :le: Evaluation of Metals Data for the Contract Laboratory Program Appendix A.l: Data Assessnent - Qontract Ocrpliance (Total Review) Date: Jan. 1992 Nunber: HW-2 Fevision: 11 YES 1.18.3 Soil/SertimPTit Circle a l l valvies on self prepared Form VI for field duplicates that sre: RPD >100%, or Difference > 2 x CRDL* Is any RPD (where sample and duplicate are both greater than 5 times •CRDL) : >100%? Is any **difference between sample and duplicate (where sanple and/or duplicate is less than 5x *CRDL ): >2X *CRDL? ACTTON: If yes, flag the associated data as estimated. m WA _ [_J Ji _ [_] Ji 1.19 r o m VII (T^hnratoiv Control Senaple) (Note: LCS required for aqueous Hg and cyanide analyses.) l.lS.l Was one LCS prepared and analyzed for: each SDG? each batch samples digested/distilled? both AA and ICP when both are used for the same analyte? - not [Ji] [-X] [XJ ACTION: If no for any of the above, prepare Telephone Record Leg and contact laboratory for submittal of results of LCS. Flag as estimated (J) all the data for which LCS was not analyzed. NJTE: If only one LCS was analyzed for more than 20 sanples, then first 20 samples close to LCS do not have to be flagged as estimated. S'jbstitute IDL for CRDL when IDL > CRDL. '* Use absolute values of sanple and duplicate to calculate the differe.nce. 304289 STANDARD OPERATING PROCEDURE E^/aluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Nunber: HW-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 Ccmpliance (Total Review) ~~" " ^ m B/h ,19.2 Agueous LCS Circle on each Form VTI the LCS percent recoveries outside control limits (80 - 120%) except for aqi.w?c»is Ag and Sb. Is any LCS recovery: less than 50%? [ ] between 50% and 79%? [ ] between 121% and 150%? [ ] greater than 150%? [ ] ACTTON: less than 50%, reject (red-line) all data; between 50% and 79%, flag all associated data as estinated (J); between 121% and 150%, flag all positive (not flagged with a "U") results as estimated; greater than 150%, reject all positive results. .19.3 Solid LCS NCTE: 1. If "Found" value of LCS is rejectable due to duplicate injectic.-is or analytical spike recovery criteria, regardless of LCS recovery, flag the associated data as estimated (J). 2. If IDL of an analyte is equal to or greater than true value of LCS, disregard the "Action" below even though LCS is out of control .limits. Is LCS "Found" value hither than the cantrol limits on Form VII? f X l ACTTON: If yes, qualify all associated positive data as estimated. Is LCS "Found" value lower than the Control limits on Form VII? ^-f^^ ACTTON: If yes, q-ualify all associated data as estimated. 304290 SIAND?>RD OPERATING PROCEDURE tie: D.'aluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Nunber: HW-2 Appendix A.l: Data Assessnent - Ccntract Revisicn: 11 Ccnpiiance (Total Review) 1.20 Form TK (ICP Berial Dilution^ - >PTE: Serial dilution analysis is required only for initial ccncentraticns equal to or greater than 10 x IDL. 1.20.1 Was Serial Dilution analysis performed for: . ^ each SDG? f X l each matrix type? f X ] each concentration range (i.e. low, med.)? f "V ) ACnCN: If no for any of the above, flag as estixated all the positive data >. lOxIDLs or >. CRDL when lOxIDL <. CRDL for which Serial Dilution Analysis was not performed. 1.20.2 Was field blank(s) used for Serial Dilution Analysis? f X l ACTTON: If yes, flag all associated data >. 10 x IDL as estirated (J). If lOxIDL <. CRDL, flag all data >. CRDL. 1.2 3.3 Are results outside control limit flagged with an "E" on Form I's and Form IX when initial concentration on Form IX is equal to 50 times IDL or greater. f X l ACTTON: If no, write in the Contract-Problem/Non- Ccrpliance section of the "IData Assessment Narrative". 1.20.4 Circle on each Form IX all percent difference that are outside the control limits for initial concentrations equal to or greater than 10 x IDLs only. Are any % difference values: > 10%? _2C_ [ 1 _ >. 100%? [JjL] 304291 STANDARD OPERATING PROCEDURE .le: D.'aluatian of Metals Data for the Date: Jan. 1992 Contract Laboratory Prtxgram Number: HW-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 cirpiiance (Total Review) ^ ^ HZK ACnCK; Flag as estimated (J) cdl the associated sample data >. lOxIDLs (or >.'CRDL when lOxIDL <. CRDL) for which percent difference is greater than 10% but less than 100%. Reject (red-line) all the associated sample results equ2d to or greater than lOxIDLs (or >. CRDL when lOxIDL < CRDL) for vhich FD is greater than or equal to 100%. Note; Flag or reject on Form I's only the sanple results vhose associated raw-data are >. lOxIDL (or >. CRDL when lOxIDIx CRDL) ..21 Furnace Atetaic Absortation (AA) OC Analysis j\j ^ |X f\ tjJOr-\<^ o/^S . . . . fC,*" vorr^iJ. ..21.1 Are duplicate injections present m furnace raw data (except-during full Method of Standard AfViition) for each sample analyzed by GFAA? [ ] ACTTON: If no, reject the data on Form I's for which duplicate injections were not performed. •1.2 Do the duplicate injection readings agree within 20% Relative Standard Deviation (RSD) or Coefficient of Variation (CV) for concentration greater than CRDL? [ ] Was a dilution analyzed for sample with analytical spike recovery less than 40%? [ ] ACTION: If no for any of the above, flag all the associated data as estimated. 11.2 Is *aralytical spike recovery outside the control limits (85-115%) for any sanple? [ ] ACTION: If yes, flag the affected sample results if the recovery is between 10-84%; if the recovery is between 115-200%, flag the associated positive sanple results as estimated; reject the associated sample __ residts if the recovery is less than 10%; reject positive sanple results if the recovery is greater than 200%. d\tical spike is not required on the pre-digestion spiked sample. 304292 STANEARD ORERAITNG PROCEDURE Le: Evaluation of Metals Data for t-he Date: Jan. 1992 Contract Laboratory Program Nunber: HW-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 C o m p l i a n c e ( T o t a l R e v i e w ) xss. m uih NCTT: Reject or flag the data only when the affected sanple (s) was not subsequently analyzed by Method of Standard Addition. .22 Fona VIII (Method of Standard Addition Rasults) .22-1 Present? [ ] If no, is any Form I result ceded with "S" or a "+"? [ ] ACnON: If yes, write request on Telephone Record Log and contact laboratory for sutamittal of Form VIII. .22,2 Is coefficient of correlation for MSA less than 0.990 for any sanple? [ ] ACTION: If yes, reject (red-line) the affected data. Was *MSA required for any sanple but not performed? [ ] Is coefficient of correlation for MSA less than 0.995? [ ] Are MSA calculations outside the linear range of the calibration curve generated at the beginning of the analytical run? [ ] ACTION: If yes for any of the above, flag all the associated data as estimated (J). Was proper quantitation procedure followed correctly as outlined in the SCW on page E-23? [ ] TACTION: If no, note exception under Contract Problem/ Non-Ccrpliance section of the "Cata Assessment Ncurrative", and pr^are a separate list. - !-'.SA is not required on LCS and prep, blank. 304293 SIJiNDARD OPERATING PROCEDURE tie: Evaluation of Metals Data for the Date: Jan. 1992 Contract laboratory Program Nunber: HW-2 Appendix A.l: Data Assessnent - Ccntract Revision: 11 cisipliance (Total Review) ~~~ " ^ m EZA" 1.23 Dissolved/Total or J-nnrinnic/Total Analytes - M / / | 1 ,23.1 Were any analyses performed for dissolved as well as total analytes cn the same fvmple(s). [ ] Were any analyses performed for inorganic as well as total (organic + inorganic) analytes cn the same sanple (s)? [ ] NOTE: 1. If yes, prepare a list corparing differences between all dissolved (or inorganic) and total analytes. Conputc the differences a s a percent of the total analyte cnly when dissolved concentration is greater than CRDL as well a s total concentration. 2. Apply the following questions only if in- organic (or dissolved ) results are (i) above CRDL, and (ii) greater than total constituents. 3. At least one preparation blank, ICS, and LCS should be sinalyzed in each analytical run. 1.23.2 Is the concentration of any dissolved (or inorganic) analyte greater than its total concentration by more than 10%? [ ] 1.23.3 Is the concentration of any dissolved (or inorganic) analyte greater than its total concentration by more than 50%? [ ] ACTION: If more than 10%, flag both dissolved (or inorganic) and total values a^ estimated (J); if more than 50%, reject (red-line) the data for both values. -.24 Fom I (Field Blank) - f\fo fi^U bU^v^C c<)il^,,l-4 (Note; Designate '^ield Blank" as guch on Form I.) 1.24.1 Circle all field blank values on Form I that are - greater than CRDL, (or 2 x IDL when IDL > CRDL). Is field blank concentration less than CRDL (or 2 X IDL when IDL > CRDL) for all parameters of associated aqueous and soil sanples? [ ] 304294 STANDARD OPERATING PROCEDURE :le: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Appendix A.l: Data Assessment - Contract Revision: 11 Ccmpliance (Total Review) ' ^^ ^ M~' If no, was field blank value already rejected due to other QC criteria? [ ] ACTICK; If no, reject (except field blank results) all as.'VY'iated positive sanple data less than or equal to five times the field blank vsdue. Reject cn Form I's the soil sanple results that when converted to ug/L on wet basis are less than or equ2d to five times the field blank value in ug/L. 1.25 Form X, XI, XII (Verification of Instniaental Parazaeters). 1.25.1 Is verification report present for: Instrument Detection Limits (quarterly)? r Y.1 ICP Interelement Correction Factors (annually)? f X l ICP Linear Ranges (quarterly)? [ X l ACTION: If no, contact TPO of the lab. 1.25.2 Form X (Instrument Detecticn Limits) - (Note: IDL is not required for Cyanide.) 1.25.2.1 Are IDLs present for: all the analytes? r /s 1 all the instruments used? f ^ 1 For both AA and ICP when both are used for the same analyte? [ ] _J^ ACTTON: If no for any of the above, prepare Telephone Record Log and contact laboratory. 1.25-2.2 Is IDL greater than CRDL for any analyte? [ J--] If yes, is the concentration on Form I of the sample analyzed on the instrument whose IDL exceeds CRDL, greater than 5 x IDL. [ ] X " 304295 STANr»RD OPERATING PROCEDURE LE: Evaluation of hfetals Data fcr the Contract Laboratory Prograa Appendix A.l: . Data Assessment - Contract Cccplianoe (Total Review) Date: Jan. 1992 Nunber: HW-2 Revisicn: 11 Action : If DO, flag as estimated a l l values less than five t i r e s IDL of the instrument %Aiose IDL exceeds CRDL. iE£ m N/A 1.25.3 Form XI (Llnfv^r Ranges) 1,25.3.1 Was any sanple result hii^ier than high linear range of ICP. Was any sanple result higher than the hit^est calibration standard for non-ICP parameters? If yes for any of the above, was the sample diluted to gbtain the result on Form I? [2^1 _ TACTION: If no, flag t.he result reported on Form T as estirated (J). 1.25 Percent Solids of sp^^'ir^^nts 26.1 Are percent solids in sadiment(s): < 50%? < 10%? ACTION: If yes, qualify as estirated all the results of a sample that has per cent solids between 10%-50% (i.e. moisture content between 50%-90%). Reject all the results of a sanple that has per cent solids less than 10% (i.e. moisture content greater than 90%). NOTE: Reject or flag (J) only the sample results that were not previously rejected or flaged due to other QC criteria. [Ah] 304296 STANDARD OPERATING PROCEDURE :le: E^/aluation of Metals Data for the Contract Laboratory Prtagram Appendix A.2: Data Assessnent Narrative Date: Jan. 1992 Nunber: HW-2 Revision: 11 sel G# ntra 2.1 ctor v&li 9n/ dation ?/| Flags- Bit* y<,li^<r,o\ ChcrmcJ lab Pc\ce RBviawar Oc A Matrix: Soil )(_ Water Other The following flags have been ^plied in red by the data validator 2ind rust be considered by the data user. J- This flag indicates the result qualified as estimated Red- Line- A red-line drawn through a sample result indicates unusable value. The red-lined data are k n a ^ to contain significant errors based on documented information and rust not be used by the data user. FMllv Usable Data- The results that do not carry "J" or "red-line" are fully \isable. Contractual Qualifiers- The legend of contractual qualifiers applied by the lab on Form I's is found on page B-20 of SOW ILMOl.O. .2 The data assessment is given below and on the attached sheets. 304297 STANDARD OISVOTNG P R D O H I R E :le: Evaluation of Metals Data for the Date: Jan. 1992 Contract laboratory Program Number: HH-2 Appendix A.2: Data AssesEment Narrative Revisicn: 11 2.2 (continuation) 304298 STANI»RD OPERATING ERDCmiRE :tle: Evaluation of Metals Data for the Date: Jan. -1992 Contract Laboratory Program Number: HW-2 Appendix A.2: Data Assessment Narrative Revision: 11 .2.2 (continuation) 304299 STANDARD 0P5RATING PRDCEDURE :le: Evaliiation of Metals Cata for the Date: Jan. 1992 Contract Laboratory Program Number: HH-2 Appendix A.2: Data Assesanent Narrative Revisicn: 11 2.3 Contract-Problem/Non-Ccxipliarce I-"-3/ESAT Rviewer: Date: Signature .-.tractor Reviewer: UJ^A^tXcT^ (^ • ^ .A/^JT}''^' Cate: i o / ^ o A ' y Signature Verified by: Date: 304300 STANDARD OPERATING PROCEDURE Title: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Nunber: HW-2 Appendix A.3: Oantract Ncn-Cccplianoe Revision: 11 (SMD Report) OCNIRACT NGN-aCMPLIANS (SHD REPCKT) Regional Review of Unccntrolled Hazardous Waste Site Ccntract Laboratory Data Package CASE NO. hardcepied (laboratory name)_ rrganic data package received at Region II has been reviewed and the quality aissurance and rformance data summarized. The data reviewed included: 3 Sample No.:_ -:c. i Matrix: -tra'ct No. ( ]_ requires that specific analytical work be done and • ssociated reports be provided ty the contractor to the Regions, IMSL-LV, and SMO. Ihe 1 criteria used to determine the performance were based on an exismination of: - Data Ccnpleteness - Duplicate Analysis Results - Matrix SpUce Results - Blank Analysis Results - Calibration Standards Results - MSA Results ems cf non-cccrpliance with the above contract are described belcw. rents: Reviewer's Initial Date 304301 STANDARD CPZRATING iWJCxLURE Evaluation of Metals Data f o r t h e Contract Laboratary Program Appendix A.4: Mailing L i s t f a r Data Reviewers Date: Jan. 1992 Number: HW-2• Revision: 11 twofxxnTi: I.TIT r s rxs. gvutja. «0 VmFcvxm.- Sxrmet lAxirrr-sn. »> 02173 U^ ti*ro (tl7) •61-43i3 rr. K. wk. KH. ja. vr t J I . t i a m K r . USk A,-nBpc::i. t o 2;<C1 C-.J£X SA.-X1S c r i ) 3ti-9:io rc. r c 7i. \-x. vv. or c«.-:t*c. Kic-uL-.. rrt. Kko^. \'rjsw^, S-.i3«ci 7*r-... >;*/ FA v$t?x RJB;:C-. V (rsr; i J t Sa-t.-. c:irk r i - ' w t Ttri,'. r ; e c r . CRI Pi*, c-.-rii:* 3 ; j - : i ; - s : e - 31. r . \ f z . K : . OK. V- 3.. t5D>A taqiv) 23 (ZS3) CtliMn, MM J c T M y OtC37 (303) aSl'^^^i W. Klf. » . V3 Caneury. OMrffTT.. US 7*rt. >iA.«BO, t r c , CMlAfln. O S , G*1»m, lOt J i r.:-j-.cr. K ^ i Dttri hcrty (j;3; :34-3E!: ZZ. KS. KE. MO Wilts-.. >gL-iii C:r>' Sc:e.-.tiiic j : i rrerorr. S-_r*et SA.-. rra.-cii=c. CA 9 O 0 i (<:5) S14-W3* A2. Ok. K ; . K.-. X-«.-i&a.-. SJL-oA. OJL-. Tr.:s-. 7 e r T : t i r i e s ol P » : i l i c :»:».-ns. v«L>.t jtiiL-ri A U . c c We^-cr.. S - O j b o i . J7-CA. V«c;«.s 4. tSCA Rubier TV OSS) Cell apt r u t i o - . RaAd kXt».-». CA 3&ei3 Tw. ae."nert. J r . (40<) M«0112 IX. GA, Klf, »S. HC. SC. TV x?5. TSI, PCSL:, t . ISl^A l ^ i t r . V3 (ES3) h a r j u ^ r>>Tk P l t u . £10;. C «l3t Hcrrvoo; Crjvt Hajr--Dn. TX 7707< (713) *i3-}43!> A«, U . W.. r c . OK AWkXK, wciAS. SPECS, c s . c: Aliiid. Kr-/ tX, CSA e. UrtTA RBc:cr. Viri Uicntcr,- BOX 3i366 Dt-vfLr r«dtnJ Ct.-^tcr uv^MQoi. cz t::2S (353) 23€-737J CC. Kt. 5r. u:. w . rz A=L-, caCU, >«kL, r a t * Cier.. Ot-vrtt 30. US7A Kaqien X TA^n-^^o^y P.O. tax. S49 K&.i::^e9r.£r, W> tt3S3 (306) 443>0370 AX, I D , Cif>, Wk U.xr,s Testui; U ^ , OE.-»r>- Itstin; U i » (Tor VOA Orjy), Ueye.-ne-i»*r Cc. OsJtftrit Ttstiiij, SUv»r v*il«y : : , 33. Cesli DE.-ps*y - I36-33CJ LSirA *C". " T " $•_-«-.. S.W. V4js.'.A.-tr.cr.. rc 2 t i i . ' TTS. 3 t ; - i - < t s*.—:t f.i.-ift5«.-«.-.* c i : ; £ « V, v.- 4.-C Cir^i-./ F.C. B:> I : £ 33. tiJ.-L-i xyt-.icr USEFA IXSl-LV 5*4 t . K&rn=r. Avtnje EX iH',6 lAi Vacaji. K.- l s : : 5 304302 STANDARD OPERATING PROCEDURE Title: Evaluation of Metals Data for the Contract Laboratory Program Appendix A.6: CLP Data Assessment Sunsnary Form (Inorganics) Date: Oct. 1989 Nun±er: HW-2 Revision: 9 Typa of Ravlawi Sice: T^jctKN.-i Cl\diy\.Ui.i Cn.P DATA ASSESSMENT SUMMARY FOIW (IWOtCAMICS) C L ? Dtt,: //)'^o-^n Caaa 4: Lab Maaai Revicwar'i I n l t l a l a : ML P,ce. AhM,.J Mtiabar o£ Saaplaa: z± Ana l y t a a Ralacted Dua to Eaceeadlnf Ravlav C r i t e r i a : * ICP 1 r i a a a AA 1 Purnaca AAI Holding Tlaaa 1 n 1 CaXlbraclonl o 1 Prap Blank! Field BUnkI n 1 K 1 1 I I I Mareurv 1 O Total CAJ Other 0 ICP F l a M AA 1 ^^ Furnace AAI Mercury 1 C^ Total lothar 1 o 0 1 O 0 1 Y-l 0 Ai>alrc< o 1 0 1 0 1 1 I n t e r - 1 fercncaa1 n 1 ^1 Y; \ y 1 tt Fla^xed ai Eaclmati o 1 X 1 O 1 )C 1 0 ly 3H 1 )^ ^ Splka RacoYarrl n 1 Q 0 td (J5 I>u< ?^ ^ n Dupllcataa LablFleld | "of 0 0 y / - X >^ I CO £zct«d lo lo r ,^ 1 ^ ^ DaCectlon LlBlta O 1 0 0 iDf C r l t e r o 1 0 1 ^ LCsl 0 0 0 S«rlAl DllutlonI o 1 y^ y^ La For:* {o p 10 1 77 1 X V HSAI V:| > > j Total Aaalrtaal ^o(^\ Z3 )c- 1)^ !>^ \S0(^ \z3 2^ R«1«ctla 0 (7 6) ,/^V ''' 0 Note: Aacarlak (*) lodleacea addltloaal exceadancea of review criteria. 304303 STANDARD OPERATING roOCEDURE Title: Evaluation of Ifetals Data for the Contract Laboratory Program Appendix A.7: CLP Data Assessment Checklist Inorganic Analysis Date: Oct. 1989 Number: HW-2 Revisicn: 9 INC5?GANIC RBGICNAL DATA ASSESSMENT Region, CASE NO. T5 h h J 6'/\ ifhii-A IABCRATORY_ SDG# saw# 2, £ 4 J U . f\rM\L ho J SITE_ NO. OF SAMPLES/ MATRIX ^J/^o/c. SRUAL:. ZLfr\02.0 REVIEHni (IF NOP ESD)_ REVIEHER'S NAME O o i \ A miL. DPO: AdTCN 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. L2. HOLDING TIMES CAKCBRATICKS ELANKS ICS LCS DOPLICRTE ANAIiSIS MATRIX SPIKE MSA SERIAL mUIYlW SAMPIE VhKlt'lCATICN UiHLk QC OVHEIALL ASSESSMENT FYI :y_ OCMPIZnCN DATE DATA ASSESSMEOT SimMAHY ICP AA 1 1 . n H . li u XL n_ -Q. n 12. n Hg J l . IL XL • ^ IL X L » Data has ro problems/or qualified due to minor prdblenaS'. « Data qualified due to major problens. = Data unaccsptable. = Problems, but do not affect data. kcncn THMS: ^'^A^/' i^n GZANILC ^ XL ± AREAS OF CCNCERN: NOTABLE FERFCPMANCE: 304304 QA/QC Review of TAL Inorganic Data for Pace Analytical SDG: 97129 October 30, 1997 Holding Times: Samples were analyzed within EPA Region II CLP holding times. Initial and Continuing Calibration Verification: All percent recoveries were within control limits (90-110% for all metals except Hg, 80-120% for Hg, 85-115% for CN), except for arsenic (112.8%) in the initial calibration. No samples were associated with this calibration. CRDL Standard for AA and ICP: Arsenic (79.4% and 79.2%), selenium (64.4% and 75.5%), and thallium (72.8%) had percentrecoveries outside Region II control limits (80-120%). Results for these metals in associated samples within effected ranges should be considered estimates (J). Blanks: Initial and continuing calibration, and preparation blanks had analyte levels less than the CRDLs as required by Region II. ICP Interference Check Sample: Arsenic (79.5%) and 78.9%)), cobalt (79.4% and 79.3%), and selenium (54.2% and 61.2%) had percent recoveries outside control limits (80-120%). Results for these metals should be considered estimates (J) in associated samples. Spike Sample Recovery: Antimony (42.7%)), mercury (131.6%)), and silver (72.5%) had percent recoveries outside control limits (75-125%)) for spike sample RG0003S. Antimony (43.1%), manganese (142.4%)), mercury (129.9%), and silver (73.0%) had percent recoveries outside control limits (75-125%) for spike sample RGOOl IS. Results for antimony, manganese, mercury, and silver should be considered estimates (J) in associated samples. Duplicates: All applicable relative percent differences were less than the allowable maximum (35%) for duplicate samples RG0003D eind RGOOl ID as required by Region II. Laboratory Control Sample: All recoveries were within control limits for the soil LCSs. Standard Addition Results: No results were quantitated by MSA in this LP. ICP Serial Dilution: Cobalt (14.9%), copper (22.1%)), lead (16.7%), nickel (20.6%)), potassium (21.7%), and zinc (19.2%)) had %)Ds above the allowable maximum (10%) for serial dilution sample RG0003L. Copper (24.6%), lead (16.4%), potassium (23.4%), and zinc (21.3%) had %)Ds above the allowable maximum (10%) for serial dilution sample RGOOl IL. Results for cobalt, copper, lead, nickel, potassium, and zinc should be considered estimates (J) in associated samples. Instrument Detection Limits: All IDLs were at or below the CRDLs as required. G:\STAFF\DANNE\IsIand\97129.IN0.wpd 304305 Cyanide Date: 9/25/97 X range 1 0.5 0.1 0.05 0.01 0 y range 0.0795 0.0463 0.0105 0.0056 0.0006 0 Slope: Intercept: Cor. Coef.: 0.080366 0.001515 0.996835 304306 Mercury Date: 9/25/97 X range 0 0.2 0.5 1 5 10 y range 1106 3393 8107 18493 76069 164994 Slope: Intercept: Cor. Coef.: 16238.81 162.3062 0.999069 304307 QA/QC Review of Semivolatiles Data for Pace Analytical SDG: 97129 October 29, 1997 Holding Times: All sample RG0003 was extracted outside Region II holding times. Results for sample RG0003 should be considered estimates (J). GC/MS Tuning and Mass Calibration: All DFTPP tuning criteria were within control limits. Initial Calibration: All compounds with contract criteria for RRFs and %RSDs met those requirements. All target compounds had average RRFs above the allowable minimum (0.050) and %RSDs below the allowable maximum (30%) as required. Continuing Calibration: All compounds with contract criteria for RRF50s met those requirements. Pyridine (28.9%) had a %D above the contractual maximum (25%) on 10-07-97 (1007J01). Pyridine (32.7%) had a %D above the contractual maximum (25%) on 10-08-97 (1008H04). 2-Methylnapthalene(31.3%) had a %D above the contractual maximum (25%) on 10-13-97 (1013J04). No action is taken on two or fewer compounds per calibration outside contract limits as long as %Ds are below 40% and RRF50s are above 0.010. All target compounds had RRF50s above the allowable minimum (0.050) as required. Pyridine (28.9%) had a %D above the allowable maximum (25%) on 10-07-97 (1007J01). Pyridine (32.7%)), 2,2'-oxybis(l-chloropropane) (35.1%), hexachlorocyclopentadiene (37.2%), and 2-nitroaniiine(25.8%) had %Ds above the allowable maximum (25%)) on 10- 08-97 (1008H04). 2-Methylnapthalene (31.3%) and 2,2'-oxybis(l-chloropropane) (26.4%) had %)Ds above the allowable maximum (25%) on 10-13-97 (1013J04). Results for these compounds should be considered estimates (J) in associated samples. Blanks: Method blanks reported all target compounds as not detected. Internal Standard Area Summary: All internal standard areas and retention times were within control limits for environmental samples. Surrogate Recovery: Sample RG004D had 1 of 4 acid extractable surrogate recoveries outside control limits but not less than 10%. No action is taken on one surrogate per fraction outside control limits as long as no recovery is less than 10%). 304308 Matrix Spike/Matrix Spike Duplicate: MS/MSD samples RE0003 and RGOOl 1 had all relative percent differences and percent recoveries within control limits. Compound ID: Checked compounds were within GC/MS quantitation and qualitation limits. All positive hit compounds had the primary and secondary ions in their mass spectra as outlined in the SOW. G;\STAFF\DANNE\!sland\97129.SVL.wpd 304309 Cone, of Internal Standard: 40 ID: J Date: 10/2/97 RRF Cone, of Compound 1,4-Dichloroben2eneKJ4 Phenol RRF Naphthalene-d8 1 Naphthalene RRF Acenaphthene-d10 Acenaphthylene RRF Phenanthrene-dlO Phenanthrene RRF Chrysene-d12 Pyrene RRF Perylene-d12 Benzo(g,h,i)perylene RRF 1002J13 Sample 1 20 187641 129872 1.384 690684 304252 0.881 342609 302723 1.767 629821 298771 0.949 522698 333964 1.278 578926 232130 0.802 1002J09 Sample 2 50 171654 298576 1.392 630679 683694 0.867 315328 695803 1.765 600611 696903 0.928 488331 770298 1.262 565479 604949 0.856 1002J10 Sample 3 80 161679 457470 1.415 613144 1099163 0.896 316455 1172934 1.853 598024 1127785 0.943 500105 1277698 1.277 599934 1000773 0.834 1002J11 Sample 4 120 174935 713618 1.360 641248 1680330 0.873 320344 1703599 1.773 551560 1593636 0.963 456936 1767302 1.289 556907 1398912 0.837 1002J12 Sample 5 160 176840 887320 1.254 626980 2069686 0.825 318578 2178756 1.710 556997 1959586 0.880 441688 2264727 1.282 536144 1723822 0.804 Average 1.361 0.869 1.774 0.933 1.278 0.827 % RSD 4.6% 3.1% 2.9% 3.4% 0.8% 2.8% Continuing Calibrations Cone, of Compound 1,4-Dichloroben2ene-d4 Phenol RRF Naphthalene-d8 Naphthalene RRF Aeenaphthene-dIO Aeenaphthylene RRF Phenanthrene-dlO Phenanthrene RRF Chrysene-d12 Pyrene RRF PeryleneHd12 Benzo(g,h,i)perylene RRF 1007J01 Sample 50 140691 253103 1.439 511329 571759 0.895 254900 570434 1.790 473744 568026 0.959 394913 601020 1.218 486430 526535 0.866 %D 5.8% 3.0% 0.9% 2.9% 4.7% 4.8% 1008J02 Sample 50 154924 282547 1.459 576289 611754 0.849 273488 597751 1.749 514459 604803 0.940 400625 643567 1.285 480061 538747 0.898 %D 7.2% 2.2% 1.4% 0.9% 0.6% 8.6% 1013J04 Sample 50 129458 257043 1.588 502190 552863 0.881 229820 511521 1.781 388716 491858 1.012 353288 515082 1.166 413591 458894 0.888 %D 16.7% 1.4% 0.4% 8.6% 8.7% 7.4% Sample #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! %D #DIV/0! #DIV/0! #DIV/0! 1 SDivra! #DIV/0! #DlV/0! Sample #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! %D #DIV/0! #DIV/0! #Divro! #DIV/0! #DIV/0! #DIV/0! 304310 Cone, of Internal Standard: 40 ID: H Date: 5/27/97 >. .::.••'-.^ R R F - • Cone, of Compound 1,4-Dichlorobenzene-d4 Phenol RRF Naphthalene-d8 Naphthalene RRF Aeenaphthene-d10 Aeenaphthylene RRF Phenanthrene-dlO Phenanthrene RRF Chrysene-d12 Pyrene RRF Perylene-d12 Benzo(g,h,i)perylene RRF 527H13 Sample 1 20 252355 177261 1.405 825312 387228 0.938 376171 336874 1.791 713509 313295 0.878 566635 332485 1.174 628054 252879 0.805 527H09 Sample 2 50 223158 404273 1.449 758498 900829 0.950 374566 769684 1.644 650158 704473 0.867 561160 849134 1.211 608823 640202 0.841 527H10 Sample 3 80 247832 730966 1.475 841422 1570428 0.933 387891 1305348 1.683 661404 1190186 0.900 596557 1444729 1.211 626306 1059884 0.846 527H11 Sample 4 120 246894 1027763 1.388 806095 2172435 0.898 350044 1922535 1.831 660962 1689423 0.852 550925 1905575 1.153 601143 1379767 0.765 527H12 Sample 5 160 226612 1231303 1.358 738525 2693690 0.912 343896 2221879 1.615 591271 2007993 0.849 511221 2408100 1.178 562629 1670891 0.742 /Average 1.415 0.926 1.713 0.869 1.185 0.800 7o RSD 3.3% 2.3% 5.5% 2.4% 2.1% 5.7% Continuing Calibrations Cone, of Compound 1,4-Diehloroben2ene-d4 Phenol RRF Naphthalene-d8 Naphthalene RRF Acenaphthene-dIO Acenaphthylene RRF Phenanthrene-dlO Phenanthrene RRF Chrysene-d12 Pyrene RRF Perylene-d12 Benzo(g,h,i)perylene RRF 1008H04 Sample 50 225206 351303 1.248 752499 810314 0.861 365211 774578 1.697 649099 711459 0.877 493811 775584 1.256 452616 353145 0.624 %D 11.8% 7.0% 0.9% 0.9% 6.0% 22.0% Sample #DIV/0! #DIV/0! #DIV/0! • #DIV/0! #DIV/0! #DIV/0! %D #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! Sample #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! %D #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! Sample #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! %D #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! Sample #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/D! %D #DIV/0! #DIV/0! #DIV/D! #DIV/0! #DIV/0! #DIV/0! 304311 SDC-- 97/^^ SOP NO. Hn-6 Revision f8 CLP O?.GA:;J :F DATA -.rvi£n _ / - _ / - ^ ZY: - .\ \. '^y ^"-^ Leon Lizariis, ^."Vircnrr.snrsi S c i E n t i s - Tcxzc ar.d Hazardous Wasre Section •=v. "UL-y^A.Q^t^.^ / i — ' / y v < <!' ?< 1 Date: . Jc^.v., -^z-;-?!. Ceorrs js^rras. C.^ems-:: Toxio 2.-0 Ha22r=ov:3 Waste Section .<k /7 */ - a t e : ^ ^ / / .' /A'c/r> Steiioo Gerazounis/ cr.snist Toxic ind HazardtiTus Waste Section Kevin .Kutiv,*^ ..^^^ef 22zr^^i:s Waste Section Date: \A^ Date; Rotrert F.unyon. C.'Liet Monitorin:; Minaqenent Srancn / / J 304312 STJwKDAJ\.u C~£..rJ>.TriI3 rHOCZ-.-wi Date: January 1392 R A V i s i c n : S YES NO H/X PACKAGE CCMPLZrrrZSS AND CZUVZSABLZS n / 1 1 1 ' / 1.0 Data Corpieteness and Daliveracies 1.1 Have any r.issinc daiivaraaies teen received and added to tne data cacXaae? i ^ Ji.. _ ACTIC:;: call lib for expianation/resunnittal c i any nissinr daliveraaias- If lab cannot prsvids tnam, r.ote tr.a effsct on review ol ti:s pacicace under t.'-.a "Contract Probiens/Non-co=pliance" section cf reviewer narrativa. 1.2 Was S.MO CZZ cnsOciist included vit.': pacJcaqe? : 1 _X. 2 . 0 C o v e " ^ *:-•••»•- c~r.^::•.-•.••» — ---p 2.1 Is tr.a Narrative or Cover Latter Present? libl — — 2.2 Are case Nunter and/cr SAS nunier contained ., in tr.a Narrative or cover letter? r ^ __„ J ^ -1 Q D a t a ^f a •< ,--3,». i - — ^ W a ^ V I ' c * - The follovinc c^.ecxlisr is divided into tr.ree parts. Part A is filled our if tha data pac>:aga contains any VOA analyses. Part S fcr any ENA analyses and Part C for Pssticida/PCBs. Does t.Ms pacXaae containr w o VOA Data? J^ w H BKA Data? ::;^ • ' ^ Pesticiia/PCB data? J^ Action: ctrpiete corraspondinc parts c: c.'-.ecJclist. STAIIDAJuj C?Z?Ji.TIIt3 P?.OCZrL.--Z l . c 1.2 D a t e : J a n u a r y 13 32 R e v i s i o n : a ^23 :;o )i/x * ' * • • • • • • - • • • 1.1 Arc t-e Traffic Rencrr: Forrs present for ail saasies? ACTIDII: If no, contact lab for rspiaccaenr cf nissinc cr l l l e a i t l a c o n e s . i ^ _ 54. lo t.'-.a Traffic .-^epcrtc or Lab Narrative i.tdicata £.-iy proolsEs vit-*". samole receipt. conoition of sampies. inaiytical proolens cr special ,-otationo affactinc tr.a cuaiity cf t.'ie data? — ij^ _ ACrrc::: if any sample analyzed as a s o i l , otiicr t.nan TCLT, contai.ns 501-90* vater, all data snouid be flagged as estituited ("J"^ . If a soil sample, other t.^.an TCLT, contains core t.'-.an 901 vater, a l l data should be qualified as unusacle (R) . ACrrc::: if z2Tr.-zlzs vara not iced upon r e c e i p t at t.*:e iaisoratcrv, flao all positive r e s u l t s "J" ir.c ail .-.on-Gstectc "TJ". • • • " . 1 2.1 Have a.ny E:IA technical .holding t i n s s , detemnea froo: date cf collection to date cf extraction, oaen exceeded? J ^ I—1 _ Continuous extraction cf vater samples fcr BNA analysis r.ust be started vit.'iin seven . days of t.'-.e cate of collection. Soil/ s«dinent zzra-ples rr.ust be extractad vithin 7 days cf collection. Extracts r.ust be analyzed vitnin 4 0 days of t.'-.a date of extraction. 304314 STA}iDA^D CPi..r.^Tm3 PROCZZL--.Z Data: J a n u a r y 1232 Revision: 3 v r £S SD :;/A Sample l i t e sasiple .Hatri:^ Sampled <GcxiO^ SOIL, ^-Ali-M^n (See T r a f f i c .^.encrt; D a t e L.ih Date Date Raceaved Z:ctractad Analyzed '\\^'^\^'\ iQl^\^"\ i> o\\^\^.*^ :.o 3 . 1 ACTTD::: i r t e c h n i c a l h o l d i n g t i r e s are exceeded. flag a i l p o s i t i v e r e s u l t s as e s t i m a t e d ("J") and sample q u a n t i t a t i o n l i r a t s as e s t i m a t e d ( " U J " ) , and doourant i n t h e n a r r a t i v e t . h a t h o l d i n g t i z e s v a r e exceeded. I f a n a l y s e s v s r e done r . c r e t.'-.an i ; days baycnc h c l d i . - g t i n a , e i t h a r on t.ha f i r s t a.-.aiysis c r upon r a a n a i y s i s . rhe r e v i e w e r r.ust usa p r c f a s s i c n a l 3udgement t o d e t e r m i n e t h e r e l i a b i l i t y c: t h e d a t a and t h e e f f e c t s cf a d d i t i o n a l s t o r a g e on t h e sample r e s u l t s . At a n i n i n u n . a i l r e s u l t s s h o u l d ba q u a l i f i e d " J " , b u t t.":a r e v i e w e r r.ay d e t e r m i n e t.iat r . o n - d s t e c t d a t a a r e ur.usaole (_;^H'').'lf h o l d i n g t i n a s a r e exceeded by n o r e t.-.an 2S d a y s , a l l non d e t e c t data a r e u n u s a c l e (R) . s u r r t r s r g cg^g...grv '^'^•rr. TZ'. Are t h e EHA S u r r o g a t e R e c c v e r y Summaries (Foro I I ) p r s s e n t for e a c h of t h e following - . a t r i o a s : a . Low Water b . low S o i l c . Mad S o i l 304315 L I L A L - — . xii sTAiiDARD :7rR.\Ti::3 PRDCZZLTJ: Date: Januar-y 1332 Revision: 3 VTer :;o N/A a. b. c. Low Low Lav Water soil soil .2 Are a i l the £HA tarries l i s t e d cn tiie apprcprtata Surrorata Recc*.-erv Surctariss fcr eacn cf the following =atri.=£s: LILAL L L 1-1-1 ACTIZ::: Call lib f:r explanaticn/rssucnittzls. If r.issing oaliveracles are unavailable. docunant erfact in data assessments. 3.3 w«re o u t l i e r s r.aLr>:Ed correctly with an asterask? fY^ ACTID:;: circle all outliers in red. 3.4 w«re tvo or r.ore hase-neutrai C^ acid surrogate reccverias cut of stecificaticn fcr a.ny samcls or r.ath=i bla.nX? " 1_1 V^ If yes. ware samples reanalyzed? i 1 "S^ Were r.arncd blanxs rsanalyzea? LX, r- ACTID::: if all B.HA surrogate recoveries are > 101 but tvo vithin t.-.e base-neutral or acid fraction do not - a c t SOW s p e c . . . . >.-..s , — - g - . acid c—ro---—s) ; 1. Flaa a i l positive results as estirated 2. Flag a i l non-cstects as e s t i r a t e d detection i i t i t s ("UJ"', vnen recoveries are less t.'-.an t.-.e lower acceptance i i n i t . 3. If recoveries are areater than the upper accaotonce l i c i t , do not qualify non-oetacts, 304316 _-wiiij<->a-.w 2TZRATII'j Pr.uCZZL.-«.i. Date: Januar-.- 1=32 Revision: 3 ^ ^ :;3 N/A If a.ny taae-reutral ^^ aaid surrccate has a recovery of <ioi: 1. Positive results for the frac^iar. with <10t surrogate reccvarv are oualifisd with "J". 2. Non-cetects for that fracrlan should ba qualified as unusaole (R) . .-rcfassional judgaiient snouid be used to qualify 'iata tr.at have natnod blanX surrogate raccveriss cut cf specification in both original and rsanaiyses. Checx the i.-.temal standard areas. 3.5 Are t.here any transcrittion/calculatian errors bttwaen raw data and For= 117 ___ ''^'' ACTTC::: If large errors exist, call lab fcr expla.nation/resubnittal. naXe any necessary corrections and doaumant effect in data assessments. " • — — - » . . C .» i V o e f ^ / » - . — r ——^ 4.1 IJ t.*".e .".atri:^ SciXe/Hatri:^ Soike Duplicate F.accvery Tzrrz ; Fcra I i r ; present? 4.2 -"ere r.atrix spikes analyzed at the rsquirsd frequencv for" eacn cf t.te follovinc r.atricas; rX, a. Lou Water i—l —^ — b. Lav Soil c. Med Soil Lh r ACTID": If any r.atrix spike data are missing taXe the action soecified in 3.2 above. 304317 J r.".'-"-.——-."> Date: January 1232 Revision: 3 YZ£ ;;a N/A How cany =HA spiXe raccverias are cutsida - f- • • • • — " - - • > Va*- o — £_Oil^ •^ r •*• r" — O out of 22 4.4 How cany RPD's for a a m : c spike a.nd a a t r t i spike c u p i i c a t a raccverias are cutside QC w »•• o — 5.0 -0. r y » 1 • ;ut AC7I2::: )io action is taken cn KS/HSD data alcng. However, using inforrad prciassicnal judgement, tha data reviewer ray usa the natri:: spike s.n± natri:; spike duplicate results in conjunction vith other CC critaraa and determine tha need for some qualification of t.ha data. - * ^ ' " - - - - . • • - • Is tne ."^athod Blanx Sumc;ary .'."cm IV', prese.nt: "rsquencv cf A n a l y s i s : • ^ 1 .Has a r a a g e n t / - e t h c d blank analysis been reportao per 2 3 samples of similar r . a t r i x . or concentration l e v e l , and for each e x t r a a t i c n - batch? x t . r.ii a ENA r.sthcd blank bean analyzed for eacn GC/y.S system used? (See SCW p. b - r9/SV, Section 8.7) ih, _ ACTID::: if any r.ethcd blank data are r.issing, call lab for Explanation/resucmittal- If not available, usa profassional judgement to detemina if the associatad sample data snouid ba qualified. 304318 5 . 4 S.ywiWi-w-vw CPi..-.ATr*T3 rr.DCZ3L-\Z Date: J a n u a r y 1=32 R e v i s i o n : 3 V r C v; Z£ NO N/A raview t h a blanx rzv d a t a - c.-.r c a t to grams (RICs'. , q u a n t r a c c r t o or d a t a system p r i n t o u t s and s p a c t r a . I s t h a c n r c a a t o g r a p n i a p a r f a r a a n c e ( b a s a i i n a s t a b i l i t y ) for eacn i n s r r u c i a n t a c c a a t a a i a f o r BIIAs? • rAi ACTTC:;: i-ze profassional judgement to datamane tha efface on tha cata. r - - - , Hota: "Water clanks", "drill bla.nks" i.nd "distilled vater blanxs" are validated like any ether sample and are pot used to qualify tha data. Da not confuse t.hen with tna ctnar CC blanks discussed belov. 6.1 Da any r.ethcd/instruaant/reagent blanks have positiva results (TCI. and/or'TlC) for B.VAs? When applied as describad belov, tha contaminant oanca.ntratian in these blanks are aultipliad by tha sample dilution factor and correctad for \ moistura vnere necessar'.'. rY.^ Zo anv tiaid.'rinse/ tlanks nave cositiva EIIA results (TCL and/cr TIC;? ' LJ. t ACTID::; prepare a l i s t of the samples associated with each of the contaminated blanks. (Attac.n a separate sneet.) Note: All field Snank results associated t a a particular graup of samples (nay exceed one per case) r.ust ba used to qualif'/ data. Blanks may not be qualified because of contamination in a'not.ner blank . Field Blanks must ba qualified for surrogate, spectral, instrument performance cr calibration QC proalems- 304319 >^v>iv>.n-'._ • - . - i r J v T - . . . ^ .r-.OC——~.">-i- Date: Ji.nuar-/ 1 = 32 Revision: 3 NO N/A ACrrc::; Follow tna d i r a c t l a n s i n t h e t a b l e b a l c v t o q--alify TCL r e s u l t s dua t o contamination. J s a t h e l a r g e s t v a l u e f r c a a i l t.'-.a a s s o c i a t a d b l a n x s . If g r o s s c o n t a a i n a t i a n e x i s t s , a l l data i n t h a a s s o c i a t a d s a m p l e s should ba q u a l i f i e d a s unusacla (R). lampia c a n e > CRQL :ut < i c x b l a n x Sample cone cCROL m is< i:x t l a n x v a l u e Sampia cona > CRwL value 6 >lOx b l a n x P h t . t a . a t a E s t e r s "lag sampia r e s u l t Report CRQL q u a l i f y "U" No q u a l i f i c a t i o n i s needed Sampia c a n a 5 CRQL but" < 5x b l a n k Sampia cona <; CRQL « i s < 5x b l a n k v a l u e ot..ar C o n t a m i n a n t s Samoie cone > CRQL value & >5 b l a n k v a l u e "lag sampia r a s u l t Repcrr c u a l i ; No q - - 3 l i f i c a t i o n i s naeaed Analytas q u a l i f i a a ' a r e s t i l l o o n s i d a r e a a s f o r c a l i b r a t i o n c r i t a r i a . t * * t t ^ ^^mm ^ \ -y ^ 41 W 4 * •>«< .-nan c--alifying concsntration in tha sample is less than five tiaas the cancantraticn in tha most contiainated associatad blank, flag tha sample data "H" (unusaole). 5.3 Are tnare field/rihse/equipmsnt blanks associatad vit.*: every sampia? ACTIO:;; For lev level samples, ncre in data assessment that t.'-.are i s no associatad field/rinse/equipmant blank. Exception: samples taken from a drinking vater tap do not nave associated f i e l d blanks. r 1 s: 304320 STAIiDARD 2?ZRATI!*3 PROCZ -.Z. Date: Ja.nuar,* 1232 Revision: s rzs NO N/A 7.1 Are t h e GC/HH Instruaant F e r r a r a a n c s Checx Forms !^?$^-.yi P-ssent for oacafluaratrapnanyiphcspnina 7.2 Are t h e enhanced bar crach s a e c t n a a and mass/ charge ( a / z ; listi.nc for tha'DFTPP provided for eacn twelve hour snift? r ^ .-.as a.n i.nstruaant tarforaanca c.-.acx solution been a n a l y z e c for everv twelve hours cf samole a n a l y s i s per i.nstruaant? r ^ ACTIO::: L i s t data, l i a a , i.tstramant IZ, and sampia analyses for v n i c h na associated GC/MS tunang data are a v a i l i b i e - DATZ TIHZ INSTRUHZJIT SAMPLZ .VUKEZRE ACTIO::: i f l a b cannot preside missing d a t a . re-ject ("R") a i l data generated outside an acceptable tvalve hour c a l i b r a t i o n inter^.'ai. ACTIO::: i f mass assignment i s i n e r r s r , flag a l l a s s o c i a t e d sample data as unusable (.R) . 7.4 Have t h a ion abundances been normalized t o m/z ^-- isa? LH 304321 Date: January 1232 Revisicn: 3 YZS NO N/A 7.5 :-:«ve tna ion aauncanca criteria been mat far eacn i.-.strua:ant usad? H^"^ _ ACTIO:;; List a l l data which do not aaet ian abunaanaa crttaria (attaan a Baparate sheet;. ACTIO::: if ian abundance criteria are nor act. the Reaion II TPO must ba notified. 7.S .-.re there any transcription/calculation e r r o r s betvaen a a s s ' l i s t s and"Fora Vs? (Checx a t l e a s t tvo values cut if errors are found, check acre.) ''^'' 7.7 Have the appropriate nuaaar of signifiaant figuras (tvo) been reportad? ' £Ll ACTIO::: if large errors exist, call lab far expianation/resubmittal, make necessary corrections and document effect in data assessments. 7.S .-.re tha spectra cf tha mass calibration compound ^, iocantaala? LJL. Jse profassional judgement to determine whet.ner associated data snouid ba accepted, qualified, cr ra'^ectad- a.l Are the organic Analysis Data Sheets (Form I BHA) present vith required header information on each page, for each cf tha follcwing: a. Samples and/or fractions as appropriate LH. b. .'^atriic spikes and matrix spike duplicates jLl c. Blanks i j ^ 304322 -TAKDARD 0P.£.j-.A.TI.T3 rROCZOL.'.Z Date: January 1232 Revision: s V T C ZS NO N/A 5.2 Has GPC oiaanup been perfarmad cn a i l s o i l / saaiaant lample e x t r a a a s ? r NS ____ ACTIO::: I I data suggasts t h a t GPO vas nat perfarman. use p r c i a s s i c n a l judgement. Make note in " C s n t r a a t rrcalaas/Non-ccmpliance". 8.3 Are tha EHA Reccnstruaaad Ion c.hraaatograms.. tha mass spactra for t h e i d e n t i f i e d compounds. and t.ha cata system p r i r . t a u t s (Quant Reportaj includad in the samoie cackaca for eacn of t h e a. Samples and/or f r a c t i a n s as appropriate 1 ^ • b. Matri:; spikes and matri:; spike d u p i i c a t a s (Mass spactra n e t raquirad") l-il- — c. Blanxs ACTIO::: if any data are missing, take action specified in 3.2 above. 8.4 Are tha resoonse factors shown in the Quant Report? i-J.. -JL — C.5 Is c-trcmatocraa.tic parfcrmanca accsptaala v i t h respect t o : Baseline s t a b i l i t y ? l l ^ - — ^ 1 Rtsolution? — Peak shape? H i - F u l l - s c a l e "graph (attenuation)? Other: ACTIO::: use p r a f s s s i c n a l judgement to determine the a c c e a t a b i l i t v of t.ha data. I l l _ 304323 STANDARD OPZPATi::! PROCZZURZ Date: Januar-/ 1232 Revision: 3 V T C NO N/A 3.6 Are t h e iib-eenerrted s t a n d a r d mass soectra cf i d e n t i f i a c E.HA coaacunds p r a s e n t for eacn s a a a i s ? i^ ACTTO::; If a.ny tass spectra are missing, take action spacifiad in 3.2 abova. If lab does not ganerate t h a i r own standard spectra, make note in "Cantraat Prcbians/ Non-ccaplianca". If spectra are missing, ra-^ect all positiva data. 8.7 Is tna K217 of aacn raaortad ccmaaund vithin COS RJIT units cf tha stancara P3.T in tha continuing ^, calibration? L ^ _ 3.E Are a l l ions present in the standard aass spectz-um at a relative i n t e n s i t y greater than . 101 also trasent i.n the samaia mass saactrum? XJ2m . ___ _ • • • 8.9 Da sample and standard relative ion i.ntensities agrae vithin 2;\? I-bl • - ACTIO::: Jsa profassional judgement ta determina accaptability cf data. If it is daterminad t.hat i.-.aarract idantifiaations ware made, ail such data should ba re-iectad (R) , flagged ">T" (Fresuaptiva evidence c: tha prasenca cf tha compound', cr cnangec to not datactad (U) at t.^a calculated detection limit. Z.i order to be positively identifiad, tha data _ must coaply with the crttaria listed in 8.7, S.8, and 8.9. ACTIO::: when sample carry-cver is a possibility, professional judgement should ba usad to determine if i.-.strumant crass-ccntaminatian has affected any positiva compound identification. c n Tenf — • ••3 1V.' T-»a,^.--•'--i^^ c~—rounds r""^' 5.1 Are all Tantativeiy Identified Compound Forms (Form I, Part B) present: and da listed TICs includa scan number or retention time, estimated v^ concentration and "J:;" qualifier? SLX, 304324 S..AI»DARD CPc_-JvTII»3 PROCZ—L.-JZ Date: Januar,* 1232 Revision: i YZS NO N/A Q -.2 Are t n a aass spectra for tha t a n t a t i v a i y idantzfiad coapouncs and a s s o c i a t e d "bast natch" spactra inaludad in t.ha aaaaia paokaae for eacn of t h a following: a. Samples and/cr fractians as appraariata ^ j ^ . - b. Blanics fN^ __ ACTIO::: if any TIC data are missing, take action spacifiad in 3.2'above. ACTIO::: Add."J::^ qualiflar if missing. 5.3 Are any TOL campounds (fram a.ny fractian) listed as TIO campounds (examaie: 1,2-dimat.nylbenzene is xylene a voA TOL - and" snouid noa ba reocrtad as a Tie; ? £ i i _ ACTIO:;: Flag vith "P." any TCI. campound listed as a TIC. 9.4 Are a l l ians prasent in t.ha reference mass spectrum vit.h a relative i.ntansity greater t.'-.an 10* also prasent in tha samole mass soectrum? '"^ Q t Do TIC and "bast r.atcn" standard relative ion i.ntansitias agrae vithin 20*7 jjil. ACTIO:;; Jsa professional judgement to determina accaptaaility of TIC identifications. If it is determined that an i.-.aarraat idantifiaatian was made, o.'-.anga idsntifiaatian to "unknown" or to some less specific identification (examaie: "C3 substitutad benzene") as apprcpriate. Also, vnen a ccmpound is not found in any blank, but is a suspected artifact of a common laboratory contaminant, cha result snouid ba cualifiad as unusaole (H). 304325 Date: January 1392 Revisicn: s YES NO N/A 10.1 Are there any transcription/calculation" errors in Form I results? Chacx at least tvo positiva values. Verify that t.he carrsct intamai standard, quantitatian ian, and RKT were used to calculate Form I result. Were any errors fcund? ___. r >3 . 10.2 Are the CRQLs adjusted to reflect sample , dilutions and, for soils, sample moisture? fHi ACTIO:;: if errors are larae, call lab far cxplanation/resunmittal, make any necessary corractions and dooumant effect in data assessments. ACTIO:;: when a sannle is analyzed at mare than one dilution, the lowest CHQLs are used (unless a QC exceedancs dictates the usa of the higher CRQL data from tha diluted sample analysis). Replace ccncentraticns t.hat exceed t.he calibration range in the original analysis by crossing cut the "Z" and ifs associated value on the original Form I and sucstituting the data from tha analysis of tha diluted samale. Specify vhich Form I is to ba used, then draw a red " X" across the entire page of ail Form I ' s t.hat should not ba used", i.nciuding any in the summary package. 11.0 Standird^ f-^.ta ^GC/^g^ 11.1 Are the Reconstructed Ion c.'-.rcmatcgrams. and L svstam prir.tauts (Quant, Reports) present -^ i n i t i a l and continuing calibration? U-l data for ACTIO::: if' any calibration standard data are missing, take action specified in 3.2 above. 304326 STANDARD OPZPATHIO PROCZOURZ Date: January 13 32 Revisicn: a YES NO N7A 12.0 GC/^'^ --^-^11 ^ , . ; u , , , . . - . , ^ ^ ^ .,.. 12.1 Are tha I.titial Calibration Forms (Fora Vi; present and coaplate far tha EHA fractian? f H ACTION: If any calibratian standard farms are missing, take action specxfied in 3.2 above. 12-2 Are respsnsa factars stable for E.HAs over tha concentration ranee of the calibration? (% Relative standard deviation (^RSDl < 30.01) r>^ _ ACTION: Circle all outliers in red. NOTZ; Althoucn 2 0 ENA comaounds have a minimum RRF a.nd na maximum "tRSD, the technical criteria are the same for all analytes. ACTION: If the K RSD is > 30.Ot, qualify positiva results for t.tat analyte "J" and non-detects using profassional judcement. When RSD > 90*, flag all non- detact results for t.'-.at a.nalyte R (unusable) . NOTZ: Analytes oreviousiy qualified "U" due ta blank contamination are still considered as "^.its" when q--alifying for calibration critaria- 12.2 Are a i l ENA compound RUFs > 0.05? lliL.. ACTID:;: Ciraie a l l o u t l i e r s in red. ACTICN: If any RRF < 0.05 1. "R" a l l n o n - d e t e c t s . 2. "T-° a l l p o s i t i v e r e s u l t s . 12.4 Are t h e r e any t r a n s c r i p t i a n / c a l c u l a t i c n e r r o r s i n the r e t o r t ma of average response factors (RIIF) .51. w~u vaj,ut±±i u u w ' "^ are found, check more.) or \ RSD? (Check at l e a s t tvo values but if e r r o r s .^^ ACTION; Circle E r r o r s in red. 304327 STANDARD CPZRATING P?.OCZirJP.Z Date: January 1232 Revision: s YES NO N/A ACTION: If errors are l a r c e , call lab for explanation/resubmattal. aake any necessary carr-acaaans and note errors in data assessments. 1 3 . 0 GC/y? C ~ r - - - " ' - - ' ' l l <u«.,^4«.. ^-r***-— ^TT'r^ r » l l l » T T I I » - 1 . - - . . . . s. - - - - - , . , . • - - . . . • - - . 13.1 Are t.ha Continuing-calibratian Forms (Form VII] present a.nd ccapleta for tha BNA fraction? r'li _ 13.2 Has a continui.ng calibration standard- been analyzed for every tvalve hours of samoie a.nalysis per instruaant? f"^ _ ACTIO::: List below a l l sample analyses that ware not within twelve hours of a continuing calibration analysis for each instrumena usad. ACTIi::: If any forms are missing cr no continuing c a l i b r a t i o n standard has been analyzed vit.hin tvalve hours of every sample analysis, call lib fcr explanation/ resubaittal. If cantinuing calibration data are not available, flag all associated sample data as unusable ("R**) . 13.3 Do any semivolatile comaounds have a * Difference (% D) between the Tnitial and continuing RRF .. which exceeds tha -r 25.01 c r i t e r i a ? I L . 1—1 ACTION: Circle a l l o u t l i e r s in red. ACTIO:;: Qualify both p o s i t i v e results and non-detects for tha outlier compound(s) as estimated (J) . When hH i s above 901, reject a l l non-detects fcr t.hat analyte (R) unusable. 304328 STANDARD C?ZPJVTI:T3 PROCZZL'P.Z Date: January 1332 Revision: S YES NO N/A 13.4 Co any semivolatile ccmpou.nds have a R21F <0.0S? rY,i ACTIO::: circle all outliers in red. ACTION: If PJ^F <o,05, qualify as unusable (R) associated non-detects and "J" associated positive values. 13.5 Are there any transcription/calculation errors in the reporting cf average response factors (RJIF") or \ difference (ID) betveen initial and continuing RRFs? (Check at least tvo values but if errors are found, chacx more) . I ^ ACTIO:;: circle errara ir. red. ACTION: If errars are large, call lab for expianation/resubmittal, aake any necessary corrections and document effect in data assessments. 1 4 - 0 T w ^ o ^ — ^ l c ^ ^ ^ r i ^ ^ u ^ / r>A..-. tTT"r—^ ^ ^ " ' ^ ' ^ — • . — - — • • " 1 . ^ - . . . . — . 14.1 Are t.he i.nternal standard areas (Form VIII] of every sample and blank vithin t.he upper and lower limits (-501 to + 1001) for each ccnti.-.uing .^ calibration? f JM ACTIO::: List all tha outliers below. Samaia = Internal Std Area Lower Limit Upper Limi (Attach additional sheets if necessary.) ACTIO:;: l. if the i.ntarnal standard area count is outside t.he ucpar cr lower limit, flag with "J" all positive results^ and non-detects (U values) quantitated with this internal standard. 304329 STANDARD 0PZRATIN3 PR0CZZL*RZ Date: Januarv 1332 Revision: a YES HO N/A 2. Non-eetects associated with i s areas > 1001 should not ba qualified. 3. If tha IS area i s balow tha lower limit (<501), qualify all associated non-detects • (U-valuas) "J«. if extremely low area counts are reaortad (<2S1) or if performance exhibits a major abrupt drop off, flag a l l associatad non-detacts as unusable (R). 14.2 Are tha retention times of tha i.ntamal standards vithin 3 0 saconas of the associated c a l i b r a t i o n standard? f^^ _ ACTION: Professional judgement should be used ta qualify data if the retentian times differ by more than 3 0 seconds. IS.O Field r-.-sli-rit &SL 15.1 Were any field duplicates submittad far BNA analysis? r i ^ ACTIO:;; compare tha reportad results fcr field duplicates and calculate t.he relative percent diffarenca. ACTIO:;; Any gross variation betveen f i e l d duplicate results must ba addressed in the reviewer narrative. However, if large differences exist, identification of field duplicates s h e u l d ^ e confirmad by contacting tha samoler. 304330 SDG No. 97130 SVOCSj VOCSy Inorganics, and Organics Checklist m 304331 QA/QC Review of TAL Inorganic Data for Pace Analytical SDG: 97130 Novembers, 1997 Holding Times: Samples were analyzed within EPA Region II CLP holding times. Initial and Continuing Calibration Verification: Sodium (111.2%) had a percent recovery outside control limits (90-110%). Cyanide (119.6%, 120.0%, 118.2%, 117.8%, 116.6%, and 119.0%) had percent recoveries outside control limits (85-115%)). Results for sodium and cyanide should be considered estimates (J) in associated samples. CRDL Standard for AA and ICP: Arsenic (79.4%, 79.0%, 77.2% and 77.0%), lead (73.8%), selenium (64.4%) , 75.2%o, and 74.8%), silver (76.2%)), and thallium (78.6%)) had percent recoveries outside Region II control limits (80-120%)). Results for these metals in associated samples within effected ranges should be considered estimates (J). Blanics: Initial and continuing calibration, and preparation blanks had analyte levels less than the CRDLs as required by Region II. Field blank FB0918 contained copper (82.8 ug/L), selenium (2.5 ug/L), and zinc (166 ug/L) above their CRDLs. Field blank FB0919 contained calcium (13000 ug/L) and zinc (381 ug/L) above their CRDLs. Field blank FB0922 contained calcium (16200 ug/L) and zinc (452 ug/L) above their CRDLs. Field blank FB0923 contained zinc (46.6 ug/L) above its CRDLs. Field blank FB0924 contained zinc (42.8 ug/L) above its CRDLs. Field blank FB0930 contained calcium (11500 ug/L) and zinc (432 ug/L) above their CRDLs. Results for these metals less than five times the associated blank level should be considered unusable (R) in samples. ICP Interference Check Sample: Arsenic (79.5% and 79.6%), cobalt (79.4%, 79.6%, 78.8%, and 78.5%o), and selenium (54.2%) and 54.4%)) had percent recoveries outside control limits (80- 120%)). Results for these metals should be considered estimates (J) in associated samples. Spike Sample Recovery: All percent recoveries were within control limits (75-125%)) for water spike samples FB0918S, FB0919S, FB0926S, and FB0930S. Antimony (41.9%), manganese (65.1%)), and cyanide (51.2%)) had percent recoveries outside control limits (75- 125%) for soil spike sample 70202S. Antimony (13.4%) had a percent recovery outside control limits (75-125%)) for soil spike sample 200204S. Results for antimony, manganese, and cyanide should be considered estimates (J) in associated soil samples. Duplicates: Calcium (39.1%o) had relative percent difference the CLP maximum (20%o) but were below the allowable maximum (100%)) for duplicate sample 702022D. Zinc (27.6%)) had relative percent difference the CLP maximum (20%)) but were below the allowable maximum (100%o) for duplicate sample 200204D. These metals were appropriately flagged as per Region II. 304332 Laboratory Control Sample: All percent recoveries were within control limits for the water LCSs. Silver (7.1 rag/kg) had a recovery outside control limits (54.6-92.1 mg/kg). Results for silver should be considered estimates (J) in associated soil samples. Standard Addition Results: No results were quantitated by MSA in this LP. ICP Serial Dilution: Copper (21.7%), potassium (22.8%), and zinc (12.8%) had %Ds above the allowable maximum (10%>) for soil serial dilution sample 702022L. Lead (13.2%)), potassium (18.8%.), sodium (11.5%)), and zinc (28.7%)) had %Ds above the allowable maximum (10%)) for soil serial dilution sample 200204L. Results for copper, lead, potassium, sodium, and zinc should be considered estimates (J) in associated soil samples. Magnesium (15.1%)), potassium (38.4%)), and sodium (12.8%)) had %)Ds above the allowable maximum (10%)) for water serial dilution sample FB0918L. Calcium (11.9%o), potassium (88.8%)), and sodium (58.8%)) had %)Ds above the allowable maximum (10%)) for water serial dilution sample FB0926L. Results for calcium, magnesium, potassium, and sodium should be considered estimates (J) in associated water samples. Instrument Detection Limits: All IDLs were at or below the CRDLs as required. Percent Solids for Soils: All soil samples had percent solids above the allowable minimum (50%)). G:\STAFBDANNE\Island\97130.INO.wpd 304333 SD6-# 91i3o Evaluation of Metals Data for the contract Laboratory Program (CLP) based on BOS?. 3/90 (SOP Revision XI) .ZFARZD BY: <-L.J ^La( DATE: Hahii S.^.eikh, Ooality Assurance Qieioist Tcxic and kazardous Waste Section - - ^ ^ - ^5 •rT.OVED BY: • - > - • N ;A.-V ?.^>DVZD BY Robert Runyon, thij^f Monitoring Management Branch DATE: I - :^^ Kevin KubiX, Chief Tcxic and Hazardous Waste Section DATE: -f-A^ 304334 STANDARD OPERATING ^DCEDURE Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Revision: 11 Socpe This procedure is applicable to inorganic data obtained frcn contractor labcrstories working for Hazardous Waste Site Contract Laboratory Program (CLP). The data validation is based upon analytical and quality assurance requirements specified in Statement of Work (SOW) 3/90 . Responsibilitiea - Data reviewers vill ccrolete the follcwing tasks as assigned ty the Data Review Ccordinator: For a total review: . 1 Data Assessment - "Total Reviev-LrvorcTanies" ChecJclist Appendix (A.IK ie reviewer must answer every question on the checklist. ^1^ Data Assessiient - Data AssesrTnpnt Karrative (Appenrtix A.2) The answer on the checklist must ratch the action in the narrative (appendix A.2) and on Form I's. Do not use pencil to write the narrative. .2 Cor.tract Non-Ccrt?liance - EM3 Report (Appp-nrfiv TV.'^) This report is to be cccpleted only when a serious contract violation is encou-.tered, or upon the request of the Data Validation Task Monitor, or Technical Proiert Officer (TPO). Forward 5 copies: one each fcr internal files, appropriate Ragic.nal TPO, Sample Management Office (SMO) and last f-'o addresses c: llailing List for Data Reviewers (Appendix A.4). In other cases, all contract violations should be appended to the end of the Data Assessment Narrative (Sec. A.2.2). .4 CLP Data Assessment Sumvsry Fofwq .1 Appendix A.5 Fill in the total n r r t e r of analytes analyzed by different analyses and the n'jrber of analytes rejected or flagged as estimated due to corresponding quality control criteria. Place an "X" in boxes where analyses were not perfcrrned, or criteria do not apply. .2 Appendix A.6 Data revie.^er is also required to fill out Inorganic Regional Data Assessnent ^ ^ f o m (Appjendix A.7) provided by EPA Headquarters. Codes listed on the form ^^B^'ill be used to describe the Data Assessnent Surnnar^'. 304335 STANDARD OFERAm^G H^OCEDURE le: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Revisicn: 11 1.5 Data Reviev Log: It is X H miifr^nded that each data reviewer should maintain a log of the reviews ccrpleted to iiclude: a. date of start of case reviev; b. date of ccnpleticn of case review c. site d. case number e. contract laboratory f. number of sanples g. matrix h. hours workad i. reviewer's initials 1.6 Telephone Record Lo? - the data reviewer should enter the bare facts of inquiry, before initiating any phone conversation with CLP laboratory. • After the case review has been ccrpleted, mail white copy of Telephone Record Log t o the laboratory and pink copy to SMO. File yellow copy in the Telephone Reoord Log folder, and attach a xerox copy of the Telephone Record Log to the ccrpleted Data Assessment Narrative (;^:pendix A.2). 1.7 Forvarded Paoervor): .7.1 Upon cccpletion of review, the follcwing are to be forwarded to the Regional Sarple Control Center (RSCC) located in the Surveillance arxi Monitoring Branch: a. data package b. ccrpleted data assessment checklist (Appendix A.l,original) c. Sl-fD Contract Cc::c:liance Screening (CCS) d. Record of Camrrunication (copy) e. CL? Reanalysis Request/Approval Record (original + 3 copies) f. Axjpendix A.6 (original). .7-2 For^-ard 2 ccpies of caipleted Data Assessment Narrative (Appendix A.2) along with Z copies of the Inorganic Data Assessment Form (Appendix A. 6) and Telephone Record Log , if any,: one each for appropriate Regior^al TPO, and the other one to EPA HJSL office in Las Vegas. The addresses of TPOs and EPA office in 1^^ Vegas cure given in Appendix A-4. .8 riled Paperwork - Upon ccsrpletion of review, the follcwing are to be filed within M:-3 files: a. TV'o copies of ccnpleted IData Assessment Narrative (Appendix A.2) each carr^'ing ~" Appendix A. 6. b. Telephone Record Log (ccpy) c. S:D Report (copy Appendix A-3) d. CLP Reanalysis Request/Approval Record (ccpy) 304336 STANDARD OPEEyOTNS PROCEDURE Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Revisicn: 11 Data Cccgileteneas Each data package is chackad by a Regional Saaple Cantrol Coordinator (RSSC) for completeness. A data package is »«^qTmoH to be caiplete when all the deliverables required under the contract are present. If a data package is inoccplete,the RSSC would call the laboratory for missing document (s). If the laboratory does not respond within a week, ShJD and hMB coordinator of Ragicn H will be notified. Re-jecricn of Data - All values determined to be unacceptable on the. Inorganic Analysis Data S.heet (Form I) rust be lined over with a red pencil. As soon as any reviev; criteria causes data to be rejected, that data can be eliminated frcn any further review or ccnsideration. ' Acceptance Criteria - In order that reviews be consistent among reviewers, acceptance criteria as stated in Appendix A.l (pages 4-25) should be used. A±iitional guidance can be fourxi in the National Inorganic Functional Guidelines of October 1, 1989. S>C Contract Cccslianee Bcreening (PCS) - This is intended to aid reviewer in locating any problens, both corrected and uncorrected. However, the validation should be carried out even if CCS is not present. Resutnittals received frcn laboratory in response to CCS rrust be used by the reviewer. Request for Reanalysis - Data reviewers must note all items of contract non-conpliance v.-itr.ir. Data Assessnent Narrative.If holding times and sample storage tines have not been exceeded, TPO ray request' reanalysis if items of non-corpliance are critical to data assessment. Requests are to be made on "CLP Re-Analysis Request/Approval Record". Record of Ccrrmmication - Provided by the Regional Sairple Control Center (RSCC) to indicate v^hich data packages have been received and are ready to be reviewed. Roundi-ng off numbers - The data reviewer will follow the standard practice. 304337 STANEARD OPERATING FROCEEURE e: Evaluation of Jfetals Data for the Contract Laboratory Program Appe-ndix A.l: Data Assessment - Ccntract Osipliance (Total Review) Date: Jan. 1992 Nunber: HW-2 • Revision: 11 1 Contract Caaplianee Screening Report- (CCS) - Present? ACTION: If no, ccntact RSCC. I£S. . m UZA 2 Record of CccTmmication (freta R30C) - Present? ACTION: If no, request frcn RSCC. 2 Trip Report - Present sind ccrplete? ACTION: If no, contact RSCC for trip report. ^^mple Traffic Report - Present? Legible? ACTION: If no, request frcn Regional Sanple Control Center (-RSCC). 5 Cy.^BT Paoe - Present? Is cc-.'er page prtperly filled in and signed by the lab ra-nager or the manager's designee? ACTION: If no, prepare Telephone Record Log, 'and contact laboratory. Do n'LTbers of samples correspond to nunbers on Record of Ccrrrunication? Do sa.Tple nambers on cover page agree with sample n'JTbers on: (a) Traffic Report Sheet? '<:'> ^Hbri (b) Form I's ON: If no for any of the above, contact RSCC for clarification. [_] _ JL [_] _ JL [ ] [ ] JL Y [JL) _ _ 304338 STANDARD OPERATING PRDCECURE le: Evaluation of Metals Data for the Contract Laboratory Program Appendix A.l: Data Assessment - Ccntract ciirpliarxs (Total Review) Date: Jan. 1992 Nun±)er: HW-2 Revision: 11 .6 Fora I to IX X ^ m BZh ,6.1 Are a l l the Form I through Form IX labeled with: Laboratory name? Case/SAS number? EPA Scuiple No.? SDG No.? Contract No.? Correct units? Matrix? ACTION: If no for any of the above, note under Contract Problem/Non-Ccrpl iance section of the "Data Assessment Narrative". Do any ccrputation/transcription errors exceed 10% of reported values on Forms I-HX for: (NOTE: Check a l l forms against raw data.) (a) a l l analytes analyzed by ICP? (b) a l l analytes analyzed by GFAA? (c) a l l analytes analyzed by AA Flame? (d) Mercury? (e) Oj-anide? ACTION: If yes, prepare Telephone Log, contact laboratory for corrected data and correct errors with red pencil and initial. _ ] Ji _ ] JL ^ — ± _] -^ _ _] X — 304339 STANDARD OPERATING P5DGEDURE e: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Nunter: HW-2 Appendix A.l: Data Assessment - Ccntract Rsvision: 11 Cccpliance (Total Review) ^. "m nzr .7 Raw Cata .7.1 Digestion Log* for flame AA/ICP (Form XIU) present? 1 X 1 Digesticn Log for fumaoe AA Form XIII present? [ ] Y Distillation log for mercury Form X H I present? f Y 1 Distillation Log for cyanides Form XIII present? f V- 1 Are pH values (pH<2 for all metals, pH>12 for cyanide) present? [ ] V> *Kei(^t:s, diluticns and volumes used to obtain values. Perce.nt solids calculation present for soils/sediments? [_XX Are r^ -ation dates present on sample preparation logs sheets? •-2 Keas-j-:_:^-t read out record present? ICP Flame AA Furnace AA Mercury • Cyanides r.3 Are a l l raw data to support a l l sample analyses and QC operations present? Legible? Properly labeled? ACTION: If no fcr any of the above questions - in sections A.1.7,1 through A.1.7.3, write Telephone Record Log and contact laboratory for resubrnittals. r ^ i rYT [ ] [ ] r Y i [X3 [XU r ^ i r > i X % 304340 STANDARD OPERATING HRDCEDURE Evaluation of Metals for the Contract Date: Jan. 1992 Laboratory Program Nunber: HW-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 Ccmpliance (Total Review) YES NO N/A Hftif^inq TJTTVPs - (aujuecus and soil samples ) (Examine sanple traffic reports and digestdcn/distillatdcn logs.) Mercury analysis (28 days) exceeded? [ Y 1 Cyanide distillation (14 d a y s ) . . . . . exceeded? [X.] Other Met:als a.nalysis (6 months).... exceeded? f )C 1 NDTE: Prepare a list of all sanples and analytes for which holding times have been exceeded. Specify the number of days from date of collection to the date of preparation (from raw data). Attach to checklist. ACTION: If yes, reject (red-line) values less than Instrument Detection Limit (IDL) and flag as estiratied (J) the values above IDL even thcxigh sample(s) was preserved properly. Is p.H of aquecus sanples for: Metals Analysis >2? [X.] cyanides Analysis <12? f )C 1 Action: If yes, flag the associated metals cind cyanides data as estimated. Fornn I (Final Data) Are all Form I's present and complete? r X 1 ACTION: If no, prepare telephone record log arxi contact laboratory for suixiittal. Are correct u-nits (ug/1 for waters and mg/kg for soils) indicated on Form I's? [ H^l Are soil sanple resultzs for each piarameter corrected for percent solids? f >• 1 Are all "less than IDL" \-alues properly ceded with "U"? [_^] 304341 STANDARD OPERATING FROCEHJRE ' - t e: Evaluation of Mstals Cata for the Contract Laboratory Program Appendix A.l: Cata Assessment - Contract Ccmpliance (Total Revia*) Date: Jan. 1992 Nunber: HW-2 Revision: 11 1.9.3 ..10 Are the correct concentraticn qualifiers used with final data? X- ^CTICN: If no for any of the above, prepare Telephone Record Log, and ccntact laboratory for corrected data. Are E?A sanple i s and corresponding laboratory sample ID S s the same as on the Cover Page, Form I's and in the raw data? Was a brief physical description of sanples given on Form I's? Was t-he dilution of any sanple diluted beyond the requirements of the contract noted on Form I or Form XIV? ACTTON: If no for any of the above, note under Contra ct-Problem/Non-Caq:liance of the"CBta Assessment Narrative". Calibration Is record of at least 2 point calibration present for ICP analysis? Is record of 5 point calibration present for Hg analysis? Is record of 4 point calibration present for: Flame AA? Furnace AA? Cyanides? Is one calibration standard at the CRDL level for all AA (except Hg) and cyanides analyses? [X [ ] [X [ ] [ ] [ X ] m u/h :L _ [_)k] X [X — — ACTION: If no for any of the above, write in the Conturact Problem/Non-CCTrpliance section of the "Cat:a Assessment Narrative". 304342 STANCftRD OPERATING PROCEDURE -1 e: E\'aluation of hfetals Data for the Contract Laboratory Program Appendix A.l: Data Assessment - Ccntract Ccmpliance (Total Review) Date: Jan. 1992 Nuntjer: HW-2 Revisicn: 11 YES .10.2 Is correlation coefficient less than 0.995 for: Mercury Analysis? cyanide Analysis? Atonic Absorption Aralysis? ACTTON: If yes, flag the associated data as estimated. NOTE: The data validator shsill calculate the correlation coefficient using concentraticns of the standards and the corresponding instrument response ( e.g. absorbance, peak area, peak heii^t, etc.). .10.3 In the instance where less than 4 standards are measured in absorbance (or peak area, peak height,etc.) mode, are the remaining standards einalyzed in concentration mode immediatiely after calibration within ±10% of the true values? [ ] ACTTON: If no, flag the associated data as estimated if standards are not within ±10% of true values. Do not flag the data as estirated in linear range indicated by good recovery of standard(s) . m [ X J [ 3 N/A X _ X Form II A (Initial and Conti-nuing Calibration Verification)- Present and complete for every metal and cyanide? Present and ccrplete for AA and ICP when both are used for the same analyte? ACTTON: If no for any of the above, prepare Telephone Record Log and contact laboratory. .11-2 Circle on each Form IIA a l l percent recoveries that are out:side the contract windcws. Are all calibration standards (initial and continuing) — within control limits: Metals- 90-110%R? Hg - 80-120%R? Cyanides- B5-115%R? [X [ ^ [ ] [X] [ ] X — X _, 304343 STANLftRD OPERATING FFOCEDURE Eval\:ation of Hetals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Appendix A.l: Data Assessment - Contract Revision: 11 Corpliance (Total Review) ' ^ m HzT ACncM: Flag as estimated (J) all positive data (not flailed with a "U") analyzed between a ® calibration standard with %R between 75-89% (65-79% for Hg; 70-84% for CN) or 111-125% (121-135% for Hg; 116-130% .for CH) recovery arxi nearest good caLLibrat:icn standard. Qualify results <IDL as estixated (UJ) if the ICV or CCV %R is 75-89% (QJ, 70-84% ; HG, 65-79%). Reject (red-line) as unacceptable data if reoovery of the ICV or CCV is outside the range 75-125% (CN, 70-130%; Hg, 65-135%). CMalify five sanples cn either side of verificat:ian standard out of cantrol limits. Ll,3 Was continuing calibration performed every 10 sanples or every 2 hours? [ J^] Was ICV for cyanides distilled? [ X J ON: If no for any of the above, write in the Contract-Problera/Non-Coipliance section of the "Data Assessment Narrative". ,12 Form II B (CKDL Standards for AA and ICP) - .12-1 Was a CRDL standard (CRA) analyzed after initial ^ calibration for all AA metals (except Ha)? [_XX Was a mid-range calib. verification standard distilled and analyzed for cyanide analysis? f Xl Was a 2XCRDL ( or 2xIDL v,hen IDL>CRDL) analyzed (CRI) for each ICP run? ' 1 yC 1 (Note: CRI for AL,Ea,Ca,Fe,Mg,Na,or K is not required.) ACTION: If no for any of the above, flag a s estimated all data falling within the affected ranges. The affected ranges are: AA Aralysis - **True Value ± C3^DL ICP Ar^alysis - **True Value ± 2(3^DL CN Analysis - **True Value ± 0.5 x True Value. rje value of CRA, (33 or mid-range standard. Substitute IDL for CPDL when IDL > CRDL. P'jte the concentiration of the missing mid-range standard fran the calibration range. 304344 STANDARD ORERAITNG IKXEURE ^tle: Evaluation of Metals Data for the Contract Laboratory Program Appendix A.l: Data Assessment - Ccntract (iT:pliarx:e (Total Review) Date: Jan. 1992 Number: HW-2 Revision: 11 1.12.2 Was CRI analyzed after ICV/ICB and before the final CCV/(OCB, and twice every eight hours of ICP run? ACTTON: If no, write in Contract ProblenvOton-Corpliance Section of the "DQt:a Assesssnent Narrative". 1.12.3 Circle on each Form H B all the percent reooveries that are outside the aooeptanoe windows. Are CRA and CRI standards within cantrol limits: YES [X Metals 80 - 120%R? Is mid-range standard wit±dn control limits: cyanide 80 - 120%R? [. ACTTON; Note: Flag as estirated all sanple results within the affected range if the recovery of the standard is between 50-79%; flag only positive data within the affected range if the reoovery is between 121-150%; reject all data within the affected range if the recovery is less than 50%; reject only positive data wit:hin the affected range if the recovery is greater than 150%. Qualify 50% of the samples on either side of CRI standard outside the control liruts. Flag or reject the finail results only when sanple raw data are within the affect:ed ranges and the CRDL standards are outside the acceptance windows. m N/A ^ — _ A ,13 Form III (Initial and Continuing calibration Blanics) .13.1 Present and ccrplete? For both AA and ICP when both are used for the same einalyte? Was an initial calibration blank analyzed? " Was a continuing calibration blank analyzed after every 10 samples or every 2 hours (which ever is more frequent)? X] [X _ [X _ _ 304345 STANDARD OPERATING PROCEDURE le: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Appendix A.l: Cata Assessment - Ccntract Revision: 11 (inpliance (Total Review) " ^ " ^ N/A ACTTCK: If no, prepare Telephone Record Log, ccntact laboratory and write in the Contract-Problems/ Non-Coipliance section of the "Data Assessment Narrative". .13.2 Circle on each Form I H all calibraticn blank values that are above CRDL (or 2 x IDL when JUL > C3?DL). Are all calibration blanks (when IDKCRDL) less than or equal to the Contract Required Detecticn Limits (<3DLs)? 1 A-1 Are all calibration blanks less than two times Instrument Detection Limit (v*ien IDL>CRDL)? [ ] '_ A ACTION: If no for any of tihe above, flag as estimated (J) positive sanple results when raw sample value is less than or equal to calibration blank value analyzed between calibration blank with value over CPDL (or 2xIDL) and nearest good calibration blaink. Flag five sanples on either side of the calibration blank outside the control limits. .14 FORM III (Preparation Blank) - (Note: The preparation blank for mercury is the same as the calibration blank.) .14.1 Was one prep, blank analyzed for: each Sanple Delivery Group (SDG)? [ "NLl each batch of digested samples? f H,1 each matrix type? f 'p^l both AA and ICP when both are used for the same analyte? [ ] ^ ACTTON: If no for a-ny of the above, flag as estimated (J) all the associated positive data <10 X IDLs for which prep, blank — was not analyzed, NOTE: If only one blcink was analyzed for more than 20 sanples, then first 20 sanples analyzed do not have to be flagged as estiirated (J). 304346 STANEARD OPEiyMTNG FRDOHJRE D.'aluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Hunter: HW-2 Appendix A.l: Data Assesanent - Ccntract Revisicn: 11 ciirpliance (Total Review) ~~~~" " ^ m U/h 1.14.2 Is concentraticn of prep, blank value greater than the CTOX when IDL is less than or equal to CRDL? r /Ci If yes, is the concentraticn of the sanple with the least concentrated analyte less than 10 i--iTTtf>«; the prep.blank? [ ] /N. ACTTCgi; If yes, reject (red-line) all associated data greater than CRDL concentration but less than ten times the prep, blank value. 1.14.3 Is concentration of prep, blank valine (Form III) less than two times IDL, when IDL is greater than CRDL? [ ] X ACTTCDN: If no, reject (red-line) all positive sanple results when sanple raw data are less than 10 times the prep, blank value. Is concentration of prep, blank below . the negative CRDL? f X l ACTTON: If yes, reject (red-line) all associated sanple results less than lOxCRDL. Form IV {TCP Interference Check R^mtpie) 1-15.1 Present and ccrplete? f X 1 (NOTE: Not required for furnace AA, flame AA, mercury, cyanide and (2a, Mg, K and Na.) Was ICS analyzed at beginning and end of run ^ (or at least twice every 8 hours)? [_i_] ACTTON: If no, flag as estimated (J) all the sanples for vAiich AL, Ca, Fe, or Mg is higher than in ICS. -.15.2 Circle all values on each Form IV that aire more than ± 20% of true or est:ablished mean value. _ Are all Interference Check Sanple results inside .^ the control IL'TU.ts (± 20%)? [ ] _£;: If no, is concentration of Al, Ca, Fe, or Mg lower .^ than xhe respective concentration in ICS? [ ] /^. 304347 T = STS^NIARD OHRATING IKXHURE :le: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Progrsm Nunber: HW-2 Appendix A.l: Data Assessment - Contract Revision: l l ccnpiiance (ipitcil Review) .15.1 YES NO N/A ^LUl'liM: II no, flag as estimated (J) those positive results for which I(S reacvery is betireen 121-150%; flag all sasapla results as estimated if ICS recovery falls vithin 50-79%; reject (red-line) those sample results for whicii ICS recovery is less than 50%; if ICS reoovery is above 150%, reject positive results only (not flagged vith a "U"). Form V A (Spiked Sample Raoovery - Pre-Dicegtion/Pre-Distillation)- ( Note: Not required for Ca, Mg, K, and Na (both matrices), Al, and Fe (soil only.) Present and ccrplete for: each SDG? f Y.1 each matrix type? f NLl each cone, range (i.e. low, med., high)? [Xs] For both AA and K^* when both are usad for the same analyte? [ ] Jx. ACTTON: If no for any of the above, flag as estirated (J) all the positive data less than four times the spiking levels specified in SCW fcr which spiked sanple was not analyzed. NOTE: If one spiked sample was analyzed for more than 20 samples, then first 20 sanples analyzed do not have to be flailed as estimated (J). .15,2 Was field blank used for spi3ced sanple? [__L] ACTTON: If yes, flag all positive data less than 4 x spike added as estimated (J) for which field blank was used as spiked sanple. 16.3 Circle on each Form VA all spiJce reooveries that are outside control limits (75% to 125%). ~' Are all recoveries within control limits? [ ] Yv If no, is sanple concentration greater than or equal to four times spike concentration? [ ] X 304348 STANDARD OI^RATING FROCETURE Le: Evaluation of Metals Data for the (Contract Laboratory Program Appe-ndix A.l: Data Assessnent - Ccntract Ccnpiiance (Total Review) Date: Jan. 1992 Nunber: HW-2 Revision: 11 16.4 xss. ACTTCa;: if yes, disregard spiJte recoveries for analytes whose ccnoentraticns are greater than or equal to four times spiJce added. If no, circle those analytes cn fdrm V for which sanple ocnoentration is less than four times the spike concentration. Are results outside the ccntrol limits (75-125%) flagged with "N" cn Form I's and Form VA? t:Si ACTTON: If no, write in the Contract - Problera/Non - Ccnpiiance sectian of "Cata Assessment Narrative". Aqueous Are any spiJce recoveries: (a) less than 30%? _ (b) between 30-74%? _ (c) between 126-150%? _ (d) greater than 150%? _ TACTION: If less than 30%, reject all associated aqueous data; if between 30-74%, flag all eissociated aqueous data as estimated (J) ; if between 126-150%, flag as estirated (J) all associated aqueous data not flat^ged with a "U"; if greater than 150%, reject (red-line) all associated aqueous data not fla^^ged with a "U". m [X] [X3 [X] tX] N/A ,16.5 Soil/Sedimfint Are any spike reooveries: (a) less than 10%? (b) between 10-74%? (c) between 126-200%? (d) greater t-han 200%? X [X] [ 3 cX 304349 STANDARD OPERATING rKXHURE itle: D/aluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Appendix A.l: Data Assesanent - Ocntxact Revision: l l Cixpliance (Total Review) ~ ~ ' ' m ^ HzF~ ACTTCgt; If less than 10%, reject all associatPd data; if between 10-74%, flag all associated data as estimated; if between 126-20{^, flag as estirated all associated data vas not flagged vith a "IT; if greater than 200%, reject all associated data not flagged vith a "U". 1.17 Form VI (Lab Duplicatea) " 1.17.1 Present and ccrplete for: each SDG? f f^] each matrix type? [ >-1 each concentration range (i.e. low, med., hi(^)? [ J h J both AA and ICP when both are used for the same analyte? [ ] T- ACTTON: If no for any the above, flag eis estimated (J) all the data >CRDL* for which duplicate sample was not analyzed. Note: 1. If one duplicate sanple was analyzed for more than 20 sanples, then first 20 sanples do not have to be flatbed as estirated. 2. If percent solids for soil sanple and its duplicate differ by more than 1%, prepare a Form VI for each duplicate pair, report concentrations in ug/L on wet weight basis and calculate RPD or Difference for each analyte. :.17.2 Was field blank used for duplicate analysis? f ^ 1 ACTTON: If yes, flag all data >CRDL* as estirated (J) for vhich field blank was used as duplicate. 1.17-3 Are all values within control limits (RPD 20% or difference < +CRDL) ? [ ] _ X If no, are all results cutside the control limits flagged with an * on Form I's and VI? f X l ACTTON: If no, uTite in the Contract - Prc±)lems/Non- Corpliance section of "Data Assessment Narrative". Substitute IDL for CRDL uhen IDL > CRDL. 304350 STANDARD OPERATING PROCEDURE .e: Ev'aluation of hSstals Data for the Cisntract Laboratory Program Appendix A.l: Data Assessment - Ccntract cixpliance (Total Review) Date: Jan. 1992 Nunber: HW-2 Revisicn: 11 KTTE; 1. RPD is xxrt; calculable for an analyte of the sanple - duplicate pair when both values are less than IDL. 2. If the result of lab duplicate analyzed by GFAA is rejectable due to coefficient of correlation of MSA, analytical spike reoovery, or duplicate injections criteria, do not apply precision criteria to Tnp^-.aiR aialyzed by GFAA. Agueous Circle on each Form VI all values that are: RPD > 50%, or Difference > CPDLA' Is any RPD greater than 50% where sanple and duplicate are both greater than or equal to 5 times *C3^L? Is any difference** between sanple and duplicate greater than «CRDL where sanple and/or duplicate is less than 5 times *CRDL? ACTTON: If yes, flag the associated data as estirated. Soil/Sedimp.nt Circle on each Form VI all values that are: RPD > 100%, or Difference > 2 x CRDL* Is any RPD (uhere sanple and duplicate are both greater than or equal to 5 times *CRDL) : > 100%? Is any **difference between sanple eird duplicate (\vhere sample and/or duplicate is less than 5x*CRDL) : > 2x*CRDL? lES m U/h [Xl [X] _ tX] _ Xl — S'jbstitute IDL for CRDL when IDL > CRDL. Use absolute values of samole and duplicate to calculate the difference. 304351 STANDARD OPERATING PROCEDURE le: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 Ccnpiiance (Total Review) YES NO N/A ACTTON; If yes, flag the associated data as estimated. .18 Field Duplicates .18.1 Were field duplicates analyzed? [ ] ACTTON: If yes, prepare a Form VI for each aqueous field duplicate pair. Prepare a Form VI for each soil duplicate pair, if percent solids for sample and its duplicate differ by more than 1%; report concentraticns of soils in ug/1 cn wet wei^t basis and calculate RPDs or Difference for each analyte. NOTE: 1. Do not calculate RPD"when both values are less t-han IDL. 2. Flag all associated data only for field duplicate pair. ,18.2 Aouecrus Circle all values on self prepared Form VI for field duplicates t-hat are: RPD > 50%, or Difference > CRDL* Is any RPD greater t-han 50% where sanple and duplicate are both greater than or equal to 5 time? *CRDL? [ ] _ _ Is any **differE.nce between sanple and duplicate greater than *CRDL where sanple and/or duplicate is less than 5 times *CRDL? [ ] ACTTON: If yes, flag the associated data as estimated. * Substirute IDL for CRDL v,hen IDL > CRDL. •** Use absolute values of samole and duplicate to calculate the differe.nce. 304352 STAJroARD OPERATING PROCEDURE :le: Evaluation of Metals Data for the contract Laboratory Program Appendix A.l: Data Assessment - Ccntract (irpliance (Total Review) Date: Jan. 1992 Nunber: HW-2 Revisicn: 11 IE£ 1.18-3 Soil/SertiTTV-nt Circle all values cn self prepared Form VI for field duplicates that are: RPD >100%, or Difference > 2 x CRDL* Is any RPD (where sample and duplicate are both greater than 5 times "CRDL) : >100%? Is any **difference between sanple and duplicate (vhere sanple and/or duplicate i s less than 5x *(3?DL ): ACTTON: >2X *CRDL? If yes, flag the associated data as estimated. m iMh [ ] 1-19 Form VTI (T^horatory Control Sample) (Note: LCS - not required for aqueous Hg and cyanide analyses.) 1.19.1 Was one LCS prepared and analyzed for: each SDG? r y i each batch sanples digested/distilled? f Y 1 both AA and ICP when both are used for the same analyte? [ ] ACTTON: If no for any of the above, prepare Telephone Record Log and contact laboratory for submittal of results of LCS. Flag as estimated (J) all the data for uhich LCS was riot analyzed. NOTE: If only one LCS was analyzed for more than 20 - sanples, then first 20 sanples close to LCS do not have to be flagged as estimated- _ X * Substitute IDL for CRDL when IDL > CRDL. •* Use absolute values of sanple and duplicate to calculate the difference. 304353 STANDARD OPERATING roDCEHIRE of 3 H Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Nunber: HW-2 Appendix A.l: Data Assessnent - Ccntract Revision: 11 Ccmpliance (Total Review) ^ m SzT" L9.2 Acrufiioua TC3 Circle on each Form VH the LCS percent recoveries outside ccntrol limits (80 - 120%) exoept for ziquaous Ag zvnd Sb. Is ciny LCS reccTvery: less than 50%? [X.3 between 50% arti 79%? [_^] between 121% and 150%? [ X ] greater than 150%? [ X ] ACTTON: Less than 50%, reject (red-line) a l l data; between 50% and 79%, flag a l l associated data as estirated (J); between 121% and 150%, flag a l l positive (not flagged with a "U") results as estirated; greater t-han 150%, reject a l l positive results. .19.3 Solid LCS NOTE: 1. If "Fcund" value of LCS is rejectable due to duplicate injecticns or analytical spike recovery criteria, regardless of LCS recovery, flag the associated data as estirated (J). 2. If IDL of an analyte is equal to or greater t.han true value of LCS, disregard the "Action" below even though LCS is out of control .limits. Is LCS "Found" value hic^er than the control limits on Form VII? f X l ACTTON: If yes, q^ualify cdl associated positive data as estirated. Is LCS "Found" value lower than the CiDntrol limits on Form VII? X [ ] ACTION: If yes, q-ualify all associated data as estirated. 304354 STANDARD OPERATING HSXHURE lie: E'.'aluation of Metals Data for the (Contract Laboratory Program Appendix A.l: Data Assessnent - Ccntract cimplianae (Total Review) Date: Jan. 1992 Nunber: HW-2 Revisicn: 11 1.20 Form rs (ICP Berial Dilution) - NOTE: Serial dilution analysis is required cnly for initial ccnoentraticns equal to or greater than 10 x IDL. 1.20.1 Was Serial Diluticn analysis performed for: each SDG? each matrix type? each concentration range (i.e. low, med.)? iE£ [X cX [X ACTTON: If no for cmy of t-he above, flag as estirated all the positive data >. lOxIDLs or >. CRDL when lOxIDL <. CRDL for whicdi Serial Diluticn Analysis was not performed. m U/h 1-20-2 Wcis field blank(s) used for Serial Dilution Analysis? ACTION: If yes, flag all associated data > 10 x IDL as estimated (J). If lOxIDL <. CRDL, flag a l l data >. CRDL. 1.23.3 Are results outside control limit flagged with an "E" on Form I's and Form IX when initial concentration on Form IX is equal to 50 times IDL or greater. ACTT(3N: If no, write in the Contract-Problem/Non- Ccrplianoe section of the "Data Assessment Narrative". 1.20.4 Circle on each Form IX all percent difference that are outside the control limits for initial conce-ntrations equal to or greater than 10 x IDLs only. _ [X _ Are any % difference values: > 10%? > 100%? [JL: % [ ] cX 304355 STANI»RD OPERATING PRDCECURE tie: Evaluation of Metals Data for the Contract Laboratory Program Appendix A.l: Data Assessment - Ccntract (isiplianc^e (Total Review) Date: Jan. 1992 Nunber: HW-2 Revision: 11 YES ACTT(a;; Flag as estimated (J) eai the associated sample data >. lOxIDLs (or >.-C3?DL when lOxIDL <. CIJDL) for which percent difference is greater than 10% but less than 100%. Reject (red-line) all the associated sanple results equal to or greater than lOxIDLs (or >. CRDL when lOxIDL <. CRDL) for which FD is greater than or equal to 100%. Note; Flag or reject on Form I's only the sanple results whose associated raw-data are >. lOxIDL (or >. CRDL when 10xIDL< CRDL) m ILLh w r..2 Fum.'ice Atmic Absorbtion (AA) OC Analysis Are duplicate injections present in fumaoe raw data (except during full Method of Standard Addition) for each sanple analyzed by GFAA? ACTTON: If no, reject the data on Form I's for which duplicate injections were not performed. Do the duplicate injection readings agree within 20% Relative Standard Deviation (RSD) or Coefficient of Variation (CV) fcr concentration greater than CRDL? Was a dilution analyzed for sanple with aneilytical spike reoovery less than 40%? ACTION: If no for any of the above, flag all the associated data as estimated. i ] 1 were [ ] [ ] Is *analytical spike recovery outside the control limits (85-115%) for any sanple? ACTION: If yes, flag the affected sample results if the recovery is between 10-84%; if the recovery is between 115-200%, flag the associated positive sample results as estirated; reject the associated sarple results if the recovery is less than 10%; reject positive sanple results if the reoovery is greater than 200%. [ ] .-2l\tical spike is not required on the pre-digestion spiked sa-^role. 304356 STANDARD OfERAUNG FRDCEDURE .e: Evaluaticn of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 C o m p l i a n c e ( T o t a l R e v i e w ) m m Hzr >PTE: Reject or flag the data cnly vhen the affected sanple (s) vas not subsequently aralyzed by Method of Standard Addition. .22 Form VTTI (Method of standard Addition Raaoilts) .22-1 Present? [ ] If no, is any Form I result coded with "S" or a "+"? [ ] ACTTON: If yes, write request on Telephone Record Log and csntact laboratory for sutndttal of Form VIII. .22.^2 Is coefficient of correlation for MSA less than 0.990 for any sanple? [ ] ACTTON: If yes, reject (red-line) the affected data. Was *MSA required for any sanple but not performed? [ ] Is coefficient of correlation for MSA less than 0.995? [ ] Are MSA calculations outside the linear range of the calibration curve generated at the beginning of the analytical run? [ ] ACTTON: If yes for any of the above, flag all the associated data as estimated (J). Was proper quantitation procedure followed cxsrrectly as outlined in the SCW on page E-23? [ ] ACTTON; If no, note exception under Contract Problem/ Non-Ccrpliance section of the "Cata Assessment Narrative", and prepare a separate list. » l-'Sh is not required on LCS and prep, blank. 304357 STANEftRD OPnyOTNG PROCEDURE tie: Evaluation of Metals Data for the Date: Jan. 1992 contract Laboratory Program Number: HW-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 Coiplianoe (Total Review) " ^ M N/A 1.23 Dissolved/Total ar- T'TY^Trranic/Total Analytas - 1.23.1 Were any analyses performed for dissolved as well as total analytes cn the same sanple (s). [ ] Were any analyses performed for inorganic as well as total (organic + inorrganic) analytes cn the same sample (s)? [ ] NCTE: 1. If yes, prepare a list coiparing differenoes between all dissolved (or inorganic) and total analytes. Caipute the differenoes as a percent of the total analyte only when dissolved cxanoentration is greater than C3©L as well as total cOT)centration. 2. Apply the following questions only if in- organic (or dissolved ) results are (i) above CRDL, aind (ii) greater than total constituents. 3. At least one preparation blank, ICS, and LCS should be analyzed in each analytical run. 1.23.2 Is the concentration of any dissolved (or inorganic) analyte greater than its total concentration by more than 10%? ' [ ] 1.23.3 Is the ccncentraticn of any dissolved (or inorganic) analyte greater th-an its total concentration by more t-han 50%? [ ] ACTTON: If more than 10%, flag both dissolved (or inorganic) and total values a^ estimated (J); if more than 50%, reject (red-line) the data for both values. 1.24 Form I (Field Blank) - (Note; Designate •'Field Blank" &3 such on Form I.) 1-24-1 Circle all field blank values on Form I that are ~" greater than CRDL, (or 2 x IDL when IDL > CRDL). Is field blank concentration less than CRDL (or 2 X IDL vhen IDL > CRDL) for all parameters ^ of associated aqueous and soil sanples? ( ] X. 304358 STANTARD 0IERATIN3 IKXEDURE -.le: Evaluation of Jfetals Data for the Date: Jan. 1992 Contract laboratory Program Number: HW-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 Ccnpiiance (Total Review) ^ . m M If no, was field blank value adreaiy rejected due to other QC criteria? [ ] 2 ) ^ ACTTOH: If no, reject (except field blank results) adl as.sociated positive sanple data less than or equal to five t-\iT*^ the field blank value. Reject cn Form I's the soil sanple results that when ccrrverted to lag/L cn wet basis are less than or equal to five times the field blank value in v>g/L. 1.25 Form X, XI. XII fVerification of InstnrvTital ParTtnvTbers). 1.25.1 Is verification report present for: Instrument Detection Limits (quarterly)? f V^l ICP Interelement Correction Factors (annually)? [_£i] ICP Linear Ranges (quarterly)? [_J_i] ACTTON: If no, contact TPO of the lab. 1.25.2 Form X (Instrument Detection T.imits) - (Note: IDL is not required for Cyanide.) 1-25.2.1 Are IDIs present for: all the analytes? [ X ^ all the instruments used? [_L_] For both AA and ICP when both are used for the same \r analyte? [X] ACTTON: If no for any of the above, prepare Telephone Record Log and c:ontact laboratory. 1.25-2.2 Is IDL greater than CRDL for any analyte? f N 1 If yes, is the concentration on Form I of the sanple analyzed on the instrument vhose IDL exceeds CRDL, greater t-han 5 x IDL. [ ] ^ ) ^ 304359 :le: STAJmARD OrzRATING HOTTTTRE Evaluation of Ifetals Data for the Contract Laboratory Program Appendix A.l: . Data Assessaent - Ocrtracc Ccnpiiance (Total Review) Date: Jan. 1992 Number: HW-2 Revisicn: 11 Action : If no, flag as estimated all values less than five times IDL of the instrument whose IDL exceeds CRDL. YES m Ulh 1.25.3 Form XI (Ti^Jifinr Ranges) 1.25.3.1 Was any sanple result hici^er than h i ^ linear range of ICP. Was any sanple result higher than the highest calibration standard for non-ICP parameters? If yes for any of the above, was the sanple diluted to gbtain the result on Form I? _ 1^1 _ t_) _ li^ ACTTON: If no, flag the result reported on Form I as estimated (J). 1.25 Percent Solids of &(v^irv>nt3 .26.1 Are perce-nt solids in sadiment(s): < 50%? < 10%? ACTION: If yes, qualify as estirated all the results of a sanple that has per cent solids between 10%-50% (i.e. moisture content between 50%-90%). Reject adl the results of a sanple that has per cent solids less than 10% (i.e. moisture content greater than 90%). NCTE: Pjsject or flag (J) only the sanple results that were not previously rejected or flaged due to other QC criteria. [X _ tx] — 304360 STANDARD OPERATING PROCEDURE :le: E'.'aluatian of Metals Data for the Contract Laboratory Program Appendix A.2: Data Assessment Narrative Date: Jan. 1992 Nunber: HW-2 Revision: 11 3e# retractor 9n/3o 8it« J j l o h J (ZnemicJ Lab Pace. Raviewer Dor\ An/it.' Matrix: Soil V Water_J(^ other .1 Validation Flaos- The following flags have been applied in red by the data validator and rust be considered by the data user. J- This flag indicates the result qualified as estimated Red- Line- A red-line drawn through a sample result indicates unusable vadue. The red-lined data are known to contain significant errors based on documented information and nust not be used by the data user. Fully Usable Data- The results that do not carry "J" or "red-line" are fully usable. Contractual Qualifiers- The legend of contractual qualifiers applied by the lab on Form I's is found on page B-20 of SOW ILMOl.O. 7r,e data assessment is given below and on the attached sheets. for Poci, ^ J y f , i j SPrr: ^'ll30 304361 STANI^RD OIERATING HOCZEURE :le: Evaluation of Metals Data for the Date: Jan. 1992 (Contract Laboratory Program Number: HW-2 Appendix A.2: Data Assesanent Narrative Pevisicn: 11 ;.2 (continuation) 3 0 4 3 6 2 STANEftRD OPERATING PROCEDURE itle: Evaluaticn of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Nunber: HW-2 Appendix A.2: Data Assessment Narrative Revisicn: 11 .2.2 (continuation) 304363 STANmRD OPERATING TOXEDURE lie: Evaluaticm of >fetals Data for the Date: Jan. 1992 Contract Laboratory Program Nunber: HW-2 Appendix A.2: Data Assessment Narrative Pevisicn: 11 2-3 Contract-Problenvnon-Caipliarx» H>3/ESAT Rviewer: • Cate: Signature ctor Reviewer: Cy/?^/a Ixi / / /VK^ Date: / / - , ? ' 7 7 :tractcr Signature Verified by: Cate:_ 304364 STANDARD OPERATING HSXEDURZ 'itle: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Appendix A. 3: Contract Ncn-Omplianoe Revision: 11 (SM) Report) CCNIRACT NCN-CCMPLIANCE (SMO REPCET) Regional Review of Uncontrolled Hazardous Waste Site Contract Laboratory Data Package CASE NO. ; hardcepied (laboratory name) \ :rga.nic data package received at Ragicn II hais been reviewed and the quality assura-nce a.nd •forrance data suncarized. The data reviewed included: : Sa.'XJle No.: " •.c. & Matrix: 'gfs No. ( 1 requires that specific analytical work be done and sociated reports be provided ty the contracrtor t o the Regions, EMSL-LV, and SMO. The A1 criteria used to determine the performance were based on an examination of: - Data Ccnpleteness - Duplicate Analysis Results -' Matrix SpiJce Results - Blank AnaLlysis Results - Calibration Standards Results - MSA Results L-s of non-compliance with the above contract aure described belcw. T"isnts: Reviewer's I n i t i a l Date 3 0 4 3 6 5 SITiNDARD CPnyOING FRDCLURZ Evaluaticn of Metals Data for the Contract Laboratary Program Appendix A.4: Mailing List for Data Reviefwers Date: Jan. 1992 Number: HW-2. Pevisicn: 11 trs/».n.nr. ITT- yy » a gTfsgs VSjyx J^icr. 3 (ISO) : iO Warrvi**' ruiKt Uxinr-=r. » . 02173 ( t n ) •61>4312 C7. M . K»., W. W. \T CAA, taaourot AJ^yr:*. york, tTTPX %tqiar. ZU (Dw) I3( ter:^t.< load >."nflpc::t. >c; j;<ci (3:i) 2t*-9:t5 tc. >c. ?;>. \"x. vv, tc C*.-:;t*C. K:r-A.-., J T t . >9«:>;. MJSW, S-.i3*r: 7«rv.. >;*/ FA VTi?x R«;-.c-. Y ( c r ; 534 SOC^.-. C:».-k S^rwtz 7t-r_r. r i c c r . OC PI*. c-..;ri::» 3 : j - 3 i 2 - 5 ; j - 21. r ; . IC. K., CK. v t XIX. t s c / i r c — / t i t ? x s ^ : = r . \-:: J i r.r-jr_3r. Jo4i Ki.-.bu City. X5 t t i l S Oein Mirr/ ( J : 3 ; ; : t - 3 E j : 3C. kS. KB. >c w;:icr.. K^.-Ai4 C;r>- Sc:e.-.t:;ic v£r?A Raqicr. rx ItSO) OJv K4.-*9e.Te.T:t S*cticr. 2 i i rrc-o-r. r i r * e t SA.-. m L - r i i = c . CA SUOS t*:5) ?-!«-WJ* >J, CA. K ; . K.'. A-ttricA.-. U-isA. OLA-. T r j r . 7 t r r : t i r i f c * ol P»:ilJc Ji:».tis. v.&>.« 3»:k.-xJ Ai:. CAl Vits-.cr.. S-C-jbaci. H-CA. tSCA taqicn ZI (tSO) Xaisen, H«w J a r M y Ott37 (203) 321>M7« KJ. W , PR, V3 OvT&s-y, aiflR«9-., IS 7>wt, K4.ia, Z3t, C«dKn. IMS, CAlaon, I W tStPA fm;itr> TV (IS5J A-«jyciex: gi».^T,i;i a.fc'ii.'. C&Uap* r u t i c r . Ik3*d AV«,-». CA 3Di33 Tttr. b t m e r t . J r . (4M) b4«-3112 Al, TX. CA. Ki, K . X . SO. TV ftrpxne:., ITS, £SI. nSLT, V5ITA J ^ i c r . VI (ISO) harrutrry Ptrk P U t t . a i d ; . C tiSt Hrrrvoai Criv« Kaj«--an. TX 7707< (713) 113-3*25 **, U . >M, TX. OK JWk3I<, WCtA,X. S H t S , TZS. Cl KeMATf,. I r c . . S7L I r e . , S - ^ AlijKl. Kr/ TX, nSA iriTA »B=:cr. %*::: Uicr»-.zr>- aox 2i36i Ofc-vtr r«dervi Ot-otr UXJSPOS:. CO i:225 (3:3) 23t-7371 CO. XO, $r. tf. wj-. K : Aoa;, cscu, ve^c. w-t o>c-.. c».-«i 10. LS:!7A Kjqion X TA"nr»cory P.O. aox U i Kfcf>es-jEr. Wk tl353 (2K) 442-0370 AX, ID. Cf., KV L«jchs T*stm; IMx, Ct-rrury Ttstirt; Uix (Tor VOA Crjy), Weytrr>e-i»*r Cc. CDlvrtii Tts-.irxj, SUvix V»Hty ::. t!_-:« oe.-ps^y - (a£-232) usrrA <c; -r- s-_r«--. s.v. Vts.M.-xr.=r.. r r 2^itC rrs 3t;-i-<£ V.V.- A.-T: C3-i£r.,- 12- li.-xn. Xi.-.icr I'SI^A &51-LV J u t . Ki.-rrr. Avenje EX 53<-8 L4J Vacrsi. hV «S::5 304366 STANDARD OPERAIING PRDCEEtIRE Title: Evaluation of Metals Cata for the Oontract Laboratory Program Appendix A. 6: CLP Data Assessment Sunstary Form (Inorganics) Date: Oct. 1989 Nuniser: HW-2 Revision: 9 Type of Review: C1.P DATA ASSESSMEKT SUMHARY rORM (IWOtCAMICS) CLP D«c.; Moo .1 m n £DCr \, qn/30 site: -Islat\ci <Xh(iiY\lOes,i Lab Mas*: Revlewer'i I n l c l i l a : bcfi Poici. A r , ^ l ^ h c J Muaber o£ Saaplaa: 3 0 Analytea Releeted Due to Exceeding Review Criteria:* TCP iFlaae KX Furnace AA Hercury \ratt\CKJ HoldlDg Tlaea o Calibration o Prap Blank o Field Blank ?> 1 o 1 o 1 o \ o 1 o \ o 1 o lother 1 1 1 0 I n t e r - fercDcei 0 1 v: 1 X Spike Recoverr o o o 1 Dupllcataa Lablricld o Q \o X K X Detection L l « l t a o o 1 ^ u:s o Serial Dllutioo Q o \o X X HSA X 1^ > Total Analytaa (cplo 3 0 3 0 Rclcctioe 26 O O AnaJYtaa f l m « d ai Eati»ated (J) Due to Cxeeedim Criteria for;* ICP Flase AA o 1 0 Furnace AA Mercury ZottlCfJ 1 o 1 o Other 1 o o o o o 0 eo I o 0 X y e3 ID o o 0 D )^ y x O o o 7 o o ^n3 X X > Y- X - _ 690 3 D 30 //3 o o Nate: Aateriak (*) lodlcatea additional exceedancee ol review criteria. 304367 STANDftRD OFERATING PROCEDURE Title: Evaluation of Metals Data for the Oantract Laboratory Program Appendix A.7: CLP Data Assessment Checklist Inorganic Analysis Date: Oct. 1989 Number: HW-2 Revision: 9 INCRCANIC RESICNAL DATA ASSESSMENT Region "2. CASE ND. lABCRAICKY SDG# SOW# Pace. ^ni:^o nnalyi/ccl iLrrioZ'O SITE NO. OF SAMPIES/ MKIKrX ^slcinJ C-ne/nicd.} as Aoii-. 'cutter ie DPO: ACnCN FfE 1. 2. 3. 4 . 5. 6. 7 . 8. 9. 10. 1 1 . 12. HOLDING TIMES CALEERATICNS BLANKS ICS ICS DUPLICATE ANALirSIS MKIRIX SPIKE MSA SERIAL D n i m c N SAMPLE VEKEFTCAnCN COHER QC OVERAU. ASSTTH'^J-gM' X DATA ASSESSMEOT SUMMARY ICP AA CL KLVliMER (IF NCT ESD) REVIEHER'S NAME l)ODcU fi/ln^ ccMPizncN Eggs A/nj 3. /f?*? no n J2- Q H. XL. XL XL X L XL O XL m Data has no problems/or gualified due to Tn-irrrf problems. « Data gualified due to major problems. = Data unacceptable. = Problems, but do not affect data. CYANTTK _ 0 (7 J2_ ^ TT ACnCJJ ITEKS: AREAS OF oa^CERN: hroiABLE PERFC5«ANCE: 304368 QA/QC Review of Semivolatiles Data for Pace Analytical SDG: 97130 October 31,1997 Holding Times: All samples were extracted and analyzed within Region II holding times. GC/MS Tuning and Mass Calibration: All DFTPP tuning criteria were within control limits. Initial Calibration: All compounds with contract criteria for RRFs and %RSDs met those requirements. All target compounds had average RRFs above the allowable minimum (0.050) and %RSDs below the allowable maximum (30%) as required. Continuing Calibration: All compounds with contract criteria for RRFSOs met those requirements. Pyridine (25.1%) had a %D above the contractual maximum (25%o) on 10-03-97 (1003J01). Pyridine (28.9%)) had a %D above the contractual maximum (25%) on 10-07-97 (1007J01). No action is taken on two or fewer compounds per calibration outside contract limits as long as %.Ds are below 40% and RRFSOs are above 0.010. All target compounds had RRF50s above the allowable minimum (0.050) as required. 2,2'- Oxybis(l-chloropropane) (52.8%)) had a %D above the allowable maximum (25%) on 09-26- 97 (0926J02). 2,2'-Oxybis(l-chloropropane) (47.4%) had a %D above the allowable maximum (25%)) on 10-01-97 (1001J02). Pyridine (25.1%) had a %D above the allowable maximum (25%) on 10-03-97 (1003J01). Hexachlorocyclopentadiene (28.6%) had a %D above the allowable maximum (25%) on 10-06-97 (1006J01). Pyridine (28.9%) had a %D above the allowable maximum (25%) on 10-07-97 (1007J01). Results for these compounds should be considered estimates (J) in associated samples. Blanks: Method blank SBLKWI contained traces of bis(2-ethylhexyl)phthalate(20 ug/L) and di-n- octylphthalate (4 ug/L). Method blank SBLKW5 contained a trace of bis(2- ethylhexyl)phthalate (1 ug/L). Method blank SBLKL4 contained a trace of bis(2- ethylhexyl)phthalate (35 ug/kg). Field blank FB0919 contained a trace of bis(2- ethylhexyl)phthalate (4 ug/L). Field blank FB0922 contained traces of dimethyl phthalate (3 ug/L) and bis(2-ethylhexyl)phthalate (3 ug/L). Field blank FB0923 contained a trace of bis(2-ethylhexyl)phthalate (1 ug/L). Field blank FB0924 contained a trace of diethylphthalate(l ug/L). Field blank FB0930 contained traces of diethylphthalate (2 ug/L) and bis(2-ethylhexyl)phthalate (1 ug/L). Results for dimethyl phthalate, diethylphthalate, bis(2-ethylhexyl)phthalate,and di-n-octylphthalateless than ten times the highest associated 3 0 4 3 6 9 blank level should be reported as not detected (U) in samples. The following are contaminated blanks and their associated samples: Method blank SBLKWI: FB0918, FB0919 Method blank SBLKW5: FB0930 Method blank SBLKL4: 200204, 200406, 300810, 30081 ORE Field blank FB0919: BOOOOl, B00002, B00003, B00004 Field blank FB0922: 5A2022, 5A2224, 6A2022, 6A2224 Field blank FB0923: 101618,102224 Field blank FB0924: 201820, 202022, 301820, 301012 Field blank FB0930: 300608, 100608, 101214,011214 Internal Standard Area Summary: All internal standard retention times were within control limits. Samples 300608 and 300608RE had 3 of 6 internal standard areas (IS4, IS5, IS6) outside control limits. Samples 300810 and 30081 ORE had 4 of 6 internal standard areas (IS3, IS4, IS5, IS6) outside control limits. Results for samples 300608, 300810, 300608RE, and 30081 ORE quantitated off internal standards with areas outside control limits should be considered estimates (J) or unusable (R) depending on the severity of the problem. Surrogate Recovery: Samples 300608,300608RE, 300810, and 30081 ORE had 1 of 4 base/neutral surrogate recoveries above control limits. Sample 300810 had 1 of 4 acid extractable surrogate recoveries above control limits. No action is taken on one surrogate per fraction outside control limits as long as no recovery is less than \Q%. Matrix Spike/Matrix Spike Duplicate: MS/MSD samples 300608 and 702022 had all relative percent differences and percent recoveries within control limits. Compound ID: Checked compounds were within GC/MS quantitation and qualitation limits. All positive hit compounds had the primary and secondary ions in their mass spectra as outlined in the SOW. G:\STAFF\DANNE\Island\97130.SVL.wpd 304370 Cone, of Internal Standard: 40 ID: J Date: 10/2/97 ,RRF Cone, of Compound 1,4-Dichlorobenzene-d4 Phenol RRF Naphthalene-d8 Naphthalene RRF Acenaphthene-d 10 Acenaphthylene RRF Phenanthrene-dlO Phenanthrene RRF Chrysene-d12 Pyrene RRF Perylene-d12 Benzo(g,h,i)perylene RRF 1002J13 Sample 1 20 187641 129872 1.384 690684 304252 0.881 342609 302723 1.767 629821 298771 0.949 522698 333964 1.278 578926 232130 0.802 1002J09 Sample 2 50 171654 298576 1.392 630679 683694 0.867 315328 695803 1.765 600611 696903 0.928 488331 770298 1.262 565479 604949 0.856 1002J10 Samples 80 161679 457470 1.415 613144 1099163 0.896 316455 1172934 1.853 598024 1127785 0.943 500105 1277698 1.277 599934 1000773 0.834 1002J11 Sample 4 120 174935 713618 1.360 641248 1680330 0.873 320344 1703599 1.773 551560 1593636 0.963 456936 1767302 1.289 556907 1398912 0.837 1002J12 Samples 160 176840 887320 1.254 626980 2069686 0.825 318578 2178756 1.710 556997 1959586 0.880 441688 2264727 1.282 536144 1723822 0.804 Average 1.361 0.869 1.774 0.933 1.278 0.827 % RSD 4.6% 3.1% 2.9% 3.4% 0.8% 2.8% Continuing Calibrations ,^ Cone, of Compound 1,4-Dichlorobenzene-d4 Phenol RRF Naphthalene-d8 Naphthalene RRF Acenaphthene-dIO Acenaphthylene RRF Phenanthrene-dlO Phenanthrene RRF Chrysene-d12 Pyrene RRF Perylene-d12 Benzo(g,h,i)perylene RRF 1007J01 Sample 50 140691 253103 1.439 511329 571759 0.895 254900 570434 1.790 473744 568026 0.959 394913 601020 1.218 486430 526535 0.866 %0 5.8% 3.0% 0.9% 2.9% 4.7% 4.8% 1008J02 Sample 50 154924 282547 1.459 576289 611754 0.849 273488 597751 1.749 514459 604803 0.940 400625 643567 1.285 480061 538747 0.898 %D 7.2% 2.2% 1.4% 0.9% 0.6% 8.6% 1013J04 Sample 50 129458 257043 1.588 502190 552863 0.881 229820 511521 1.781 388716 491858 1.012 353288 515082 1.166 413591 458894 0.888 %D 16.7% 1.4% 0.4% 8.6% 8.7% 7.4% 1003J01 Sample 50 158489 I 284781 1.437 596715 645311 0.865 290904 652830 1.795 528817 634084 0.959 454569 696288 1.225 516788 514995 0.797 VoD 5.6% 0.4% 1.2% 2.9% 4.1% 3.6% 1006J01 Sample 50 241003 450856 1.497 829839 883316 0.852 374913 799675 1.706 659393 762991 0.926 501945 803552 1.281 573455 631668 0.881 %D 10.0% 2.0% 3.8% 0.7% 0.2% 6.6% 304371 Cone, of Internal Standard: 40 ID: J Date: 9/29/97 RRF Cone, of Compound 1,4-Dichlorobenzene-d4 Phenol RRF Naphthalene-d8 Naphthalene RRF Aeenaphthene-d10 Acenaphthylene RRF Phenanthrene-d10 Phenanthrene RRF Chrysene-dl2 Pyrene RRF Perylene-d12 Benzo(g,h,i)perylene RRF 0902J06 Sample 1 20 175685 145676 1.658 617657 268558 0.870 282899 221842 1.568 494360 224364 0.908 385907 221290 1.147 450381 154488 0.686 0902J02 Sample 2 50 212382 461368 1.738 823919 910476 0.884 341909 735686 1.721 537590 673570 1.002 401316 629044 1.254 430964 424797 0.789 0902J03 Sample 3 80 180946 634471 1.753 666651 1254619 0.941 294293 1067414 1.814 467214 937752 1.004 357082 998673 1.398 373440 616842 0.826 0902J04 Sample 4 120 183237 891635 1.622 725764 1828629 0.840 311169 1575233 1.687 497941 1387750 0.929 377501 1296991 1.145 393577 939257 0.795 0902J05 Sample 5 160 174313 1154864 1.656 639928 2243292 0.876 287049 1934620 1.685 491497 1960050 0.997 398786 1926677 1.208 442164 1280596 0.724 Average 1.686 0.882 1.695 0.968 1.230 0.764 % RSD 3.4% 4.2% 5.2% 4.7% 8.5% 7.5% Continuing Calitirations 0926J02 Sample %D 1001J02 Sample %D Sample %D Sample %D Sample %D Cone, of Compound 50 50 1,4-Dichloroben2ene-d4 181285 186003 Phenol 325964 14.7% 332361 15.2% #DIV/0! #DlV/0! #DIV/0! RRF 1.438 1.429 #DIV/0! #DIV/0! #DIV/0! Naphthalene-d8 674957 691867 Naphthalene 736652 1.0% 755962 0.9% #DIV/0! #DIV/0! #DIV/0! RRF 0.873 0.874 #DIV/0! #DIV/0! #DIV/OI Aeenaphthene-d10 323045 330634 Acenaphthylene 699675 2.2% 705253 0.7% #DIV/0! #DIV/0! #DIV/0! RRF 1.733 1.706 #DIV/0! #DIV/0! #DIV/0! Phenanthrene-dlO 569477 580694 Phenanthrene 698125 1.3% 727858 3.6% #DIV/0! #DIV/0! #DIV/0! RRF 0.981 1.003 #DIV/0! #DIV/0! #DIV/0! Chrysene-dl2 514786 520568 Pyrene 775867 2.0% 776937 3.0% #DIV/0! #DIV/0! #DIV/0! RRF 1.206 1.194 #DIV/0! #DIV/0! #DlV/0! Perylene-d12 575723 606490 Benzo(g,h,l)perylene 524406 4.6% 625527 8.0% #DIV/OI #DlV/0! #DIV/0! RRF 0.729 0.825 #DIV/0! #DIV/0! #DIV/0! 304372 QA/QC Review of Volatiles Data for Pace Analytical SDG: 97130 October 31, 1997 Holding Times: All samples 102224RE, 200204RE, and 200406RE were re-analyzed outside Region II holding times. Results for samples 102224RE, 200204RE, and 200406RE should be considered estimates(J). GC/MS Tuning and Mass Calibration: All BFB tuning criteria were within control limits. Initial Calibration: All compounds with contract criteria for RRFs and %>RSDs met those requirements. All target compounds had average RRFs above the allowable minimum (0.050) as required. Methylene chloride (42.1 %>) had a %RSD above the allowable maximum (3 0%) on 08-26-97. Acetone (35.1 %) and 2-butanone (42.8%) had %RSDs above the allowable maximum (30%)) on 10-09-97. Methylene chloride (37.6%), 2-butanone (26.3%), and 4-methyl-2-pentanone (58.1%)) had %RSDs above the allowable maximum (30%) on 09-19-97. Results for these compounds should be considered estimates (J) in associated samples. 2-Hexanone( 108.5%) had a %)RSD above an acceptable maximum (90%)) on 09-19-97. Results for 2-hexanone should be considered unusable (R) in associated samples. Continuing Calibration: All compounds with contract criteria for RRF50s met those requirements. Bromodichloromethane (25.4%o),dibromochloromethane(33.0%o), trans-l,3-dichloropropene (26.1 %)), and bromoform (38.3%)) had %)Ds above the contractual maximum (25%)) on 10-01 - 97 (1001K03). Carbon tetrachloride (26.2%)) bromodichloromethane (26.5%), dibromochloromethane (36.8%)), trans-l,3-dichloropropene (27.2%)), and bromoform (44.9%) had %Ds above the contractual maximum (25%) on 10-02-97 (1002K03). Bromodichloromethane (29.1 %), dibromochIoromethane(3 8.2%o), trans-1,3-dichloropropene (32.2%)), and bromoform (47.4%)) had %)Ds above the contractual maximum (25%)) on 10-03- 97 (1003K03). These calibrations had greater than to compounds outside contract requirements. These calibrations were not compliant with the CLP statement of work. All target compounds had RRF50s above the allowable minimum (0.050) as required. Methylene chloride (25.8%), 2-butanone (25.2%)), 4-methyl-2-pentanone (59.7%), and 2- hexanone (86.6%) had %Ds above the allowable maximum (25%) on 09-23-97 (0923L04). 2-Butanone (34.1%), 4-methyl-2-pentanone (57.3%o), and 2-hexanone (82.3%) had %Ds above the allowable maximum (25%) on 09-24-97 (0924L03). 2-Butanone (32.2%) and 2- hexanone (35.8%) had %Ds above the allowable maximum (25%) on 09-29-97 (0929L01). Methylene chloride (26.4%)), acetone (35.3%)), bromodichloromethane (25.4%)), dibromochloromethane (33.0%)), trans-1,3-dichloropropene (26.1%)), bromoform (38.3%)), 4-methyl-2-pentanone (42.9%)), and 2-hexanone (47.9%)) had %)Ds above the allowable 304373 maximum (25%) on 10-01-97(1001 K03). Methylene chloride (3 6.2%), carbon tetrachloride (26.2%)) bromodichloromethane (26.5%), dibromochloromethane (36.8%)), trans-1,3- dichloropropene (27.2%o), bromoform (44.9%)), and 4-methyl-2-pentanone(39.0%) had %>Ds above the allowable maximum (25%) on 10-02-97 (1002K03). Methylene chloride (29.9%), acetone (31.6%)), 2-butanone (38.3%)), bromodichloromethane (29.1%)), dibromochloromethane (38.2%)), trans-l,3-dichloropropene (32.2%)), bromoform (47.4%o), 4-methyl-2-pentanone (41.2%)), and 2-hexanone (35.7%)) had %)Ds above the allowable maximum (25%) on 10-03-97 (1003K03). Acetone (50.1%) had a %D above the allowable maximum (25%)) on 10-10-97 (1010K03). Results for these compounds should be considered estimates (J) in associated samples. Blanks: Method blank VBLKL1 contained a trace of methylene chloride (11 ug/kg). Method blank VBLKL2 contained traces of methylene chloride (14 ug/kg) and acetone (12 ug/kg). Method blank VBLKL3 contained traces of methylene chloride (9 ug/kg) and acetone (21 ug/kg). Method blank VBLKL4 contained a trace of methylene chloride (8 ug/kg). Method blank VBLKL5 contained a trace of methylene chloride (18 ug/kg). Method blank VBLKL6 contained traces of methylene chloride (7 ug/kg) and acetone (4 ug/kg). Method blank VBLKL7 contained traces of methylene chloride (7 ug/kg) and acetone (2 ug/kg). Method blank VBLKWl contained traces of methylene chloride (2 ug/L) and acetone (10 ug/L). Method blank VBLKW2 contained traces of methylene chloride (3 ug/L) and acetone (5 ug/L). Method blank VBLKW3 contained traces of methylene chloride (4 ug/L) and acetone (7 ug/L). Trip blank TB0918 contained traces of methylene chloride (4 ug/L) and acetone (11 ug/L). Trip blankTB0919containedtraces of methylene chloride (25 ug/L) and acetone (14 ug/L). Trip blank TB0922 contained a trace of methylene chloride (27 ug/L). Trip blank TB0923 contained a trace of methylene chloride (4 ug/L). Trip blank TB0924 contained traces of methylene chloride (3 ug/L) and acetone (7 ug/L). Trip blank TB0926 contained a trace of methylene chloride (4 ug/L). Trip blank TB0930 contained traces of methylene chloride (5 ug/L) and acetone (6 ug/L). Field blank FB0918 contained a trace of methylene chloride (6 ug/L). Field blank FB0919 contained a trace of methylene chloride (4 ug/L). Field blank FB0922 contained traces of methylene chloride (14 ug/L) and acetone (39 ug/L). Field blank FB0923 contained traces of methylene chloride (4 ug/L) and acetone (22 ug/L). Field blank FB0924 contained traces of methylene chloride (4 ug/L), acetone (40 ug/L), and 2-butanone (11 ug/L). Field blank FB0926 contained traces ofmethylene chloride (3 ug/L), 2-butanone (4 ug/L), and xylene (3 ug/L). Field blank FB0930 contained traces ofmethylene chloride (5 ug/L) and xylene (3 ug/L). Results for acetone and toluene less than ten times the highest associated blank should be considered not detected (U) in samples. Trip blank TB0922 contained an unacceptable level of acetone (110 ug/L). Field blank FB0918 contained an unacceptable level of acetone (62 ug/L). Field blank FB0919 contained an unacceptable level of acetone (69 ug/L). Field blank FB0926 contained an unacceptable level of acetone (190 ug/L). Field blank FB0930 contained an unacceptable level of acetone (92 ug/L). Results for acetone less than ten times the highest blank level should be considered unusable (R) in associated samples. The following are listed the contaminated blanks and associated samples: Method blank VBLKLl: 702224, BOOOOl, B00002, B00003, B00003RE, B00004 304374 Method blank VBLKL2: 5A2022, 5A2224, 6A2022, 6A2224, 702022, 702224DL Method blank VBLKL3: 101618, 201820, 202022, 301012,301820, 5A2224DL Method blank VBLKL4: 102224, 200204, 301012RE Method blank VBLKL5: 200406,300810 Method blank VBLKL6: 100608, 101214, 102224RE, 200204RE, 200406RE, 300608, D11214 Method blank VBLKL7: 300608RE, DI 1214RE Method blank VBLKWl: FB0918, FB0919, FB0922, TB0918, TB0919, TB0922 Method blank VBLKW2: FB0923, FB0924, TB0923, TB0924 Method blank VBLKW3: FB0926, FB0930, TB0926, TB0930 Trip blank TB0918: 702022, 702224 Trip blank TB0919: BOOOOl, B00002, B00003, B00004 Trip blank TB0922: 5A2022, 5A2224, 6A2022, 6A2224 Trip blank TB0923: 101618,102224 Trip blank TB0924: 201820,202022,301820,301012 Trip blank TB0926: 200204, 200406, 300810 Trip blank TB0930: 300608, 100608, 101214, DI 1214 Field blank FB0918: 702022,702224 Field blank FB0919: BOOOOl, B00002, B00003, B00004 Field blank FB0922: 5A2022, 5A2224, 6A2022, 6A2224 Field blank FB0923: 101618,102224 Field blank FB0924: 201820, 202022, 301820, 301012 Field blank FB0926: 200204, 200406, 300810 Field blank FB0930: 300608, 100608, 101214, DI 1214 Internal Standard Area Summary: All intemal standard retention times were within control limits. Sample DI 1214 and DI 1214RE had 3 of 3 intemal standard areas (ISl, IS2, IS3) outside control limits. Sample301012RE,300608RE,andB00003had2of3 intemal standard areas (IS2, 1S3) outside control limits. Samples 300608, 301012, and B00003RE had 1 of 3 intemal standard areas (IS3) outside control limits. Results for samples D11214,D11214RE, 301012RE, 300608RE, B00003, 300608, 301012, and B00003RE quantitated off intemal standard with areas outside control limits should be considered estimates (J). Surrogate Recovery: Sample B00003RE had 2 of 3 surrogate recoveries outside control limits. Sample D11214RE had 1 of 3 surrogate recoveries outside control limits. Results for samples DI 1214RE and B00003RE should be considered estimates (J). Matrix Spike/Matrix Spike Duplicate: MS/MSD samples 300608 and 702022 had all relative percent differences and percent recoveries within control limits. Compound ID: Checked compounds were within GC/MS quantitation and qualitation limits. All positive hit compounds had the primary and secondary ions in their mass spectra as outlined in the SOW. G:\STAFF\DANNE\lsland\97130. VOL.wpd 304375 Cone, of Intemal Standard: 50 ID: K Date: 10/9/97 RRF Cone, of Compound Bromochloromethane Vinyl Chloride RRF 1,4-Difluorobenzene Triehloroethene j RRF 1 Chlorobenzene-d5 Tetrachloroethene RRF 1009K04 Sample 1 10 639742 129095 1.009 3097512 310827 0.502 2224315 353847 0.795 1Q09KQ2 Sample 2 20 771107 268154 0.869 3580223 734938 0.513 2564585 766370 0.747 1009K07 Sample 3 50 621468 524508 0.844 3018181 1467186 0.486 2270397 1551428 0.683 1009K03 Sample 4 100 731897 1147217 0.784 3434892 3321478 0.483 2565484 3494071 0.681 1009K05 Sample 5 200 780724 1920937 0.615 3302809 7149955 0.541 2727871 7661025 0.702 Average 0.824 0.505 0.722 % RSD 17.4% 4.7% 6.8% Continuing Calibrations - • ' • Cone, of Compound Bromochloromethane Vinyl Chloride RRF 1,4-Difluorobenzene Triehloroethene RRF Chlorobenzene-d5 Tetrachloroethene RRF 1010K03 Sample 50 767840 602076 0.784 3418979 1635586 0.478 2488971 1682552 0.676 %D 4.9% 5.3% 6.3% • Sample #DlV/0! #OIV/0! #DlV/0! %D #DIV/0! #DIV/0! #DIV/0! Sample #DlV/0'. #DlV/0! #DIV/0! %D #DIV/0! #DIV/0! #DlV/0! Sample #DlV/0! #DIV/0! #DIV/0! V.D : #DIV/0! #DIV/0! #DIV/0! Sample #DIV/0! #DIV/0! #DIV/0! ,;:v%D-..- #DIV/0! #DIV/0! #DIV/0! 304376 Cone, of Intemal Standard: 50 ID: K Date: 8/26/97 R R F . ' Cone, of Compound Bromochloromethane Vinyl Chloride RRF 1,4-Difluorobenzene Triehloroethene RRF Chlorobenzene-d5 Tetrachloroethene RRF 0826K07 Sample 1 10 271486 86886 1.600 1086101 125322 0.577 896773 140331 0.782 0826K06 Sample 2 20 258409 142622 1.380 1043398 206470 0.495 840502 232258 0.691 0826K04 Sample 3 50 230277 256709 1.115 898106 444951 0.495 724344 476865 0.658 0826K10 Sample 4 100 288988 779699 1.349 1170177 1227788 0.525 987744 1337155 0,677 0826K08 Sample 5 200 297013 1421132 1.196 1180685 2604003 0.551 1034678 2939330 0.710 Average 1.328 0.529 0.704 7. RSD 14.1% 6.8% 6.8% Continuing Calibrations Cone, of Compound Bromochloromethane Vinyl Chloride RRF 1,4-Difluorobenzene Triehloroethene RRF Chlorobenzene-d5 Tetrachloroethene RRF 1001K03 Sample 50 585872 762352 1.301 2723990 1284533 0.472 1959065 1352323 0.690 •/oD 2.0% 10.8% 1.9% 1002K03 Sample 50 746374 907581 1.216 3569198 1629717 0.457 2499677 1604903 0.642 %D 8.4% 13.6% 8.8% 1003K03 Sample 50 610227 741921 1.216 2896976 1315797 0.454 2074703 1341455 0.647 %D 8.4% 14.1% 8.1% Sample #DIV/0! #DIV/0! #DIV/OI %D #DIV/0! #DIV/0! #DIV/0! Sample #DIV/0! #DIV/0! #DIV/0! V.D #DIV/0! #DIV/0! #DIV/0! 304377 Cone, of Intemal Standard: 50 ID: L Date: 9/19/97 . . ^ , • ; • ; • • ; R R F , ; : • • • , • • Cone, of Compound Bromochloromethane Vinyl Chloride RRF 1 1,4-Difluorobenzene Triehloroethene RRF Chlorobenzene-d5 Tetrachloroethene RRF 0919L05 Sampte 1 10 325198 68455 1.053 1724399 175858 0.510 1441655 182502 0.633 0919L03 Sarhple2 20 320639 139753 1.090 1677946 327341 0.488 1439373 340179 0.591 0919L02 Sample 3 50 287146 366307 1.276 1611119 759729 0.472 1367960 811715 0.593 0919L04 Sampte 4 100 320764 779684 1.215 1681899 1638721 0.487 1435104 1689683 0.589 0919L06 Samples 200 315462 1555796 1.233 1648146 3161653 0.480 1376883 3270481 0.594 Average 1.173 0.487 0.600 V. RSD 8.2% 2.9% 3.1% Continuing Calibrations 1 Cone, of Compound 1 Bromochloromethane Vinyl Chloride RRF 1 1,4-Difluorobenzene I Triehloroethene RRF 1 Chlorobenzene-d5 1 Tetrachloroethene 1 RRF 0923L04 Sample 50 317143 299383 0.944 1722560 766209 0.445 [ 1482775 836093 0.564 %D 19.5% 8.7% 6.0% 0924L03 Sample 50 328129 353165 1.076 1704050 757322 0.444 1 1496828 793286 0.530 %D 8.3% 8.8% 11.7% Sample #DIV/0! #DIV/0! #DIV/0! V.D #DIV/0! #DIV/OI #DlV/0! Sample #DIV/0! #DIV/0! #DIV/0! 'y-y%D-:-: #DIV/0! #DIV/OI #DiV/0! Sample #DlV/0! #DIV/0! #DIV/0! .:::\.%D:4.- #DIV/0! #DIV/0! #DIV/0! 304378 Cone, of Intemal Standard: 50 ID: L Date: 9/26/97 -.;•.•. RRF:-- Cone, of Compound Bromochloromethane Vinyl Chloride RRF 1,4-Difluorobenzene Triehloroethene RRF Chlorobenzene-d5 Tetrachloroethene RRF P926L04 Sample! 10 552220 109258 0.989 2805652 235852 0.420 2360617 240796 0.510 0926L02 Sample 2 20 579499 254777 1.099 2846434 539091 0.473 2448393 559302 0.571 0926L01 Sampie 3 50 610791 651924 1.067 2932968 1314166 0.448 2523023 1340009 0.531 0926L03 Sample 4 100 567230 1275933 1.125 2825003 2663113 0.471 2398336 2649736 0.552 0926L05 Sample 5 200 550173 2523783 1.147 2768989 5338884 0.482 2398860 5299839 0.552 Average 1.085 0.459 0.543 V. RSD 5.7% 5.5% 4.3% Continuing Calibrations Cone, of Compound Bromochloromethane Vinyl Chloride RRF 1,4-Difluorobenzene Triehloroethene RRF Chlorobenzene-d5 Tetrachloroethene RRF 0929L01 Sample 50 370336 349830 0.945 1808094 796867 0.441 1634344 771898 0.472 V.D 13.0% 4.0% 13.1% 1003L01 Sample 50 521869 568236 1.089 2577991 1177039 0.457 2145463 1140884 0.532 V.D 0.3% 0.5% 2.1% Sample #DIV/0! #DIV/0! #DlV/0! V.D #DlV/0! #DlV/0! #DlV/0! Sample #DlV/0! #DIV/0! #DIV/0! V.D #DIV/0! #DlV/0! #DlV/0! Sample #DIV/0! #DlV/0! #DIV/0! V.D #DlV/0! #DlV/0! #DIV/0! 304379 QA/QC Review of 8270 Pyridine Data* for Pace Analytical SDG: 97130 November 3, 1997 Holding Times: All samples were extracted and analyzed within Region II holding times. GC/MS Tuning and Mass Calibration: All DFTPP tuning criteria were within control limits. Initial Calibration: All SPCCs and CCCs were within control limits. Pyridine had average RRFs above the allowable minimum (0.050) and %RSDs below the allowable maximum (30%) as required. Continuing Calibration: All SPCCs and CCCs were within control limits. Pyridine had RRFSOs above the allowable minimum (0.050) and %Ds below the allowable maximum (25%) as required. Blanks: Method blanks reported pyridine as not detected. Intemal Standard Area Summary: All intemal standard areas and retention times were within control limits. Surrogate Recovery: All percent recoveries were within control limits. Matrix Spike/Matrix Spike Duplicate: MS/MSD samples did not include pyridine as a target compound. Compound ID: All samples reported pyridine as not detected. * only four field blanks were analyzed for pyridine by 8270, all others pyridine was included as part of the CLP semivolatile analyses. G:\STAFF\DANNE\Isiand\97130.PYR.wpd 304380 SOP NO. Krf-6 Revision 18 SD<^ : 97(30 ^ ^ ' 3Y: - -^ .1 \ . T T ^ ^ ^ ^ ' ' L e o n ^ L i i a r u s . lr.vir=r.r.an"Cii S c i e n r i s " Tcxzc and K a z a r i c u s Wasre Secri=r. Al /7 GTeorcs I-s^rras. c.^eniisr Tcxic ar.i Hazarccus Waste Secticr. Date . Jc2.^ ^ ;•;?!. Date •j!X^IX!±2±f'*' - '^^ fa. / ' < . ex.;- .^y. V*-. s!L-c -i/ .••< 1 5 t e i i c £ G e r a z c u r . i s / c r . e n i s t T c x i c 2nd H a z a r d e d Wasre Secricr. Kevin Kufai,^ _a!^ei D a t e : /Jwz. iz-2rrc^.::s Waste S e c t i c r . / ' D a t e : . JA<I^ R o b s r t P.unyon. criief M o n i t c r i r . q hlanageinent Srar.cr. 304381 Date; J a n u a r y 1292 R e v i s i o n : 8 YES HO H/A PACKAGE ccitPLErz-rzss XKD czxjr.TSABizs o /O / / • 1 SAfiS ^UHBIS: ^ n i ' ^ 0 T^p. Mace /-foQ!.^ftca ( K 1.0 Data cczipieteness and Daliveranies 1.1 Have any r.issinc dalivaraalES teen received and added tc tr.s data pacxage? I 1 ACTID::: call lab fcr expianaticn/resutssittai cf any nissinc daliveraaias. II lab cannot prsvida tham, r.cta tna effact cn review of ti:a package under t:;a "Contract Probians/Non-ccspiianca" section of reviewer narrative. 1.2 Was SHO CZZ. cr.ackiist included -•it^. package? '_ 1 JL. 2.1 Is tr.s Karrctiva or Ccver Latter Present? i"^ __- — 2.2 Arc Case Nunbar and/or SAS nusibar contained x/ in tba Narrative cr ccver letter? r •< ^ -Ji. -> n D a t a r / a i ; - J n » « - — r-*.ai-V^1 » <?•• The fcllcvinc checxli'sr is divided into tr.ree parrs. Part A is filled out if tr.a data package contains any VOA analyses. Part S fcr any EKA analyses and Part C for Peaticida/PCBs. to Does this packaqe ccntainr ^ VOA Data? _^. 00 B.S'A Data? lEi —-• Peatic:ia/PCB data? _^ 2 ^ Action: ccrtlate ccrraspcndinc parts cf cr.ecklist. STA}IDAAD CPBPJkTmC PHGCZZI..%Z Date: Januar*/ 1332 Revisicn: £ Y£S SO N/A ^ • ' • • • -I n r^t n . . 1.1 Are the Traffic Report ror=s present fcr I_l _^L all samples? ACrrc::: if r.c. contact lab fcr rapiacenent of -issinc cr illegioie copies. 1.2 Do tr.e Traffic Reports or Lab Narrative indicate any problems vitii saniple receipt, condition of samples, analytical problems or special circurstances affecting the quality of t.he data? _ LL _ ACnc::: if any sampie analyzed as a soil, other than TCLP, contains SOt-90% . water, all data should be flagged as estimated (J]. If a soil sample. other than TCLP contains more than 90% vater. ill data snouid ba qualified as u.-.usable (R) . ACTID::: if samples vare not iced upon receipt at the laboratory, flag all positive results "J"' and all Non- Detects '"JJ". ACTIDH: If both VGA vials fcr a sample have air bubbles^r the VOA vial analyzed had air bubbles, flag all positive results "J" and all non-detects "R". 304383 •) — O 00 1 > STANDARD 0PBRATIK3 PROCZBZ^ D a t e : January 1992 R e v i s i c n : 8 YES HO H/A 2.0 HQldir.r --~r.«^ 2 . 1 Have any VOA t e c h n i c a l h o l d i n g t i m e s . determined from d a t e of c o l l e c t i o n t o d a t e of a n a l y s i s , b e e n exceeded? f- r 1 If u n p r e s e r v e d , i q u e o u s samoles m a i n t a i n e d a t 4'C vhich are t o be analyzed f o r a r o m a t i c h v d r o c a r c c n s must be analyzed v i t h i n 7 days of c o l l e c t i o n . If p r e s e r v e d v i t h -4C1 (?.H<2) and s t o r e d a t 4*C, t h e n aqueous samoles must be a n a l y z e d v i t h i n 14 days cf c o l l e c t i c n . If u n c e r t a i n a b o u t p r e s e r v a t i o n , c o n t a c t sampler t o d e t e r m i n e whether or n o t s a m p l e s were p r e s e r v e d . The h o l d i n g t i m e for s o i l s i s 10 d a y s . Table a - " - I d i r - - ^ r ^ v^ >^1 » t i c n s Samole Samoie Matrix Preser^.-ed? ZOO'iOloRE So) (S«e Traffic Report; Date Date Lab Date Sampled Received Analyzed a M o L f/3oMn j^lmiaiL AC.^ .1. w.>: If technics positive re quantitatio the narrati analyses we tine, eithe the reviewe daterr.ine t additional all results determine t holding tim detect data in 1 holding times are exceeded, flag all suits as estimated ("J") and sampie n limits as estimated ("UJ") , and document ve that holding times vare exceeded. If re done more than 14 days beyond holding r cn the first analysis or upon re-analysis, r must use professional judgement to he reliability of the data and the effects of storaoe on the samole results. At a minimum, must'be q-ualified" "J", but.the revievar^r.ay -.at ncn-detect data are unusable (R). If es are exceeded by'more than 2S days, all ncn are unusable (R) . STAIiDAUD CPi.-JvTI^iG PROCZZ'JP-Z Date: January 1932 Revisicn: 8 YES HO H/A 3.1 Are the VCA SMC Reccvery Summaries (Form II") present for each cf the folloving matrices: a. Low Water r^j ___, b . Low £ 2 i l i"^"! c. Med Soil i_J. 2L. 3.2 Are fill the VOA samples listed cn the appropriate System Kcnitoring Ccmpound Reccvery Summary fcr each of the follcwing matrices: a. Low Water r N _ _ ___ b. Lowsoil L i l c. Med Soil L-i - ^ ACTi:::: c a n lab fcr expianaticn/ resucmittals. If missing deliveraclss are unavailable, document effect in data assessments. 3.3 Were outliars marked correctly with an ^ asterisk? L l l ACTIC": Circle a l l outliers in red. Was one cr mere VOA system r.cnitcring compound recovery outside of ccntract specifications fcr any sampie or method blank? —b_ LX. If yes, were samples re-analyzed? Libi Were nethcd blanks re-analyzed? 3 . 4 _L _ ^ 304385 - 4 - STANDARD Crr,iO\TZ^G PROCZZL.-^ Date: J a n u a r y 1232 Revision: 8 YES HO N/A ACnZM: If recoveries are > 101 but 1 or more compounds fail to meet SOW specifications: 1. All positiva results are qualified as estimated (j) . 2. Flag all ncn-detects as estimated detecticn limits ("UJ") where recovery is lass t.han the lever acceptance limit. 3. If SHC recoveries are above ailcvaole levels, do not qualify non-detects. If any system monitoring compound reccvery is <lOt : 1. Flag all positive results as estimated ("J") . 2. Flaa all non-detects as unusable ("R"). Professional judgement should be usad tc qualify data that cnly have method blank SHC raccverias cut of specification in bot.h original and ra-anaiyses. Checx t.na i.-.tarnal standard areas. 3-5 Are t.hare any transcription/calculation errors betveen raw data and Form II? ACTID:;: if large errors exist, call lab fcr expianaticn<iresubmittal, .-ake any necessary corrections and note errors in the data assessment. Xl 4.0 M a t r l v g-^-iVoe ^f^,— TTT^ ' ' * " * • " • • • • • - . • ^ : : ' . . . . . . . . ; 4.1 Is the Matrix Soike/Matrix Soike Duolicate Recovery Term (Form III) present? iX 304386 STANDAJID CPZRATIK3 PROCZZLIIZ Date: Januar-/ 1292 Revisicn: a YES HO H/A 4.2 Were matrix spikes analvzed at the required frequency for eacn cf t-he follcwing matrices: a. Low Water r T ___^ V. b. Low Soil r'^ c. Med Soil jr_j_ Y ACTIC::: If any matrix spike data are m>issing, take the action specified in 3 - 2 above. 4.3 How many VOA spike recoveries are outside QC limits? Ha^ex 2^2X2. out cf 10 O out cf 10 4.4 Kow many RPD's fcr matrix spike and matrix spike duplicate reccverias are outside QC limits? out cf £ O out cf £ ACTIDI?: .Vo action is taken based cn MS/MSD data alone. Hovever, using i.-.formed professional judgement, t.he MS/MSD u> r e s u l t s may be used i.n conjunction o with ether'CC c r i t e r i a t o determine ; |^ t h e need fcr'-qualificaticn of the ' c» d a t a . * <> . 0 Blanks ^~^r-. ^rr) 5.1 I s the Method Blank Summary (Form IV) p r e s e n t ? rYJ _ _ 5.2 Frequency of Analysis: fcr t h e a n a l y s i s of VOA TCL compounds, has a reagent/method blank been analyzed fcr each SDG or every 20 samples of similar matrix (low water. low s a i l , -adium s c i l ) , vnichever is,more freaue.nt? i^Si STAKDAJID CPZRATIMG ?ROCZZL"RZ D a t e : J a n u a r y 1392 R e v i s i o n : 8 YES NO H/A 5.3 Has a VOA method/instrument blank been analyzed at least cnca every twelve hours for eacn concentratrcn lavel and GC/>!S system usaa? rr-^ ACTIC::: If any method blank data are missing, call lab fcr explanation/ resummittal. If -ethod blanx data are not available. reject (R) all associated positive data. However, using professional judgement, the data reviewer may substitute field blank or trip blank data fcr missing method blank data. 5.4 Chrcnatcgrapny: review the blank raw data - chromatograms (RICs), quant reports or data system printouts and spectra. Is the chromatographic performance (baseline stability) for eacn i.-.strument accectable w. for vcAs? ' 1X1 nCZZZIl: Use professional judcament tc determ.ine t.te effect cn t.he data. 6.0 Cor.tti-t I I *< T « r ' I l.'OTZ; "Water blanks", "drill blanks", and distilled vater blanxs" are validated like any other sampie, and are not usad tc qualify data. Do not confuse t.hem vit.h the ether CC blanks ttiscussad balow. 6.1 Do any method/instrument/reagent blanks have positive results (TCL and/or TIC) for VOAs? When applied as described balow, tha contaminant ccncentraticn in these blanks are multiplied- by the sample dilution factor and . w corracted fcr t m.cistura vnen necessary. _2_i i — ^i, OJ 6.2 Do anv f i e l d / t r i p / r i n s a blanks have positive V , m VOA results (TCL and/or TIC)? —LL LX. 1 Prepare a l i s t cf tha samples associated vit.h eacn cf t.ha contaminated blanks- (Attacn a separata sheet.) STAKDAJID CPZilATIh'G PROCZZ'JRZ Date: J a n u a r y 1332 R e v i s i o n : S YES NO N/A NOTE: A l l f i e l d blank r e s u l t s a s s o c i a t e d t o a p a r t i c u l a r group cf samples (may exceed one p e r case) c u s r b a used t c q u a l i f y d a t a . T r i p blanks a r e u s e d t o q u a l i f y only t h e s e samples w i t h which t h e y w e r e shipped and a r e n o t r e q u i r e d f c r non-aqueous m a t r i c a s . Blanxs may n o t be c i a l i f i e d b e c a u s e of contaminaticn i n a n o t h e r b l a n k . Field E l a n x s i T r i ' Blanks must ba q u a l i f i e d f c r system mcnitcrir-g compound, i n s t r u m e n t performance c r i t e r i a , s p e c t r a l o r c a l i b r a t i o n QC p r o b l e m s . ACTZZ::: Follow t h e d i r e c t i o n s i n t h e t a b l e below- t o q u a l i f y TCL r e s u l t s due t o c o n t a m i n a t i c n . Use t h e l a r g e s t v a l u e from a i l t h e a s s o c i a t e d b l a n k s . I f any b l a n k s a r e c r o s s l y c o n t a m i n a t e d , a l l a s s o c i a t e d d a t a s h o u l d be q u a l i f i e d a s u n u s a b l e (R). sampie cone ? CRQL Samnle cone < CRQL Sample cone > CRQL b u t < iQx blank i <iox blank value S >10x blank value value .^'.atnylene Chloride Flag sampie result Report C.~QL i Acetcne with a "U; qualify "U" Toluene 2-Eutanone No q-uaiification is needed samoie cone > CRQL sammle cone < CRQL i sample cone > CRQL but" < 5x blank is < 5x blank value value & > 5x blank value Other Flag samnle result Report CRQL i Ccntam- with a "U" qualify "U" i n a n t s NO q - u a i i f i c a t i o n i s n e e d e d NOTE; .nalvtes Q u a l i f i e d "U" f o r blank c o n t a m i n a t i o n a r e II k 4 . . . _ 11 s t i l l ccnsidarea as "hits calibration c r i t e r i a . „ .^'-.— hen q--:ai-ifying i c r 304389 STANDARD C?ERATI::G PROCZZTPJI Date: January 1392 Revision: a ACTICM: YES NO N/A For TIC compounds, if t h e concentration in t h e sample is less than five times the concentraticn i n the c o s t contaminated a s s o c i a t e d blank, flag t h e sample data "R" (unusable) . 6.3 Are t h e r e f i a l d / r i n s e / e o u i t m e n t blanks ^ associated vith everv* sampie? fXi ACTIC:.': For low level samples, n o t e in data assessment t h a t t h e r e i s no associated field/rinse/equipment b l a n k . Exception: samples taken from a drirJting water t a p do not have associated f i e l d blanks. •W M l i I M . . I - . . - , . - . - - . . . . . . . . . . 7 . 1 Are t h a CC/MS Instrument Performance Check Forms (Form V) present f c r Eromoflucrcbenzene (BFB)? x;ii 7.2 Are t h a ennanced bar cramh smectrum and r.ass/c.harcs (r./z; l i s t i n c fcr tha EF3 provided f:r eacn tvalve hour shift? r V 7-3 Has an instrument performance ccmpound been analyzed f i r every t v a l v e hours of samcle ^ a n a l y s i s per instrument? r M 304390 STA},'DARD CPZrJ^TIMG PROCZZ'JRZ Date: January 1392 R e v i s i c n : 8 YES NO N/A ACTIC::: List date, time, instmment 13, and sample analysis for vhich no associated CZ/yjs. tuning data, are available.' DATE TI^TZ INSTRL"HZHT SAMPLE KUHBERS ACTIO::: if lab cannot provide missing data, reject ("R") all data generated cutside an acceptable twelve hour calibration interval. 7.4 Have t.ha icn abundances been normalized tc ^ m/z 9 5? ilX. * qualify all associated data as unusaole (R) . 7.5 Have t.he icn abundance criteria been met fcr ./ each i.-.strument used? f ^'' _—^- • ACTIO:.': List all dzzz vhich do not meet icn abundance criteria (attach a separate sheet). ACTIc:r: If icn abundance criteria are not met, the Regicn II TPO r.ust be notified. 7.6 Are there any transcription/calculation errors betveen mass lists and Form Vs? (Check at least tvo values but if errors are fcund, check N^ nore.) i-ij 304391 STA:«DAR.D CrZPj^.Ti-rG PROCZZJP.Z Date: January 1=32 Revision: s YES HO H/A ' ^ 7.7 Have the appropriate number cf sicnificant ^ figures (two) been.reported? ' l2i ACno::: if large errors exist, c a l l lab for explanaticn/resucmittal, make • necessary corrections and document effect ir. data assessments. 7.8 Are the spectra of the mass calibration compound acceptable? _ _ ACTIc:i: UsB. professional judgement to determine whether associated data should be accepted, qualified, or rejected. 8.1 Are rha organic Analysis Data Sheets (Form I VOA) present vit-h required header information cn each page, fcr eacn cf the fcllcving: a. Sanples a.id/cr fractic.ns as appropriate rY.' ___ _ b- Matrix spikes and r.atrix spike duplicates * fX^ _ c. Blanks IXl - 8.2 Are Che VOA Reconstructed Ion Chromatograms, tha mass spectra fcr the identified compounds, and tha data system printouts (Quant Reports) included in the sample package fcr each of t.he following? a. Samples and/cr fractions as apprcpriate f"^^ . b. Matrix spikes and matrix spike duplicates (Mass spectra not .required) i_ji . c. 31anks ££l . ACTIC": If anv data are missinc, take action . soecified in 3.2 above.' 304392 STAKDAR.U C?ZRATi:rG PROCZZ'JRZ Date: J a n u a r y 1392 R e v i s i o n : 3 YES NO H/A 8.3 Are t h e r e s p o n s e f a c t o r s shown in t-he Quant Report? r i 8.4 I s c.-.romatccraphic p e r f c r c a n c e a c c e o t a b l e w i t h r e s o e c t t o : Baseline s t a b i l i t y ? R e s o l u t i o n ? Peak shape? F u l l - s c a l e g r a p h ( a t t e n u a t i o n ? ? O t h e r : JUI r 1 >^ _ -X ACnc::: use professional judgement to datermine tha acceptability of the data. 3-5 Are the lab-generated standard r.ass spectr; 'cresent fc: 8.6 8 -7 of tna idantifiaa eac.i samole? ACTIi::: If any mass spectra are missing, take action specified in 3.2 above- If lab does not generate their own standard spectra, make note in "Contract Prohlems/Non-compliance". Is the RRT cf each reported ccmpound vithin 0.06 RRT units of the standard RRT in the conti.-.uing calibration? Are all ions present in the standard r.ass spectrum at a" relative intensity greater than i z \ also present in the sampie mass ,spectrum? iii , i^ _ lA . 304393 Si^liDARD OPERATING PROCZZL---i Date: J a n u a r y 1392 Revisicn: s YES HO N/A 8.8 Do sample and s t a n d a r d r e l a t i v e ion i n t e n s i t i e s agree v i t h i n 20*7 T^T ___ ACTICK: Use p r o f e s s i o n a l j u d g e m e n t t o datermine a c c a p t a b i l i t y of data- If i t i s determined t h a t i n c o r r e c t i d e n t i f i c a t i o n s w e r e made, a i l such data snouid be r e - j e c t e d (R) , flagged "N" (presumptive e v i d e n c e of t h e presence cf t h e ccmpound) cr changed t o net d e t e c t e d (U) a t t h e c a l c u l a t e d d e t e c t i c n l i m i t - In order t o be p o s i t i v e l y i d e n t i f i e d , the data must comply v i t h t h e c r i t e r i a l i s t e d i n 8 . 6 , 8 . 7 , and 8 . 8 . ACTICJi: When sample c a r r y - o v e r i s a p o s s i b i l i t y , p r o f e s s i o n a l judgement should be used t c d e t e r m i n e if instrument c r o s s - c c n t a m i n a t i c n has a f f e c t e d any p o s i t i v e compound i d e n t i f i c a t i o n . 9.1 Are a l l Tentatively Identified Compound Forms (Form I Part 2) present; and do listed TICs include scan number or r e t e n t i o n time, y estimated concentration and "JM" qualifier? ^^'' 9.2 Are the r.ass spectra for t h e tentatively identified compounds and associated "best match" spectra included in the sample package for eacn of the following: a. Samples and/or fractions as appropriate f^*! __— b . Blanks L t l —— ACTION: If any TIC data are missing, take action specified in 3.2 above. ACTI0:i: Add ":vr q - a l i f i e r if missing. 304394 STANDARD CPZPATi:iG PROCZZL':iE D a t e : January' 1 = 92 R e v i s i o n : 8 YES HO H/A 9.3 Are any TCL ccmpou.nds (from any f r a c t i o n ) l i s t e d a s TIC compounds (exammle: 1 , 2 - d i m e t h y l b e n z e n e i s x v l e n e - a VOA TCL a n a l y t e - and s h o u l d ' n o t ba r e p o r t e d a s a TIC)? ''X'' A C T I O : : : F l a g w i t h "?." any TCL ccmpound l i s t e d as a TIC. 9.4 Are a l l ions present i.n the reference mass spectrum vith a relative intensity greater than lot also present in the samcie mass spectrum? JJ± 9.5 DO TIC and "best match" standard r e l a t i v e ion i n t e n s i t i e s agree wit-hin 2 0t? TAT ___. ^ _ ACTIO:;: use professional judgement to determine acceptability of TIC identificaticns. If i t i s determined that an incorrect identificaticn vas made, change icenti^icaticn tc unknown cr w.. some less specific identification (example: "C3 suDStituted benzene") as appropriate. Also, vhen a ccmpound i s not fcund in any blank, but is detected in a sample and i3_ a suspected a r t i f a c t of a common laboratory contaminant, the result should be qualified as • unusable (R). ( i . e . Common Lab Contaminants: CO, (M/E 44), Siloxanes (M/E 73) Hexane, Aldol Condensation Products, Solvent Preservatives, and related by products - see Functional Guidelines for more guidance). 304395 STA:CDA:RD CPZPJSWTI::: PROCZZL'P.Z Date: January 1=92 Revision: 8 YES HO H/A r \ 10.0 Comrcun:^ r"^--* —•«-^ ••- »«,< oa»»,.^—«,< T^'^t.^'"^' ^iT. 10.1 Are there any transcription/calculation. errors in Form I results? c::&cx. at least tvo positive values. Verify that tha correct intemal stancard, q-antitaticn icn, and RRF vare used tc calculate Form I result. Were any errors fcund? 10.2 Are the CRQLs adjusted to reflect sample dilutions and, for soils, sampie moisture? r^^ „___ ___ ACTIO::: if errors are large, call lab for explanaticn/resutmittal, make any necessary ccrrections and note errors under "Conclusions". ACTIi::; When a sample is analyzed at r-ore than ene diluticn, t.he icvast CRQLs are usad (unless a QC exceedanca dictates t.he use of t.he hig.her CRQL data from t.ha diluted sample analysis). Replace ccncentraticns t.hat exceed the calibration range in t-he original analysis by crossing out t.he "Z" and its associated value on t.he original Form I and substitutinc the data from t-he analysis of the diluted sample. Specify vhich Form I is to be used, t-hen draw a red "X" acrcss Sie entire page of all Form I's that should not be used, including any in the summary package. 11.0 ' sta^'*''--''^ p3'«-« fi^-c/y'^ 11.1 Are the Reccnstructed Icn Chromatograms, and data system printouts (Quant. Reports) present for i n i t i a l and continuing .^'• calibration? l2± ACTIC::: If any calibraticn standard data are n i s s i n c , take action soecified in on/ioo^ • 3.2 above. ' 304396 STANDARD CPEPJ^TIIIG PRDCZZURZ Date: January 1=92 Revision: S YES HO H/A 12.1 Are the I n i t i a l C a l i b r a t i c n Forms (Form VI) present and complete for t h a v o l a t i l e fraction a t c o n c e n t r a t i c n s of 10, 20, 50, 130, 2 00 ug/1? Are t h e r e saoaratc c a l i b r a t i o n s for low water/med c o i l s ^, and low s o i l sammles? r K rwWA ..k.w*a • If any calibration standard forms are missing, take action specified i.n 3.2 above. 12.2 Were ail lev level soil standards, blanks and samples analyzed by heated purge? f/\i ACTIO::: if icv level s o i l samples ware not heated during purcs, qualify positive h i t s "J" and non-detects "R«, 12.3 Are response factors stable for VGA's over tha concentration range cf the calibraticn (^Relative standard Deviation (\RSD) <30,Ci )? I I _ ^ ACTICN: Circls a l l c u t l i a r s in red. NOTZ; Althcucn 11 VOA compounds have a minimum RR.F ana no maximum "%RSD, the technical c r i t e r i a are t.he same fcr all analytes. ACTIC::: if \RSD > 30.0l, qualify associated positive results for t h a t analyte "J" and non-detects ^ using professi^onal judgement. When RSD > 90%, o flag a l l non-cetects fcr that analyte R (unusable) . *• NOTE: Analytes previously qualified "U" for blank -^ contaminaticn are s t i l l considered as " h i t s " when qualifying fcr i n i t i a l calibraticn c r i t e r i a . U) 12.4 Are the RRFs above 0.05? iii _ Action: Circle a l l o u t l i e r s in red. Action: If any RRF are < 0.05, q-jalify associated non-detects (R) and flag associated positive data as estimated (J). - 1 fi - STANDARD OPZPATIKG PROCZZURZ Date: January 13 9 2 Revision: 8 ~~~" YES NO N/A 12.5 Are thare any t r a n s c r i p t i o n / c a l c u l a t i o n e r r o r s in t h a reportino of averace resoonsa factors (RRF) or tRSD? (Check a t l e a s t 2 values, but if e r r o r s are fcund, check more.) rTN? 1 3 . C G C / y = ^ - ~ - ' ' - . i < v . - , - 4 — fT " - - « 13.1 Are the ccntinuinc calibraticn Forms (Form VII) present and ccmmlete fcr the volatile fraction? * JjSl 13.2 Has a continuing calibraticn standard been analyzed fcr every twelve hours of ^ sample analysis per instrument? r N _ _ ^ ACTIO::: List balov all sample analyses t.hat were not vit-hin twelve hours of the previous ccntir-uing calibraticn anaivsis- u> ;.CTII::: if any forms are missing or no continuing ^ calibration standard has been analyzed vithin tvalve Q hours of every sample analysis, call lab for j ^ expianation/resubmittal. If continuing calibration ^ data are not available, flag all associated sample co data as unusable ("R") . 13.3 Do any volatile compounds have a % Difference {\ D) betveen the initial and continuing ^ RRF vhich exceeds the + 251 criteria? _jL -^—^ ACTIO::: circle all outliers in red. ACTION: Qualify both positive results and non-detects fcr t.he outlier compound(s) as estimated. When I D is above 90%, reject all r.cn-deteets fcr that analvte (R) unusable. STA;-;DARD C?Z?ATI:IG PP.OCEZ-'P.Z Date: January 1332 Revision: S YES HO HTA 13.4 DO any v o l a t i l e cocpounds have a KRF <0.0S? J 1 "A ACnCH: Circle all cutliers in red. ACTIO::: if the FJIF <o.OS, qualify associated non-detects as unusable (R) and "3" associated positive values. 13.5 Are t h e r e any transcription/calculation errors in the repcrtir.g of average response factors (RRF) cr difference (%D) betveen i n i t i a l and continuing RRFs? (Check at least two values but if errors are found, ^ check more.) IflL ACTIO::: c i r c l e errors in red. ACTIO::: if errors are large, c a l l lab for explanaticn/resubmittai, make any ' ^ necessary corrections and note Q errors under "Ccnclusic--.s" . *• . W 1 . . . - , . . . - - . _ - . . . . V - - - . , M . ' 14.1 Are t h e i-nternai standard areas (Form VIII) of every sample and blank v i t h i n the upper and lower limits (-50% to + 100%) for each continuing calibration? -I—1 - ^ ACTIO::: List a i l t.he outliers below. Sampie i l.hternai Std Area Lower Limit Upper Limit .' /on 9(^6^ l £ l . /5'6qo^o ^^03 63 6 ^ 2o\oiZ mniis ^si 119£3Z 3iif\i3o— p (Attacn additional sheets if necessary.) W^^p/e^ .. _3_oo6o8. ... jooGog/e/f. k WiZfi R^ ... i| '/ BoQ^3 Q06Oo3RE,_ H • ._ Jn'^mJ S(A . Hn(oZ3i lioSdH^'A U3(o/cl /7597„V 8 anClA : 8?c39Y ^s^ai^iQ _ GGZznS' 3 o o / 6 l • • - - - — • f^rtc. :ES 3 I6Z. .._...1^3 .^.._I^/ IS 2. ...^JXsl _ J S 3 r£z _ I ^ 3 • • Lcxo?r.. A'^'i _ ..nssnQ^ _. ino?\^%o^ ... i^HMA'.U, 3S3^Lo inoji'^io IZ'i^HQ.O OH 1 see _. g6/2^0. ... nnm^ . . . — . Ujoper AiOil ..^ A.SHQ/J^H- . __<:k8i'_7-9.ie_ ...Al3nilBHA._ .lS3S.C.Bo^^ (^R.3 99-375 ^^in^HZ- z^^^sso AH'^5:JW ._ .3AASS£D .._. ... 304400 STA:;DARD CPZPJ.TI:IG PROCZZLT.Z D a t e : J a n u a r y 1=92 R e v i s i o n : s YES HO H/A ACTIO::: i . i f t h e i n t e r n a l s t a n d a r d a r e a c o u n t i s o u t s i d e t h e umper o r l o w e r l i m i t , f l a g w i t h " j " a l l p o s i t i v e r e s u l t s q u a n t i t a t e d w i t h t h i s i n t e m a l s t a n d a r d . 2. Non-detects associated with IS area counts > 100% should not ba qualified. 3. If. IS area is belov t.he lower limit (< £0%), qualify ail associated non- detects (U values) "J". If extremely low area counts are reported, (< 25%) or if performance exhibits a major abrupt drop off, flag a l l associated non-detects as u.nusable ("R"). 14.2 Are the retention times of the i n t e m a l standards v i t h i n 3 0 seconds of the associated calibration standard? f^i ACTIc::: Professional judgement should be used tc qualify data if the retention times differ by more t.han 30 SBCcr.zz. ^ - " ^ f « t « • t - . i - - » • T ,rT » -T » T r 15.1 Were any field duplicates submitted fcr .. VOA analysis? _ i_J. r^ ACTIO::: compare the reported results .for field duplicates and calculate the r e l a t i v e percent difference. ACTIO::: Any cross variation betveen duplicate results must be addressed in the rsviever narrative. However, if large differences exist, identification of field duplicates should be confirmed by contacting the sampler. 304401 Date: January 1=32 Revision: a YES HO H/A 1.0 iTif'*'' - To-.- — — ...... » ,'U^.i„,»««_- vJ«',~.-»''«'>*0 ' * * * * - • ' ' • • » » « • • M U M • [ - • • • f c M M g a l I I • • • ! • 1.1 Are tha Traffic Rencrt Forms prssent fcr all samples? f ^ _ Its. ACTIO::: if no, contact lab for replacement of missing cr illegible copies. 1.2 Ie tha Traffic -Reports or Lab Narrative indicate a.ny prcclans with sample receipt, ccnciticn cf samples, anaiyticai prcmiems cr special nctaticns affacti-tg the quality ci the data? ACTIO::: if anv samcle analyzed as a soil, ether t-han TCLP." contai-ns £0%-90% vater, all data snouid be flaaged as estimated ("J"). If a soil sampie. ether than TCLT, contains more than 9 0% vater, all data should be q-jaiified as unusaole (R) . £fi _ /%W^.. w.l If sammles vare not iced upon receipt at the laboratcr-.-, flag ail positiva results "J" ano all .-.cn-cetectc "UJ". 2.0 Hcldinr ---«« 2.1 Have any ENA technical holding times, determinec from date cf collecticn to date cf w_^ extraction, been exceeded? . 1 L ^ Conti-hucus extraction cf vater samples fcr EHA analysis must be started vithin seven days of the date of collecticn. Soil/ sediment samoles must ba extractad vithin 7 days of coil ection. Extracts r.ust ba analyzed vit-hin 4 0 days of the date of extraction. 304402 •TANDARD CPZPJ^7Z::G PROCZrJRZ Date: Januar-/ i = 3 2 Revision: 3 Yzi HO ){/T « • • • » T . i i » « w » i i - i « » i i i M • • • • • • • » l ' " (See Traffic Report; Sample late Date ^->>^ Date Data Sampia Matri:i Samoied Received Zirtractad Analyzed ACTIO::: ir tec-hmcal holding times are exceeded. flaa all positive results as estimated ("J") and samoie quantitation limits as estimated "("UJ"), and dooumant in the narrative that holding times vare exceeded. If analvses vsre dene more t.han 14 days tayonc holding"tine, eithar en the first analysis cr upon reanalysis, ihe reviewer must usa prcfessicnai judgement tc determine the reliabilitv cf t.he data and tha effects cf additional'storage on t-he sample results. At a minimum, all results should ba qualified "J", but tha reviewer mav determine that ncn-cstect data are unusaole (j:R")."lf holdi.ng times are exceeaed by more t.-.an IS days, adl non detect data are unusac.e (R) . 1,0 Surrcrstp c^r^verx' '-^rr-r. ^Z' 3-1 Are the ENA Surrogate Reccvery Summaries (Form I I ) present fcr each cf t h e fcllcwing - . a t r i c a s : f^l a. Low Water -^— ' r>i . b . I-ow S o i l -'-' c . Med Sci 304403 STA::DARD z?i.rj\.zzi'z PP.OCZZUP.Z Date: Januar".* 1 = 92 Revision: 3 yrer ^ HO H/A 3.2 Are a l l tha ENA caroies l i s t e d cn t-he a p p r o p r i a t e Surrcgita Recc-er-/ Summaries for eacn cf tha fcllcving marrtmas: a. Low Water f'Yj b . Low Soil j ^ low Soil j _ j ^ y c ACni::; c a l l lab fzr e x p l a n a t i c n / r e s u c m i t t a l s . If r.issinc e a l i v e r a c l e s a r e unavailable, document effect in data assessments. 3.3 Ware c u t l i a r s marked c o r r e c t l y w i t h an a s t e r i s k ? _r^ ACTIO::: c i r c l e a i l o u t l i e r s i n r e d . 3.4 Were t v o or more base-neutral 02, acid surrogate r e c o v e r i e s cut cf s c e c i f i c a t i c n f c r any samcie or method bla.nk? ' £_2 J L I - y s s . vare samples reanalyzed? .; 1 ^ Were matncd bla-nxs raanalyzea? ' ^ h ACTIO::: Z I a l l ENA surrogate r e c o v e r i e s are > 10% but tvo vit.hir. t.-.e base-neutral or acid fraction do not meet SOW 3 p B C « . . « _ — » - . _ . . 5 , , w - a . . f r ' a r - — • — > - . - — I . , ( ^ a — •» « o — r » o » i ^ — ^ » '- — ^ • ^ ^ • - • • _ • ' - . c . ^ ' ^ . . . acid rcmccu—s) ; !• Flao a l l positive r e s u l t s a s estimated ( " J " ) . 2. Flag a l l .non-cetects as estimated d e t e c t i c n limits ("UJ") vhen recoveries a r e l e s s than the lover acceptance l i m i t . 3. If r e c e v e r i e s are g r e a t e r t.han tha upper acceptance limit, do not q u a l i f y non-detects- 304404 3.5 STA::DARD C?ZPJ.TI::G PROCZZL'P.Z Date: Januar-.- 1 = 32 Revision: 3 ^ES y.z H/A If a.ny base-neutral £^ acid surrccate has a recovery ef <io%: 1. Positiva results for tha fraction vith <10% surrogate reccvarv are cualifiad with "J''. 2. Hon-detects for t.hat fraction should ba qualified as unusaale (R) . Profassional judcament snouid be used tc qualify iata tr.at have net-nod blank surrogate recoveries cut cf scecificaticn in both c r f i n a l and rsanaiyses. Checx the i.ttemal standard areas. Are thare a.ny transcritticn/calculation errors between raw data and Form IZ7 . ^ rX^ ACTIO::: I I large errors exist, call lab fcr expianation/resubmittal, make any necessary corrections and document effect in data assessments. Mitr-.'r^ C ~ W V a e ^ T ^ — -r — ^ 4.1 Is tha .Matrix Scike/Matrix Scike Duolicate ^ .-.eccvery Frrm (Form III', present? L A 4.2 •-••«re r.atrix spikes analyzed at tha required frequency fcr eacn cf t-ha fcllcwing matrices: a. Low Water LX. JL. b. Low Soil . i£l- — c. Med Soil ACTIO::: I I any matrix spike data are missing, take the action soecified i-n 3.2 above. r 1 t 304405 Date: January 1 = 32 Revision: 5 ~~~" ~ YES HO HTA" 4.3 How cany EHA spike raccvarias are cutsida. W»tS- Soil2 Q out cf 2: 4.4 Haw many RPD's fcr matrix soike and matri:c spike cupiicata receveries are cutside QC limits? V »••=•- C/-.<ie ~ • • • r • •- ___ cut cf 11 Q cut cf 11 ACTIO::: HO action is taken cr. MS/MSD data a^cr.g. However, using informed professional judgement, tha data reviewer may use t.he matrix spike B.nd. matrix spike duplicate results in conjunction with other QC criteria and determine the need fcr some qualification of t.ha data. 5.0 o i « - v « .--.— •'•'"y Is the Method Elanx Summary {Form IV) present? r" _ ."requency cf Analysis: Has a raaaent/methcd blank analvsis been repcrtcd per 2 0 samples of similar matrix. or con: batch? or concantrcticn level, and fcr each extraction ^ £.3 Has a ENA mathed bl^nk been analyzed fcr v each GC/MS system usad? LlL — — — (See SOW p. b - 53/SV, Section 8.7) ACTIO::: if any method blank data are missing, call lab fcr explanaticn/resucmittal. If not available, usa professional judgement tc determina if the associated sampie data snouid ba qualified. 304406 S .yvnu/%^i; OPZPJ^TI**! PROCZZUZZ Date: J a n u a r y 1=32 R e v i s i o n : 3 YES HO H/A 5.4 Chromatcgrapny: raview the blank riv data - chromatcgrams (RiOsi , quant raoorts cr data system printouts and spectra. Is tha c.trcmatograpnim performance (baseiina stability) for each insrrumant accsotaole for ^. Biyis? • rNi ACTIO::: Usa professional judcament tc datarmi.r-a the effect on the cata- £.0 C-- •< Note: "Water blanks", " d r i l l blanks" and "distilled vater blanks" are validated like any ether sampia and are not used to qualify tha data. Do net confuse them vith t.ha other QC blanks discussed balow. 6.1 Do any method/instrument/reagent blanks have positive results (TCL.and/or'TIC) for ENAs? When applied as describad balow, tha contaminant ccncentraticn in t.hese blanks are multiplied by tha sample diluticn factor and . corractad for t mcistura vnere necessar".'. _jli. 1 1 5.2 Co any tiald/rir.se/ blanks nave positive SNA rasults (TCL and/or TIC)? J:. I-i ACTIO::; prepare a list cf the samples associated with each cf the contaminated blanks. (Attacn a separata snaet.) Note: All field tlank results associated te a particular group of samples (may exceed one per case) rust ba used te qualif"/ data. Blanks may not ba qualified because of contamination in another blank - Field Blanks must be qualified for surrogate, spectral, instrument perfcrmance cr calibraticn QC proeiems. ,0440-7 ii>/w— -~irJwT...lIG PP.OCZZ---t Date: J a n u a r y 1=32 Revision: 3 l i s H-0 H/A ACTIO::; FCIIC-- tna diracticns ir- the table balcv te qualify TCL rasults dua tc contamination. Use the largest value from ail the associated blanks. If gross contamination exists, ail data in t.ha associated sammles should ba qualified as unusacle (R) , Sampia cone 5 cRQL cut < icx bla.nx Sampia cene.«:c:iOL i is< i:x Clank value Sample cone :- CRQL value & >lQx blanx Cemmcn Phthaiata Estars Flaa sammla result vith a "U"; Repcrt CRQL qualify "U" No qualification is needed Sampia cone 5 CRQL Sampia cone < CRQL < but < 5x blank is < 5x blank value Sample cenc > CRQL value & >5 blank value Cthar Contaminants .-.ag sampia rasult Repcrt CRQL a. cualifv "U" No qualification is naeaed .> v..^ ^ > . . vnaivtas c-»aiifiaa ~cr canx ccntaminatic: are s t i l l ecnsidared as "hits" vt;en qualifying for calibration c r t t a r i a . ACTi:::: For TIC ccmpcu.-.ds, if the concentraticn i-n t-hc sampie is less than five times the ccncentraticn in tha most contaminated associatad blank, flaa tha sample data "P." (unusacle). 6.3 Are thare field/rinse/equipmant blanks associated vit-h every sampie? £k ACTIO::: For lev iayei samples, note in data assessment that t h e r e i s no associated field/rinse/equipm.ent blank- Zxcapticn: samples taken frem a drinking vater tap do net have associated field blanks- 304408 SirfJiDA-au CPZPJ^TI"! PP.'DCZ—-.-.Z Date: Ja.nuar.* 1=32 Revision: S vrc HO H/A :£^kL . . • • - . , - . . - • , . » , • - . - ^ l i l t ' 7.1 Are t h e cz/y.z I.-.strumant Perrsrmancs Checx Forms (Fort: V) p r e s e n t for Oecaflucrcmrtpnanvlphestnina (DFTPP)? i ^ 7.2 Are t h e enhanced bar erap-h smectrum and mass/ charge (m/z; l i s t i n c for t-he" DFTPP provided fcr eacn twelve hour snift? J j l 7.3 Has an i.-.strumant parfcrmanca chacx solution been analyzec fcr everv t v a l v e hours cf sampie ^ a n a l y s i s c a r i.nstruman't? r M ^ ^ ACTIO::: L i s t data, lima, l.tstrument IZ, and sampia analyses fcr vnich no associated CZ.HS tuning data are a v a i l a b l e . DATZ TIHE INSTRUHZ^rr SAMPLE :rJHBZP.S ACTIO::: i f l a b cannot prc.'ide missing data. re-^ect ("R") a i l data generated outside an acceptable tvalve hour c a l i b r a t i o n inter^.'ai. ACTIO::: i f mass assignment i s in e r r o r , flag a l l a s s o c i a t e d sampie data as unusaole (R)• 7.4 Have t.ha icn abundances been normalized t c r./z 138? L t l 304409 Date: Januar-.* 1332 Revisicn: s ^ES HO H/A Have t.ha ion acundanca criteria been mat for eacn instrumant usad? LLH ACTIO::: List a l l data which do not meet icn abuncanca c r t t a r i a (attacn a separate sheet). ACTIO::: if ion abundance c r i t e r i a are not met. the Reaion II TPO must ba notified^ 7.5 .\re there any transcrittion/calculaticn errors betvaen mass"lists and" Form Vs? (Checx at l e a s t tvo values cut if errors are found, check mere.) __ 7.7 Have tha apprcpriate number cf significant figuras (tvo) been reported? ' 111 r> ACTIO::: if large errors exist, call lab for expianation/resubmittal, make necessary corrections and document effect in data assessments. 7.S .-.re tha spactra cf tha mass calibration compound acceptacle? ^ jM ACTIO::; use profassional judcament te cetermine vhet.ner associated data should ba accepted, qualified, er re-^ectad. o n — 5 tmma^ ^-«..-... — J T : 5.... , — — » ^ > „ , 1 , , » o , . 8.1 Are the organic Analysis Data sheets (Form I BNA) present vith raquirad header information cn each page, fcr each cf tha fcllcving: a. Samples and/or fractions as appropriate L t l b. Matrix spikes and matrix spike duplicates J i l c. Blanks ij^ 304410 Date: January* 1 = 32 Revisicn: 2 V T C HO H/A 8.2 His GPC Cleanup been perfermsd cn ail soil/ seaimcnt lampie extracts? r^*^ ___ . ACTIO::: I I data suggests that GPC vas not periermea- use prctessional judgement. Make note in "Cmntract Frcoiems/Non-Ccmpliance*. 8.3 Are the E.HA Reccnstructed Icn chromatograms.. the mass spectra for t h e identified compounds, and tha data systam printouts (Quant Reports) includad in tha samoie oackaae fcr each cf the a- Sampias a.nc/cr frhcticns as apprcpriate f^ . — b. Matrix spikes and matrix spike duplicates (Mass spectra not required") JXil- — . — c. Blanxs I ^ . — ACTIO::: if any data are missing, take action specified in 3.2 above. 8.4 Are the resocnse factors shcvn in tha Quant Report? I—1. Jk- — Is chremctccrap.nic parfcrmanca acceptacle viti resoect tc: Easeiine s t a b i l i t y ? Resolution? Peak shape? Full-scale ••graph (attenuation)? O t h e r : ^ _ • CL iX ^f1 — :i ACTIO::: use prefsssional judgement tc determine the acceptability of the data. 304411 STAoiDARD OPiriATIirO PROCZ—«.-.Z Data: January 1=32 Revision: 3 ' T C HO H/A 3.6 Are tha iab-ceneratad standard mass soectra cf i d e n t i f i a c E.NA ccmtounds p r a s e n t fcr eacn sample? r>? ACTIO::: I I my tass s p e c t r a are missir-g, take action specified i n 3.2 abova. if lab does not ganerate t h a i r own standard spectra, cake n o t e in *'Cehtract Problems/ Hon-compiianca««. If spectra are missing, re-^ect a l l p o s i t i v e d a t a . 8.7 Is t h a RRT ef eacn rapcrtad compound vithin COS •RRT u n i t s cf tha stancarc RRT ir. the ccntinuinc -^ c a l i b r a t i o n ? r >< 3.B Are a l l lens present ir. t h e standard mass spectrum at a r e l a t i v e i n t e n s i t y greater t.han v^ 10% a l s o present in t-he sample mass spectrum? i"^ 8.9 Do sampia and standard r e l a t i v e ion i n t e n s i t i e s agree v i t h i n 2C%? r |a ACTIO::: Usa professional judgement t c determina accaptability cf d a t a . If i t i s determined t.hat i n c c r r o c t i d e n t i f i c a t i o n s were made, a l l such data snouid ba re'iectad (R) , flagged "N" (Presumptive evidence cf tha presence cf tha compound) or cna.-.gec t e n e t datectad (U) at the calculated d e t e c t i o n limit- In order t o ba positively i d e n t i f i a d , the data must comply with t.he c r t t a r i a l i s t e d in 8.7 , 0-8, and 8.9. ACTIO::: when sample c a r r y - c v e r i s a p o s s i b i l i t y , prcfessicnai judgement should ba usad t o determine if instrument cross-ccntamination has affected any p o s i t i v a compound i d e n t i f i c a t i o n . 9 . 0 T e n t S t • V ? ^ V T - » a n i - - •*• ^'^ 9.1 Are a i l Ta.ntativeiy I d e n t i f i a d Ccmpound Forms (Form I , Part SJ present: and do l i s t e d TICS includa scan number cr r e t e n t i o n time, estimated ^. q-ualifier? l H 304412 STAlJDARu CPi.-JiTIiro PP.OCZZL.-^ Data: Januar-,* 1 = 32 R e v i s i o n : a VES HO HVA 9.2 Are t h e mass s p e c t r a f c r t.ha t e n t a t i v e l y i - a n t i f i a d ccmpcuncc and a s s o c i a t e d " b e s t match" s p a c t r a i n c l u d a d i.- t.ha sammla p a c k a o e f o r aacn of t h e f c l l c v i n g : a. Samples a.nd/cr f r a c t l c n s a s a p p r c p r i a t e x i i b. Blanks rN, ACTIO::: i f any TIC data a r e missing, take action soacifiad i n 3.2'above. 3.3 Q C ACTIO::; Add.-j::" qualifier if missing. '^"^^^y "^^L compounds (from a.ny fraction; listed as TIC compcuncs (exammle: 1,2-dimethvlbenzene is xylene a vOA TOL - and" should net ba reportad as ., a TIC) 7 *^ jrNj^ ACTIO::: Flag vith "R« any TCL compou-nd listed as a TIC- 9.4 Are all ions present in tha reference mass spectrum vith a relative intensity greater t.han 10% also prasent in t.ha samoie mass spectrum? ill Do TIC and "bast r.atch" standard relative icn .^^ i.ntansitias agrae vithin 2C%? ill. -^CTIO::; Use profassional judgement tc determina accapttbiiit'/ of TIC identifications, ir it is daterminad that an ir.ccrract identification was made, change identification to "unknown" cr to some less specific identification (example: "C3 substitutad benzene") as appropriate. Also, -'hen a ccmpcund is not fcund in any blank, but is a suspected artifact of a common laboratcr-/ contaminant, z^.i result snouid ba cualifiad as unusaole (R). 304413 STANDARD OPx.r.ATi:'! PROw^^^.'..^ Date: January 1392 Revisicn: a YES HO H/A 12.0 T w i i i v - - . . . . n i l - . - - T, m , v < ^ » - - - . . 1« • • 10.1 Are there any transcription/calculation errors in Form I results? Chacx at least t*vo positiva values. Verify t.hat the correct intemal standard. qaantitaticn icn, and RRF were used t a calculate Form I r e s u l t . Here any errors fcund? . _ . f">^ 10.2 Are the CRQLs adjusted ta reflect simple diluticns and, fcr soils, sample moisture? fn ___ ACTIO::: if errors are large, call lab for expianaticn/resubmitthl. make any necessary corrections and document effect in data assessments. ACTION: When a sample is analyzed at mere than one dilution, the lowest CRQLs are used (unless a QC exceedance dictates t-he usa of the higher CRQL data from the diluted sample analysis). Replace ccncentraticns that exceed t-he calibraticn range i-n the original analysis by crossing out the "E" and it*s associated value cn t.he original Form I and sucstituting the data frem the analysis of tha diluted sample- Specify vhich Form I is te be used, then draw a red " X" acrcss the e.ntirs page of all Form I ' s that should not be used, i.-.ciuding any in the summary package- 11.0 Standard;; r>.ta rcc/V?> 11.1 Are the Reccnstr-uctad Icn Chromatograms, and data systam printcuts (Quant, Reports) present for initial and continuing calibration? S2tl — • ACTIO::: if' any calibration standard data are missing, take action specifiad in 3.2 above. 304414 STA}JDARD OPZrATi:iG PROCZZZP.Z Date: January 12 92 Revisicn: 8 YES NO H/A 12.0 GC/M5L "-''-"'•» •" '-ll <i-_,«4-« cr^— tr-" 12.1 Are the i.-.itial Calibration Farms (Form VI) present and compiata for the EHA fraction? f Ki _ ACno::: if any calibraticn standard forms are missing, take action specified in 3.2 above. 12.2 Are response factors stable for SNAs over the coneantraticn ranee of the calibration? (% Relative standard deviation (%RSD) < 30.0%) rKi ACTIO::: circle all outliers in red. NOTZ: Althougn 2 0 BNA compo'unds have a minim*.mc RRF a.nd no maximum '%RSD. t-he technical criteria are the same for all analytes. ACTIO::: if the % RSD is > 3 0.0%, qualify positive results for that analyte "J" and non-detects using professional judgement. When RSD > 90%, flag all non- detect results fcr t-hat analyte R (unusable) . NOTZ: Analytes previously qualified "U" due tc blank contamination are still considered as "hits" vhen qualifying fcr calibration 12.3 Are ail E.NA ccmpound RRFs > 0.05? ijEl.. ACTIO::: circle all outliers in red. ACTION: If any RRF < 0.05 1. "R" all non-detects. 2. "T-° ail positive results. 12.4 Are there any transcription/calculation errcrr in the reporting of average response factors (RRF) or % RSD? (Check at least t*,*o values but if errors >j; are fcund, check more.) L Q ACTIO::: circle Errors in red. 304415 STANDARD CPZRATIITG PROCEZUPJ: Data: January 1232 Revision: s YES HO H/A ACTION: If errors a r e l a r g e , c a l l l i b fcr expla.-.aticr./resuEmittrl. make any necessary c s r r e c t i c n s and note errors in d a t a assessments. 1 3 . 0 G C / y ? C - - - - — - - - '-1^ < v-.».^4 — /••e-^^— xTTTy 13.1 Are t-ha Continuing-calibraticn Forms (Form VII) present and compiata for tha BHA fraction? r T^ 13.2 Has a continuing calibrmticn standard- been analyzed fcr every f-aive hours of sampie .^• analysis, per i.-.strumant? f N ACTION: List balov all sampie analyses that vare not 'vithin twelve hours of a contir.-uing calibraticn analysis for each ir.strument usad. ACTIO::: if any fcr=s are missing cr no continuing calibration standard has been analyzed vithin tvalve hours of every sampia analysis, call lab fcr explanation/ resubmittal. If contir-*uing calibration data are not available, flag all associated sample data as unusacle ("R"). 13.3 Do a.ny semivolatile compounds have a % Difference (% D) between tha Tnitial and centihuir.g RRF -^^ which exceeds the i- 25.0% criteria? -J^ i—1 ACTIO::: circle all outliers in red. ACTIO::: Qualify both positi'/e results and non-detects for t.he outlier compound(s) as estimated (J). When %D is above 90%, reject all non-detects fcr t.hat analyte (R) unusable. 304416 STAKDARD C?ZPJ^TI:TO PROCEZLTJ: Date: January 1392 Revision: s YES HO H/A 13.4 Do any seaivolatila ccmpeunds have a RRF <0.057 fl^'' ACTIO::: circia all outliers in red. ACTION: If PRF <o.0S, qualify as unusable (R) associated non-detects and "J" associated positive values. 13.5 Are there any transcription/calculation errors in the reporting of average response factors (RRF) or \ difference (%D)' between initial and continuing RRFs? (Check at least tvo values ^ but if errors are fcund, checx more). Jtl ACTIO::: circle errers ir. red. A C T I O N : If errors are large, call lab for expianaticn/resubmittal, make any necessary corrections and document effect in data assessments. 1 4 . 0 Ti^t'o*—^! er^«*.M«-^.4.. ^r/s»— irT^—i 14.1 Are the i-nternal standard areas (Form VIII) of every sampie and blank wit-hin t.he upper and- lowar limits (-50% to + 100%) for each continuing y calibraticn? LX. J X ACTIO::: List all the outliers below. Sampia = Internal Std Area Lower Limit Upper Lim: 'lowdto _ S ± ^ j n ^ ^'^ Z2n?.9^ jo2Jj± 3QTO7O fo j ^ Z £ ± ^ ^ o ^ Ti>6 • Z^Bl^^ /03?>5% (Attach additicnal sheets if necessary.) ACTIO::: l. if the i.nternal standard area count is outside the uoper cr lower limit, flag with "J" all positive results and non-detects (U values) quantitated with this i.nternal standard. 304417 ^Icfm/j/e^ ^JLQ_OOO9 3O0S/0 Re JooQ/0 Re .jQoQlo Re 30oC^o2>RS_ 3oo6oQ/^B i^._._ .__ ^ % - • ' - Josvpz / C 203C 1^^303 Z29/^o — — JS3 arsr xsG . - • — , Z ^ Q Z 9 H /67vr6 Zro9'7L /033> S % 7V?^2(^ [003^90 IHGI/O IVMd.G lpo:3^Cfo_ _ 3 04418 STA2:DARD OPERATI::G PROCZZL*RE Datef Januarv 1333 Revision: s YES NO N/A 2. Non-detects associated with. IS areas > 100% should not ba q u a l i f i e d . 3. If tha IS area i s balow t h a lower l i a i t (<50%), qualify a l l a s s o c i a t e d non-datacts • (U-valuas) "J«, If extremely l e v area counts are reportad (<2S%) or i f parfcrmanca e x h i b i t s a major abrupt drop csf, flag a l l associated non-detacts as unusable (R). 14.2 Are tha r e t e n t i o n times of tha i.ntamal s t a n d a r d s vithin 3 0 seconds of t.ha associated c a l i b r a t i o n . . stancard? r yo ACTION: Professional judgement should b e usad t o qualify data if t h e r e t e n t i o n times d i f f e r by more t h a n 30 seconds. 15.0 nei^i r — V P-i 15.1 Were any field duplicates submittad for SNA .^ analysis? LX, A ACTION: Compare the reportad rasults fcr field dupiicatas and calculate the relative percent diffarence. ACTION: Any gross variation between field duplicate rasults must ba addressed in tha reviewer narrative. However, if large diffarencas exist, identification of field duplicates should-:ba confirmad by contacting tha samoler. 304419 m SDG No. 97135 SVOC and Inorganic Checklist 304420 QA/QC Review of Semivolatile Data For Pace Analytical SDG: 97135 November 20, 1997 Holding Times: Samples CSD002RE and CSD003RE were reanalyzed outside the Region II holding time of seven days. The results were qualified as estimated (J). GC/MS Tuning and Mass Calibration: All DFTPP tuning criteria were within control limits. Initial Calibration: All compounds had percent relative standard deviations (%RSD) below 30 % and all relative response factors (RRF) were above 0.05 units. Continuing Calibration: All compounds had percent differences (%D) below 25% and all RRFs were above 0.05 units. Blanks: No target compounds were detected in the method blanks and field blank FBI00797. No sample data were qualified based on the tentatively identified compounds (TIC) detected in the method blank. TICs qualified (A) were rejected as these are identified as aldol condensation products. Intemal Standard Area Summary: All internal standard retention times and area counts were within acceptable limits. Surrogate Recovery: Samples CSD002 and CSD003 had recoveries for 4 acid volatile surrogate compounds below acceptable limits. 2 of these recoveries were below 10% in both samples. The samples were re-extracted and analyzed by the laboratory. The re-extracted samples met all surrogate recovery criteria. Since the results showed disparity, both sets of results were reported by the laboratory. For sample CSD002, results from the re-analyses are acceptable for use and were qualified as estimated (J), if detected and (UJ) if not detected. For sample CSD003, results from the re-analyses were found acceptable for use. All data were qualified as estimated for sample CSD003 RE. Matrix Spike/Matrix Spike Duplicate: MS/MSD samples had all percent recoveries and percent differences within control limits. Compound ID: All reported compounds were correctly identified and quantitated accurately. H:\chemrislc\island\SVOC_QA. doc 304421 SD^; "iliSS SOP NO. -Trf-* Revision iS CLP OROA::J :F DATA -.rviZn* BY: "^^^^^'^ -^ v.T^'<^— Date: Leon^Liiarus. z.-.vircnmental S c i e n t i s t TCXIC and Hazardous Waste Section BY: \ ^ ' y ^ ^ 2 ^ L-<A .^ ^-occ/f Caorge :<^rras. Chemist Tcxic ar.d Haiarccus Waste Section S t e l i c s G c r a c c u n i s / Chemist Tcxic and H a z a r d e d Waste Section CO::CUP.P.ZZ BY: '4.~'.. ' O • ^^ILU Date Kavin .Kubyy _''^^ef ind .Hazzr^tus Waste Section r.rrr.^.X2 EY: \ y ^ ^ l ' : ^ - ^ .Ar^tr-A-^'^ Date: Robert .°unyo.h. Chief Manitcring -Management Branc.-. Jet.... -::^^^z. .4 /7 ^^ ' ^ • ^ " • ' ' • ^ /J.z. / / . '/^/^ / ^ 304422 STANDARD CPZRATINO PROCZZURZ Date: January 1392 Revision: a YES NO N/A PACKAGE C0HPLZ:TZ::Z£S A N D DZIZ-.-ZSABLZS n A) , I siTZ: Jslc(A\ ChemiLo\l 1.0 Data Ccmpieteness and Caliveraoies 1.1 Have a.ny missing daiiveramles baen received . and added t c t.ha data package? I 1 >X _____ ACTION: Call lab fcr expianation/resubmittal cf any n i s s i n g d a l i v e r a a i a s . I I lab cannot prcvida tham, r.cta tha effact cn review of tha package under t.ha "Contract Probiacs/Non-commlianca" section of reviewer n a r r a t i v e . 1.2 Was s.MO CZZ cnacklist i.-.cludad v i t h package? l _ l J L 2-0 Ccver :.art;r ?-:c V ^ - > ^ - - - P 2.1 Is tha Narrative or cover Latter Present? r % _ _ 2.2 Are C^&a. Numbar and/cr SAS number contained in tha Narrative cr ccvar letter? 3.0 Data Va•»•>•-»•.•••<-- .-*.B,-V» .' «r-<- The fcllcwing chacklist is divided i.-.ts three parts. Part A is fillad out if tha data package contains any VOA analyses, ?art 3 fcr any ENA analvses and Part C for Pesticida/PCBs. Does this pacxage ccntainr •. % VOA Data? i i ti BNA Data? j;5; Pesticida/PCB data? S^ Action: ctmpiate corraspondinc parts cf checklist. Data: January Revision: a ^2^ :;o s/A -•0 ! ! ^ f f i r -^a... «.... '•,u..—,« v^, ' » • • • • » I II • , 1.1 Arc tha Traffic Report .^crms present for all samcies? I-l _ i. ACTION: If no, contact lah for raplacement ef missing or i l l e g i b l e c o p i e s . 1.2 :c t.ha Traffic Reports or Lab Narrative i.hiicata any preelams with sampia r e c e i p t , ccnoiticn of samoles. i n a i y t i c a l preelams c r special r.ctaticnc affacti.-.g tha c u a l i t y of tha data? ___ r^^ ACTION: If a.ny sampie analyzed as a soil, other t-han TCLP. contains £01-90% vater, all data snouid ba flagged as estimated ("J") . If a soil sample, ether t.han TCIT, contains more t.han 9 01 vater, all data should be q-califiad as unusaole (R) . ACTION: If samples vare not iced upon receipt at the laboratory, flag all positive results Lnc all .-.cn-cetectc •".'J". 2.1 Have a.ny ENA tachnical holdi--.g times. daterminad from date of collection to date cf extraction, been exceeded? Y Contihucus extrzctich cf vater samples fcr ENA analysis must be started vithin seven days of the cate of collection- Soil/ sediment samples must ba extractad vithin 7 days cf ccilsction. Zxtracts must ba analyzed vit-hin 4 0 days of the date of extraction. 304424 :A:;DARD OPZPATI-IO pp.oczrjp.z Data: J a n u a r y 1332 Revision: 3 fZS ;;0 )l/K — i W ^ o ^ " ' V - . 1 J < — — ' " ' — a <r< • • > « . • • - - - • S a s t l a same l a M.atrii: lata ; ABOled c^mL_kc Soil C^Mo2Rei>L ikL 10 |£2il'^ (See Traffic Report; Date Lah Date R a c e i v a d Zictrtctad ^4^ Data Analyzed _L£li2l37 :.o ACTION: If tsc-nnical holding times are exceeded, flaa all positive results as estimated {"J") and sammle quantitation limits as estimated ("UJ"), and document in the narrative that holding times vare exceeded. If analyses vara C.CT.& more than 14 days cayonc helding" tima. aithar cn the first a.-.aiysis cr upon raanalysis, -he reviewer must usa prcfessicnai judgement te determine the reiiabilitv cf t.ha data and tha effacts cf additional'storage cn t-ha sample results. At a minimum, all results should ba qualified "J**, but tha reviever r.av determine that r.cn-oetect data are u.-.usaoie TR") . If holdi.-.g times are exceeaed by more t.han 22 days, all ncn detect data are unusacle (R) . Surrcrstg c^r-ver^-r f T"«»- :.l Are the ENA Surrccate Reccvery Summaries (Form :i) present fcr each cf the fcllcving .T.atricas: a . Low Wdter b . Low S o i l c . ."led S o i l 304425 J ^ r^L — .'v-> ^.rurvu > .'—i'J^T.-i-J .f .~.OC.:.Z...^ D a t e : Januar*/ 1 3 3 2 Revision: i V f C iZS ;iO .N/A :.2 Are a l l tha SNA carpies l i s t e d on t.he appremriata Surrerata Recc*ery summaries for eacn of tha fcllcving matrtcas: a. Low Water £;;^ b. Low soil £h. c. Low Soil . . j _ j , X ACTIO::: c a n lab fir axplanaticn/resucmitttls. If r.issinc caliveraoies are unavailable, dooumant effact i--. data assessments. 3.2 v«re c u t l i a r s marked correctly v i t h an asterisk? ^^^ ACTIO::: circle all cutliars in red- 2.4 w«re tvo cr mere tase-neutrai 02 acid surrogate rBcc*.*erias cut cf scecif icaticn fcr a.ny samcle or mathed bla.nk? ' JtX^ .. If yes. --are samples reanalyzed? 'X' Were mathed blanxs raanalyzac? J<X ACTIO::: I I a i l BHA surrogate rsccveries are > 10 \ but tvo VIthin the base-reutrzl or acid fractien do net meat SOW specifieati=.-.s, ^;r rhg affscted ^ - ^ - . j . r . . C . - - « • . . - - t » . « . - . ^^^- ccmttuntsi: 1. Plao all positiva results as estimated ("J") . 2. r i a a all non-cetects as estimated detecticn limits. ("UJ"1 vnen reccveriss are less than t.-.e Icvar acceptance limit. 3- If recoveries are greater than tha upper accaotanca limit, do not q-uaiify ncn-detects. 304426 sTA::DA.r... cPzpj^Tiiro PP.OCZ.——."—^ Date: Januar-.- 13 32 Revision: i VES •.;: N/A If any caae-reutral ^j^ acid surrogate has a recovery cf <101: 1. Positiva results fcr tha fractten vith <10^ surrogate recovery are q-califiad wit-h " J " . 2. Non-detacts fcr t.hat fraction should ba qualified as u.-iusaole (R) . Professional judcament sncuid be usad tc qualify data that have cetncd blank surrogate reccverias rsanaiyses. Checx tha i.-.tamal stancard areas- 3.5 Are t.hare a.-.y transcription/calc-ulatien errers ^ batwaen raw data and Form IZ? — lijl ACTIO::; if large errers exist, call lab for expianaticn/resucmitthl, make any necessary corractions and doc-cment effect in data assessments. i » l » « n « i i - r - - > r • • • ! •;.l Is tha .'^.itrix Scike/Matrix Spike Duplicate Recc-.-er-/ .^orm ('orm III*, present? 4,2 '-'ftre matrix spikes a.nalyzed at tha required frequency fcr" es-cr. cf the fcilo-ving matricas: a. Low Water b. Low Soil c. Med Soil vCTIo::: If any r.atrix snike data are r.issing, take the action" soecified in 3-2 above, iii f 1 X _ , i h • - f 1 J x 304427 STA:;DAP.D CPZPATI::I PROOZZL"P-Z Date: January 1332 Revision: a YZS ;;o ^;/A •i. 3 Hsv many BNA spike r a c c ' a r i a s are cutsida H i i ^ SQils c-.:t cf : i O cut cf 02 4.4 Hcv many RPD's for matrix spike a.nd matri:^ spike c u p i i c a t a r a c c v e r i a s are cutside QC o cut cf 11 ACTIO::: S'O action is taken on .".S/KSD data a lens. However, using informad profassional judcament, tha data reviewer may usa tha matrix spike and matrix spike duplicate results in conjunction -vith other QC criteria and datermine tha need fcr some qualification of tha data. . . . . .J r , a 11 III *; Is tha .".2thcd Blanx Summary •'.Term IV', present? _iL "requancy cf A n a l y s i s : Has a reagent/mathed blank analysis been reported per 2 3 samples of similar matrix. or c o n c a n t r c t i c n l e v e l , a.nd fcr each e x t r t c t i c n ^ batch? 5.3 Has a E.NA r.ethcd blank baan analyzed fcr eicn GO/MS system usad? (Ste SOW D. b - cS/SV, Section 8.7) X ACTIO::: if any method blank data are missing, call lab fcr explanaticn/resucmittal. If not available, usa profassio--.al judcement tc determina if the associatad sampie data snouid ba q-ualified. 304428 S.wvitu<-w-\.j OPZ^ATIIiO PP.OCZUZ.^ Date: Januar-/ 13 32 Revision: 3 v r c ZS >iO N/A 5.4 C.hrcmatcgrapn-/: raview t.ha blanx rzv data - c-tremctcgrams (RICs*. , q-cant rapcrts or data system printc-uts anc s p a c t r a . Is tha c.tremategrapnim parfermenca (basaiina s t a b i l i t y } fcr eacn ir.strumant accsotaole f c r B:IAS? Jf^ ACTIO::; 'Jsa professional judgement tc datermtna the effact on t.ha cata. ~ * *- 1 II • • 111 » I I • » « M I I Note: "Water cla-nks" , "drill blanks" a.nd "distilled water blanxs" are validated like any ct.har sampia a-nd are net -used to qualify the data. Oo not ccnf-cse them wit.h t.ta other QC blanks discussed below. 6.1 Da any r.ethcd/i.-.strument/reaaent blanks have pcsitiva results (TCI. and/or'TIC) for SNAs? When applied as describad below, zha contaminant ccncentratie.-. in these blanks are multiplied by tha sample diluticn factor and corractad fcr \ mcistura vnere necessar-.*. _jL 1 1 Ic any :iald/rinse/ tlanks r.ave positive ENA rasults (TCL and/cr TIC, n Xi^ ACTIO::; prepare a l i s t of t.he samples associated with each cf t.he contaminated blanks. (Attacn a separata sneat.) Note: All field "tlank results associatad t e a particular group of samples (may exceed one per case) r.-ust ba used t e qualify data. Blanks r.ay not ba c-.^3lified because of contamination in a'notner blank - ."ield Blanks must ba qualified fcr surrogate, spectrci. i.-.str-cmant paricrmancB cr calibraticn QC prcmiems. 304429 viiw.->_'.., .-.-i.rw%..-.-t«j i-.-.uu———- Date: January 1=32 Revision: 3 ;o };/A ACTIO::; rcllov t.'-.a diracticns ir- the table balov tc qualif-/ TCL r e s u l t s dua tc contaminazicn. Usa the largest value from all zr.a associated blanxs- If gross contamination e x i s t s , all data in tha associatad samoles should ba qualified as unusacla (R) . ;ampia cone 5 CROL :ut < iCx blank Sampia cone cc^OL « is< :;x clank value Sanpia cone > CRQL value & >l0x blanx ^cmmcr. .-ht-ta-ata Bstars n lag sample result - a I I T » i » . Report CRQL i qualify ' " j " No qualificaticn is naeaed Sampia cone 5 c:iQL b'ut < 5x blank Sampia cone c CRQL i is < 5x blank value Sample cone > CRQL value & >S blank value ^..c -...«wa.~...ants .-.ac sampia r e s u l t , 1 W> 4 ^ . Anaivzas —laiifiac No qualification is naeaed cr clanx ccntcmir.a-.-—- are s t i l l ccnsidarea as "hits" for calibration c r t t a r i a - .•hen qua!--/••*- 6.3 concantrcticn in t.he sampie is less than five times t.ha ccncentraticn in tha rest contaminated associated blank, flag tha sample data "P." (unusaole). Are there fiald/rinse/equipmant blanks associatad vit-h every sampie? ACTIO::: For lev level samples, note in data assessnent that t h a r e i s no associated field/rinse/equipmant blank. Zxcapticn: samples ta.*cen from a drinking vater tap do not have associatad field blanks. Ck 304430 STAIiDA-al C?ZPJwTIITI r?.OCZZL.-JI Data: Ji.-.uar.* 1332 Revision: £ •re •:3 NY A v C r r '--TT-:-:— "^---r^--r-^ c-gcx . 1 Are t h e CZ/y.Z I.-.str-cmant Perfcrmcncs Checx Forms (Form V) p r e s e n t for Oacaflucrctrtphanvlphcsenina (DTTPP^? f>l 7.2 Are t h e enhanced bar erapn smectrum and mass/ charga (m/z; listi.ne for the'DFTPP provided fcr eacn twelve hour snift? i2ii 2 Has an i.-.strumant parfcrmanca c.-.acx solution been analyzec fcr every t--aive hours of sample ^ a n a l v s i s c a r i.-.strumant? ^ r'^ ACTIO::: L i s t Cate. zima, i.-.strument IZ, and sampia analyses fcr --nich ne a s s o c i a t e d co/XS tuning data are a v a i i a b l e - DATZ T I K Z IKSTRLZ-nijrr SAMPLZ -NUKBZPJ ACTIO::: I I lab ca.nnct p r c ' i d e missing data. r e j e c t ("R") a i l data generated cutsida an acceptable f-aive hour c a l i b r a t i o n inter-'.'ai. ACTIO::: if mass assignment is in errsr. flag^^all associated sampie data as unusaole (R) . 7.4 Have t.ha icn abundances been nermaiized te m/z isa? ixL 304431 STTClZX^u opzpjwTr.ro PROCZZ*JP>Z Date: Januar-,- 1332 Revision: s ^23 .iO ;i/A ' . S ;-:ave tna icn acundanca c r i t e r i a been met f c r eacn instrument usaa? f^ ACTIO::: L i s t a l l data vhich do not meet i c n abuncanca c r i t e r i a ( a t t a c t a s e p a r a t e sheet) . ACTIO::: if ion abundance c r t t a r i a a r e n o t n e t . the Recion I I TPO m-ust ba n o t i f i e d . "•6 .-.re t h a r e any t r a n s c r i p t i o n / c a i c u l a t i o n e r r e r s catvaen mass l i s t s and Form Vs? (Checx a t l e a s t tvo values cut if e r r e r s are fc-jnc. zir,zcx mere.) f n 7.7 Have t h a a p p r c p r i a t e numcer of s i c n i f i c z r . t figuras (fvo) been reportad? ' J^X 0::; If l i r g e errors e x i s t , c a l l l a b f o r expianation/resubmittal, make necessar-/ corrections and document e f f e c t in data assessments. 7.3 ."-.re tha s p a c t r a cf tha mass c a l i b r a t i c n ccmpound. accaptacia? J ^ / - k W 4 . _ - ' « ; L'sa p r c i a s s i c n a l judgement t e d e t e m i n e vhetnar associatad data snouid be accepted, q-ualifiad, cr r e j e c t e d . ^ * " • - * - • - - " - ' • • - . I T — - - ~ s i % - g H 3.1 Ar« the Organic Analysis Data Sheets (Form I SHA) present --ith requirad header infcrmaticn cn each pace, fcr eacn cf tha fcllcving: a. Samples and/or fractions as a p p r o p r i a t e i l l b. .Matrix spikes and matrix spike d u p l i c a t e s i l l c. Blanks L t l 304432 -lANDARZ CPZRATi::0 PROCZZTP-^ Date: Januar-/ 13 32 Revision: H YZS .O S/A 3.2 r.ts GPC Cleanup baen parfcrmad cn ail soil/ staimcnt sampie extracts? f>.i ____ ACTIO::: I I data suggests that CPC '-as not perrormac. usa protassionai judgement. Make note in "Csntrmct Prcciems/Non-ccmpiiance". 8.3 Are t.he sHA Raccnstrumtad Icn Chromatograms.. tha mass spactrm fcr tha identified compounds, and t.ha cata syBtam printcuts (Quant Reportsj included in the samole cackaoe fcr eacn cf the fcllcvir.-' * " ' a. Samples and/or frsctiens as appropriate 'V b. Matrix spikes and matrix spike duplicates (Mass spectra net required") xil. — —. c. Blanxs ' I ^ . — ACTIO::: II any data are r.issing, take actien spccified in 3.2 above. 8.4 Are the resoonse factors shc-n in the Quant Raport? L_J.. - ^ c.£ Is cnrcmctccrzp.-.ic parfcrmanca accaptaole vit-h respect tc: Baseline stability? LiL- — Resolution? 1X1 — Peak shape? U l - — !%L _ Full-acale "graph (attenuation)? Other: I—1 -^ ACTIO::: 'Jze prefsasicnal judcement tc determine the acceptaoility of t.he data. 304433 a. 6 8 . 7 S.fi -iA.lw/^-r.u OPiivATi:*! PP.OCZZZP.Z Date: Januar-/ 13 32 Revision: 3 YZS -O N/A Are t h e iab-eenerataa s t a n c a r c mass soectra cf I d e n t i f i a c E.NA compc-uncs p r e s e n t fcr aacn s»n=ie? £ ; ^ ACTZO::: If ir.y tass spectra are missir-g, take action spacifiad in 3.2 abova. if lab does not canerate thair own stancard spectra, cake note in "Ccntract Problems/ Non-cemeiianca". If soectra are missinc, re-ject all pcsitiva data. Is tha RRT cf aacn rapcrtcd cemmcund vithin C O S RJIT units cf tha stancarc -R:IT in the cc.-.ti--.uinc ., calibration? ' r > Are all i=ns present in the standard mass spectrum at a relative i---tensity greater t.han ^ 10% also prasent in tha samoie mass Boactr-cm? f >^ . 8.9 DO sampie and standard relative ion i.-.tansities agree vithin 231? Sjl . _ ACTIO::: 'Jsa profassic-.al judgement tc determina accaptaoiiity cf data. If it is determined that incorrect idantif icaticns v«ra made, all such data snouid ba reTectad (R) , flagged "N" (Presumptiva evidence of tha presence cf tha ccmpc-und) or c.-.angec tc net datectad (U) at t.he calculated detecticn limit. I.~. order to ba positively identifiad, the data must comply vith t.he crttaria listed in 8.7, 0.8, and S.9. ACTIO::: when sample carry-cver is a possibility, prcfassicnxl judgamant should ba usad to datermine if instrumant crcss-contaminatisr. has affected any pcsitiva compound idantificaticn. 9 . 0 T e n t "^ — * - ' A 1 V r J ^ r . , ^ , .t i ^ ^ , - - - . « « . . —.J— , — p . , 9-1 Are all Tantativaiy Identifiad Ccmpound Forms (Form I, Part 2) present: and do listed TICs include scan nucber cr retention time, eatimeted concentration and "IN" qualifier? IJl . _ -- ^ 304434 STAI«DARD Z7zXkZZl'Z PRQCZZL--JI Data: Januar-/ 1332 Revision: z YZS .-,-0 N7A 5.2 Are tna mass spectra fcr tha t a n t a t i v a i y idantifiaa ccmpcur.zc and associated "bast match" spactra includad i- t.ha sampia package for eac-- of tha fcllcvine: S.3 LS a. Samples a.nd/cr fractions as apprcpriate x i l b. Blanks r"^ __ ACTIO::: if any TIC data are missing, take actic.n spacifiad ir. 3.2"abov6- ACTIO::; Add.-J::'' qualifier if missing- Are a.ny TOL ccmpeunds (frem a-ny fractien; listed as TIC ccmpcunes (example: 1.2-dimatnylbenzene ii xylene a VOA TOL - -nd' should not ba reported as -^ a Tic;? XXI ACTIO::; riag vith "R" any Td. csmpcund listed as a TIC. 9.4 Are a l l icns prasent in tha reference mass spactrum vith a raiativa i n t e n s i t y greater t.han lot also trasent in t.ha samoie mass suactrum? J l . — • • • Do TIC and "bast r.atct" standard r e l a t i v e icn ^v/ i n t a n s i t i a s agrae vit-hin IZM i l l - ACTID::; 'Jsa profassional judgement tc determina acceptamility of TIC identifications- IJ i t is daterminad that an ir.ccrract identification was made, change identification to "unknown" cr to soma less specific identification (example: "C3 substituted benzene") as apprcpriate. Also, vhen a compc-und i s not fcund in any blank, but is a suspected artifact of a cccmcn laboratcr-/ contaminant, zha result snouid ba qualified as u.nusaoie ( R ) • Q t 304435 Date: January 1332 Revision: s YZS NO H/A 12.C Cfr.eeur.d Cu^r.r*-^---- ^^^^ oa^,-—,»- no*-p^—--- f'-.^.,. 10.1 Are t h a r e any t r a n s c r i p t i o n / c a l c u l a t i o n e r r o r s in Form I r e s u l t s ? Chacx a t l e a s t f-'o p o s i t i v a values. Verify t h a t t h e c o r r a c t i.-.temal standard. q u a n t i t a t i o n ion, and Rjil vare usad t o c a l c u l a t e Form I r e s u l t . Were any errers found? _ _ . f^ 10.2 Are the CRQLs adjusted to reflect saanple dilutions and, for soils, sample moisture? rn ACTION: If errors are large, call lah fcr expianatien/resucmitttl. make any necessary corractions and dccument effect in data assessments. ACTIO::: when a sample is analyzed at mere than one dilution, the lowest c:iQLs are used (unless a QC exceedance dictates t.he usa of tha higher CRQL data frem the diluted sample analysis). Rapiace ccncentraticns t-hat exceed tht calibraticn range i-n t-he original analysis by cressing out the "Z" and it's associated value cn tha original Form I and sucstifuting tha data frem the analysis of tha diluted sample- Specify vnich Form I is te be used, then draw a red " X" acrcss the e.ntirs page of all -^orm I ' s t-hat should not ba used, including any in the summery package. 11.0 stand"*—'"^ nai-a /nr/^c^ 11.1 Are the Reccnstr-ueted Icn Chromatograms, and data system printcuts (Quant, Reports) present for initial and continuing calibration? i H — _ . ACTIO::: I-' any calibraticn standard data are missing, take action specified in.3.2 above. 304436 STA:JDA:ID OPZPATHTO PROCZZZP-Z Data: January 13 32 Revisicn: a ' T C v; 0 ,\VA T W I I I . . , 1 - - - . . - . _ , . _ . 12.1 Are tha l.-.itial Calibration Forms (Fore Vl^ present and compiata fcr t.ha ENA fractien? f K^ _ ACTION: If any calibration standard forms are missing, take action specified in 3.2 above. 12.2 Are response factors stable for EHAs over the concentration range of the calibration? (\ Relative standard deviation (\RSD) < 30.01) rXj ACTIO::: circle all cutliars in red. NOTZ: Althougn 2 0 BNA cc::pcunds have a minim-urn RRF and no maxim-cm "iRSD. the technical criteria are the same for all analytes. ACTION: If the \ RSD is > 3 0.0t, qualify positive results for that analyte "J" and non-detects using professional judgement. Whan RSD > 901, flag all nen- datect results for t-hat analyte R (unusable) . NOTZ: Analytes previously qualified "U" dua to blank contamination are still considered as "hits" vhen qualifying fcr ealibratisn critaria. 12.2 Are ail BNA cempeund RRTs > 0.05? IIL. _ ACTIO::: circle all outliers in red. ACTION: If any RRF < 0.05 1. "R" all non-detects. 2. "J" all positive results. 12.4 Are thare any transcripticn/calculaticn errors in tha reporting of average response factors (RRF) or 1 RSD? (Check at least fvo values but if errers M are found, check more.) —.-.lil _ ACTIO::: circle Errors in red. 304437 STANDARD OPZPJiTIITO PP.0CZZTP.Z Date: January 1292 Revision: s ^ ^ :vO .VA ACTIO::: if errors are l a r g e , c a l l l i b fcr expia.-.aticn/resucmittal. make any necessary c e r r e c t t c n s and note errers in data assessments. 13.0 GC/y? Crnr-- —-— "ii^i—,-4— < T — «f-p-ri 13.1 Are t-he Continuing-calibration Forms (Form vri; present a.nd compiata for tha BHA fraction? r"^ 13.2 Has a contir.ui--.g calibraticn standard- been analyzed fcr every t--aive hours of sampie . • analysis, per i.-.str-cmant? r N ACTION: List belov a l l sample analyses that ---are not -vithin twelve hours of a contir-'uing calibraticn analysis for each instrument -used. ACTIO::: if any forms are missing cr no continuing calibration standard has been analyzed vit.hin f-alve hours of every sample analysis. call lab fcr explanation/ reaubmittal. If ccntin-uing calibration data are not available, flag all associated sample data as unusaole ("R"). 13.3 Do a.ny semivolatile ccmpeunds have a 1 Difference (1 D) between tha Tnitial and continuing RRF y which exceeds t-he T 25.01 c r i t e r i a ? _*—izSl ACTIO::: circle a l l o u t l i e r s in red. ACTID::: Qualify both positive results and non-detects for t.he outlier coopaund(s) as estimated (J). When *D i s above 901, reject a l l non-detects for that analyte (R) unusable. 304438 Si,vvhu.(VAij CPZPATi::! ?ROCZIL.--i Date: January 1392 Revision: a :ZS KO H/A 13.4 Oc any samivolatila ccmpo-unds have a RJIF <o.0£? f> ACTIO::: Clrela all cutliers in red. ACTIO::: if PJir <0.0£, qualify as unusable (R) associated nen-detects and "J" associatad positiva values. 13.5 Are there any transcripticn/calculaticn errors ih t.he reporting cf average response factors (RRFl cr S diffarenca (ID) batwaan initial and centin-uing RRFs? (Chacx at least tvo values ^ but if errers are fcund. cnecx msrej . ''X'' ACTIO::: Cirela errors in red. ACTTON: If errers are large, call lab fcr expianaticn/restibmitt2l, make any necessary cerrsctisns and document effect in data asaassmants. * " ^ ~ - - ' - - — .. — — » — _ M « i i i ' i i r - - 14.1 Are t-ha i--.ternai standard areas (Form VIIi; of every sampie and blank vithin t.he upper a.nd- lower l i m i t s (-501 te + 1001) fsr each eentinuing rXl calibration? ACTIO::: List ail tha cutliars below. Sampia = Internal Std Area Lower Lizit Upptr Litif (Attach additional sheets if necessary.) ACTIO::: l.lf tha i.-.tamal standard area ccunt is cutsida tha uoper cr lower lisit, flag vith "J" all positive results and non-detacts (U values) quantitated with t.his internal standard. 304439 STA::DA:VD OPZRATI::G PROCZZLTJ: Date: Januar*/ 1232 Revision: 3 YZS NO N/A 2. Non-cetects associated with. IS areas > 1001 should not ba qualified. 3. If tha IS area is balow tha lowar lisit (<501), qualify all associated non-datacts • (U-vaiuas) "J", if extreaaiy low area counts ara reportad (<251) or if parforsanca exhibits a major abrupt drop off, flag all aaaociatad non-detacts ax unusable (R). 14.2 Are tha retention times of t.ha i---tamai standards vithin 20 saccncs of tha associated calibration ,, stancard? jr^ _^_ ACTION: Prcfessicnai judcement should ba usad te q-ualify data if tha retention times differ by more than 3 0 seconds. 15.1 W«re any field dupiicatas submittad for SNA analysis? r 1 ____ J^^^ ACTIO::: compare tha reportad rasults fcr field dupiicatas and calculate the relati'.-a percent diffarence. ACTIO::: Any gross variaticn batvaan field duplicate results must ba addressed in tha reviewer narrative. However, if large diffarencas exist, idantificaticn of field d-uplicates should-ia confirmed by contacting tha samoler. 304440 QA/QC Review of TAL Inorganic Data For Pace Analytical SDG: 97135 November 21, 1997 Holding Times: Samples were analyzed within the EPA Region II CLP holding times. Initial and Continuing Calibration Verification: All percent recoveries were within control limits. CRDL Standard for ICP: All compounds had percent recoveries within the Region II control limits. Blanks: Initial and continuing calibrations and preparation blanks had detected analyte levels that were below the CRDLs as required by Region II. Field blank FBI00797 reported 63.7 ug/L of zinc which is above the CRDL. Zinc result in sample SSDOOl was less than five times the amount detected in the field blank. Therefore, the zinc result in sample SSDOOl was rejected as unusable. ICP Interference Check Sample: Cobalt (76.7%) and selenium (68.4%) had percent recoveries outside the control limits. Results for these metals in all samples were qualified as estimated (J). Spike Sample Recovery: Spike recovery for antimony (23.2%) was outside the control limits (75-125%)). Antimony results in all soil samples were qualified as estimated (J). Duplicates: All compounds had percent differences that were acceptable. Laboratory Control Sample: Percent recoveries for beryllium, copper, and manganese were below acceptable criteria in the solid laboratory control sample. The results for these metals were qualified as estimated in all soil samples. Standard Addition Results: No results were quantitated by MSA in this SDG. ICP Serial Dilution: The ICP serial dilution was conducted on sample SSDOOl. Recoveries for calcium (14.3%), potassium (24.4%)), and sodium (60.8%) were above the acceptable level of 10%). Calcium results were qualified estimated (J) in all soil samples with results greater 304441 than the CRDL. Potassium and sodium results in all samples were below the CRDL and therefore, not estimated. Instrument Detection Limit: All IDLs were at or below the CRDLs as required. Percent Solids for Soils: All soil samples had percent solids above the allowable minimum (50%)). H:\chemri sk\island\IN_QA.doc 304442 ^€\cur\d. (2h,crY\i (uA - -Sol Evaluation of Metals Data for "the Contract Laboratory Program (CLP) bzised on SCW. 3/90 (SOP Revision XI) PREPARED BY Hahif Sheikh, Quality Assi DATE Assurance Chemist Toxic and kazardous Waste Section •• i - - - ^ o - ^ s APPROVED BY : Yy -^3% VL!- • < ' ^ ^ \ , - \ L APPROVED BY Ruhyon, Monitoring Managestvent Branch DATE: 1-S Kevin Kubik, Chief Toxic and Hazcundous Wast:e Section DATE: / / " ^ dx 304443 STANDARD -.i^FPJ'^'G P-rcCEGURE Title: Evaluation of hfetals Cata'ivor .liia Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Revision: 11-' 1.0 Socpe 1.1 This procedure is applicable to inorganic data obtained fran contractor laboratories working for Hazcurdous Waste Site Contract Laboratory Program (CLP). 1.2 The data validation is based upsn analytiical and quality assurance requirementis specified in Statement of Work (SCW) 3/90 . 2.0 Responsibilities - Data' reviewers will ccrplete the follcwing tasks as assigned by t Data Review Coordinator: 2.1. For a total review: 2.1.1 Data Assessment - "Total Review-Inorganics*' Checklist Apperi^ix (A.l). The reviewer must answer every question on the chec3clist. 2.1.2 Data T^seafjnvnt - Data Assessment Narrative (Apperf^-ix A.2) The answer on the checklist must match t±ie action in the rarrative (appendix A.2) and on Form I's. Do r a t tase pencil t:o write the narrative. 2.1.3 Contract Non-Cctnpliance - SM3 Report (Rppenrtix A.3) This report is to be conpleted only when a serious contract violation is encoimtered, or upon the request of the Data Validatu-on Task Monitor, or Technical Project Officer (TPO). Forward 5 copies: OT>e each for intemal files, appropriate Regioral TPO, Sample Management Office (SMO) and last two addresses of. Mailing List for IData Reviewers (Appendix A.4). In other cases, all contract violations should be appended to the end of the Dat:a Assessment Narrative (Sec. A.2.2). 2.1-4 CLP Data Assesanent suianary Fonna 2.1.4.1 Appendix A.5 Fill in the total ruirober of analytes ancLIyzed by different ancilyses and the number of amalytes rejected or flcigged as estJjnated due to corresponding quality control criteria- Place an "X" in haxps where analyses were not performed, or criteria do not apply. 2.1.4.2 Appendix A.6 Data reviewer is also required to fill cut Inorganic Regional Data Assessment form (Afpendix A.7) provided by EPA Headquarters. Codes listed on the form will be used to describe the Data Assessment Summary: 304444 STANDARD OPERATING PKXEDURE Title: Evaluation of Metals Dat:a for the Date: Jan. 1992 Contract Laboratory Program Nuntoer: HW-2 Revision: 11 2.1.5 Data Review Lag: It is reoaaaended that each data reviewer should maintain a log i the reviews ccrpleted to include: a. date of start of case revii b.-date of ccnpleticn of case review c. site d. case number e. contract laboratory f. number of sanples g. matrix h. hours worked i- •reviewer's initials 2.1.6 Telephone Reoord Log - the data reviewer should enter the bare facts of inquiry, before initiating amy phone conversation with CLP laboratory. After the case review has been corpleted, mail white copy of Telephone Record Log to the laboratory and pink ccpy tn S^D. File yellow ocpy in the Telephone Record Log folder, and attach a xerox copy of the Telephone Record Log to the caipleted Data Assessment Narrat:ive (Appendix A.2). 2.1.7 Forvarded Paperwork . .'' 2.1.7.1 Upon completion of review, the following are to be forwarded to the Regional Sample Control Center (RSOC) located in the Surveillance and Monitoring Brar£h: a. data package b. completed data assessment checklist (Appendix A.l,origir^al) c. SMO Contract Ccnpiiance Screening (CCS) d. Record of Conmunicatdon (copy) e. CLP Reanalysis Request/Approval Record (original + 3 cx:pies) f. Appendix A.6 (original). 2.1.7.2 Forward 2 copies of ccrpleted Data Assessment Narrative (Appendix A.2) along with 2 copies of the Irorganic Data Assessment Form (Appendix A. 6) and Telephone Record Log , if any,: ene each for appropriate Regional TPO, and the other one to EPA WSL office in Las Vegas. The addresses of TPOs and EPA office in Las Vegas are given in Pjppendix A-4. •' 2.1.8 Filed Paperwsrk - Upon conpletion of review, the following are to be filed within MMB files: a. Two copies of caipleted Data Assessment Narrative (Appendix A.2) each carrying Appendix A. 6. b. Telephone Reoord Log (copy) c. S!/D Report (copy Appendix A-3) d. CLP Reanalysis Rec^estyApproval Record (copy) 304445 STANDARD OPERATING PRDCECURE r . Title: Evaluation of Metals Data for the Data: Jan. 1992 Contract laboratory Program Number: HW-2 Revision: 11 3.0 Data Occpleteness Each data package is checked by a Regional Sanple Cantrol Coordinator (RSSC) for ccnpleteness. A data package is as.s3,Tmed to be cccplebe when' all the deliverables required under the contract are present. If a data package is int:oiplete, the RSSC would call the laboratory for missing document (s). If the laboratory does not respc within a week, S^D and MMB coordinator of Regicn II will be notified. 4.0 Rejection of Data - All values determined to be unacceptable on the IrxDrganic Analys Data Sheet (Form I) must be lined over with a red pencil. As soon as any review critaria causes data to be rejected, that data can be eliminated fran any further revi or consideration. 5.0 Acceptance Criteria - In order that reviews be consistent among reviewers, acceptan criteria as stated in Appendix A.l (pages 4-25) should be used. Additional guidan can be found in the National Inorganic Functional Guidelir>es of October 1, 1989. 6.0 SM3 Contract Coppliance Screening (CCS) - This is intended to aid reviewer in locati any problems, both corrected arxi uncorrected. However, the validation shculd be carri out even if CCS is not present. Resuhniitrtals received frtm laboratory in respor^se CCS must be used by the reviewer. 7.0 Request for RearaLLysis - Cata reviewers must note all items of contract non-compliani within Cata Assessment Narrative. If holding times and sample storage times have not be. exceeded, TPO may request reanalysis if iters of rx3n-catrpliarx:e are critical to da- assessment. Requests are to be made on "CLP Re-Analysis Request/Approval Record". 8.0 Record of Omrniinioation - Provided by the Regional Sanple Control Center (RSCC) to indicate which data packages have been received and are ready to be reviewed. 9.0 Roxmdinc off mmbers - The data reviewer will follow the standard practice. 304446 STANDARD OPERATING PROCEDURE •^gs 4 of 34 Title: Evaluatd.on of Mstals Dat:a for the Contract Laboratory Program Appendix A.l: Data Assessment - Contract Ccnpiiance (Total Review) i:&te: Jan. 1992 Nvmt)er: HW-r2 Revision: 11 a s [ 1 NO N/A A. 1.1 Contract Coppliance Screenina Report (CCS) - Present? ACTICN: If no, ccntact RSCC. A. 1.2 Record of Orrminlcation (from R3C3C) - Present? ACTION: If no, request fran RSCC. A. 1.3 Trip Report - Present and ccrplete? ACTION: If no, contact RSOC for trip report. [ ] X \ A. 1.4 Sample Traffic Report - Present? Legible? ACTTON: If no, request from Regioncd Sanple Control Center (RSCC). A. 1.5 Cover Page - Present? Is cover page properly filled in and signed by the lab manager or the manager's designee? ACTION: If no, prepare Telephone Record Log, and contact Iciboratory. Co numbers of samples correspond to nuabers on Reoord of Cammunication? Do sample numbers on cover page agree with sanple numbers on: (a) Traffic Report Sheet? (b) Form I's? ACTION; If no for any of the above, contact RSCC for clarification. [ 3 [ ] [ ] [ ] [ X ] __ X A 304447 STANDARD OPERATING PKXEDURE Title: Evaluation of Hetals Data for the Contract laboratory Program Appendix A.1: Data Assessjaent - Ccntract Coiplianoe (Ttotal Review) Date: Jan. 1992 Nuntaer: HW-2 Revision: li A.1.6 Form I to rr Yes No N, A. 1.5.1 Are all the Form I through Rarm IX labeled with: Laboratory name? Case/SAS nunber? EPA sanple No.? SDG No.? Contract No.? Correct units? Matrix? ACTION; If no for any of the above, note under Contract Problem/Non-Conpliance section of the "Data Assessment Narratu.ve". A. 1.6.2 Do any conputiation/transcription errors exceed 10% of reportad values on Forms I-IX for: (N3TE: Check all forms against raw data.) (a) all analytes anzdyzed by ICF? (b) all analytes analyzed by GFAA? (c) all analytes analyzed by AA Flame? (d) Mercury? (e) Cyanide? ACTION: If yes, prepare Telephone Log, contact laboratory for corrected data and correct errors with red pencil and initial. ^ X.3 X] Ai X J A. _ J J J i X 304448 STANDARD OPERATING PROCEDURE Title: Evaliiation of Hetals Data for the Contract Laboratory Program Appendix A.l: Data Assesanent - Ccntract Compliance (Total Review) Date; Jan. 1992 Nui±)er; HH^2 Revision: 11 A.1.7 Raw Data A. 1.7.1 Digestion Log* for flame AA/ICP (Form x m ) present? Digestion Log for fumaoe AA Form x m present? Distillation Log for mercury Form x m present? Distillation Log for cyanides Form XHI present? Are pH values (pH<2 for cill metals, pH>12 for cyanide) present? *Weights, dilutdlons ard volumes .used to obtain values. Percent solids calculation present for soils/sediments? Are preparation dates present on sanple preparation logs/bench sheets? A. 1.7.2 Measurement read out record present? ICP Flame AA Fumaoe AA Mercury Cyanides A. 1.7.3 Are eill raw data to support ciU sample anadyses and QC operations present? Legible? Properly Labeled? ACTION: If no for any of the above questions in sections A.l.7.1 through A.1.7.3, write Telephone Record Log and contact laboratory for resubmittals. XSS. J 2<] A 21] A] m NZA A X ] Ax XJ .^- J L 304449 STANDARD OPERATING PRDCECURE Title: Evaluation of Metals for the Contract Date: Jan. 1992 Laboratory Program Number: HW-2 Appendix A.l: Data Assessment - Contract Revisicn: ll-* Conplianoe (Total Review) YES m ^/h A. 1.8 Holding Times - (ciqueous and soil sanples ) (Examine sanple traffic reports eind digestion/distillation logs.) Mercury analysis (28 days) , . exceeded? iJSj cyanide distillation (14 d a y s ) . . . . . exceeded? [ .X ] Other Metals, analysis (6 months). . . . exceeded? [.Aj NOTE: Prepare a list of all sanples and analytes for which holding times have been exceeded. Specify the number of days fran date of collecticn to the date of prepsuration (fran raw data). Attach to checklist. ACTION; If yes, reject (red-line) values less than Instrument Detection Limit (IDL) and flag as estimated (J) the values above IDL ever). though sanple (s) was preserved properly. A. 1.8.2 Is pH of aqueous sanples for: ^ Metals Analysis >2? [ Xl cyanides Analysis <12? [ A ] Action: If yes, flag the associated metals aind cyanides data as estimated. A.1.9 Form I (Final Data) A. 1.9.1 Are all Form I's present and caiplete? IISL] ACTION: If no, prepare tPlpphcaTe record log aind contact laboratory for submittal. A. 1.9.2 Are correct units (ug/1 for waters and mg/kg for soils) , indicated on Form I's? r >^1 Are soil sanple results for each pairameter corrected for . - percent solids? [AsX Are CLLI "less than IDL" values properly ceded with "U"? [_2S] 304450 STANDARD OPERATING F5?DCEDURE Title: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Nunijer: HW-2 Apperxiix A.l: E>ata Assessment - Contract Revision: 11 Compliance (Total Review) XE£ . m NTT Are the correct concentration qualifiers used with . . final data? , f X 1 ACTION: If no for. any of the' above, prepare Telephone Reoord Log, and contact laixDratory for corrected data. A. 1.9.3 Are EPA sanple # s and corresponding laboratory sanple ID # s the same as on the Cover Page, Form I's and .^^ in the raw data? [ A.] Was a brief physical description of sanples given on Form I's? • [ ] X Wcis the dilution of any sanple diluted beyond the requirements of the contract noted on Form I or .^ Form XIV? IxAi ACTION: If no for any of the above, note imder Contract-Problem/Non-Cccplianoe of the"Data Assessment N^u^^ative". A.1.10 Calibration A. 1.10.1 Is record of at least 2 point calibraticn present for ICP analysis? [_Xj Is record of 5 point ccLLibration present for -^ Hg analysis? [ X 1 Is record of 4 point calibration present for: - Flanfi AA? [ ] _ _ Fumaoe AA? [ ] Cyanides? f X 1 X X Is one calibration standard at the CRDL level for ^ all AA (exoept Hg) and cyanides cinalyses? [ j _ijx ACTION: If no for airy of the above, write in the Contract Problem/Non-Oaipl iance section of the "Data Assessment Narrative". 304451 STANDARD OPERATING FRXEXIRE Title: Evaluation of Metals Data for the Contract Laboratory Program Appendix A.l: Data Assessment - Contract Conplianoe (Total Review) Date: Jan. 1992 Nunfcer; KW-2 RevisicHi; 11 YES A. 1.10.2 Is correlaticn coefficient less than 0.995 for: Mercury Analysis? cyanide Analysis? Atomic Absorption Aralysis? ACTION; If yes, flag the associated data as estimated. NOTE; The data validator shall calculate the correlation coefficient using concentrations of the standards cind the corresponding instrument response ( e.g. c±sorbanoe, peak area., peak height, etc.). A.1.10.3 In the instance where less than 4 stand2unis are measured in absorbance (or peeik area, peak height,etc.) mode, are the remaining standards analyzed in concentration mode immediately after calibration within ±10% of the true values? [ ] ACTION; If no, flag the associated data as estimated if standards are not within +10% of true values. Do not flag the data as estimated in linear range indicated by good reoovery of standard (s). NO N/A t2Si X X A.1.11 Form II A (Initial and Continuing Calibration Verification)- A. 1.11.1 Present and complete for every metal and cyanide? Present and ccnplete for AA and ICP v^en both are usad for the same analyte? ACTION; If no for any of the eibove, prepare Telephone Record Log and contact laboratory. A. 1.11.2 Circle on each Form IIA all percent reooveries that are outside the contract windows. Are all calibration standards (initial and continuing) within control limits: Metals- 90-110%R? Jig - 80-120%R? Cyanides- 85-115%R? [X] Cii] [ 3 304452 STANEftRD OPERATING PRDCECURE Title: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 COTpliance (Total Review) _ _ _ _ ACTION; Fleig as estimated (J) a l l positive data (not flacjged with a "U") aneilyzed between a calibration standard with %R between 75-89% (65-79% for Hg; 70-84% for CN) or 111-125% (121-135% for Hg; 116-130% for CN) recovery and nearest good calibration standard. QusLLify results <IDL as estimated (UJ) if the ICV or CCV %R is 75-89% (CN, 70-84% ; HG, 65-79%). Reject (red-line) as unacceptable data if reoovery of the ICV or CCV is outside the range 75-125% (CN, 70-130%; Hg, 65-135%). Qualify five samples can either side of verification staindard cut of control limits. A. 1.11.3 Was continuing calibration performed every 10 sanples . or every 2 hours? C X 1 Was ICV for cyanides distilled? [ X^l ACTION; If no for any of the above, write in the Contract-Prcblem/Non-Coiplianoe section of the "Data Assessment Narrative". A.1.12 Form II B (CRDL Standnrds for AA and ICP) - A. 1.12.1 Was a CRDL standard (CRA) analyzed after initial calibration for all AA metals (except Hg)? [_Xj Was a mid-range calib. verification standard distilled and analyzed for cyanide analysis? [ -A] Was a 2xCRDL ( or 2xinL v*ien IDL>CRDL) aneilyzed (CRI) for each ICP run? f X. (Note: CRI for AL,Ba,Ca,Fe,l^,Na,or K is i>ot required.) ACTION: If no for any of tha above, flag as estimated all data falling within the affected ranges. The affected ranges are: AA Analysis - **True Value + CRDL ICP Analysis - **True Value + 2CRDL OJ Anaaysis - **True Value + 0.5 x True Value. yf- **True value of CRA, CRI or mid-range standard. Substitute IDL for CRDL when IDL > CRDL. Compute the concentration of the missing mid-range standard frem the calibration range. 304453 STANDARD OPERATING PROCEDURE Title: Evaluation of Metals Data for the Contract Laboratory Program Appendix A.l: Data: Assessment - Contract Ccnpiiance (Total Review) Date: Jan. 1992 Number; HW-2 Revisicn: 11 A. 1.12.2 Was CRI analyzed after ICV/ICB and before the final CCV/OCB, and twice every eight hours of ICP run? ACnON: If no, write in Contract PrcbleaVNcn-Cccpliance Section of the "Cata Assessment Neirrative". A. 1.12.3 Circle on each Form IIB all the percent reooveries that are outside the aoceptance windows. Are CRA ard. CRI standards within control limits: Metals 80 - 120%R? Is mid-range standard within control limits: Cyanide 80 - 120%R? X [-£\] [A] ACTION; Flag as estimated all sanple results within the affected range if the recovery of the standard is between 50-79%; flag only positive data within the aif f ected range if the recovery is between 121-150%; reject all data within the affected range if the recovery is less than 50%; reject only positive data within the affected range if the recovery is greater than 150%. C^Jalify 50% of the sanples on either side of CRI standard outside the control limits. Note; Flag or reject the final results only when sanple raw data cure within the affected ranges and the CRDL stamdards are outside the aoceptance windcws. m N/A A.1.13 Form i n (Initial and Cont-JnuiTyT Calibration Blanks) A.1.13.1 Present and ccnplete? For both AA and ICP when both are used for the same analyte? Was an initial calibration bleink analyzed? Vas a continuing calibratian blemk analyzed after every 10 samples or every 2 hours (which ever is more frequent)? CXJ [2x [ J ^ 304454 STANDARD OFERATING PRDCECURE Title: Evaluation otiyttzJjs Data for the Date: Jan. 1992 Contract Lahoratx;!/ :.rcgram Number: HW-2 Appendix A.l; Data Assessment - Ccntract Revision: 11 Ccnpiiance (Total Review) ^ ^ NZA ACTICN; If no, prepare Telephone Reoord Log, contact laboratory and write in the Contract-Problems/ Non-Ccrpliance section of tha "Data Assessnent Naunrative". A. 1.13.2 Circle on each Form I H all calibration blank veilues •that are above CRDL (or 2 x IDL when IDL > CRDL). Are all calibration blanks (when IDLcCRDL) less than or v, equal to the Contract Required Detectirai Limits (CRDLs)? [_Xj Are all calibratian blanks less than two ti"mps ^ Instrument Detection Limit (vhen IDOCRDL)? [ ] X ACTION: If no for ciny of the above, flag as estimated (J) positive sample results when raw sample vcdue is less than or equal to ccilibration blank value analyzed between calibration blcink with value over CUDL (or 2xIDL) and nearest gocd_ calibration blank. Flag five sanples on either side of the calibration blank outside the control limits. A.1.14 FORM III (Preparation Blank) - (Note; The preparation blank for mercury is the same as the calibration blank.) A. 1.14.1 Was one prep, blank analyzed for: each Sanple Delivery Group (SDG)? f X ] each batch of digested sanples? r X l each matrix type? [ ^ 1 both AA and ICP when both are used for ^^^ the same analyte? f /\1 ACTION: If no for any of the above, flag a s estimated (J) all the associated positive data <10 X IDLs for which prep, blank Weis not aralyzed. NOTE: If only one blank was einalyzed for more than 20 sanples, then first 20 sanples cuvilyzed do not have to be fleagged cis estimated (J). 304455 .STANTARD 'OPERATING PROCEDURE Title: Evaluation of Hetals Data for the Date: Jan. 1992 Contract Laboratory ProQjam Nuntaer: HW-2 Appendix A.l: Cata Assessment - Ccntract Revisicsi: 11 diplianoe (Totad. Review) _ _ _ ^ ^ A. 1.14.2 Is concentration of prep, blank val\ie greater than the CRDL when IDL is less than or equal to CRDL? f X ] If yes, is the conoentratJ.on of tha sanple with the least concentrated analyte less than 10 times ^ the prep.blank? [ ] X ACnON: If yes, reject (red-line) all asfvx:iatpri data greater th2in CRDL concentraticn but less than ten times the pri^. blank valine. A. 1.14.3 Is concentration of prep, blank Vcilue (Form III) less v/" than two tiines IDL, when IDL is greater than CRDL? [ ] _£_ ACTION: If no, reject (red-line) all positive sanple results when sanple raw data are less than 10 times the prep, blank value. A.1.14.4 Is concentration of prep, blaink below v/ the negative CRDL? r r\] ACTION: If yes, reject (red-line) all associated sanple results less than lOxCEDL. A. 1.15 Form IV (ICP Interference Check gt^'mple) A.l. 15.1 Present and complete? [_Xj . (NOTE: Not required for furnace AA, flame AA, mercury, cyanide and Ca, Mg, K and Na.) Was ICS aovilyzed at beginning and end of run (or at least twice every 8 hours)? 1 /^l ACTION: If no, flag as estimated (J) all the sanples for which AL, Ca, Fe, or Mg is hi^^er than in ICS. A.1.15.2 Circle all values cn each Form IV that are more than + 20% of true or established mean value. Are all Interference Check Sanple results inside y/ the cantrol limits (+ 20%)? [ ] JjL If no, is concentration of Al, Ca, Fe, or Mg lower than the respective concentration in ICS? [ ] X 304456 STANDARD CPEPATING PROCEDURE Title: Evalijiation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Appendix A.l: Data Assessment - Contract Revision: 11 Compliance (Total Review) _ _ _ _ AcncM: If no, flag as estimated (J) those positive results for which ICS reoovery is between 121-150%; flag all sanple results as estinated if ICS recovery falls within 50-79%; reject (red-line) those .sanple results for which ICS reoovery is less than 50%; if ICS reoovery is above 150%, reject positive results cnly (not flagged with a "U"). A. 1.16 Form V A (Spike<i K:<Tnp1ft Reoovery - Pre-Edgestion/Pre-Distillation)- ( Note: Not required for Ca, Mg, K, and Na (both matrices), Al, and Fe (soil only.) A. 1.16.1 Present and caiplete for: each SDG? f X 1 each matrix type? [_£lJ each cone, range (i.e. low, med., hic^)? f X ] For both AA aind ICP when both are usad for - the same analyte? [ J ', X ACTION: If no for amy of the above, flag as ^-. estimated (J) all the positive data less than four times the spiking levels specified in SCW for which spiked sanple was not analyzed. tcrrs: If one spiked sanple was analyzed fcr more than 20 sanples, then first 20 sanples analyzed do not have to be flagged as estimated (J). "X A. 1.16.2 Was field blank used for spiked sanple? , C___3 ACTION: If yes, flag all positive data less than 4 x spike added as estimated (J) for vAiicii field blank was used as spiked sanple. A. 1.16.3 Circle on eacii Form VA all spike recoveries that are outside control limits (75^ to 125%). Are all recoveries within cantrol limits? [ ] A [ ] K If no, is sanple concentration greater than or equal to four times spDce concentration? 304457 STANDARD OPERATING PSDCEaroE Title: Evaluation of tfetals Data for the Contract laboratory Program Appendix A.l: Data As.'yfv=3npnt - Caitract Coiplianoe (Total Review) Date: Jan. 1992 Number: HW-2 Revisicn; 11 YES ACncM: If yes, disregaLrd spi3ce recoveries for aralytes \i)CGe concentraticns zire greater tham or equal to four times ^ i k e added. If no, circle those analytes on Form V for which sanple conoentration is less than four times the ^ i k e ocnoentration. Are results cutside the ccntrol limits (75-125%) flagged with "N" on Form I's and Form VA? [ ^ A.1.16.4 ACTION; If no, write in the Oontract - Problenv/Non - Caipliance section of "Data Assessment Narrative". Agueous Are any spiJce recoveries: (a) less than 30%? _ (b) between 30-74%? _ (c) between 126-150%? _ (d) greater than 150%? _ ACTICN; If less than 30%, reject all associated aqueous data; if between 30-74%, flag all associated aqueous data as estimated (J); if between 126-150%, flag as estimated (J) all associated aqueous data not flagged with a "U"; if greater than 150%, reject (red-line) all associated aqueous data not flagged with a "U". m N/A (AJ _ (_><j [A] _ i2ii _ A.1.16.5 Soil/Sedimflnt Are any spike recoveries: (a) less than 10%? (b) between 10-74%? (c) between 126-200%? (d) greater than 200%? X [21] r_,j tA] [ X J 304458 STANCftRD OPERATING PROCEDURE Title: Evaliaation of Metals Data for the Contract Laboratory Program Appendix A.l; Data Assessment - Contract Ccirpliance (Total Review) Date: Jan. 1992 Number; HW-2 Revision; 11 US ACTION: If less than 10%, reject all associated data; if between 10-74%, flag jiU f^agnr-j^st^^i data as estimated; if between 126-200%, flag as estinated adl associated data was not flagged with a "U^; if greater than 200%, reject all associated data not flagged with a "U". m N/A A.1.17 A.1.17.1 A.1.17.2 A.l.17.3 Fonn VI (lah Duplicates) Present and caiplete for: each SDG? each matrix type? each concentration range (i.e. low, med-, hi<^)? both AA cind ICP when both aune used for the same ainalyte? AcncN; [ X J [ ] If no for any the above, flag as estimated (J) all the data >CRDL* for which duplicate sanple was not analyzed. Note; 1. If one duplicate sanple was analyzed for more than 20 sanples, then first 20 sanples do not have to be flagged as estimated. 2. If percent solids for soil sanple and its duplicate differ by more than 1%, pr^aare a Form VI for each duplicate paiir, report concentrations in ug/L on wet weic^t basis and calculate RPD or Difference for each analyte. Was field blank xised for duplicate analysis? ACTION; If yes, flag all data >CRDL* as estimated (J) for which field blank was used ais duplicate. Are all values within control limits (RTO 20% or difference <. ^CRDL) ? f ^ If no, are all results outside the cuntiol limits flawed with an * on Form I's and VI? [ ; ACTION: If no, write in the Contract - Problems/Non- Coipliance section of "Data Assessment Narrative". 2S. (Xj JL * Substitute IDL for CRDL when IDL > CRDL. 304459 STANDARD OPERATING PROCEDURE Title: Evaliaation of Metails Data for the Date: Jan. 1992 Contract Laboca±Dry Program Number: P&J-2 Appendix A-1: Data Assesaaent - Ccntract Revision: 11 Compliance (Ttrtal Review) f NOTE: 1. KPD is not calculable for an euvilyte of the saaiple - duplicate pair *4ien both values are less than IDL. 2. If the result of lab duplicate anaLLyzed by GFAA is rejectable due to coefficient of correlation of MSA, anadytical ^ike recovery, or duplicate injections criteria, do not apply precisicm criteria to wipfcslg analyzed by GFAA. A. 1.17.4 Aguecwjs Circle on each Form VI all values that are; RPD > 50%, or Difference > CRDL* Is any RPD greater than 50% where sanple and duplicate are both greater than or equal to 5 times *CRDL? Is any **difference between sanple and duplicate (where sanple and/or duplicate is less than 5x*C3y3L) > 2x*CRDL? m. Mh. X Is any difference** between sanple and duplicate greater than *CRCiL where sanple and/or duplicate is less than • 5 times *CRDL? Q X J ACTION; If yes, flag the associated data as estimated. A.1.17.5 Soil/Sed-imflnt Circle on each Form VI all values that are; RPD > 100%, or Difference > 2 x CRDL* Is any RPD (v^vere sanple and duplicate are both greater than or equal to 5 times *CEDL) : > 100%? f Xl tXj _ * Substitute IDL for CRDL when IDL > CRDL. ** Use absolute values of sanple and duplicate to calculate the difference. 304460 X STANDARD OPERATING PRDCECURE Title: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Number: KW-2 Appendix A.l: Data Assessment - Contract Revision: 11 Compliance (Totad Review) _ _ _ _ ACnaST: If yes, flag the associated data as estimated. A.1.18 Field Duplicates A. 1.18.1 Were field duplicates analyzed? [ ] ACTION; If yes, pr^>are a Form VI for each aqueous field duplicate pair. Prepare a Porm VI for each soil di:plicate pair, if percent solids for sanple aind its duplicate differ by more than 1%; report ccncentraticrjs of soils in ug/1 on wet wei(^t basis and calculate RPDs or Difference for each anailyte. NPTE: 1. Do not calculate RPD when both vailues aure less than IDL. 2. Flag all associated data only for field di43licate pair. A.1.18.2 Aqueous Circle all values on self prepared Form VI for field duplicates that are: RPD > 50%, or Difference > CRDL* Is any RPD greater than 50% where sanple and duplicate . are both greater than or equail to 5 times *CRDL? [ ] A Is any **difference between sample and duplicate greater than *CRDL where sanple and/or duplicate is less thaui y 5 times *CRnL? [ ] A ACTICN; If yes, flag the associated data as estinated. X- * Substitute IDL for CRDL when IDL > CRDL. ** Use absolute values of sanple and duplicate to calculate the difference. • 304461 STANEftRD OPERATING HSDCECURE Title: Evaluation of Metals Cata for the Contract Laboratory Program Appendix A.l: Data Assessment - Ccntract Coiplianoe (Itotal Review) Date: Jan. 1992 Number: HW-2 Revisicn: 11 A.1.18.3 Soil/S^impnt Circle all values on self prepared Form VI for field duplicates that are: RPD >100%, or Difference > 2 x CRDL* Is any RPD (where sanple and dijplicate are both greater than 5 times *CRDL) ; >100%? Is any **difference between sanple aind duplicate (where sample and/or duplicate is less than 5x *CRDL ): >2x *CRDL? ACTTCN; If yes, flaig the atssociated data as estimated. m N/A C ] X X A. 1.19 Fonn VTI (lahnratory Control Sanple) (Note; LCS required for aqueous Hg aind cyanide analyses.) A. 1.19.1 Wcis one LCS prepared and analyzed for: each SDG? each batch sanples digested/distilled? both AA and ICP when both are used for the same analyte? - not tX] [. X ACTION: If no for any of the above, prepeure Tel^±ione Record Log and contact laboratory for submittal of results of ICS. Flag as estimated (J) aill the data for which LCS was not analyzed. NOTE: If only one LCS was ainalyzed for ntare than 20 sanples, then first 20 sanples close to LCS do not have to be flagged as estimated. * Substitute IDL for CRDL when IDL > CRDL. ** Use absolute values of sanple and duplicate to calculate, the difference. 304462 STANDARD OPERATING PROCEDURE Title: Evaduation of Metals Data for the Contract Laboratory Program Appendix A.l: Data Assessment - Ccntract Coiplianoe (Total Review) Date: Jan. 1992 Number: HW-2 Revision: 11 YES NO N/A A. 1.19.2 Aqueous ICS Circle on each Form V H the LCS percent recoveries outside control limits (80 - 120%) exoept for aqueous Ag and Sb. Is any LCS reoovery: less than 50%? between 50% and 79%? between 121% and 150%? greater than 150%? cK: [ ^ [A) [21] ACTION: Less than 50%, reject (red-line) all data; between 50% and 79%, flag all associated data as estimated (J); between 121% and 150%, .flag all positive (not flagged with a "U") results as estimated; greater than 150%, reject all positd.ve results. A.1.19.3 Solid LCS NOTE: 1. 2. If "Found" value of LCS is rejectable due to duplicate injections or analytical spike recovery criteria, regardless of LCS recovery, flag the associated data as estimated (J). If IDL of an analyte is equail to or greater than true Vcilue of LCS, disregard the "Action" below even though LCS is out of control limits. Is ICS "Found" value hi^ier than the cantrol limits on Form V H ? ACTION; . If yes, quadify all atssociated positive data ais estimated. Is LCS "Found" value lower than the Control limits Ol Form VH? ACTTCN; If yes, qualify a l l associated data as estimated. [ ^ X [ ] 304463 STANDARD OPERATING PRDCECURE Title: Evaluation of Metals Data for the Date; Jan. 1992 Contract Laboratory Program Number: HW-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 Caipliance (Total Review) A.1.20 Fonn IX (ICP Serial Dilution) - NcrrE; Serial diluticn anadysis is required only for initial ccncentraticsTs .equal to or greater than 10 x IDL. A. 1.20.1 Was Serial Diluticn anadysis performed for: ., each SDG? [_AJ " each matrix type? C X l each conoentration range (i.e. lew, med.)? [ A \ ] ACTION: If no for any of the above, flag as estimated all the positive data >. lOxIDLs or >. CRDL when lOxIDL <. CRDL for which Serial Diluticsi Analysis was not performed. A. 1.20.2 Was field blank(s) used for Serial Dilution Analysis? F X ] ACTICN; If yes, flag all associated data >. 10 x IDL as estimated (J). If lOxIDL <. CRDL, flag all data >. CRDL- A. 1.20.3 Are results outside control limit flagged with an "E" on Form I's and Form IX when initial concentration on Form IX is equal to 50 times IDL or greater. [_Xj ACTION; If no, write in the Contract-Prcblem/Ncn- Conpliance section of the "Data Assessment Narrative". A. 1.20.4 Circle on each Form IX all percent difference that are outside the cantrol limits for initial concentrations equal to or greater than 10 x IDLs only. Are any % difference values: > 10%? 2^ { ] _ > 100%? [A] 304464 STANDARD OPERATING PROCEDURE Title: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Nundaer: HW-2 Appendix A.l: Data Assessment - Contract Revision: ll Conplianoe (Total Review) _ _ g2K~ ACTTCN; Flag as estimated (J) aill the associated sanple data > lOxIDLe (or > CRDL when lOxIDL < CRDL) for which percent difference is greater than 10% but less than 100%. Reject (red-line) all the ?i«^snri?itpri sanple results equal to or greater than lOxIDLs (or > CRDL vhen lOxIDL < CRDL) for which PD is greater than or equal to 100%. Note: Flag or reject on Form I's only the sanple resiilts whose associated raw data are >: lOxIDL (or >, CRDL when lOxIDIx CRDL) A.1.21 Furnace Atcndc Absortation (AA) QC Analvsis A. 1.21.1 Are duplicate injections preserrt in fumaoe raw data (except during full Method of Standard Addit:ion) for x/ each sanple analyzed by GFAA? [ ] _ X ACTION; If no, reject the data on Form I's for which duplicate injections were not performed. A. 1.21.2 Do the duplicate injection readings agree within 20% •^' Relative Standard Deviation (RSD) or Coefficient of -^ Variation (CV) for concentration greater than CRDL? [ ] ^^ Was a dilution analyzed for sanple with analytical spike recovery less than 40%? ACTTON: If no for any of the above, flag all the associated data as estimated. A A. 1.21.3 Is *2malytical spike recovery cutside the control ^ ^ limits (85-115%) for any sanple? [ 3 £x ACTTON; If yes, flag as estimated the affected sanple results if the recovery is between 10-84%; if the recovery is between 115-200%, flag the ?issnriatiM positive sanple results as estimated; reject the associated sanple results if the recovery is less than 10%; reject positive sanple results if the recovery is greater than 200%. * Analytical spiJce is not required on the pre-digestion spiked sanple. 304465 STANDARD OPERATING PROCEDURE T i t l e : Evaluaticn of Metads Data for t h e Date: Jan. 1992 Coniiract Laboratory Program Nunber: HW-2 Afpendix A . l : Data Assessment - Ccntract Revision: 11 C o m p l i a n c e ( T o t a l R e v i e w ) _ _ _ _ NOTE: Reject or flag the data cnly when the aiffected sanple(s) was not subsequently anadyzed by Method of Standard Addition. A.1.22 Fonn v m (Method of Stand^L^a Mditlon Raaiilta) A.1.22.1 Present? [ ] _X_ If no, is any Form I result coded with "S" or a "+"? [ ] X ACTION: If yes, write request on TelephoTe Record Log cind contact laboratory for submittal of Form VIII. A. 1.22.2 Is coefficient of correlation for MSA less than 0.990 for any sanple? ACTTCN; If yes, reject (red-line) the aLffected data. A. 1.22.4 Wcis proper quantitation procedure followed correctly as outlined in the SCW on page E-23? ACTION: If no, note exception vmder • Contract Prcbleny' Non-Cccpliance secticn of the "Data Assessment Naurrative", and prepare a separate list. * MSA is not required on LCS and prep, blank. A V A. 1.22.3 Was *MSA required for any sanple but not pierformed? -.[ ] "^ Is coefficient of correlation for MSA less than 0.995? [ ] X. Are MSA calculations outside the linear range of the calibratian curve generated at the beginning of the ^^ analytical run? [ ] A ACTION: If yes for any of the above, flaig all the associated data as estimated (J). ><s 304466 STANDARD OHRATING PROCEDURE Title: Evaluation oivMstals Data for the Cate: Jan. 1992 Contract Lc-bor^raujry Program Number: HW-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 Compliance (Total Review) ^ ^ m NTA" A.1.23 Diasolved/Total or morganic/Total Analyteg - A. 1.23.1 Were any analyses performed for dissolved as well as total ancilytes on the same .sanple(s). [_ Were any analyses performed for inorgainic as well as total (orgainic + inorganic) analytes on the same sanple(s)? [_ X NOTE; 1. If yes, pr^aare a list cccparing differences between all dissolved (or inorganic) and total aralytes. Ccnpute the differenoes as a percent of the total analyte only •v*ien dissolved concentraticn is greater than CRDL as well as total concentratioi. 2. Apply the following questions cnly if in- organic (or dissolved ) results are (i) above CRDL, and. (ii) greater than total constituents. 3. At least one prepauration blaink, ICS, and LCS should be aralyzed in each analytical run. A. 1.23.2 Is the conoentraticn of any dissolved (or inorganic) analyte greater than its totail ccnoentratian by nore than 10%? [ ] 2L. A. 1.23.3 Is the conoentration of amy. dissolved (or inorganic) analyte greater tham its total conoentraticn by more than 50%? [ ] ACTION; If more than 10%, flag both dissolved (or inorganic) and total vedues as estimated (J); if more than 50%, reject (red-line) the data for both valiies. A.l.24 FomiJELfild_El5BiSl- (Note: Deajgnata 'Tield Blank** as such on F o m I.) A. 1.24.1 Circle all field blank values on Form I that are greater than CRDL, (or 2 x IDL .when IDL > CRDL). Is field blank concentration less than CRDL (or 2 X IDL when IDL > CRDL) for all parameters y of associated aqueous and soil sanples? [ ] A X 304467 STAND.ARD OPERATING PRDCECURE Title: Evaluation of Metals'Data for the Date: Jan. 1992 Contract Laboratory Program Nunijer: HW-2 Appendix A.l: Data Assesanent - Ccntract Revision: 11 Compliance (Total Review) _ _ ^/^ If no, was field blank value already rejected due to other QC criteria? [ ] /K^ ACTTCN; If no, reject (except field blank results) all associated positive sanple data less than or equal to five times the field blank value. Reject cn Form I's the soil sanple results that when converted to ug/L on wet basis eure less tham or equal to five times the field blank value in ug/L. A.1.25 Form X, XI. X U (Verification of InstniMntal Parameters). A. 1.25.1 Is verification report present for: Instrument Detection Limits (quarterly)? [ A 1 ICP Interelement Correction Factors (annually)? f X 1 ICP T.irvar Ramges (quarterly) ? [_LSJ ACTION; If no, contact TPO of the lab. A.l.25.2 Form X (Instrument Detection Limits) - (Note: IDL is not required for Cyanide.) A. 1.25.2.1 Are IDLs present for: all the analytes? [-X 1 add the instnnnents used? f X 1 For both AA and ICP when both are used for the same y analyte? [ ] /\ ACTTCN; If no for any of the above, prepare Telephcaie Record Log and contact laboratory. A. 1.25.2.2 Is IDL greater than CRDL for any analyte? F A l If yes, is the conoentration on Form I of the sanple analyzed on the instrument vAvase IDL exceeds CRDL, ^ greater than 5 x IDL. [ ] JS:^ 304468 STANDARD QPE.RATTr.'G H^DCEDURE rr: Title: Evaluation of Metals Cata Contract Laboratory Progra:u Appendix A.l: Data Compliance (Total Review) — Contract Cate: Jan. 1992 Number: HW-2 Revision: 11 Action : If no, fla«g as estimated adl vadues less than five tines IDL of the instnnnent vhose IDL exceeds CRDL. iE£ m N/A A.1.25.3 Fom XI (LlnPMir Ranges) . A. 1.25.3.1 Was any sanple result hi^ier than high linear range of ICP. Was any sanple result higher than the hit^^est calibration standard for non-ICP parameters? If yes for any of the aibove, was the sanple diluted to cbtain the result on Form I? [ ) A ACTTON; If no, flag the result reported cn Form I cis estimated (J). A.1.25 Percent Solids of Sedinvpints X- A.1.26.1 Are percent solids in sediment(s): < 50%? < 10%? ACTTON; If yes, qualify avs estimated all the results of a sanple that has per cent solids between 10%-50% (i.e. moisture content between 50%-90%). Reject all tha results of a sanple that has per cent solids less than 10% (i.e. moisture content greater than 90%). NOTE: Reject or flag (J) only the sample results that were not previously rejected or flaged due to other QC criteria. 304469 STANDARD OPERATING PROCEDURE Title: Evaluation of Metals Data for the Contract Laboratory Program Appendix A.2: Cata Assessment Narrative Date: Jan. 1992 Nuntyr: HW-2 Revision: 11 Case# SDG# Contractor ^7/36" Matrix: soil Sit. T^a^d OKmiuLJ Lab nxC-C Avxi/AAA^^Loul^'l'gJ^J^. X 'atar X Rsviower U f ^ O ^ TkAAt^cA- Other A.2.1 Validation Flags- The following flags have been applied in red by the data validator amd must be considered by the data user. J- This flag indicates the result qualified as estdmated Red- Line- A red-line drawn through a sanple result indicates unusablt value. The red-lined data are known to contain significan errors based on documented information and must not be used by the data liser. Fully Dsable Data- The results that do not carry "J" or "red-line" are fully visab] Contractaial Qualifierg- The legend of contractual qualifiers applied by the lab cn Form I's is found on page B-20 of SOW IIMOl.O. A.2.2 The data assessment is given below and on the attached sheets. 304470 STANDARD OPERATING IKXEDURE Title: Evaluation of htetals Data for the Date: Jan. 1992 Contract Laboratary Program v^umber; HW-2 Appendix A.2: Data Assessment Narrative Revisicn: 11 A.2.2 (continuation) 304471 STANDARD OPERATING IROCEDURE Title: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program I^iSxir; HW-2 Appendix A.2: Data Assessment Narrative Revision; 11 A.2.2 (continuation) 304472 STANDARD OPERATING PROCEDURE Title: Evaluaticn of Metals Data for the Date: Jan. 1992 Contract Laboratary Program Number; HW-2 Appendix A-2: EBta Aseesanent Narrative Revision: 11 A.2.3 Contract-ProblenyTfcn-Caiplianoe M-IB/ESAT Rviewer: [ Date: Signature ; jXniJL. ]9<J^.J^-^^^ Date: l^ I'll /^7 Contractor Reviewer _ Signature Verified by: Date: 304473 STANDARD OKRAUNG PRDCEHIRE Title; Evaluation of Metals Data for the Date: Jan. 1992 Contract Labaratory Program Number: HW-2 Appendix A.3: Contract Ncn-Ccoplianoe Revision: 11 (SMO Report) COTIRACT NQN-CEMPLIANCE (SMD REPCRT) Regional Review of Uncontrolled Hazardous Waste Site Contract Laboratory Data Package CASE NO. The hardcopied (laboratory name) _^_ Inorganic data package received at Region II has been reviewed and the quality assurance a performance data summarized. The data reviewed incluied: SI-X) Sample No.: Cone. & Matrix: _ _ _ _ ^ Contract No. ( )_ requires that specjific aralytical work be done and that associated reports be provided by the contractor to the Regions, EMSL-LV, and S^D. T general criteria used to determine the performance were based on an examination of: - Data Ccnpleteness - Duplicate Analysis Results - Matrix Spike Results - Blank Analysis Results - Calibration Standards Results - MSA Results Items of non-ccnpliance with the above contract are described below. Comments; Reviewer's Initial- Date 304474 STANDARD OPIFAIING EROCEIXIRE itle: Eval\:iaticn of Ifetals Data far the contract Laboratary Program Appendix A.4: Mailing List for Data Reviewers Date: Jan. 1992 Number: HH-2 Revision: 11 ira/>Rm>c m ? y j VKTX MrrPKeyt, 1. Vsn>X »«9icr J (ESD) D t t SZATS <«17) «61-4312 CT, KE. >ft, HH, W , v r t 3 1 , iKUVMT. IJft 3 . VSTPK Mgion I I I {C3C) A.-n«pcii«, JO 2KC1 (3C1) 26t-9:i0 EC. r o . PA. VX. V.', DC CM.-r:jK. Ki'o-*.-,, JTC. Wko;. VEJSXR, 5 . USEPA R«;icr. V fEED 53t SaL.-v. c:«rk $tr«rr T«.-rJi n o c r , OC OUCigc. 11. 606^5 Pit QiuTi::* 312-3«3-95ZT IL, u;, t c . K:. CH. V- KIE. XAI/ITC •7. USI?A Ji^qicn M I lASomtary KA.-1SAS City. XS 64115 Deir* Morry (S:3) 236-38il 10. »CS, KB. t o Wjl»ar., >;t.-)fcu Cit>' ScjcTTific E>:tArpTi»*», Eii^lt Pitd^tr ». VSEPA Rjiqicn IX (ESD) 215 n m.-unz SUrart SAn rrmrciAco, Ok 9A\0i (415) 974-0>2« X2. CA, KI, Kif. A,r«rican &&.•»>, Ou«.r: Trust T i m t x i r i a * ol P t c i i i c Itlft.ndx, W4>.« Island AU. CAT WMTLon. S-Cub«l, IT-CX, V«3U l&LPA taqion I I (ESD) WorrfPT-i^ Xv«rx)« Zduon, Mw JmzT*y MI3? (201) 321-*»7* W . Ky. PR. VI Cmrraary, QwBiM:t\, US T>MX, M«.ieD, X7C. CMteon, O S , CAl«cn, 204 UEkU'A Aaqivi TV (ISD) AnfclyticaU gmr^'^ B.*-»-i. Q3ll«9« r u t i o n Aaad A t h w , U 30613 Tor a«.-sTrrt, J r . (4CM) S4t-3112 AL, IX, GA, JQf, » . HC, SC, TH CavoaT^r., EPS, ESE, F K ^ . 7ri4n;l« Lai» vswx »«;icr VI (ESD) Hrnmrrf Ptrfc Plat*, a i d ; . C •i3( HsTTMaoj Criv* KxtKm. TX r7074 Cavid r u O c u r . (713) 153-3425 XR. LA, W., TX, » AW^DDK, JUDIMC, SHTS, n s , Clochgr. PmakTOi. I r e . , 5PL Inc., S^iJC, AlliKl, Y^Ti' TX, HXX USIPA ^ i o n VIII LibBntrcy BOX 25366 Dinv«r radcnU Qvuxr U)u».«od, 03 10225 Ev» Hofto*.-) (303) 236-7371 CD, KD. S3. UT, Wi-, tC AOr, C2CU, R9U., Ctti Otas., Oa.-\mi 10. USEPA K«qian X lahnrmtory P.O. BOX S49 Minc^MUx. Hk 91393 Otzmld RAh {204) 442-0370 AX, XD, Ok, U\ lA\xt\M T w t i n ; L i ^ , Cft.*)tury Trstlrq lAhB (POT VQik crUy), w»y«rr»«ii*tr Ca. ColMrti^ THting, SUv«r Valley 1 1 . Carl* Oe.-pMy - (05-230) USEPA 4C; " r - S t r r r : , S.V. V4*.Mng-.or.. OC 2 « 6 3 rrS 3£2-57<6 13. S*.-;::* fJc^OK-tm Ciiica V.'i.- jL-ri Ccr^a.—/ P.O. EX Ell 12. Etf-mrd Ka.-rtar USEPA D5L-LV 944 E. Karaon Av«.tj« BDX 9347B U s V«gu. »r.' 69119 304475 4 •' \ STANDARD OPERATING PRCCEDURZ tie; Evaluation of MetzQs Data for the Contract Labaratcry Program Apendix A.5: CLP Data Assessnent Sunsnary Form (Inorganics) Date: Jan. 1992 Number: HH-2 Revision: ii y* • ! ktvlvw: t « : C L / ^ Bat.. A/»V CU , l " ) ^ ! M^lcK.'\nd C h er W C A X vi«««r'a I n l t i i l a : U ^ uhtu—i raccL A^^cLX^i-icoJL IhM^r af taafl«*i 5" AwilTt>« t«jtftt< Out te t i f tdlnt t«»lr> CfittTl«!< CT M e l ^ l S f 0 • \ t m t KK 'uTAtCt kX ( t r e u T v .-.t.i cf\; 1 0 6) C i l l k r » t I o n o 0 o ) t h » r 1 1 f r t f l l * n k n t i 4 l l i n k a / o 0 o o I n t t T - f t r t n r t i o X X t ^ l k t o o o D u r l i c a t t t L«blri(i4 o o o X X X 04t*etl«> H a i t i o o 1 o LCJ o 0 0 t<rl«l C l l u t l e n o X. >c HSA Tet«l A n « l T t f 1 K i i ^ X X 1 5- 5" « It Wetlofl ; o O <Ln«lTt«« r ) « n » 4 «t t n i a i t t < ( J ) Pu* to t i t » « 4 t B t C r l t t f l i Ter:* 0 M t » * 4> 1 'uTnact /u <«TturT Total Cf\i 3th»r 0 0 0 0 0 0 0 0 o 0 o \o 0 0 ^ X X 0 X 0 0 X. ^ 0 . 0 0 (2- (:) c? 4 X X 1 X X X /IS- 3 0 c? d Mettt •atarlak. (•} ln41c«tta a441tlanal aict«4aa<aa af ft»lt« c r i t a r i a . 304476 STANDARD OPIRATING PROCEDURE Title; Evaluation of Metals Data for the Contract Laboratary Program Appendix A.6: CLP Data Assessment Qiecklist Inorganic Analysis Date: Jan. 1992 Number: HM-2 Revision: ll CASE NO. INCKGANIC REGIONAL DATA ASSESSMENT Region X SITE XA\{K^(L Clne/yyic&A • LABORATORY l(KcO n y n O - l u A c ^ - NO. OF SAMPLES/ MAIRIX ^/Sail 'INAUA. SDC? sa^/ jLmo'^' 0 REVUHER ( I F NOT ESD) REVIEWER'S NAME ////Tl^ / a t a ^ ^ r DPO: 1. 2. 3 . 4. 5. 6. 7. 8- 9. 10. 1 1 . 12. AcncN ] HOLDING TIMES CAT.TRRATTnN.S BLANKS ICS LCS DUPLICATE ANAL:£SIS MAIRIX SPIKE MSA RFRTAT, DTTITTTCN SAMPU: ViRUlCAIlON OTHER QC OVFRATL AS.STH.'TmTr Ffl X DATA ASSESSMENT SUMMARY ICP o AA OCMPLETICN DATE_ XL PA n. XX XL XX XL XX XL NOV , ^ 1 /"^^7 CYANIDE o XL H O O XL XL XL XL O 0 = Data has no problems/or qualified due to minor problems. M = Data qualified due to major problems. Z = Data unacceptable, X = Problems, but do not affect data. YL ACTION rrms: ' z A c /yjuoi^Uc /\JUt(A i'V^ .4A-wui^ CS>hOO I ^ • • PS^US OF CONCERN: NOTABLE PERFORMANCE: 304477 • SDG No. 97162 VOC Checklist m m 304478 QA/QC Review of Volatile Data For Pace Analytical SDG: 97162 ISLAND CHEMICAL Reviewer: Uma Parasar January 27, 1998 Holding Times: Samples PPl (25'-27'), PP2 (10'-12'), PP3 (24'-26'), PP4 (8'-10'), PP4(21'-23'), andPP4D (2r-23') were re-analyzed outside the Region II holding time often days for soil samples due to intemal standard area counts outside acceptable limits in the original analyses. Both the original and re-analyzed results were included in the data package. The results from the re-analyses were qualified as estimated (J) for the detected compounds and (UJ) for compounds that were not detected. GC/MS Tuning and Mass Calibration: All BFB tuning criteria were within control limits. Initial Calibration: The percent relative standard deviations (%RSD) for methylene chloride were 45.2% and 48%, respectively, in the initial calibrations run on December 11th and December 12th, 1997. Positive detects for methylene chloride in associated samples were qualified as estimated (J). All other compounds had %RSDs below 30 %> and all relative response factors (RRF) were above 0.05 units. Continuing Calibration: The following compounds had percent differences (%iDs) that were greater than 25% in the continuing calibration run on December 19, 1997: Acetone 110.2% 2-Butanone 70.8% 2-Hexanone 55.6% Positive results for acetone in samples FB1210, TB1210, and TB1297 were qualified as estimated (J). Non detect results for 2-butanone in samples FB1210, TB1210, and TB1297 were qualified as estimated (UJ). All other compounds had %Ds below 25%) and all RRFs were above 0.05 units. Blanks: All method blanks associated with both aqueous and soil analyses reported elevated concentrations ofmethylene chloride. Methylene chloride data in all samples were qualified as not detected based on method blank contamination. 304479 Field blanks were associated with the soil samples only. Field blanks 1297, 1208, and 1203 reported acetone at concentrations of 310, 120, and 98 micrograms per liter (ug/L), respectively. Acetone results in samples 121820, 122224, 131820, 132426, BAST12, and P12527 were qualified as not detected based on field blank contamination. Field blanks also reported concentrations of methylene chloride but samples were already qualified based on method blanks. Field blank FB1203 reported toluene at a concentration of 1 ug/L. Toluene detected in associated samples PI2527 RE and P21012 RE were qualified as not detected (U). The following tentatively identified compounds (TIC) were rejected in all samples based on being laboratory artifacts: l,l,2-trichloro-l,2-ethane, unknown hydrocarbon (retention time: 17.67), and carbon dioxide. Three trip blanks were collected along with the soil samples. They were not used to evaluate blank contamination. Trip blanks reported low concentrations ofmethylene chloride, acetone, and toluene. Intemal Standard Area Summary: Intemal standard area counts were below acceptable limits in the initial analyses of samples P12527, P21012, P30810, P32426, P42123, and PD2123. Samples P30810 and P21012 reported recoveries that were below 25%) of the acceptable limit for bromochloromethane, and therefore data associated with this intemal standard were rejected. Sample P30810 was re-analyzed the same day and reported recoveries that were unacceptable, but higher than 25%) of the acceptable limit. The remaining samples were re-analyzed outside holding time. The intemal standard recoveries in the re-analyses were within acceptable limits. All other intemal standard retention times and area counts were acceptable. Surrogate Recovery: All surrogate recoveries were acceptable. Matrix Spike/Matrix Spike Duplicate: The recoveries for 1,1-dichloroethene were above acceptable limits in one MS/MSD pair evaluated for the soil samples. No data were qualified based on MS/MSD data alone. All other percent recoveries and percent differences were within control limits in all MS/MSD samples. Compound ID: All reported compounds were correctly identified and quantitated accurately. Field Duplicates: Three soil field duplicates were collected in this data set. The data were compared and the relative percent differences calculated. Chloroform was detected in samples PP5 and PP5D at concentrations that differed by 128%. The validity of the identification of the replicate was confirmed with the sampling personnel. No data were qualified as per the guidelines. 3 0 4 ^ 80 Re-analyses/Dilutions: The following is a tabulation of the samples that were re-analyzed or diluted in this data set with an explanation of which analyses is better representative for further use. Sample P1212527 (PPl 25-27) P21012 (PP2 10-12) P30810(PP3 8-10) P32426 (PP3 24-26) P40810(PP4 8-10) P42123 (PP4 21-23) PD2123(PP4D 21-23) P11113 (PPl 11-13) RE/DL RE RE RE RE RE RE RE DL Reason Low IS area counts Low IS area counts Low IS area counts Low IS area counts Low IS area counts Low IS area counts Low IS area counts Acetone out of range Data Set To Use Re-analyses' Re-analyses Re-analyses^ Re-analyses Re-analyses'* Re-analyses Re-analyses'* Initial analyses RE - Re-analyses DL= Dilution IS = Intemal Standard ' Sample was re-analyzed outside holding time. IS area counts in re-analyses were acceptable. Chloroform was detected in re-analyses only. •^ Sample was re-analyzed outside holding time. IS area counts in initial analyses were severely low requiring rejection of data. IS area counts in re-analyses were acceptable. Chloroform was detected in re-analyses only. Sample was re-analyzed within holding time. IS area counts in initial analyses were severely low requiring rejection of data. IS area counts in re-analyses were not acceptable but required only estimation of data. '' Sample was re-analyzed outside holding time. IS area counts in re-analyses were acceptable. Sample was re-mn at a dilution due to acetone concentrations exceeding the calibration range. Acetone was outside the calibration range in the re-analyses also. Acetone result in this sample is qualified EJ to account for the uncertainty of the result. G\stafI\uparas\DVMEMO\971621C_VOC 304481 SOP NO. 'ry;—o Revision ?a C—r 0.-.UAJI~ '.~ DA'.r/-. ••.:.\'J. — Tx '\ \ . Leon Liiaru-s. I.v Tcxzc 3.-:d .Hazartcus Wasre Secric: ..A. BY: ^^""^^Jx y^ ^ 2—L^ .^. /^y ^ - ^ z .•"- 1 - ^ A CXI ^- -a *-» ri vr , Wasze £ec-::icr. Kevin .Kub;J::. -_"^£r Date: Ji!^^.. — ^'/-/Z_ Date ^r-iv C e o r r s :<-l'rris. C h e m i s i rcxic 2.-C .Hz2artcu3 Wasra Sectirr. / 7 .-'/?5^; Zate; 5teiic3 Garazou.-.zs/ c.'isnisi. Date: 2-2Tct.us Wasza SacTlcn r\e rr.^-i v .;L_; Date: // MW_Z- / / RotTHr- .^.unyo.n, C.'ii.ei H o n i i c r i r . c .'^.i.naceme.n-:: Hrznc." / 304482 S i.^vNui_r^.D CPi.r'..ATrZ^I3 ?HOC.i_w.-^-i. Dat£: J a n u a r y 1392 R a v i s i c n : S YES >Io H/A 1-0 Data CccclsTier.ess and Caliveraoies 1.1 Have any r.issinc dslivericles bean received .^ and addad rc zT.z cara cac>:ace? i 1 ^ ACTir::: call lab f::r expl2.naT:icr./resut=:i--2l of any nissir.c daliveraclas. II lab canncr provide tham, .-.era -che effacr cn review cf tha packaoe under zha "CZ7*z.rzzrz Prcblams/Non-CcmcliancE" saczicn cf reviewer narrzTiva. 1.2 Was sy.a CZ^ c.-.acXlisz i.-cludad virh pacXace? : 1 JL. 2-0 Ccver '_£-':sr STG-N'^—-rtvg 2.1 Is rha N'arra-iva or caver Larrar Fresenr? f^ 2.2 Arc Case NurJzar and/or SAS nur±:er ccr.zained x^ in tha Narra*iva cr Caver letter? i 1 -J— The fcllcvine chacXlisr is divided intc three carrs. Parr A is filled ouz if tha data package contains any VOA analvses. ."arx B fcr any EHA analyses and Farr C fcr Pssricida/PCHs. Does t.Ms packaoe conzainr VOA Data? Xf!l. — Y B-KA Data? -Ci - w o >(^ c» CO Pesriciia/PCH data? - } 5 iwi>D/T_r\ij —.-i.T'.AT—• Iw f ~.wC———•'—i- Date: Jinua—,' 1332 Revisicn: S _ _ _ _ _ PI'S" 1 . i'ni IMITVCT-^ T T - S - ' - ' - — Oai-i, r ,--! T , V,.--..,..--. — • v;^ .r-—-••^•••••0 • • " ' • " • ^ i l i r n - T » « » ....- — ^ . _ , • - _ I - 1.1 Are rhe Traffic -Reccrr: Fores presenc fcr i 1 Y". all sacples? ACTIcri; If T.c. ccr.zzcz lab fcr r3i3iac£cenr. of zissinc cr illeqidle ccp.ies- 1-2 Do the Traffic P.spcrrc or L-ab Harrc-cive indica-E i.ny prcbians vit-h sanple receipt, conditicn cf sanples. analytical problens or special cirrurstances affecting' the cuality of the data? _ Acnc::: if any sanple analyzed as a soil. other't.'-.an" TCL?, contains 50\-9QX vater, all data should be flagged as estirated (J) , If a soil sanple ot.'-.Er than TCI? contains -ere than 90% vater, all data sncuid be qualified as u.-.usable (?0 • ACTICrr; If sanples vare .",ct iced upon receipt at t.'-.e laboratcr-/, flag all positive results "J"' and all Hon- Detects '"JJ". ACTICN: If both VGA vials fcr a sanple have air bubbles-or the VOA vial analyzed had air tubties, flag all positive results "J" a.nd all ncn-detects "P.". iX 304484 STAXDAJID O?Z?JVTI::G ??.0CZZ*J7JE: D a t e : J a n u a r - / 1S92 R e v i s i c n : s YES .SO .S7A 2 . 0 1 *J -' - * — rr> J . Hgl^-Tl Have any VOA t a c h n i c a l holdi.-.g t i e e s . d e t e r e — . e d f r c n d a t e cf c o l l e c t i o n t c 2 . 1 Have a d e t e m a n a l y s i s , b e e n e x c e e d e d ? I f unpreser-.'eri d a t e cf X r 1 e c , ac-ceous s a n c l e s c a i . ' - . t a i n e d a t 4 * C v h i c h a r e t c be a n a l y z e d f c r a r c r a t i c . V / d r c c a r c c n s n u s t b e a n a l v z e d v i t h i n TZ ^" ^ = ' - ^ - ' - = - ' '-' preser-.-ed v i t h HCl •(p.4<2i and s t o r e d a t 4 C^ t h e n a q u e o u s s a n c l e s r u s t b e a n a l y z e d v i t h i n 14 d a y s ^ c f c o l l e c t i c n . I f u n c e r t a i n a b c u t p r e s e r v a t i o n , c c n t a c t s a n p . e r t c d e t e r c i n e w h e t h e r c r n e t s a n p l e s v a r e p r e s e r v e d . The h o l d i n g t i r e f c r s o i l s i s 10 d a v s . I i ^ • c - ^ ~ \ t ^ T - - ' - - v ^ ^ . , > . - - . S a n p i a S a n p i a ID .Matrix i'Pi(2.Ao,i')f^e"'so\'L P P x ( i o ' - i 3 j f i £ PPL, ( 8'-'0 (KB P r £ s e r".' e d ? N O (See Traffic -Repcrt; Date Date Lab Date Sanded Received Analvred ' A A l^jA\9j ^ ^ L OJ o 00 Ul t\\Lx ^.1 II t£ posit quant the n analy tinia"', the r deter addit all r deter holdi chn; i-.-E - — -1 •" arr; ses ei svi :su V th ew e al It e al holding tites are exceeded, flag all ssults as estinated ("J") and sanple CT. iinits as esti-ated ("UJ") , and docunent ive that holding tines vere exceeded- • If ere done nore than 14 days beyond holding er cn t.^.e first analysis'or upon re-enalysi er rust use prcfessicnai judgement to the reliability of the data and the effects storage on t.'-.e sanple results- At a nininu s nust'be qualif ied" "J" , but. the reviewer r. t.'-.at ncn-detect data are unusable (R) . If res are exceeded b-.''Tncre r-'^n i~ Have: aii o: av Date: J a n u a r ' / 1S32 R e v i s i c n : S HO N7A W I i r r T i " 1 . ^ . . - - - • - - . . - , ~ - ^ . . . — ......., . ^ _ . . . , . , - » ' V . i . f a i n i » l 3.1 Arc the VCA S>{C Recc-.-ery Sunnaries (Fom II") present for each ct the fcllcving ratrices: a- Lev Water '^ ^^ b. Lov Scil f XT c. Med Scil '' "i 3-2 Are all the VOA sanples listed cn the apprcpriate Systen Mcnitcring ccnpeund Reccvery Snr.nary fcr each of t.'-.e fcllcving r.atrices: a. Lov Water iJx. b. Lov Soil rX^ __«. c "ed c^'ii r 1 ____ ACT*"''!" ^ r > ' , ^ •< ^ K - - - pxz^'^ 2.^ •* ^ • — / resucrittals- If r.issi.ng deliveracles are unavailable. docurant effect in data assessne.nts- 3.3 Were cutliars narked ccrrectl'/ vith an y asterisk? i—1 ACTIC".: Circle all outliers in red- 3-4 Was one cr rcre VOA systen ncnitcring contc'cnd reccvery cutside cf ccntract specifications fcr a.ny sanple cr nethod xir bla.nk? If yes, vere sanples re-analyzed? L_l - ^ Were nethcd blanks re-analyaed? L—1 — ' - 304486 S.:-O^DAR.D 3PXP-ATZli>-i x-.-.OC: -vj;. Date: J a n u a r - / 1 = 32 R e v i s i o n : s " \ YZS HO H/A ACnD:J: I f r e c e v e r i e s a r e > 101 b u t 1 c r n o r e cetrpcunds f a i l t e n e e t SD'n s p e c i f i c a t i o n s : 1- A l l p o s i t i v e r e s u l t s a r e q u a l i f i e d a s e s t i r a t e d ( J ^ . 2 . " l a g a i l . - . c n - c e t e c t c a s e s t i r a t e d d e t e c t i c n U n i t s ( " U J " ) v h e r e rec=-.-ery i s l e a s t h a n t h e l e v e r a c e a p t a n c e U n i t . 3 - I f s k c r e c e - . - e r i E s a r e a b o v e a i l c v a h l e l e v e l s , de n o t q - c a l i f y n e n - d e t e c t s . I f any s y s t e n n c n i t c r i n g ccnpeund recc-.-ery i s < 1 0 1 : 1- F l a g a l l p o s i t i v e r e s u l t s a s e s t i r a t e d " ("J"^ . 2 . F l a a a l l n c n - d e t e c t s a s u n u s a b l e ( " R " ) . Profassional judeenent should be usad tc qcalifv data that cnly have nethcd blank sy.C raccveries cu: of specification in botn criginal and ra-ar.alyses. Checx t.-.a internal standard areas. 3-5 Are there a.ny transcripticn/calculaticn errors betveen rav data and Fcrr 117 ACTIC::: If large errers exist, call lab fcr explanaticn^resubnittal, rake a.ny necessary ccrrectiens and note errors in the data assessnent. lA _ -t . u I r g J»» a n ^ r- « • I - ' - - I f ^ m » A. 4 . 1 I s t h e .Matrix S p i k e / M a t r i x S p i k e Duplicate Reccverv Fcrr (Forr I I I ) p r e s e n t ? ,y. 304487 STAKDARJ: CRZRATI^'D PROCZZL-RZ Date: Januar-/ 1392 Revisicn: s YZS HO H/A 4.2 Were n a t r i x s p i k e s a.nalvzed a t t h e r e c u i r a d f r e q u e n c y f c r eacc =f t.he f c l l c v i n g r a t r i c a s : a. Lov Water -i -^^^ 5" At^.^w^pl^ ^y<) b . Ucv s o i l 3 /Y15/r»^7> j c \ -Xl A6i^yfi€^- f ^ c- Med S o i l r i ^v.!..,:;: zz any r . a t r i x spike d a t a a r e r . i s s i n g , t a k e t-he a c t i c n s p a c i f i a d i n 3.2 a b o v e . 4.3 .Mov n a n y VOA spike r e c o v e r i e s a r e o u t s i d e QC l i n i t s ? Hi^sx s o i l s ^ out cf 10 J out cf 10 4.4 Hov nany RPD's fcr r a t r i x s c i k e and r a t r i x s e i k e d u p l i c a t e r e c c v e r i a s a r e c u t s i d a QC l i r i t s ? Water c«-<-; i > ; • • • . » » O out cf £ I o u t CI £ AV..LIJ::: .\'O a c t i c n is taken b a s e d cn MS/HSD d a t a a l o n e . Hovever, u s i n g i.-.ferred p r c f E s s i o n a l j u d g e n e n t , t.he MS/KSD r e s u l t s nay fce used i n c e n j u n c t i e n w i t h e t h e r -^C c r i t a r i a t e d e t e m n e t h e need f c r ~ - q u a l i f i c a t i c n of t h a d a t a . 3 , Blanks ^ ^ — - ^-^ 5.1 I S t.he Mathed Elank Sunnary (Fort: IV) p r e s e n t ? ' ry^i -•2 Frequenc-/ of A n a l y s i s : for t.he a . n a l y s i s of VOA TCL cz-ccur.cs, has a r e a g e n t / n e t h e d b l a n k b e e n analyced fcr each SDC o r e v e r y 3 0 4 4 8 8 20 s a n p l e s or s l n i l a r r a t r i x (IcV v a t e r , " l e v s o i l , - a d i u r s c i i ) , v n i c h e v e r i s . n c r e ^^ frecruent? STAKDAR.D CPZPJwTIKC PR0CZZ'J7JZ D a t e : J a n u a r y 1332 R e v i s i c n : 3 YZS HO K/A 5.3 .Mas a VOA n e t h c d / i n s t r - c r e n t b l a n k b e e n a n a l y z e d a t l e a s t c.-.ce e v e r y t v e l v e h o u r s f o r eacn c c n c e n t r a t i c n l e v e l and GC/HS s v s t e n usad? sX Acrrz::: i r a.ny r a t h e d blank data a r e n i s s i n g , c a l l l a b f o r ax-planatien/ r a s u e n i t t a l - I f ret.hcd hla.nx data a r e n e t a v a i l a b l e , r e n e c t (R) a l l a s s o c i a t e d p o s i t i v e d a t a . However, u s i n g p r c f e s s i c n a i j u d g e n e n t , t h e d a t a r a v i e v e r ray E U t s t i f u t a f i e l d b l a n k or t r i p b l a n k data f c r r i s s i n g zzR-chcd b l a n k d a t a . 5.4 Chrcrategrapn-y: r e v i e v t h e blank r a v d a t a - c h r c r a t c g r a n s (RICs), qcant r e p o r t s o r d a t a s y s t e n p r i n t c u t s and s e e c t r a . I s tha c h r c r a t c g r a p h i c p e r f c r r a n c e ( b a s e l i n e stacilit-.-) for VOAs? 1.-^.., ^^^ eacn i n s t f c r a n t a c c e n t a b l e iX 4 n u i .1 •Jse e r c f a s s i c n a l iudeanent t c 5 . 0 6 . 1 6 . 2 d e t e m i n e t n e e f f e c t cn t h e d a t a . c o p t i r - ~ a t ; c - "Water blanks", "drill blanks", and distilled vater blanxs" are validated like any other sample, and are not -sed tc q-calify data. Jo'net ccnfuse tham vith the ct.her QC blanks Hiscussad balov. Do any r.ethcd/instr-crent/reagent blanks have positive results (TCL and/or'TIC) for VOAs? When applied as describad balov, the contani.nant ccncentraticn in these blanks are nulticlied bv t.he sanele diluticn facter and corractad for % ncistura vnen necessary. X<. Do a.ny f i e l d / t r i p / r i n s a blanks have p o s i t i v e . ^ VOA r e s u l t s (TCL a n d / o r TIC)? * / V Prepare a l i s t cf t h a sanples a s s o c i a t e d vit-h eacn c: t h a c e n t a n n a t e d iilankc /it-.*--.— - r 1 r 1 U) o 00 fiiz^d /Sfa'vvic PBi20^^7 h^odode^d ga^w^pieA: Ac.<2iALz. 3:io&£: 1 ^ - 7 - 0 .SfbLP 2. C^'" ' ^ ' ) S&fi.ST l l . p 7^er(.A.i_£yM_X- / J" FllLd. f^io^yAL Ff6'^o2^~i f^e.A\Ljiov\^ ct^L&^^^ ^ e>^ 9<3 huouioAcd SoiA^Y m PPLi ( " g - (o') ??± [ l l ~ ' ^ ^ PP± (35'-517') f P ^ (/o'-ys^O 6/5A6r io(i^-'^o) 6e>hST M (»g-3o) vSBA^T /( (30-3?.) S^/V^r /3 (18-So) PPb3> ( d . A ' ^ ^ ' ) 304490 PrtfX^' i O P Ps M l ^ d BtCwuc NoJkA. ^;f6LKio± ^^/n/c^i M ^ K u ^ U ^ Cia(Wd^ 3 ^ - k^4,0iiAi<A ^CWvY'LU : fe>}GL03 m IA; 8-575" [/M i^'-« (^ 1' 5^)] Tt^lX03 rk\xv<^ ' "-^^ . . - TIC - LA.r\Kr^auyn. H C ( ^ n - ^ 7 ) S^o-S /'PI (25'-Z7') 7FX (io ' / i ) PPX ( ^ B ' - l s O ?P3 ^^ (8'- /^O ? P ' 5 ( 2 q ' - : i 4 ) PP ^^ (-i^-S'- /oO ?P^ (ai-P^30 P P ^ i ^ (;^i- ;i-5) m ' 304491 6^-3.5;) - 2.^<rr\i # ^/S^cXcc -R^ ^ (?WVU? Lu : S6A5T ix(^is'-2D^ ?PZ/-^ (a/'Z3)^e PP^(liA2>0'^L Pn(zA-^7^R(B ^^-^ (10'-17') RE ^P3C^Ao.(J)fiG (V[tHy^oL%Lc^^ ^SiX V/^LkL?, l^ll(ol^-j huou(\Xce{ Aot/vw^lu: SftASr /of/§-:it?) 6P)LP 1 (z^-'iv'J) 6/^/\Sr /I (as-^o';) ^'^^^ ^ (S-'-/oj) S/6hSr 13 (I'd'-20) 5feLP z (g-'_,c5J) PP6 ( 2 S - s o 3 6/5L/^ 'i (/3'-/5'; PAtrAOcL f ^ t c v ^ iAJaJ<j. l/^Lkh/a / a / / ^ / ^ 7 _ Not-^VOUGU^I • kUoAOAtd. l(X/v\A^iUx : 304492 r n ,^^ ^ (^ "^ U) o STA^'DARD CPZPATIh'C RROCZZL'RZ D a t e : J a n u a r y 1332 R e v i s i c n : 8 YZS HO H/A NOTZ: A l l f i e l d b l a n k r e s u l t s a s s o c i a t e d t e a p a r t i e - e l a r g r o u p of s a n p l e s ( r a y e x c e e d one c e r c a s e ) r - a s r b e u s e d t c q u a l i f y d a t a . T r i p b l a n k s a r e u s e d t e q u a l i f y o n l y t h e s e s a m p l e s v i t h v h i c h t h e y v e r e s h i p p e d a.nd a r e n o t r a o r u i r e d f c r n e n - a o u e o u s r . a t r i c a s . B l a n k s r a y n e t b e c - . : a l i f i e d b e c a u s e of c c n t a r i n a t i c n i n a n o t h e r bla.nk. F i e l d B l a n k s i T r i p Bla.nks r u s t b e q - c a l i f i e d f c r s y s t e r r c n i t c r i n g c e r p c u n d , i . n s t m i r e n t p e r f c r r a n c e c r i t e r i a , s p e c t r a l o r c a l i b r a t i c n QC p r e b l e n s . F o l l c v n-he d i r e c t i o n s i n t-he t a b l e belov- t e q - c a l i f y TCL r e s u l t s d u e t e c e n t a n i n a t i c n . Usa t.he l a r g e s t v a l u e f r c n a l l t h e a s s o c i a t e d b l a . n k s . I f a n y b l a n k s a r e c r e s s i y c e n t a n i n a t e d , a l l a s s o c i a t e d d a t a s h o u l d be q c a l i f i e d a s u . n u s a b l e (R) . S a n p l e c e n c ? CRQL S a m p l e c e n c < CRQL S a m p l e c e n c > CRQL b u t < l o x b l a n k i < i o x b l a n k v a l u e i > i o x b l a n k v a l u e v a l u e . M e t h y l e n e - c r i c e F l a g s a n p i a r e s u l t R e p c r t CRQL k No q - c a l i f i c a t i c n A c e t c n e v i t h a " i j ; q u a l i f y "'J" i s n e e d e d T o l u e n e 2 - = u t a n c n e s a n p l e c e n c ? CRQL S a m p l e c e n c < CRQL i S a m p l e c e n c > CRQL b u t < £x b l a n k i s < 5x bla.nk v a l u e v a l u e & > 5x b l a n k v a l u e O t h e r F l a g sa.npie r e s u l t R e p o r t CRQL a No q u a l i f i c a t i o n C e n t e r . - w i t h a "12" q u a l i f y "U" i s n e e d e d i . n a n t s NOTZ: A n a l y t e s q - - : a l i f i e d "U" f o r b l a n k c e n t a n i n a t i c n a r e s t i l l c c n s ' i d a r s d a s " h i t s " v h e n q-caldfying f c r c a l i b r a t i c n c r i t e r i a . STAKDARD 0~Z?-A7r!TC PROCZZURZ Date: J a n u a r y 1392 Revisicn: a YES HO N/A ACrrch': For TIC ccnpcunds, i f t h e c c n c e n t r a t i c n i n t-he sample i s l e s s than f i v e t i m e s t-he c e n c s n t r a t i e n i n t h e n e s t centaninated a s s o c i a t e d blank. H a g t h e samnle data "?." ( u n u s a b l e ) . ^ , „ ^ ^,^At. 6.2 Are t h e r e f i a l d / r i n c e / e a u i e r e n t bla.nks 'S^^-f'-^ ^ S . r ^ ^ ' t associated vith ever%- samcie? J L ^ ^ ^ L ^ P H T ^ ACTID::: For l e v level sanples. n o t e in data assessnent t-hat t h e r e i s no associated f i e l d / r i n s e / e q u i p n e n t blank. Exception: samples taken fret: a drinking v a t e r t a p do n e t .have associated f i e l d blanks. 7 . 1 Are t h e GC/>{S Instrunenr Perferranca Check Forms (Forr V) present f c r Sromeflucrctcnzene (BFE)? l A l 7.2 Are t.he ennanced bar graph s p e c t r c r and nass/c.harca (r/2* l i s t i n g f c r t.he EF3 prc-.'ided far each tvalve hcur s.nift? i X l Has an i n s t r c r e n t perfemar.ce ccnpeund been analyzed fcr every f - a i v e hours of sample a n a l y s i s per instrument? 304494 STA:;DARD C?Z?.ATI:IG RRDCZZZTJI Date: January 13 32 Revision: S YZS HO H/A ACTIc::: List date, time, i-nstr-crent ID, and sample analysis for vhich ne associated bz/y.s tuning data, are available.- DATZ TIIDZ IHSTRL-:MZ>rr SAHPIZ ^-UHEZR ACTION: If lab cannot provide nissing data, reject ("R") all data generated cutside an acceetable tvalve hcur calibration i.ntcr\'al. 7.4 Have the icn acundances been ncrraliced tc "./z 35? OO. nCTUN: If rass assicnrent is in errcr, cu^iiiy s l l associated data as unusable (R). 7.5 Have t h e ien abundance c r i t e r i a been net fcr each instr-crent used? X2iL ACTICN: List a l l drta vhich d= n e t r e e t icn abunda.nce c r i t e r i a ( a t t a c h a separate s h e e t ) . ; o ACTION: If icn abundance c r i t e r i a are net |^ n e t , the Regicn I I TRO .rust tn be n o t i f i e d . 7.5 Are t h e r e any t r a n s c r i p t i c n / c a l c u l a t i c n e r r e r s betveen r.ass l i s t s and'Form Vs? (Check at l e a s t tvo v a l u e s but if errers are fcund, check . -=re.) . jjL. UJ o STAJJDARD C~Z~_\TI1TD RROCZZITRZ Date: Januar-/ 1332 R e v i s i o n : S YES HO H/A 7.7 Have t h e a p p r c p r i a t e number cf s i c n i f i c a - h t fig-ores (fwo) been, r e p o r t e d ? FAl ACTION: I f l a r g e e r r o r s e x i s t , c a l l l a b f c r e x p l a n a t i e n / r e s x i e n i t t a l , r a k e • n e c e s s a r - / c c r r e c t i e n s and dec-enent e f f a c t i n data a s s a s s n e n t s . r & 7.3 Are t.he s p e c t r a of t h e nass c a l i b r a t i c n ccnpcund a c c e p t a b l e ? ACTION: Use p r c f e s s i c n a i judgenent t e d e t e m n e v h e t h e r a s s o c i a t e d d a t a s h o u l d be accepted, q u a l i f i e d , c r r e j e c t a d . 8.1 Are rha Organic Analysis Data Sheets (Forr I VOA) present vit.h requirad .header inferratien cn each pace, fcr eacn cf the fcllcving: a. Samples and/cr fracticns as apprcpriate Xii b. Matrix spikes and ratrix spike ^^ duplicates I" ^ c. Blanks rXl « • 3.2 Are the VOA Reccnstruetad Icn Chrcratcgrans, the nass spectra fcr the identified ccmpeunds, and the data system printcuts (Quant Reports) included in the sannle eackace fcr each of t.ha fcllcving? a. Samcies and/or fracticns as apprcpriate j ^ b- Matrix spi.kes and natrix spike dumlicates (Mass soectra not ranuired) SXl c- aianks . i2ll ACTIO:.': If any data are nissing, take acticn seecifiad i.n 3.2 above. Date: J^nuazr/ 13 3 2 R e v i s i o n : 3 ~ ~ ~ Yzi HO H/A 8.3 Are the response factors shc-m in t-he Quant R«pcrt? I 1 X 8.4 I s C h r c r a t c g r a p h i c p e r f c r r a n c e a c c e p t a b l e v i t h r e s p e c t t c : Baseiina stabilit*.-? '' ^ R a s o i u t i c n ? X^. Peak shape? ^^"^ F u l l - s c a l e crap.h ( a t t e n u a t i c n ) ? ^XT- Other: ^ '' . ACTION: Use p r o f e s s i o n a l judgenent t c d e t e m n e t h e a c c e p t a b i l i t y of t.he d a t a . Are the l a b - g e n e r a t e d s t a n d a r d nass s p e c t r a of tha i d e n t i f i e d VCA cenpeuncc p r e s e n t f c r eacn sanpia? l3cX ACTION: I f any r.ass s p e c t r a a r e n i s s i n g , t a k e a c t i c n s p e c i f i e d in 3.2 abovc- i r l a b d e e s n o t g e n e r a t e t h e i r cvn s t a n d a r d s p e c t r a , .take note in " C o n t r a c t P r c b l e n s / K o n - c c n p i i a n c e " . B-6 I s tha PJIT cf each r e p o r t e d ccnpeund vit-hin 0.06 FJ^T u n i t s cf t h e s t a n d a r d RRT in t h e c o n t i n u i n g c a l i b r a t i o n ? 8.7 Are a i l i o n s p r e s e n t i.n t h e s t a n d a r d r.ass spectrum a t a" r e l a t i v e i n t e n s i t y g r e a t e r t h a n IZX a l s o p r e s e n t i n t h e sanple nass s p e c t r t r ? X jVx, 304497 ^ A.^-ii-i/xR.D 0?i..rLATHiC f-ROCZZL-"-:. Date: Januar-/ 13 32 Revisicn: S YES HO H/A 8-8 Do sample and s t a n d a r d r e l a t i v e ion i n t e n s i t i e s agree v i t h i n 2 0*7 rX; ACTICK: Use p r o f e s s i o n a l judgement t c d e t e m n e a c c e p t a b i l i t y of data- If i t is d e t e r m i n e d t h a t i n c o r r e c t i d e n t i f i c a t i o n s v e r e made, a l l such- data sncuid be r e j e c t e d (R), flagged "N" (presurpti-.-e e v i d e n c e of t h e presence cf .the ccmpccnd) c r changed t e net d e t e c t e d (U) a t t h e c a l c u l a t e d d e t e c t i c n l i m i t . In order t e be p o s i t i v e l y i d e n t i f i e d , t h e data r u s t cempiy v i t h t h e c r i t a r i a l i s t e d i n 8 - 6 , 8 . 7 , and S . 8 , ACTION: When sample c a r r y - o v e r i s a p o s s i b i l i t ' / , p r c f e s s i c n a i judgenent should be used t e d e t e r m i n e if i n s t r t r e n t c r e s s - c e n t a n i n a t i c n has affectad any p e s i t i ' / e ccnpeund i d e n t i f i c a t i c n - 0 " ^ e n f - * - * ? 1 V "^-" •= •n r •• -^ ••• o-^ C .— —.- —-I5 / — " r - l 9.1 Are a l l Tantati'/ely Identified Ccmpcu.nd Forms (Form I Part B) present: and do listed TICs include scan number or r e t e n t i o n time, y e s t i r a t e d ccncentraticn and "JM" qualifier? 'Ai « ^__ 9.2 Are t.he r.ass spectra fcr the. tentatively identified compe-unds and associated "best ratch" spectra included i.n the sample package for each of the folloving: a. Samples and/cr fracticns as apprcpriate /"Xl b. Blanks IXX ACTION: If any TIC data are missing, take acticn specified in 3.2 above. 304498 ACTION: Add "JN" cualifier if rissirir- STANDARD O^ZFJ^TING PROCZZLIIZ Date: January 1332 R e v i s i c n : S YZS HO H/A 9.3 Are any TCL ccmpeunds (frem any fractien) l i s t e d as TIC ccmpeunds (exammle: 1,2- dimet.hylbenzene ik xvlene- a VOA TCL analyte - and should" net ba reported as a TIC) 7 J^I. •"'-•'• ——••'• ^ ~2.c '-Ith "R" inv TCL cereeund l i s t e d as a TIZ- 5.4 Are a l l icns present in the reference nass spectr-cr v i t h a relati-.-e intensit-/ greater than 101 also cresent in the samcle nass spectr-cm? " ' jXl 5.5 Do TIC and "best ratch" standard r e l a t i v e ion i . n t e n s i t i e s agree wit-hin 20\7 I ^ ACTIO.N: Use prcfessicnai judgement t e d e t e m i n e accaetability of TIC i d e n t i f i c a t i c n s - If i t i s d e t e m n e d t.hat an i n c e r r a c t ide.ntificaticn vas made, change some l e s s specific i d e n t i f i c a t i o n (example: "C3 s u b s t i t u t a d benze.ne") as apprcpriate- Also, vhen a cempeund i s not fcund in any blank, but i s d e t e c t e d in a sample and i-§_ a suspected a r t i f a c t of a cemmcn laboratcry contaminant, t-he r e s u l t should be q u a l i f i e d as " unusable (R) . ( i . e . Commen Lab Contaminants: CO^ (M/Z 44), Siloxanes (M/Z 73) Hexane. Aldol Concensatich Products, Solvent Preservatives, and r e l a t e d by products - see Functicnal Guidelines f o r mere guidance). 304499 STA::DAR.D OPZ?J.TINO PROCZZLTLZ D a t e : J a n u a r y 1332 R e v i s i c n : a YES HO .\'/A ^ ° - ° '^gr-IrP-':: C-:2ht:T-rlcn -^-^ ^grrcrt^d D°r.gcticn L i l . . . 1 - p 10-1 Are t h e r e a.ny t r a n s c r i r t i c n / c a l c u l a t i c n e r r e r s i.n F c r r I r e s u l t s ? C^-.ec^ a t l e a s t f - o pcsiti-.-a v a l u e s . Verifv t-hat t.he c o r r e c t i n t e r n a l s t a n c a r d , q c a n t i t a t i c n i c n , and PJU vare used t c c a l c u l a t e Fcrr I r e s u l t . W«re any e r r e r s fcund? pXa 10.2 Are t h e CRQLs a d j u s t e d t e r e f l e c t s a m p l e d i l u t i c n s and, f c r s o i l s , sample n a i s t - e r e ? f^' ACTION: If e r r e r s a r e l a r g e , c a l l l a b f c r e x p i a n a t i c n / r e s u b m i t t a l , r a k e any n e c e s s a r y c c r r e c t i e n s and n o t e e r r e r s u n d e r " C c n c l u s i c n s " . ACTION: When a sample i s analyzed a t mere t h a n one d i l u t i c n , t.he l e v a s t CRQLs a r e u s e d ( u n l e s s a QC exceedanca d i c t a t e s t h a u s e of t.he hig.her CRQL data frem t.ha d i l u t e d sample a n a l y s i s ) . Replace c c n c e n t r a t i c n s t-hat exceed t h e c a l i b r a t i c n r a n g e i n t h e o r i g i n a l a n a l y s i s by c r e s s i n g c u t t.he "Z" and i t s a s s o c i a t e d v a l u e cn t-he o r i g i n a l Form I and s u b s t i f c t i n g t.he d a t a frem t.he a n a l y s i s of t.he d i l u t e d s a m p l e . Specif-/ which Form I i s t e be used, t.hen d r a v a CO o red "X" a c r c s s 1Sie e n t i r e cane of a l l Form rf^ o I's that should not be used, including a.ny 1 1 in t-he summary package. o 1-0 • standard?^ n^t?. (C-c/y.^) 1 1 . 1 Are the R e c e n s t r - c c t a d Icn C h r e n a t o g r a m s , and data s y s t e m p r i n t o u t s (Quant. R e p o r t s ) p r e s e n t f o r i . n i t i a l and e e n t i n u i n g c a l i b r a t i c n ? rX^ ACTION: I f any c a l i b r a t i c n s t a n d a r d d a t a a r e n i s s i n g , t a k e a c t i c n s p e c i f i e d i.n • 3.2 a b o v e - STANDA:ID OPEPJiTINu PROCZZL-RZ Date: Januar-/ 1352 R e v i s i o n : s YES HO N/A 12-0- 12.1 Are the Initial Calibraticn Forms (Form VI) present and cemplete for tha volatile fractich at cencentrations of 10, 20, 50, 130, 200 ug/1? Are thare senarate calibraticns fcr lev vater/med coils and law soil sammles? rX; If any calibraticn standard fcrrs are nissine, take acticn specified in 3.2 above. 12.2 Were all lev level soil standards, blanks and samples analyzed by heated purge? rX^ kCT^DN: If iz-j level soil samples vere not heated durine purga, q-calify positive hits "J" and ncn-detects 12.3 Are raspcnse factors stable fcr VGA's over the cencantration range of t.he calibraticn (\Relative standard Deviatien (%RSD) <30.0^ )? rX^ ACTION: Circle all cutliers in red. .NOTZ; Although 11 VOA ccmpeunds have a ninir-cm RR? ana ne maximum tRSD, the technical critaria are the same fcr all analytes. U) ACTION: If \RSD > 30.01, qualify associated p c s i t i v a results fer t h a t analyte "J" and ncn-detects. : o using professional judgement. When RSD > 9 0%, m flag a l l nen-d^tects fcr t-hat analyte R (unusable), o NOTE: Analytes previously qualified "U" fer blank centaninaticn are s t i l l considered as " h i t s " vhen c-ualifying fcr i n i t i a l calibraticn c r i t a r i a . 12.4 Are tha RRFs above 0.05? i2jL ., Acticn: circle a l l o u t l i e r s in red- Acticn: If any RRF are < o.05, q-jalify associated non-detects (R) and flag' associated ecsitive data as estimated (J). STANDARD OPZRATIKG PROCZZL'RZ Date: Januar-/ 1=92 Revision: 8 •> '"; YES NO H/A 1 2 - 5 Arc t h a r e any t r a n s c r i p t i c n / c a l c u l a t i c n e r r e r s i n t h a r e p o r t i n g o ; a v e r a c e r e s o c n s e f a c t e r s (RUT) or IRSD? (Check a t l e a s t 2 v a l u e s , b u t , , if e r r o r s are fcund, chec^fz mere.) ^7% G C / y ^ ^ ' - - . i < i - i — / • - - > — • ' — • 1 3 . 1 Are t h e e e n t i n u i n g C a l i b r a t i c n F c r r s (Form VII) p r e s e n t - a n d c e m e l e t e f c r t h e v o l a t i l e f r a c t i e n ? " f)<J 1 3 . 2 Has a e e n t i n u i n g c a l i b r a t i c n s t a n d a r d baen a n a l y z e d f c r everv f - c l v e h e u r s of / sample a n a l y s i s per i n s t m i m e n t ? f/>^ ACTICN: L i s t balov a l l s a m p l e a n a l y s e s t.hat v a r e not vit-hin f - ' a l v e h e u r s cf t h e p r e v i c u s c c n t i n - i n g c a l i b r a t i c n a n a l v s i s . CJ o ^^I"IJN': ZI any fcrrs are nissing cr ne eentinuing , o calibraticn standard has baen analyzed vithin tvalve ' lo hours of every sanple analysis, call lab fcr explanaticn/resubmit-al- If continuing calibraticn data arc net available, flag a l l associated sample data as u.nusable ("R"). 13.3 De any volatile ccmpeunds have a k Diffarence (1 D) betveen the i n i t i a l and eentinuing .^ RRF vhich exceeds the ± 251 c r i t a r i a ? ' A i _ l ACTICJI: Circia ail outliers i-n red- -ACTIQN: Qualify both pesiti'.'e results and non-dstects fcr t.he o u t l i e r ccnpeune(s) as estirated- When % D is above 901, reject a l l • STAI'iDARD 0~.L.-_\TIliG .r.-.DC.:_Z---.Z D a t e : Januar-/ 1392 R e v i s i c n : S YES HO H/A 13.4 Do any v o l a t i l e cerpcmds have a RRF <Q.05? ^ 1 X ACTICN: C i r c l e a i l c u t l i e r s i n r e d . ACTION: I f t.he PJIF <3.05, qualif-/ a s s o c i a t e d n o n - d e t e c t s as u n u s a b l e (R) and "J" a s s o c i a t e d t c s i t i ' / e v a l u e s . 13.5 Are t h e r e any t r a n s c r i p t i c n / c a l c u l a t i c n e r r o r s i n t h e r s p c r t i n g of a v e r a g e r e s p o n s e f a c t o r s (PJIF) cr ^difference (ID) b e t v e e n i n i t i a l and eentinuing RJRFs? {cr^eck a t l e a s t tvo v a l u e s but i f e r r o r s a r e fc'-ind, ^ check m e r e . ) LcX- ACTION: C i r c l e e r r e r s in r e d . o ACTION: If errers are larce, call lab fcr expla.naticn/resubmittal, rake any »^ necessar-/ ccrrectiens and nete \ ^ errors under "Ccnel'-isicns" . co - ^ • ^ A II r - - • • - -. - - V • - - • 14.1 Are t.he i.nternal standard areas (Forr VIII) of every sanple and blank vithin the upper and Ic-wer lirits (-501 te + 1001) fcr each contintiing calibraticn? -I 1 -A- ACTION: List all t.he outliers belov. Samnle ? I.hternai Std Area Lower Limit Upper Limit 6 z t (xVr^cM^ S h c e ^ • ^ P , r A P i e P i i i i 3 P x i o i x P3 0<& lO P^O'^iOf^^ P3^^3.6 P^OS-lO pm\^3 ?3>aia-3 P / i i i 3 P-2.J01^ P30^/O p 3 a H a ^ Pa;^iai) 7i)-5^i^3 T'W 113 Paioio- P^or/o ?30<^/0Re y^^nx^ ? ^ a i ^ 3 P j : ) a ) ^ 3 IN3T e/^MAL T ^ T l ^ xs± •v / x;-S'2_ \ / X-SS <\ / s m t ^ - b h i ^ p AAEA 9 8 6S3 6 5 6 ^ ' ! 5g-8rifS- ^3Sr-4-| ' ^ l ^ l l /Q.0^^-7 l O l O h L i ^ ^ o o " ^ 5-^13-0 G 3-5-/1^6 3 ^ ^ ^ 3 S ^(^I'o'Ao SK^oSC. S l I ' ^ ] 1 2. 3 ^ ^ ^ q X 5 . 1 11 if 5" ^ ^ 6 ( 9 ^ 2 - ^ ^ ' l ^ ^ 4 - 3^5"3^5' ^ O ' ^ ^ a i f 35i7a<^ C U T L / C /^o Lo^^>^ L\rY\n 1 / 5~^^-^C'2. \ / m b ^ 5 i \ / UPPBd. Liry\ 5 7 / 3 ^ ^ f •sl^ .33^S2.C \ / /C^'^^^C \> / 304504 STAliDARD CRi.-JvTI-iG x'ROCZZL--w:. Date: J a n u a r y 13 32 R e v i s i o n : s YES HO H/A ACTION: 1. If the internal standard area ccint is outside t-he upper cr lever limit, flag vith "J" all positive results quantitated vith this internal standard. 2. Hon-dstects associated vith IS area ce-cnts > 10 01 Ehould net ba q-ealified. 3. If IS area is belcv the lover limit (< 501),•qualify all associated nen- detects (li values) "J". If extremely lov area counts are reported, (< 251) or if perfcrmance exhibits a major abr-ept drop off, flag all associated non-cetects as unusable ("Tl") . 14.2 Are the 'retentien times of the intemal standards vit-hin 3 0 saccnds cf the ^ associated calibration standard? ^/S^ — ACTION: Frcfessicnai judgenent should be used tc qualif-/ data if t.ha retentien tires diffsr by mere than 3 0 seccnes. 15.0 Field D-Jrlicat o «r 15.1 Were anv field duelicates submittad fcr \ , VOA analysis? " _ 1X1 - ACTION: Compare the reported results fcr field duplicates and calculate the relati'/e percent difference. ^^ o ACTION: Any cress variaticn betveen |^ duplicate results r.ust be addressed o in* t-he reviever narrative- Hovever, ^ if large differences exist, identification of field duplicates should be cenfirred by centacting the sampler- # SDG No. 97187 VOC, SVOC, and Inorganics H Checklist # 304506 \ ^ ^ o o ^ ^ QA/QC Review of Volatiles Data for Pace Analytical SDG: 97187 December 19, 1997 Holding Times: All samples were analyzed within Region II holding times. GC/MS Tuning and Mass Calibration: All BFB tuning criteria were within control limits. Initial Calibration: All compounds with contract criteria for RRFs met those requirements. Vinyl chloride (22.0%) had a %RSD below the contractual maximum (20.5%) 06-23-97. No action is taken on two or fewer compounds outside contract requirements as long as no %RSD is above 40% and no RRF is below 0.010. All target compounds had average RRFs above the allowable minimum (0.050) as required. Acetone (39.4%) had a %RSD above the allowable maximum (30%) on 06-20-97. Results for acetone should be considered estimates (J) in associated samples. Continuing Calibration: 1,1,2,2-Tetrachloroethane (0.489) had an RRF50 below the contractual minimum (0.500) on 06-22-97 (0622L01). 1,1-Dichloroethene (36.3%) and 1,1,2,2- tetrachloroethane (32.0%) had %Ds above the contractual maximum (25%)) on 10-01-97 (0622L01). Bromomethane (31.2%) and vinyl chloride (39.0%) had %Ds above the contractual maximum (25%) on 06-23-97 (0623L03). Vinyl chloride (31.0%) had a %D above the contractual maximum (25%o) on 10-03-97 (0627L04). No action is taken on two or fewer compounds outside contract requirements as long as no %RSD is above 40% and no RRF is below 0.010. All target compounds had RRFSOs above the allowable minimum (0.050) as required. Chloroethane (26.6%), methylene chloride (42.7%), carbon disulfide (38.8%), 1,1- dichloroethene (36.3%), 1,2-dichloroethene (40.0%), and 1,1,2,2-tetrachlroethane (32.0%) had %Ds above the allowable maximum (25%)) on 06-22-97 (0622L01). Chloromethane (33.2%), bromomethane (31.2%), vinyl chloride (39.0%), chloroethane (26.1%), and 1,2- dichloroethene (28.5%) had %Ds above the allowable maximum (25%) on 06-23-97 (0623L03). Chloromethane (40.2%), vinyl chloride (31.0%), chloroethane (25.5%), and methylene chloride (32.4%) had VoDs above the allowable maximum (25%) on 06-27-97 (0627L04). Results for these compounds should be considered estimates (J) in associated samples. Blanks: Method blank VBLKLl contained a trace ofmethylene chloride (6 ug/kg). Method blank VBLKL2 contained a trace ofmethylene chloride (10 ug/kg). Method blank VBLKL3 contained traces of methylene chloride (3 ug/kg) and toluene (2 ug/kg). Method blank 304507 t^^X' "" <- VBLKL4 contained a trace of methylene_chloride (12 ug/kgp Method blank VBLKWl contained^a triicelS^f riTetliyrenFchTorrde^(2 ug/L). MethodTblank VBLKM1 contained a trace A of methylene chloride (250 ug/L). Trip blank TB0611 contained a trace of methylene ^ ^ 1 ^ chloride (1 ug/L). Trip blank TB0612 contained a trace of methylene chloride (2 ug/L). Trip blank TB0616 contained a trace of methylene chloride (1 ug/L). Trip blank TB0617 contained a trace ofmethylene chloride (2 ug/L). Trip blank TB0618 contained a trace of methylene chloride (2 ug/LJj'Rinseate blank RB0611 containM-^tracErofTTieihylene ~ """cHloride (1 ug/L)r Rinseate blank RB0612 contained a trace of methylene chloride (1 ug/L). Rinseate blank RB0613 contained a trace ofmethylene chloride (1 ug/L). Rinseate blank RB0616 contained a trace of methylene chloride (1 ug/L). Rinseate blank RB0617 contained a trace of methylene chloride (2 ug/L). Rinseate blank RB0618 contained a trace of methylene chloride (2 ug/L). Results for acetone, methylene chloride, and toluene less than ten times the highest associated blank should be considered not detected (U) in samples. Rinse blank RB0617 contained an unacceptable level of acetone (76 ug/L). Results for acetone less than ten times the highest blank level should be considered unusable (R) in associated samples. The following are listed the contaminated blanks and associated samples: Method blank VBLKL 1: S10318, S12628, S1810, 82810, S281 ORE, S31820, S32224 Method blank VBLKL2: SI 1012, S12224, S12426, S23032, S2810DL1, S468, S81416, S81820 Method blank VBLKL3: S146, S21012, S21618, S3810, S42224, SD2022 Method blank VBLKL4: S32628, S32628MS, S32628MSD Method blank VBLKWl: RB0611,RB0612,RB0613,RB0616,RB0617,RB0618,TB0611, TB0612, TB0616, TB0617, TB0618 A ^ Method blank VBLKM 1: S2810DL2 ^ ' ^ ^O'^'XA!-^ Trip blank TB0611: SI810, SI2628 ^ ' ^ ^ ^ Trip blank TB0612: S2810, S23032, S31820, S10318, S32224 ^A" Trip blank TB0616: S468, S42224, S81416, S81829, SI 1012, S12224, S21012, S22022 \5- Trip blank TB0617: S146, S12426, S21618, SD2022 Trip blank TB0618: S3810, S3812, S32628 Rinseate blank RB0611: S1810, S12628 Rinseate blank RB0612: S2810, S23032, S31820, S10318, S32224 Rinseate blank RB0613: S468, S42224, S81416, S81829 Rinseate blank RB0616: SI 1012, S12224, S21012, S22022 Rinseate blank RB0617: S146, S12426, S21618, SD2022 Rinseate blank RB0618: S3810, S3812, S32628 Intemal Standard Area Summary: All intemal standard areas and retention times were within control limits. Surrogate Recovery: Samples S2810, S2810RE, and S2810DL2 had 1 of 3 surrogate recoveries outside control limits. Results for samples S2810, S2810RE, and S2810DL2 should be considered estimates (J). 304508 Matrix Spike/Matrix Spike Duplicate: MS/MSD sample S32628 had all percent recoveries within control limits but had 1 of 5 relative percent differences outside control limits. No action is taken on MS/MSD data alone to qualify or reject an entire set of samples. Compound ID: Checked compounds were within GC/MS quantitation and qualitation limits. All positive hit compounds had the primary and secondary ions in their mass spectra as outlined in the SOW G:\STAFF\DANNE\Island\97187. VOL.wpd 304509 Cone, of Internal Standard: 50 ID: L Date: 6/20/97 RRF Cone, of Compound Bromochloromethane Vinyl Chloride RRF 1,4-Difluorobenzene Triehloroethene RRF Chlorobenzene-d5 Tetrachloroethene RRF 0620L06 Sample 1 10 605444 81288 0.671 2425076 265128 0.547 1916077 282026 0.736 0620L08 Sample 2 20 531239 129928 0.611 2164944 4022?? 0.464 1688423 369383 0.547 0620L07 Sample 3 50 546104 384455 0.704 2351141 1156282 0.492 196///3 1187893 0.604 0620L05 Sample 4 100 563257 728629 0.647 2427419 2439278 0.502 1996681 2538995 0.635 0620L04 Sample 5 200 580881 1724508 0.742 2434336 5074801 0.521 2099223 5487379 0.654 Average 0.675 0.505 0.635 % RSD 7.5% 6.1% 10.9% ' • .:.•' • Continuing Calibrations Cone, of Compound Bromochloromethane Vinyl Chloride RRF 1,4-Difluorobenzene Triehloroethene RRF Chlorobenzene-d5 Tetrachloroethene RRF 0622L01 Sample 50 676406 401246 0.593 2709458 1261202 0.465 2091956 1195697 0.572 %D 12.1% 7.9% 10.0% 0623L03 :: Sample 50 530050 218288 0.412 2287905 1152278 0.504 1925614 1164133 0.605 %D 39.0% 0.3% 4.8% 0627L04 Sample 50 586001 273339 0.466 2642517 1207459 0.457 2176952 1282775 0.589 <:-::;;%Dv::;- 30.9% 9.6% 7.2% iSample #DIV/0! #DIV/0! #DIV/0! ;::•:;: %D|:;:;.;- #DIV/0! #DIV/0! #DIV/0! Sample #DIV/0! #DIV/0! #DIV/0! %D #DIV/0! #DIV/0! #DIV/0! 304510 Cone, of Intemal Standard: 50 ID: M Date: 6/23/97 RRF Cone, of Compound Bromochloromethane Vinyl Chloride RRF 1,4-Difluorobenzene Triehloroethene RRF Chlorobenzene-d5 Tetrachloroethene RRF 0623M05 Sample 1 10 1468100 164068 0.559 4921565 478811 0.486 4394212 513779 0.585 0623M04 Sample 2 20 1445007 381666 0.660 4818828 957638 0.497 4131600 980967 0.594 0623M01 Sample 3 50 1318115 1019239 0.773 4406720 2147533 0.487 3848702 2045731 0.532 0623M03 Sample 4 100 1272475 2318950 0.911 4664494 4572065 0.490 4059735 4463221 0.550 0623M02 Sample 5 200 1202084 4659111 0.969 4456095 8575395 0.481 3869328 8032718 0.519 Average 0.//b 0.488 0.556 % RSD 22.0% 1.2% 5.9% Continuing Calibrations Cone, of Compound Bromochloromethane Vinyl Chloride RRF 1,4-Difluorobenzene Triehloroethene RRF Chlorobenzene-dS Tetrachloroethene RRF Sampie #DIV/OI #DIV/0! #DIV/0! %D #DIV/0! #DIV/0! #DIV/0! Sample #DIV/0! #DIV/0! #DIV/0! %D #DIV/0! #DIV/0! #DIV/OI Sample #DIV/0! #DIV/0! #DIV/0! %D #DIV/0! #DIV/0! #DIV/0! Sample #DIV/0l #DIV/0! #DIV/0! %D #DIV/0! #DIV/0! #DIV/0! Sampie #DIV/0! #DIV/0! #DIV/0! %D #DIV/0! #DIV/0! #DIV/0! 304511 QA/QC Review of 8270 Pyridine Data* for Pace Analytical SDG: 97187 November 12, 1997 Holding Times: All samples were extracted and analyzed within Region II holding times. GC/MS Tuning and Mass Calibration: All DFTPP tuning criteria were within control limits. Initial Calibration: All SPCCs and CCCs were within control limits. Pyridine had average RRFs above the allowable minimum (0.050) and %RSDs below the allowable maximum (30%) as required. Continuing Calibration: All SPCCs and CCCs were within control limits. Pyridine had RRFSOs above the allowable minimum (0.050) and %)Ds below the allowable maximum (25%>) as required. Blanks: Method blanks reported pyridine as not detected. Intemal Standard Area Summary: All intemal standard areas and retention times were within control limits for reported data. Surrogate Recovery: All percent recoveries were within control limits. Matrix Spike/Matrix Spike Duplicate: MS/MSD data was not provided in this SDG. Compound ID: All samples reported pyridine as not detected. * only six rinse blanks were analyzed for pyridine by 8270, for all other samples pyridine was included as part of the CLP semivolatile analyses. G:\STAFF\DANNE\Island\97187.PYR.wpd 304512 QA/QC Review of Semivolatiles Data for Pace Analytical SDG: 97187 November 12, 1997 Holding Times: All samples S21012 and S23032 were extracted outside Region II holding times. Results for samples S21012 and S23032 should be considered estimates (J). GC/MS Tuning and Mass Calibration: All DFTPP tuning criteria were within control limits. Initial Calibration: All compounds with contract criteria for RRFs and %RSDs met those requirements. All target compounds had average RRFs above the allowable minimum (0.050) and %RSDs below the allowable maximum (30%) as required. Continuing Calibration: All compounds with contract criteria for RRF50s met those requirements. Pyridine (25.4%) had a %D above the contractual maximum (25%) on 06-30-97 (0630J07). Pyridine (28.9%) had a %D above the contractual maximum (25%)) on 10-07-97 (1007J01). No action is taken on two or fewer compounds per calibration outside contract limits as long as %Ds are below 40% and RRF50s are above 0.010. All target compounds had RRF50s above the allowable minimum (0.050) as required. 2,2'- Oxybis( 1 -chloropropane) (3 5.8%) had a %D above the allowable maximum (25%)) on 06-25- 97 (0625H04). 3-Nitroaniline (29.7%), 4-nitroaniline (43.3%), and carbazole (28.8%) had %Ds above the allowable maximum (25%) on 06-18-97 (0618J04). 3-Nitroaniline(25.3%), 4-nitroaniline (47.1%), and carbazole (31.9%) had %Ds above the allowable maximum (25%) on 06-19-97 (0619J05). Pyridine (25.4%), 2,2'-oxybis(l-chloropropane) (32.4%), 2,4-dinitrophenol (34.6%), and 4,6-dinitro-2-methylphenol (25.3%) had %)Ds above the allowable maximum (25%) on 06-30-97 (0630J07). 2,2'-Oxybis(l-chloropropane) (29.3%) and 2,4-dinitrophenol(25.2%) had %)Ds above the allowable maximum (25%)) on 07-01-97 (0630J07). Results for these compounds should be considered estimates (J) in associated samples. Blanks: Method blank SBLKW3 contained a trace of bis(2-ethylhexyl)phthalate (1 ug/L). Rinse blank RB0612 contained a trace of bis(2-ethylhexyl)phthalate (22 ug/L). Rinse blank RB0613 contained a trace of diethylphthalate (1 ug/L). Rinse blaiik RB0616 contained traces of diethylphthalate (2 ug/L) and bis(2-ethylhexyl)phthalate (2 ug/L). Rinse blank RB0617 contained traces of diethylphthalate (6 ug/L) and bis(2-ethylhexyl)phthalate (4 ug/L). Rinse blank RB0618 contained traces of diethylphthalate (2 ug/L) and bis(2- 304513 ethylhexyl)phthalate (2 ug/L). Results for diethylphthalate and bis(2-ethylhexyl)phthalate less than ten times the highest associated blank level should be reported as not detected (U) in samples. The following are contaminated blanks and their associated samples: Method blank SBLKW3: RB0618 Rinse blank RB0612: S2810, S23032, S31820, SI0318, S32224 Rinse blank RB0613: S468, S42224, S81416, S81820 Rinse blank RB0616: SI 1012, S12224, S21012, S22022 Rinse blank RB0617: S146, S12426, S21618, S22022 Rinse blank RB0618: S3810, S3812, S32628 Intemal Standard Area Summary: All intemal standard areas and retention times were within control limits. Surrogate Recovery: All surrogate recoveries were within control and advisory limits. Matrix Spike/Matrix Spike Duplicate: MS/MSD sample S32628 had all percent recoveries within control limits but had 2 of 11 relative percent differences outside control limits. No action is taken on MS/MSD data alone to qualify or reject an entire set of samples. Compound ID: Checked compounds were within GC/MS quantitation and qualitation limits. All positive hit compounds had the primary and secondary ions in their mass spectra as outlined in the SOW. G:\STAFRDANNEysland\97187.SVL.wpd 304514 Cone, of Internal Standard: 40 ID: H Date: 5/27/97 RRF Cone, of Compound 1,4-Dichlorobenzene-d4 Phenol RRF Naphthalene-d8 Naphthalene RRF Aeenaphthene-d 10 Acenaphthylene RRF Phenanthrene-dlO Phenanthrene RRF Chrysene-d12 Pyrene RRF Perylene-d12 Benzo(g,h,i)perylene RRF 527H13 Sample 1 20 252355 177261 1.405 825312 387228 0.938 376171 336874 1.791 713509 313295 0.878 566635 332485 1.174 628054 252879 0.805 527H09 Sample 2 50 223158 404273 1.449 758498 900829 0.950 374566 769684 1.644 650158 704473 0.867 561160 849134 1.211 608823 640202 0.841 527H10 Sample 3 80 247832 730966 1.475 841422 1570428 0.933 387891 1305348 1.683 661404 1190186 0.900 596557 1444729 1.211 626306 1059884 0.846 527H11 Sample 4 120 246894 1027763 1.388 806095 2172435 0.898 350044 1922535 1.831 660962 1689423 0.852 550925 1905575 1.153 601143 1379767 0.765 527H12 Sample 5 160 226612 1231303 1.358 738525 2693690 0.912 343896 2271879 1.615 591271 2007993 0.849 511221 2408100 1.178 562629 1670891 0.742 Average 1.415 0.926 1.713 0.869 1.185 0.800 % RSD 3.3% 2.3% 5.5% 2.4% 2.1% 5.7% Continuing Calibrations Cone, of Compound 1,4-Dichlorobenzene-d4 Phenol RRF Naphthalene-d8 Naphthalene RRF Acenaphthene-dIO Aeenaphthylene RRF Phenanthrene-d10 Phenanthrene RRF Chrysene-d12 Pyrene RRF Perylene-d12 Benzo(g,h,i)perylene RRF 1008H04 Sample 50 225206 351303 1.248 752499 810314 0.861 365211 774578 1.697 649099 711459 0.877 493811 775584 1.256 452616 353145 0,624 %D 11.8% 7.0% 0.9% 0.9% 6.0% 22.0% 0625H04 Sample 50 231649 377811 1.305 724076 824558 0.911 361116 783718 1.736 623230 699573 0.898 444845 707122 1.272 477996 526118 0.881 %D. 7.8% 1.7% 1.4% 3.3% 7.3% 10.1% Sample #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! %D #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DlV/0! Sample #DIV/01 #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! %D #DIV/0! #DIV/OI #DIV/0! #DIV/OI #DIV/0! #DlV/0! Sample #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! , %D #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DlV/0! 304515 Cone, of Intemal Standard: 40 ID: J Date: 4/9/97 RRF Cone, of Compound 1,4-Dichlorobenzene-d4 Phenol RRF Naphthalene-d8 Naphthalene RRF Acenaphthene-dIO Aeenaphthylene RRF Phenanthrene-dlO Phenanthrene RRF Chrysene-d12 Pyrene RRF Perylene-d12 Benzo(g,h,i)perylene RRF 0409J20 Sampie 1 20 228652 176576 1.544 823312 354022 0.860 359452 292002 1.625 632930 284821 0.900 596568 302416 1.014 703129 243227 0.692 0409J16 Sample 2 50 229953 465248 1.619 875897 1052503 0.961 396804 924666 1.864 727128 869749 0.957 668952 931049 1.113 718735 704460 0.784 0409J17 Sample 3 80 237256 774680 1.633 912435 1819207 0.997 426559 1607291 1.884 766572 1509354 0.984 635622 1601558 1.260 701965 1239884 0.883 0409J18 Sampie 4 120 238036 1167641 1.635 927977 2645593 0.950 390110 2325749 1.987 692977 2155240 1.037 670516 2328080 1.157 723844 1737069 0.800 0409J19 Sampie 5 160 219263 1479771 1.687 855660 3407800 0.996 403856 3061075 1.895 707185 2903918 1.027 638199 3027844 1.186 636172 2306968 0.907 Average 1.624 0.953 1.851 0.981 1.146 0.813 % RSD 3.2% 5.9% 7.3% 5.7% 8.0% 10.5% Continuing Calibrations;:?' : :••:::•••;•! ::/;,; :;;-'-^ Cone, of Compound 1,4-Dichlorobenzene-d4 Phenol RRF Naphthalene-d8 Naphthalene RRF Aeenaphthene-d 10 Acenaphthylene RRF Phenanthrene-dlO Phenanthrene RRF Chrysene-d12 Pyrene RRF Perylene-d12 Benzo(g,h,i)perylene RRF 0618J04 Sample 50 153523 309063 1.611 619230 794329 1.026 290213 665278 1.834 544988 645680 0.948 411506 646498 1.257 430284 474928 1 0.883 %D 0.8% 7.7% 0.9% 3.4% 9.7% 8.6% 0619J05 Sample 50 153694 321639 1.674 595602 750946 1.009 275495 627205 1.821 478562 561748 0.939 356408 582459 1.307 349826 395650 0.905 %D ; 3.1% 5.9% 1.6% 4.3% 14.1% 11.3% 0630J07 Sample 50 123803 284501 1.838 473718 606572 1.024 234288 514289 1.756 416220 484173 0.931 342654 511512 1.194 370522 394735 0.852 ; %D 13.2% 7.5% 5.1% 5.1% 1 4.2% 4.8% 0701J05 Sample 50 97789 222924 1.824 383023 470509 0.983 178597 401712 1.799 328013 372293 0.908 265160 414158 1.250 283510 314849 0.888 %D 12.3% 3.1% 2.8% 7.4% 9.0% 9.3% Sampte #DlV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! %D #DIV/0! #DIV/0! #DIV/0! #DIV/0! #D1V/Q! #DIV/0! 304516 QA/QC Review of TAL Inorganic Data for Pace Analytical SDG: 97187 November 13, 1997 Holding Times: Samples were analyzed within EPA Region II CLP holding times. Initial and Continuing Calibration Verification: Sodium (84.7%) had a percent recovery outside control limits (90-110%). Results for sodium should be considered estimates (J) in associated samples. CRDL Standard for AA and ICP: Antimony (75.5% and 73.1%), arsenic (78.4%), mercury (145.0%), selenium (39.5%, 24.4%, and 60.0%), and zinc (134.6%) had percent recoveries outside Region II controHimits (80-120%). Results for these metals in associated samples within effected ranges should be considered estimates (J). Blanks: Initial and continuing calibration, and preparation blanks had analyte levels less than the CRDLs as required by Region II. Rinse blank RB0611 contained sodium (9940 ug/L) and zinc (37.5 ug/L) above their CRDLs. Rinse blank RB0612 contained zinc (35.0 ug/L) above its CRDL. Rinse blank RB0613 contained zinc (30.5 ug/L) above its CRDL. Rinse blank RB0616 contained zinc (31.0 ug/L) above its CRDL. Rinse blank RB0617 contained zinc (115.0 ug/L) above its CRDL. Rinse blank RB0618 contained zinc (61.7 ug/L) above its CRDL. Results for these metals less than five times the associated blank level should be considered unusable (R) in samples. ICP Interference Check Sample: Thallium (78.2% and 76.5%) had percent recoveries outside control limits (80-120%). Results for these metals should be considered estimates (J) in associated samples. Spike Sample Recovery: Mercury (58.3%) had a percent recovery were within control limits (75- 125%) for water spike sample IBWOOIS. Results for mercury should be considered estimates (J) in water samples. Antimony (41.8%), arsenic (71.5%), beryllium (61.6%), cobalt (72.8%), lead (73.5%), manganese (271.5%), nickel (74.9%), selenium (68.3%), silver (51.4%)), thallium (69.8%), and zinc (1135.2%) had percent recoveries outside control limits (75-125%) for soil spike sample S32628S. Results for antimony, arsenic, beryllium, cobalt, lead, nickel, selenium, silver, and thallium should be considered estimates (J) in soil samples. Positive results for manganese and zinc should be considered unusable (R). Duplicates: All applicable relative percent differences were less than the CLP maximum (20%)) for duplicate water sample RB061 ID. Barium (55.4%),calcium (68.5%)), manganese (71.9%), and vanadium (23.9%) had relative percent difference above the CLP maximum (20%)) but were below the allowable maximum (100%) for duplicate sample S32628D. These metals in soil samples were appropriately flagged as per Region II. Cadmium (101.9%), copper (115.0%), lead (140.0%), and zinc (23.9%) had relative percent difference above the CLP 304517 maximum (20%) and the allowable maximum (100%)) for duplicate sample S32628D. Results for cadmium, copper, lead, and zinc should be considered estimates in soil samples Laboratory Control Sample: All recoveries were within control limits for the soil LCSs. Sodium (79.4%)) had a percent recovery outside control limits (80-120%)). Results for sodium should be considered estimates (J) in water samples. Standard Addition Results: No results were quantitated by MSA in this LP. ICP Serial Dilution: Cadmium (15.7%), potassium (20.8%>), sodium (16.2%), and zinc (65.3%) had %)Ds above the allowable maximum (10%)) for soil serial dilution sample S32628L. Results for cadmium, potassium, sodium, and zinc should be considered estimates (J) in soil samples. Instmment Detection Limits: All IDLs were at or below the CRDLs as required. Percent Solids for Soils: All soil samples had percent solids above the allowable minimum (50%). G:\STAFRDANNE\Island\97187.INO.wpd 304518 Mercury Date: 7/8/97 X range 0 0.2 0.5 1 5 10 y range 199 4033 11381 23199 136416 264336 Slope: Intercept: Cor. Coef.: 26710.03 -1082.25 0.999765 304519 Mercury Date: 79/97 X range 0 0.2 0.5 1 5 10 y range 1827 10257 21491 39321 202997 387314 Slope: Intercept: Cor. Coef.: 38771.85 2619.517 0.999763 304520 Mercury Date: 79/97 X range 0 0.2 0.5 1 5 10 y range 5817 16802 29891 48934 310412 599056 Slope: Intercept: Cor. Coef.: 60095.92 1218.369 0.999524 304521 ^DGi 9T87 Evaluation of Hetals Data for the Contract Lalxiratory Program (CLP) based on SOR. 3/90 (SOP Revision Xli ZFARZD EY ^.•.AAXXXJX DATE: Harm SneiXh, QJall'z^y Assuranca Q-iemist. Tcxic and kazardo'us Waste Secticn -^^^- ?s ; IT.avZD BY: N r . . - V >_ *\ •:.IA FrJDVZD EY •r.yx. Robert Runyon, t h ^ f Monitoring Kanagenent Branch DATE: Kevin K'Obik, Quef Tcxic and Hazardous Waste Secticn DATE: -y-A^ 304522 STW,TWRD OPERXniiG roOGETURE Evaluation of Metals Data for the Date: Jan. 1992 Contracc J-aboratory Pxuyidm Number: HW-2 Revision: 11 Scope lhis procedure is applicable to inorganic data obtained frem contractor laboratories wor>arxg for Hazardous Waste Site Contract Laboratory Program (CLP) . Ihe data validation is bsLsed upoi analytical and quality assurance requirements specified in Statenent of Work (SOW) 3/90 . Rasponsibilitiea - Cata reviewers vill ccrplete the following tasks as assigned by the Data Review Coordirator: For a total rgview; 1 Data Assessment - "Total Reviev-InonTanies" Checklist ygpeTirf-Jv (A.l). ^ I ^ e reviewer rust answer every question on the checklist. - i^ta Assessment - Data Assessment Karrative (Appendix A.2) Ihe answer on the checklist nusr ratch the action in the narrative (appendix A.2) and on Form I's. Do not use pencil to write the rarrative. .3 Contract Non-CcrzJliance - EM3 Report (Appendix A.3) This reixDrt is to be ccrpleted only when a serious contract violation is encc-ar.t.ered, cr upon the request of the IData Validation Task Monitor, or Technical Projert Cfficer (TPO). Forward 5 ccpies: one each for intemal files, apprcpriate Regional TPD, Sample Manageiient Office (SMO) and last fwo addresses cf Mailing List for Data Reviewers (Appendix A.4). In other cases, all contract violations should be appended to the end of the Data Assessment Narrative (Sec. A.2.2), . 4 CLP Data Assessment Sunnary Fonns .1 Appendix A.5 Fill in the total njmber of analytes analyzed by different analyses arxi the n'JTPer of analytes rejected or flagged as estimated due to corresponding quality control criteria. Place an "X" in boxes where analyses were not performed, cr criteria do not apply. .2 Appendix A. 6 C&ta revier;er is also required to fill out Inorganic Regional Data Assessment ^ ^ o r m (Appendix A.7) provided by EPA Headquarters. Codes listed on the form ^ ^ i l l be used to describe the Data Assessment Summary. 304523 STMiTARD OFERATING FTOCEIURE :e: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Nuniber: HW-2 Revisicn: 11 ..5 Data Rgview log; It is reoccinended that each data reviewer sixuld maintain a log of the reviews ccrpleted to inclxx3e: a. date of start of case reviev.' b. date of ccnpleticn of case review c. site d. case nuniber e. contract laboratory f. nuEber of sanples g. natrix h. hours worked i. reviewer's initials 1.6 Telephone Record Log - the data reviewer should enter the bare facts of inquiry, before initiating any phor« conversation with CLP laboratory. ' After the case review has been ccrpleted, mail white copy of Telephone • Record Log to the laboratory and pink copy to SMD. File yellcw copy in the Telephone Record Log folder, and attach a xerox copy of the Telephone Record Log to the ccrpleted Data Assessment Narrative (f'jppeiriix A.2). 1.7 Forvarded Paperwork .7.1 Upon completion of review, the follcwing are to be forwarded to the Regional Sarple Control Center (RSCC) located in the Surveillance and .Monitoring Branch: a. data package b. ccrpleted data assessment checklist (Appendix A.l,original) c. S:-:o Ccntract Ccrpiiance Screening (CCS) d. Record cf Canrrjru.cation (copy) e. CL? Reanalysis Request/Approval Jlecord (original + 3 copies) f. Appendix A.6 (original). .7.2 Foru-ard 2 copies of ccrpleted Data Assessment Narrative (;^Dpendix A.2) along with 2. copies of the Inorganic Data Assessment Form (Appendix A. 6) and Telephone Record Log , if any,: one each for appropriate Regional TPO, and the other one to EPA EMSL office in Las Vegas. The addresses of TPOs and EPA office in T^gg Vegas are given in Appendix A-4. .8 Filed Papeivork - Upon coTpletion of review, the follcwing are to be filed within M:-3 files: a. TV'O copies of ccrpleted Data Assessment Narrative (Appendix A.2) each carr^'Lng — Appendix A. 6. kb. Telephore Record Leg (copy) rc. Sl-yD Report (copy Appendix A-3) d. CLP Reanalysis Request/Approval Record (copy) 304524 STANEftRD OFERATING PFSXHURE Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Revisicn: l l Data Cnnpleteneas Each data package is checked by a Regicnal Sanple Ccntrol Coordinator (RSSC) for completeness. A data package is n'^^-mt^t^ to be ccnplete when zill the deliverables required under the contract are present. If a data package is inccnplete,the RSSC would call the laborat:ory for missing document(s). If the laboratory does not respond within a week, aiD and hMB coordinator of Regicn H will be notified. Reiecrcion of Data - All VcLLues determined to be unacceptable on the Inorganic A.nalysis Data S.heet (Form I) must be lined over with a red pencil. As soon as any reviev.' criteria causes data to be rejected, that data can be elirdnated frcn any further review or cc'isideration. ' Acceptance Criteria - In order that reviews be consistent among reviewers, acceptance ^criteria as stated in Appendix A.l (pages 4-25) should be used. Additional g'uidance Fcan be found in the National Inorganic Functional Guidelines of October 1, 1989. EHD Contract C=gplianee Scrrvninq (0C3) - This is intended to aid reviei^er in locating any problem's, both corrected and uncorrected. However, t.he validation should be carried out even if CCS is not present. Resutnittals received frcn laboratory in response to CCS .—ust be used by the reviewer. Request for Reanalysis - Data reviewers must note all items of contract non-compliance v.-ithm Data Assessment Narrative.If holding times and sample storage tiroes have not been exceeded, TPD ray request reanalysis if items of non-corpl iance are critical to data assessment. Requests are to be nade on "CLP Re-Analysis Request/Approval Record". Record of Ccmunication - Provided by the Regional Sample Control Center (RSCC) to indicate which data packages have been received and are ready to be reviewed. Roundi-na off r.umJpers - The data reviewer will follcw the standard practice. 304525 STANDARD 0PERATIJX3 FRDCEDJRE Ev'aluation of Metsils Data for the Contract Laboratory Program Appendix A.l: Data Assessment - Ccntract Ccmpiiarxfi (Total Review) Date: Jan. 1992 Nunter: HW-2 Revision: 11 1 Contract Cccpliance Screer'iTY7 Rjeport- (CCS) - Present? ACTION: If no, ccntact RSOC. YES 2 Reoord of Cecimmication (frees RSCC) - Present? ACTION: If no, request frcn RSCC. [_] _ JL J Trip Report - Present and ccrplete? ACTION: If no, contact RSCC for trip report. ^Knple Traffic Report - Present? Legible? ACTION: If no, request frcn Regional Sample Control Center (RSCC). 5 Cc.'er Pane - Present? Is ccr.'er page properly filled in and signed by the lab manager or the manager's designee? ACTION: If no, prepiare Telephone Record Log, "and contact laboratory. Do n'umbers of samples correspond to numbers on Record of Ccrrrurj.cation? Do sarple numbers on cover page agree with sample n'umiers on: (a) Traffic Report S.heet? ^P^n (b) Forro I ' s ? ON: If no for any of the above, ccntact RSCC for clarification. [ ] [ ] [ ] V tJL: _ (X: _ [ ] [ ] _ J)L X 304526 STANDARD OFERATING PROCEDURE le: Evaluation of htetals Data for the Contract Laboratory Program Appendix A.l: Data Assesanent - Ccntract Ccrnpliance (Total Review) Date: Jan. 1992 Nuntcr: HW-2 Revision: 11 .6 Fona I to IX X S Ha liZA .6.1 Are a l l the Form I through Form IX labeled vith: laboratory name? Case/SAS number? EPA sample No.? SDG No.? Contract No.? Correct units? Matrix? ACTION: If no for any of the a^ove, note under Contract Problem/Non-Ccrpl iance section of the "Data Assessment Narrative". Do a.'^y ccmputation/transcription errors exceed 10% of reported values on Forms I-IX for: (NCTE: Check all forns against raw data.) (a) a l l analytes analyzed by ICP? (b) a l l analytes analyzed by GFAA? (c) a l l analytes ai^yzed by AA Flame? (d) Mercury? (e) Oy-anide? ACTION: If yes, prepare Telephone Log, contact laboratory for corrected data and correct errors with red pencil and i n i t i a l . [ J ^ [ ] [JL.] [ X J [ ] [JL] J ^ JL ] j ^ _ ] _ : L ] J L __ _ ] JL _ 304527 SriANEftRD OPERATING IKXH3URE Evaluation of Metals Data for the Contract laboratory Program Appe-ndix A.l: Data Assessment - Contract Ccxpliance (Total Review) Date: Jan. 1992 Nuntier: HW-2 Revision: l l .7 .7.1 •,2 Rav Data Digestion Log* for flame AA/ICP (Form XIU) present? Digestion Log for fumaoe AA Form XIII present? Distillation Log for mercury Form XIII present? Distillation Log for cyanides Form XIII present? Are p.4 values (pH<2 for all metals, pH>12 for cyanide) present? *Keights, diluticns and volumes used to obtain values. Perce.'it solids calculation present for soils/sediments? Are V' -ation dates present on sample preparation logs sheets? l-'eas.::: _:.^-.t read out record present? ICP Flame AA Furnace AA Mercury • cyanides Are all raw data to support all sample analyses and QC operations present? Legible? Properly Labeled? ACTION: If no fcr any of the eibove questions in sections A.1.7.1 through A.1.7.3, uTite Telephone Record Log and contact laboratcry for resubinittals. YES JL] J is N/A _ JL \ JL] _ : L ] _ X.] _ ] ] JL] _ JL] _ _J^] _ AL] _ JL] _ JL 304528 STANDARD OFERATING TPOCEDJRE Evaluation of Itetals for the Contract Date: Jan. 1992 Laboratory Program Number: HW-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 Compliance (Total Review) YES NO HZA Hoi diner Timf>*i - (aqueous and s o i l sanples ) (Examine sample traffic reports and digesticn/distillaticn logs.) Mercury ansdysis (28 days) exceeded? [ Y 1 cyanide d i s t i l l a t i o n (14 d a y s ) . . . . . exceeded? [ \: 1 Other Metals analysis (6 m o n t h s ) . . . . exceeded? f ^C ] NOTE: Prepare a l i s t of all samples and analytes for which holding times have been exceeded. Specify the number of days fran date of collection to the date of preparation (fran raw data). Attach to checklist. ACTION: If yes, reject (red-line) vadues less than Instrument Detection Limit (IDL) and flag as estimated (J) the values above IDL even though sample(s) vas preserved properly. Is p-H of aqueous samples for: Metals Analysis >2? [JC_] Cyanides Analysis <12? [ J ^ J Action: If yes, flag the associated metals and cyanides dat:a as estimated. Form I fFinal Data) Are a l l Form I ' s present and ccrplete? f X1 ACTION: If no, prepare telephone record log and contact laboratory for sutnittal. Are correct units (ug/1 for waters cind mg/kg for soils) indicated on Form I's? [JL] Are soil sample results for each parameter corrected for v^ percent solids? [JL] Are a l l "less than IDL" x-alues properly coded with "U"? [ J ^ ] 304529 STANDARD OPERATING H»ZEEURE tie: Evaluation of Metals Data for the Date: Jan. 1992 Contract laboratory Program Number: HW-2 Appendix A.l: Data Assessment - Contract Revision: 11 Compiiance (Total Review) ~~~ xss. m HZT Are the correct conoentraticn oualifiers used vith . final data? * f A 1 KTlC&i: If no for any of the above, prepare Telephone Reoord Leg, and ccntact laboratory for corrected data. 1.9.3 Are EPA sample # s auTd corresponding laboratory sample ID * s the same as on the Cover Page, Form I's and in the raw data? [ A 1 Was a brief physical description of samples given on Form I ' s ? F X1 . Was the dilution of any sample diluted beyond the requiremients of the contract noted on Form I or y Form XIV? [J^] ACTION: If no for any of the above, note under Contract-Prcblem/Non-Ccrpliance of the"Data Assessment Narrative". •-. 10 Calibration --i:.l Is record cf at least 2 point calibration present for IC? aralysis? Is record of 5 point calibration present for Hg aralysis? Is record of 4 point calibration present for: Flaire AA? Furnace AA? Cyanides? Is one calibration standard at the CRDL level for - all AA (except Hg) esxd Cy-anides analyses? [J_] ACTICN: If no for any of the above, write in the Contract Problen/Non-Ccrrpliance section of the "Data Assessment Narrative". 304530 tX, r^.j [ ] [ ] [ Y l JL Y STANDARD OFERATING IRDCEDURE .le: Evaluation of Metals Data for the Contract Laboratory Program Appendix A.l: Data Assessment - Ccntract cirrplianoe (Total Review) Date: Jan. 1992 Nui±er: HW-2 Revisicn: 11. .10.2 Is correlaticn coefficient less than 0.995 for: Mercury Analysis? cyanide Analysis? Atonic Absorption Analysis? If yes, flag the associated data as estimated. 10.3 YES ACTION: NOTE: ACTTON: The data validator shall calculate the correlation coefficient using concentraticns of the standards and the corresponding instrument response ( e.g. absorbance, peak area., peak heii^t, etc.). In the instar>ce where less than 4 standards are measured in absorbance (or peak eurea, peak height,etc.) mode, are the remaining standards euialyzed in concentration zvode imrnediately after calibration within +10% of the true values? [ ] If no, flag the associated datia as estimated if standards cire not vithin +10% of true values. Do not flag the data as estimated in linear range indicated by good recovery of standard(s). m CL] X N/A y K Form II A (Initial zmd Contir.'jinq Calibration Verification)- Present and complete for every metal and cyanide? Present and ccrplete for AA and ICP when both are used for the same analyte? ACTTON: If no for any of the above, prepare Telephone Record Log and contact laboratory. 1.11.2 Circle on each Form IIA all percent recoveries that cure outside the contract windcws. Are all calibration stiandards (initial and continuing) — within control limits: Metals- 90-110%R? Hg - eO-120%R? Cyanides- e5-115%R? [A] [ ] [ ] [JL] tJL] X X w o O l CO STANDARD OIERAITNG PROCEDURE t Evaluation of >Setals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Appendix A.l: Data Assessment - Ccntract Revisicn: 11 Ccnpiiance (Total Review) '• " ^ ^ H z l ACnCM: Flag as estiiaatfid (J) all positive data (not flagged with a "IT) analyzed between a Ccilibration standard vith %R between 75-89% (65-79% for Hg; 70-84% for CN) or 111-125% (121-135% for Hg; 116-130% .for OJ) reacrvery and nearest good calibraticn standard. Qualify results <IDL as estimated (UT) if the ICV or CCV %R is 75-89% (CN, 70-84% ; HG, 65-79%). Reject (red-line) as unacceptable data if recovery of the ICV or CCV is cutside the range 75-125% (CN, 70-130%; Hg, 65-135%). &ialify five sanples cn either side of verification standard out of control limits. L1.3 Was continuing calibration performed every 10 samples ^ or every 2 hours? r X l Was ICV for cyanides distilled? f A 1 ON: If no for any of the above, vrite in the Contract-Problem/Non-Ccrpliance section of the "Data Assessment Narrative". .12 Fom II B (CRDL Standards for AA and ICP) - .12.1 Was a CRDL standard (CRA) analyzed after initial .. calibration for all AA metals (except Hg)? f A 1 Was a mid-range calib. verification standard distilled and analyzed for Cj'anide analysis? [ ] A Was a 2XCRDL ( or 2xIDL vhen IDL>CRDL) analyzed (CRI) y for each ICP run? ' f A 1 (Note: CRI for AL,Ea,Ca,Fe,Mg,Na,or K is not required.) ACTION: If no fcr any of the above, flag as estimated all data falling vithin the affected ranges. The affected ranges are: AA Analysis - **True Vcdue + CRDL ICP Ancdysis - -'•True Vcdue + 2CRDL CN Ancdysis - **True Value + 0.5 x True Value. — to o Ol LO NJ rue value of CRA, CRI or mid-range standard. Substitute IDL for CRDL when IDL > CRDL. cute the concentration of the missing mad-range standard fran the calibration range. STANDARD OPERATING FRDCEDURE itle: Evaluation of Mstals Data for the Date: Jan. 1992 Contract Laboratory Program Nunter: HW-2 Appendix A.l: Data Assessnjent - Ccntract Revisicn: 11 Ccnpiiance (Ttotal Review) " ^ m N/A .1.12.2 Was CRI analyzed after ICV/ICB and before the final ,. CCV/OCB, and tvice every eight hours of ICP run? r A ^ ACTION: If no, vrite in Contract Problenv/Non-Ccnpliance Section of t.he "Data Assesanent Narrative". .1.12.3 Circle on each Form IIB all the pertaent reooveries that are outside the aooeptanoe winckaws. Are CRA and CRI standards vithin control limits: Metals 80 - 120%R? [ ] 2L. Is mid-range standard vithin control limits: cyanide 80 - 120%R? [ ] X ACTTON: Flag as estimated all sample results vithin the affected range if the recovery of the standard is between 50-79%; flag only positive data within the affected range if the recovery is between 121-150%; reject all data vithin the affected range if the recovery is less than 50%; reject only positive data vithin the affected range if the recovery is greater th^an 150%. Qualify 50% of the samples on either side of CRI standard outside the co.ntrol limits. Note: Flag or reject the final results only when sanple rav data are within the affected ranges and the CRDL standards are outside the acceptance windows. Form III (Initial and Continuing Calibration Blan)c3) .1 Present and ccnplete? [ X 1 For both AA and ICP when both are used for the . samve analyte? f K1 Was an initial calibration blank analyzed? f \ ] Was a continuing calibration blank analyzed after every 10 samples or every 2 hours (which ever is more frequent)? tjy 304533 STANEftRD OPERATING FRDCHURE .e: Evaluatian of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 cinplianoe (Total Review) ^ ^ "^ N/A ACTTCK: If no, prepare Telephone Record Log, ccntact laboratory zuxi write in the Ccntract-Problems/ Non-Ccnplianoe secticn of the "Data Assessnent Narrative". .13.2 Circle on each Form I H all calibraticn blank valxies that are above C323L (or 2 x IDL vhen IDL > CRDL). Are all calibraticn blanks (when IDLcCRDL) less than or ^ . equal to the Contract Required Detecticn Limits (O^Le)? f A l Arc all calibration blanks less than two tirnips Ir.strument Detection Limit (when IDL>CRDL)? [ ] '_ \ ACTION: If no for any of the above, flag as estirated (J) positive sanple results when raw sample value is less than or equal to calibration blank value analyzed between calibration blank vith value over CRDL (or 2xIDL) and nearest good calibration blank. Flag five samples on either side of the calibration blank outside the control limits. :A FORM III (Preparation Blank) - (Note: The preparation blank for mercury is the same as the calibration blank.) L4.1 Was one prep, blank analyzed for: each Sample Delivery Group (SDG)? [ X 1 each batch of digested samples? f X 1 each matrix type? f X 1 both AA and ICP vhen both are used for the same analyte? [ ] /\ ACTION: If no for any of the above, flag as estirated (J) edl the associated positive data <10 X IDLE for vhich prep, blank — was not analyzed. H7TE: If only one blank was analyzed for more than 20 samples, t.hen first 20 samples analyzed do not have to be flagged as estimated (J). 304534 STANDARD OPERATING PROCEDURE :ic. D/aluation of hSetals Data for the Date: Jan. 1992 Ci^ntract Laboratory Program Nuntaer: HW-2 Appendix A.l: Data Assessnent - Contract Revisicn: 11 Ciirpliance (Total Review) _ _ ^ ^ 1.14.2 Is ccncentraticn of prep, blank value greater ^ than the CRDL when IDL is less than or equal to CEDL? f X l If yes, is the concentraticn of the sanple vith the least ct3>oentrated analyte less than 10 t-i-mf^ the prep.blank? [ ] j ^ ACncg;: If yes, reject (red-line) all ?e«=ry'-i a+or^ data greater than CRDL ccncentraticn but less than ten times the prep, blank Vcdue. 1.14.3 Is concentration of prep, blank value (Form III) less than r^o tires IDL, when IDL is greater than CRDL? [ ] X ACTION: If no, reject (red-line) all positive sample results vhen sample rav data are less than 10 times the prep, blaink value. Is concentratian of prep, blank below the negative CRDL? [JL] ACTTON: If yes, reject (red-line) all associated sample results less th.an lOxCRDL. 1.15 Fom IV (ICP Interference Check Sample) 1.15.1 Present and cemplete? f A l (R7TE: Not required for f'umaoe AA, flame AA, mercury, cyanide and Ca, Mg, K and Na.) Wcis ICS analyzed at beginning cind end of run (or at least f.;ice every 8 hours)? [JX.] ACTION: If no, flag as estimated (J) all the samples for vhich AL, Ca, Fe, or Mg is higher than in ICS. 1.15.2 Circle all values on each Form TV that are more than + 20% of true or established mean value. __ Are all Interference Check Sample results inside ^ the ccntrol limits (+ 20%)? [ ] J\^ If no, is concentration of Al, Ca, Fe, or Mg lower , than the respective conce.ntration in ICS? [ ] X 304535 STANDARD OfERATING FRDCHURE .le: Evaluation of >5etals Data for the Date: Jan. 1992 Contract Laboratory Program Nuniper: HW-2 Appendix A.l: Data Assessnent - Ccntract Revision: 11 oipliance (Ttttal Review) .YES NO N/A ACTICK: If no, flag as estimated (J) those positive results for vhich ICS reocTVEry is between 121-150%; flag all sanple results as estimated if ICS reoovery falls vithin 50-79%; reject (red-line) those sample results for which ICS reoovery is less than 50%; if ICS reoovery is above 150%, reject positive results only (not flagged vith a "U"). 15 Fora V A (gpiked Sample Reoovery - Pre-Diqegtion/Pre-Distillatio'n)- ( Note: Not required for Ca, Mg, K, and Na (both matrices), Al, and Fe (soil only.) ,l£.l Present, and ccrplete for: each SDG? f X l each matrix type? f X 1 each cenc. range (i.e. low, r e d . , hic^)? [ J L J For both AA and ICP vhen both are used for the same analyte? [ ] X ACTION: If no for any of the above, flag as estimated (J) all the positive data less than four tines the spDdng levels specified in SCW fcr vhich spiked sanple vas not analyzed. NOTE: If one spiked sample vas analyzed for more than 20 samples, then first 20 samples amalyzed do not have to be flawed as estimated (J). 15.2 Was field blank used for spi3ced sample? [JL] ACTION: If yes, flag all positive data less than 4 X spike added as estimated (J) for which field blank vas used as spiked sample. 15.3 Circle on e^ch Form VA all spike recoveries that are outside control limits (75% to 125%). Are all recoveries vithin control limits? [ ] If no, is sample concentration greater than or equal to four tines spike concentration? [ ] ^ _ 304536 STANDARD OPERATING PROCEDURE .e: Evaluation of Metals Data for the Contract Laboratory Program Appendix A.l: Data Assessment - Oontract Corpliance (Total Review) Date: Jan. 1992 Number: HW-2 Revision: 11 16.4 IIS ACTICg;: If yes, disregard spike reocMeries for analytes whose ccnoentraticns are greater than or equal t o four times spike i^dded. If nm, circle those analytes cn Fom V for which sanple cxnoentration i s less than four times the spike ooncexTtraticn. Are results outside the control limits (75-125%) flagged vith "N" on Form I's and RDrm VA? ACTION: If no, vrite in the Contract - Prcblenv/Non - Ccnpiiance section of "Data Assessment Naun^tive". Aqueous Are any spike recoveries: (a) less than 30%? (b) between 30-74%? (c) between 126-150%? (d) greater than 150%? ACTION: If less than 30%, reject all associated aqueous data; if between 30-74%, flag all associated aqueous data as estirated (J); if between 126-150%, flag as estimated (J) all associated aqueous data not flagged with a "U"; if greater than 150%, reject (red-line) all associated aqueous data not flagged with a "U". m [JL] _ [JL] [LjL] [JL] [JL] N/A .16.5 Soil/Se^^-iTTv^nf- Are any spike reooveries: (a) less than 10%? (b) between 10-74%? (c) between 126-200%? (d) greater than 200%? JL X [X] [ ] [JL] [ ] 304537 STANDARD OFERATING PROCEDURE :tle: Evaluation of Metals Cata for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 Corpliance (Total Reviev) ^ ^ N/A ACTIO;: If less than 10%, reject a l l ;^eer^ia^-cH data; if between 10-74%, flag a l l associated data as estimated; if between 126-200%, flag as estimated a l l associated data was not flagged vith a "U"; if greater than 200%, reject cdl associated data not flagged vith a "U". 1.17 Form VI (Lab Duplicatgg) " 1.17.1 Present and ccnplete for: each SDG? [_^] each matrix type? [_jL] each concentration range ( i . e . low, med., high)? [ J L ] both AA and ICP vhen both are used for the same analyte? [ ] X. ACTTON: If no for any the above, flag as estimated (J) all the data >CRDL* for vhich duplicate sample vas not analyzed. Note: 1. If one duplicate sanple vas analyzed for more than 20 samples, then first 20 samples do not have to be flagged as estimated. 2. If percent solids for soil sanple and its duplicate differ by more than 1%, prepare a Form VI for each duplicate pair, report concentrations in ug/L on vet veight basis and calculate RPD or Difference for each analyte. ,17.2 Was field blank used for duplicate analysis? f A 1 ACTTON: If yes, flag all data >CRDL* as estimated (J) for which field blank vas used as duplicate. .17.3 Are all values vithin control limits (RPD 20% or difference < +CRDL) ? [ ] Ji. If no, are all results outside the control limits flagged with an * on Form I's and VI? f X 1 ACTION: If no, write in the Contract - Prc±)lems/Non- Ccnpliance section of "Data Assessnent Narrative". * Substitute IDL for CRDL when IDL > CRDL. 304538 STANDARD OPERATING PROCEITTRE Evaluation of Metals Data for the Contract Laboratory Program Appendix A.l: Data Assessanent - Ccntract Corpliance (Total Review) Date: Jan. 1992 Number: HW-2 Revisicn: 11 KTTE: 1. RPD is not calculable for an einalyte of the sample - duplicate pair T^ien both values are less than IDL. 2. If the result of lab duplicate analyzed by GFAA is rejectable due to coefficient of correlation of hEA, cinalytical spike recovery, or duplicate injections criteria, do not apply precision criteria to miPtiilR analyzed by GFAA. Aqueous Circle on each Form VI a l l values that are: RPD > 50%, or Difference > CRDL* Is any RPD greater than 50% where sample and duplicate are both greater than or equal to 5 times *CRDL? Is any difference** between sample and duplicate greater than «CRDL where sample and/or duplicate is less thcin 5 tires *CRDL? ACTION: If yes, flag the associated data as estimated. Soil/Sediment Circle on each Form VI all values that are: RPD > 100%, or Difference > 2 x CRDL* Is any RPD (where sample and duplicate are both greater than or equal to 5 times *CRDL) : > 100%? Is any **difference between sample and duplicate (where sample and/or duplicate is less than 5x*CRDL) : > 2x*CRDL? YES m MA [JL] [JL] JL [_] _ [ ^ ] - S'ubstitute IDL for CRDL when IDL > CRDL. Use absolute values of samcle and duplicate to calculate the difference. 304539 STANDARD OPERATING PROCEDURE le: Evaluation of Metcds Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Appendix A.l: Data Assessment - Contract Revision: 11 Conpliance (Tttal Review) _ _ _ ^ ^ ACTTON: If yes, flag the associated data as estimated. .18 Field Duplicates .13.1 Were field duplicates analyzed? [ ] J \ ACTION: If yes, prepare a Form VI for each aqueous field duplicate pair. Prepare a Form VI for each soil duplicate pair, if percent solids for sample and its duplicate differ by more than 1%; report ccncentraticns of soils in ug/1 on wet weight basis and calculate RPDs or Difference for each analyte. NOTE: 1. Do not calculate RPD'when both values are less than IDL. 2. Flag all associated data only for field duplicate pair. LS.2 Aqueous Circle all values on self prepared Form VI for field d-uplicates that are: RPD > 50%, or Difference > CRDL* Is any RPD greater than 50% where sample and duplicate are both greater than or equal to 5 time? *CRDL? Is any **differe.'vce between sanple and duplicate greater than *CRDL where sample and/or duplicate is less than 5 tines *CRDL? [ ] ACTTCN; If yes, flag the associated data as estirated. * S'abstitute IDL for CRDL when IDL > CRDL. ** Use absolute values of sample and duplicate to calculate the difference. 304540 STANDARD OFERATING JROCHURE :le: Evaluation of Metals Data for the Contract Laboratory Program Appendix A.l: Data Assesanent - Ccntract Corpliance (Total Review) Date: Jan. 1992 Nunber: HW-2 Revisicn: 11 YES ..18.3 6oil/Set1i.TTy*nt Circle a l l values cn self prepared Form VI for field duplicates that are: RPD >100%, or Difference > 2 x C3^L* Is any RPD (where sample and duplicate a r e both greater than 5 times *CRDL) : >100%? Is any **difference between sample and duplicate (where sample and/or duplicate is less than 5x *CRDL ): >2x *CRDL? ACTTON: If yes, flag the associated data as estimated. m NZA _ [_] X [ ] X .-19 Fom VTI (Tj^traratorv Control Saaple) (Note: ICS - not required for aqueous Hg and cyanide analyses.) ..13.1 Was one LCS prepared and analyzed for: each SDG? [LjL] each batch sanples digested/distilled? f X 1 both AA and ICP when both are used for the same analyte? [ _] _ X ACTTON: If no for any of the above, prepare Telephone Record Log and contact laboratory for submittal of results of LCS. Flag as estimated (J) cdl the data for which ICS was not analyzed. NOTE: If only one LCS was analyzed for more thsin 20 samples, then first 20 samples close to LCS do not have to be flagged as estimated. •* S^ubstitute IDL for CRDL when IDL > CRDL. •* Use absolute values of sample and duplicate to calculate the difference. 304541 STANI^RD OPERATING FRDCHJRE Ev'aluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Nunber: HW-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 Conplianoe (Tctal Review) ,19.2 Aqueous Ica Circle cn each Form VII the LCS percent recoveries outside control limits (80 - 120%) except for aqueous Ag and Sb. Is any LCS recovery: less than 50%? [_X_] between 50% and 79%? _ ^ [ ] between 121% and 150%? [_^] greater than 150%? fX 1 ?CTTOT: Less than 50%, reject (red-line) all data; between 50% and 79%, flag all associated data as estinated (J); between 121% and 150%, flag cdl positive (not flagged with a "U") results as estirated; greater thcin 150%, reject all positive results. ,19.3 Solid LOS NOTE: 1. If "Found" value of LCS is rejectable due to duplicate injecticrjs or aral\tlcal spike recovery criteria, regardless of LCS recovery, flag the associated data as estimated (J). 2. If IDL of an analyte is equal to or greater than true value of LCS, disregard the "Acticn" below even though LCS i s out of ccntrol .limits. Is LCS "Found" value higher than the control limits on Form VII? [ J L ] ACTION: If yes, qualify all associated positive ciata as e s t i r a t e d . Is LCS "Found" %'alue lower than the Control ,. limits on Form VII? [JiX] ACTION: If yes, qualify all associated data as estimated. 304542 STANDARD OFERATING raOCEDURE de: I>/aluation of Metals Data for the Contract Laboratory Program Appe-ndix A.l: Data Assessment - Ccntract ciJrplianoe (Total Review) Date: Jan. 1992 Nunber: HW-2 Revisicn: 11 ..20 1.20.1 Fom TS. (ICP serial Dilution^ - NOTE: Serial diluticn anedysis is required cnly for initial ccnoentraticns equzd to or greater than 10 x IDL. Was Serial Diluticn analysis performed for: each SDG? each matrix type? each concentration range (i.e. low, med.)? YES [ J p iJL.] [JL] ACTION: If jTo for any of the above, flag as estimated all the positive data >. lOxIDLs or >. CRDL when lOxIDL < CRDL for which Serial Dilution Analysis was not performed. m N/A 1.20.2 Was field blank(s) used for Serial Dilution Analysis? [ X l .20.4 ACTION: If yes, flag all associated data >. 10 x IDL as estirated (J). If lOxIDL <. CRDL, flag all data > CRDL. Are results outside control limit flagged with an "E" on Form I's and Form IX when initial concentratian on Form IX is equal to 50 times IDL or greater. ACTION: If no, write in the Contract-Problem/Non- Ccnpliance section of the "Data Assessnent Narrative". Circle on each Form IX all percent difference that are outside the control limits for initicd concentrations equal to or greater than 10 x IDLs only. Are any % difference values: > 10%? > 100%? iX _ _ ) ^ I 1 304543 SDMiARD OFERATING PROCEDURE :le: E'.'aluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Appendix A.l: Data Assessment - Contract Revision: 11 Conplianc^e (Ttotal Review) Yg ^ H2A" ACTTCM; Flag as estimated (J) edl the associated sample data >, lOxIDIs (or >.'CRDL vhen lOxIDL <. CRDL) for which percent differenoe is greater than 10% but less than 100%. Reject (red-line) £dl the 2issociated sample results equal to or greater than lOxTDLfi (or >. CRDL when lOxIDL <. CRDL) for vhich PD is greater than or equal to 100%. Note; Flag or reject on Form I's only the sample results v*iose associated raw data are >. lOxIDL (or >. CRDL when 10xIDL< CRDL) .^x Furnace Atonic Absorbtion (AA) OC Analvsis ^ Q £af(\p^^S UUeCC p .21^.1 Are duplicate injections present in fumaoe raw data Q.r\(\l^'?:^0 oy 'CK p (except during full Method of Standard Addition) for fj-rj . each sample analyzed by GFAA? [ ] ACTTON: If no, reject the data on Form I's for which duplicate injections were not performed. Do the duplicate injection readings agree within 20% Relative Standard Deviation (RSD) or Coefficient of Variation (CV) fcr concentration greater than CRDL? [ ] Was a dilution analyzed fcr sample with anedytical spi)<e recovery less than 40%? [ ] ACnON: If no for any of the above, flcig edl the cissociated data as estimated. Is *a-nalytical spike recovery outside the control limuts (85-115%) for any sample? [ ] ACTTON: If yes, flag the affected sample results if the recovery is betv^een 10-84%; if the reoovery is between 115-200%, flag the associated positive sample results as estimated; reject the eissociated sa.'Tole results if the recovery is less than 10%; reject positive sample results if the recovery is greater than 200%. .-.alNtical spike is not required on the pre-digestion spiked sample. 304544 r/)At' STANDARD OFERATING PROCEDURE Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Nunber: HW-2 Appendix A.l: Data Assesssnent - Ccntract Revisicn: 11 C o m p l i a n c e ( T o t a l R e v i e v ) IE£ NO N/A NOTE: Reject or flag the data only vhen the affected sanple(s) vas not subsequently analyzed by Method of Standard Addition. ,22 Form VITI (Met^vsd of gtandard Additicm Rearults) .22.1 Present? [ ] If no, is any Form I result coded vith "S" or a "+"? [ ] ACTTCN: If yes, vrite request on Telephone Reoord Log and contact laboratory fcr submittal of Form VIII. .22,2 Is coefficient of correlation for MSA less than 0.990 for any sample? [ ] ACTION: If yes, reject (red-line) the affected data. Was •.^iSA required for any sanple but not perlormed? [ ] Is coefficient of correlation for MSA less than 0.995? [ ] Are MSA calculations outside the linear range of the calibration curve generated at the beginning of the analytical run? [ ] ACTICN: If yes for cmy of the above, flag all the associated data as estimated (J). Was proper quantitation procedure followed correctly as outlined in the SCW on page E-23? [ ] ACTTON: If no, note exception under Contract Problem/ Non-Ccnpliance section of the "Data Assessnent Narrative", and prepare a separate list. !-'-SA is not required on LCS and prep, blank. 304545 STANDARD OFERATING FROCEDURE :le: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Nunber: HM-2 Appendix A.l: Data Assesanent - Ccntract Revision: 11 Ccnpiiance (Total Review) ^ ^ HzT 1-23 Dissolved/Total QT J-nrij-<7axiic/Totil TUalvtaa - 1 .23.1 Were any analyses performed for dissolved as well as total cinalytes cn the same Eaiiple(s). [ ] ^ Were cUTy analyses performed for inorganic as well as t o t a l (organic + inorganic) anedytes cn the same sample (s)? [ ] X NOTE: 1. If yes, prepare a l i s t corparing differenoes between a l l dissolved (or inorganic) and total analytes. Ccnpute the differences as a percent of the total anadyte only v*ien dissolved concentration is greater than CRDL 2is v e i l as t o t a l concentration. 2. Apply the follcwing questions only if i n - organic (or dissolved ) results are (i) above CRDL, and (ii) greater than total constituents. 3. At least one preparation blamk, ICS, and LCS should be analyzed in each analytical run. 1.23.2 Is the concentration of any dissolved (or inorganic) analyte greater than i t s total conoentration by - . Z.J - J. nore than 10%? [ 1 JL Is the concentration of any dissolved (or inorganic) a-nalyte greater than its tctal concentration by ^ more" than 50%? [ ] A ACTTON: If more than 10%, flag both dissolved (or inorganic) and total values a^ estimated (J); if more than 50%, reject (red-line) the data for both values. 1.24 Fom I (Field Elank) - (Note; Designate 'H^ield Blan>:^' aa such on Fom I.) 1.24.1 Circle all field blank values on Form I that are " greater than CRDL, (or 2 x IDL when IDL > CRDL). Is field blank concentration less than CRDL (or 2 X IDL when IDL > CRDL) for all parameters ^ of associated aqueous and soil sanples? [ ] /x 304546 STANEftRD OFERATING PROCEDURE :le: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program - Number: HW-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 Corpliance (Total Resriew) ~ ~ ~ ~ ISS. m N/A If no, was field blank valiie already rejected due t o other QC criteria? [ ] j£_ ACTTOH: If no, reject (except field blank results) a l l associated positive sample data less than or equal to five times the field blank value. Reject on Form I ' s the soil sample results t h a t when converted to ug/L on wet basis are less thsm or equal to five times the field blank value in ug/L. •-.25 Form X, XI. XII (Verification of Instnraental Paraeaeters). 1.25.1 Is verification report present for: Instrument Detection Limits (quarterly)? f X 1 ICP Interelement Correction Factors (annually)? [JL.] ICP Linear Ranges (quarterly)? [ J L ] ACTTON: If no, contact TPO of the lab. 1.25.2 Form X (Instrjcgnt Detection Limits) - (Note: IDL i s not required for Cyanide.) 1.25.2.1 Are IDLs present for: a l l the analytes? [ J L ] a l l the instruments used? [ J _ ] For both AA and ICP when both are used for the sane analyte? [ ] X TACTION: If no for any of the above, prepare Telephone Record Log and contact laboratory. 1.25L_2.2 Is IDL greater than CRDL for any analyte? [ X 1 If yes, is the conce-ntration on Form I of the sanple analyzed on the instrunent whose IDL exceeds CRDL, greater than 5 x IDL. [ ] 304547 STANEARD OPERATING HSXEDURE :le: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Progran Number: HW-2 Appendix A.l: . Data Assessaent - Oontract Revisicn: 11 Conpliance (Total Review) iE£ m Rlh Action : If no, flag as estimated all values less than five tires IDL of the instrument whose IDL exceeds CRDL. ..25.3 F o m XI (TiinfMir Ranqes) ..25.3.1 Was any sample result hJ.aher than h i ^ linear range ^ of ICP. ' r A 1 Wais any sample result h-igher than the hit^est w calibration standard for non-ICP parameters? [ J L ] If yes for any of the above, was the ^ sample diluted to qbtain the result on Form I? [ ] J_^ ACTION: If no, flag the result reported on Form I as estimated(J). .26 Percent Solids of Sp^'i'-v^ts .2{S.l Are percent solids in sadirent(s): < 50%? [J^] < 10%? [JL ACTTON: If yes, qaalify as estirated all the results of a sample that has per cent solids between 10%-50% (i.e. moisture content between 50%-90%). Reject adl the results of a sample that has per cent solids less than 10% (i.e. moisture content greater than 90%). NOTE: .^eject or flag (J) only the sample results that were not previously rejected or flaged due to other QC criteria. 304548 STANDARD OPERATING PROCEDURE lie: Evaluation of Mstals Data for the Contract Laboratory Program Appendix A.2: Data Assessment Narrative Date: Jan. 1992 Nunber: HW-2 Revisicn: 11 se* ntractor S^fg7 Bit. Xslat^A rIp>n.lJ Matrix: Soil X I*i> P^^r.P dn^UjicJ Water Roviewer Dor\ (\-r\f\t • I other ? T Validation Flaqs- The follcwing flags have been applied in red by the data validator and must be considered by the data user. J- This flag indicates the result quadified as estimated Red- Line- A red-line drawn through a sample result indicates unusable value. The red-lined data are known to contain significant errors basnd on documented information and must not be used by the data user. Fully Usable Data- The results that do rxjt C2rry "J" or "red-line" are fully usable. Contractual Oualifiers- The legend of contractual qualifiers applied by the lab on Form I's is found on page B-20 of SOW IIMOl.O. .2 -The data assessment is given belcw and on the attached sheets. Pnc^ ft/)aLf/cA W r : 9 7 / ^ 7 o tn vo STANTARD OPERATING PRDCEEURE :le: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Nunber: HW-2 Appendix A.2: Data Assessment Narrative Revisicn: 11 .. 2 (continuation) 304550 STANEftRD OPERATING FRDCHURE .tie: Evaluation of Metals Data for the Date: Jan. • 1992 Contract Laboratory Program Nunber: HW-2 Appendix A.2: Data Assessment Narrative Revisicn: 11 2.2 (continuation) w o »{^ tn tn STANDARD OFERATING FRDCEDURE tie: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Nunber: HH-2 Appendix A.2: Data Assessment Narrative Revisicn: 11 .3 Contract-Problem/Non-Ccnpliance I---3/ESAT Rviewer: ' Date:_ Signature -.tractor Reviewer: Date: " Signature Verified by: Date: 304552 STANDARD OFERATING PRDCUURE .Utle:' Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Nunber: HW-2 Appendix A. 3: Contract Non-Ccnplianoe Revisicn: 11 (SM) Report) CCNIRACT NCN-CCKPLIANCE (SMD REPCKT) Regional Review of Unccntrolled Haizardous Waste Site Ccntracx Laboratory Data Package CASE NO. 2 hardcepied (laboratory name) • rrganic data package received at Regicn II has been reviewed and the quality assura-nce and .-formance data summarized. The data reviewed included; } Samole No.: ' ^.c. & Matrix: ^iTs No. ( )_ requires that specific analytical vrork be done and sociated reports be provided try the contracxor t o the Regions, EHSLrLV, and S>D. The 1 criteria used t o determine the performance were based on an examination of: - Data Ccnpleteness - Duplicate Analysis Results - Matrix SpiJce Results - Blank Analysis Results - calibration Standards Results - MSA Results r-s of no.n-compliance with the above contract are described belcw. Reviewer's I n i t i a l Date 304553 SD^NDARD C5=ERATING tWXlLURZ Evaluaticn of Metals Data for the Contract Labcoratcry Program Appe.nQix A.4: Mailing List for Data Reviewers Date: Jan. 1992 Nomber: HW-2. Revision: 11 tm^nrx: IATT-Kt t»^ iiui^i^ i . ISWX r ^ i e r . I (ES3) *0 Urn/TVx^- r w t Uadnr-a-.. W. C21"J3 cr. K.. ».. w, w, vr (It aen.i;at4 te«:3 C-.JZX £4.-ils ( 3 : : ) 2 t i - 9 : t D t c . K r . ?*.. \ X . v v . EC c«.-.t*c. K;r-4.-.. rrr, KJ-ty. \T7SWI. S-.i3»c-. 7«cr... t ^ y FA i . VTr?A Rac;:=r. V f t s r ; 53i Sa-t.*. C : i r k S^-»«t Ttrv. r;ocr. cv:. 3::-3S3-s;t- : i . S : . >C. >?•. CH. v - ; f'TT^t.sri t i l l Un7A Ka::=r. \ - : K.L-JA» C ; r / . >3 Ctir* rcrry (s:3, ; j t - : E ! : 3:. KS. K5. K: Vrr?A K«;:cr. DC (ISO) Oiv Ki.-»^-e.-r: s*cr:jcr. 5:i rrc-o-r. S--r*et SA.-. m n c i i s c . CA S«iOS (<:i) s^^-w:* A2. CV. K". SV. A-«r:cA.-. S A - T M . OLA-. T T J S - . ZtSTZ'—TitA Di P%ZiiXC A : ^ . CAl Vcs-.cr.. S-Cubod, 17-CA. Xlliacn, N M J s T M y O t t 3 7 (301) 3 3 1 - M ? ( KJ, W . PR. V3 C v n u r y , OT»T»-r., US T « c t . 10.130, n c , telAon. O S , telJkcn, IQ*. USTPA Hiqicn TJ (TSZ) A . - ^ y T i a . : g4<ii."i a . v » J . AViKY. CA 30«13 T » . fttinert. J r . (4M) fr4i-3112 Al. n . . CA, lor, « s , X . s c , T V CapjCTier., C 5 . E S I , f B L J , USt?A lte;icr. VI (ESO: ttot Hcrrwocii trjv« H a u n J T . TX 7707< (7:3) tS3-3«25 JkR. u . }f.. rx Ri-wfirj-.. Irn. X:ii«:, Kry TX. OK SPECS, izs. c: I . Un7A RBc:a-. VIZZ l A i c n z r r / BOX 31366 DtTver- r « c ! t n J O t - x t r r v i K:!i-*.-. (3:3) 2 : 6 - 7 3 7 : CC. Ko. $r. vr. v\. yc A=Z;. C^CU, » < M . CBtJ Cier., O t , - « : 30. US3'A Ka[;:cR X l A i o n t a r y P.O. SOX &4» Ki.tSTes-.«r. Wk t ! 3 5 3 C*.-TUd « j y i (206) 442-0370 AX. I D . Of^, Wk U J O U Ttstin; Lai*, Ct-Ttury- Ttsti-ij Ui» (Tor VCA Oc.:y), Ueyt.-T>ftj»*r Cc. CS5j\rti« Tts'.irq, Silvtx v»:iley 3 : . Ci.-:* De.-pa<>- - (a£-23w) L'SrrA 4c: " r - s-_-«-.. S.V. Vti.M.-ic--=r.. OC J U t t rrs 3e;-i-ie 33. Si-?:e r«^-^3e-e-.^ c:;;=« v,i.- ere Cs-^£.-.,- T.z. E ) £:E 33. t i . - K n Xi.-.tcr l'SI7A t>31-LV m t. Hi_-nr-. Avtnje BOX t3<-;8 lAi Vegii. K"." J S : : 5 304554 STANDARD OFERATINC FRDCEDURE Title: Evaluation of hJetals Data for t ^ Contract Laborarory Program Appendix A.6: CLP Data Assessment Summary Form (Inorganics) P a g e 3 4 o f 3 5 Date: Oct. 1989 Number: HW-2 Revision: 9 Type of Hcvlcw: S i t e ; X ^ l a r ^ A C / l P m i C a l CLP DATA ASSESSMENT SUMMAKY rOIW (INOtCXJilCS) t^r.^MX Revlewar't I n l c l a l a : D6A U b N«»a; rOCe, H / ) C \ l A i c 4 27 Kuabar of Saaplaa: Analytai H«1«cc«d Due to Exeeadlm tavl«» Criteria:* ICP Flaaa AA rurnacc AA Mercury Total C ^ / Holding Tlaea o C»llbratlor o Prep ilBlank Field SUnk 1 o 1 ^ I n t e r - fereccea o 1 I I I 1 n 1 0 1 0 1 O 1 o \o 1 o\o Y 1 X [other ' 1 I I I Splka 1 Dupllcataa Reeove rr 1 Lab 1F1eId HZ \o\ X 1 ^ 1 0 , ol X ol yc Detection Ll>lta o 0 0 LCS o \0 o r Serial Dilution o yc 1 )" HSA y- r- |y l o c a l Aaalytea STi zn 27 KcleetloB V7 0 o Analftta Flamed a« Eitlmaced (J^ Due to ticeedlm Criteria For:* ICP 1 O 1 iZ- 1 o 1 o 1 ria»e AA 1 1 Furnace AAI [Mercury T ) Total CK/ 0 lOther 1 o 0 O 1 0 0 1 0 o X X IZ Iva 1 O 0 X O y; o \o yc 0 o 0 // 0 0 X % ^ )C y -f9v Zl Zl 137 0 6 Note: Aaterlik (*) lodlcatea a d d i t i o n a l azceedancea of review " c r i t e r i a . 304555 STANDARD OPERATING FRDCEHIRE T i t l e : Evaliiaticn of Metals Data for t h e Contract: Laboratory Program Appendix A.7: CLP Data Assessment Checklist Inorganic Aralysis Date: Oct. 1989 Number: HW-2 Revisicn: 9 INCffGANIC REGIONAL DATA ASSESSMENI CASE ND. SITE 3 1 S I Cind CJiimixxL Region 2. LABCRAIDRY pQco f^nJifhr./^l SDG# ?«ffl7 'r NO. OF SAMPIZS/ MAIRIX a/. 6 CiU ^LUFlieR SOW* 3Lfno3. O REVIEHER (IF NOT ESD)_ REVIEHER'S NAME f ) o n hi /le DPO: ACTICN TH. 1. HOUIENG TIMES 2. CALIBRATiaG 3. BLANKS 4. ICS 5. ICS 6. DCMJCATE ANAKiTSIS 7. MAIRIX SPIKE 8. MSA 9. SERIAL DninrcN 10. SAMPLE VERHTCAirO^ 11. OlHtR QC 12. OVERALL ASSESSHEOT A CCMPLETiai DATE A/oV ^ / 9 ^ 7 DATA ASSESSMEOT SU-IMARY TJ ICP AA IX x ML * o :n: & o XL S I 0 = Data hcis no problems/or qiial if ied due t o Tninrrr probleans. M »= Data quadified due t o major problems. Z = Data unaccmnable. X = Problems, but do not affect data. CTaNTTF. & .Q. ACTION ITEMS: AREAS OF OZNCERN: NOTABLE ItRtUWiANCE: 304556 --• SO(^i^ 97/8'7 SOP NO. Kr7-6 Revision iS CLP ORG A:; J :.<: DATA -.rviin _ / • • ^ - ^ BY: ^^*-^--.\ \ . 'Xl^ ^^^ Leon^L^iarus. Z.-.vircr.r.en-cal sciEn"L:.st T C X I C and Hazardous Kasre Secticn 3V: M-^.^IA. Ceorce Ki^rras, c.'^.eriist Tcxic a.".d .Harardcus Waste Sec-> / 1 — ' / yy. < 'il' ? < t cc::cLT.?.rr- BV: '^^-.^ ' ^ • \ ^ Kevin .Kubiii^—^lef Date: , Ji2.^. J-ry'^i, Da teJ:?^2:±5^j-- / ^ ^ i - r- S t a l l OS G e r a z c u . n i s / C'-.enist T c x i c and Hazardous Wasre S e c t i c n Date:, Uk^ azarrc^iis Waste S e c t i o n ) Rotrert .Runyon. C.'xief M o n i t o r i n g .Management Eranci Date / ' / 304557 STAKDARD CPZHATXIIG rHOCZCL^ Date: J a n u a r y 12 92 R a v i s i o n : 8 — — ^ ^ : ^ H/A PACKAGE CZXPIZmrZSS AND DILIVZllABLES o A , > I efeSr- >rJHB£R: qn \ 9-.n TAR; /"r;^.& Ar.rJ.. HC^' SITZ: -i.s/^MvJ Ch^n.-'^ rrv' K 1«0 Data Completeness and Daliveracies 1.1 Have any r.issinc deliverables been received and added tc t.'".e data package? I I ACTIc:;: Call lab fcr explanation/resubrittal cf any nissinc deliverables. If lab cannot provide tham, note t.'-.e effact on review of the pacicace under tha "Ccntract Probi£Es/Non-Ccc:piiance" sacticn of reviewer narrative. 1.2 V a s sy.Q CZZ chacklist included with paOcage? 1 1 JL, 2.0 ccver :.;tt5r STC •'••srr-t'.vg 2.1 Is t.^'.s N'arrziive or cover Letter Present? f^"* 2.2 Are Ci&e Nunbar and/or SAS nur±ier contained s ^ in the Narrative or Ccver letter? r ^ - _ j L 1 Q Data v= 1'•'^•»•••'-- '-'-of-v-t •• c« The fcllcvine checklist is divided i.-.tc three p a r t s . Part A is filled out if tha data package contains any VOA analyses, Fart S fcr any E.KA analyses and Part C for Pssticida/PCBs. Does t.Ms packaoe ccntainr ^ Ul LP CX3 VOA Data? _J:i. WI BKA Data? X Pesticida/PCB data? JL Acticn: ctr.plcte ccrraspcndinc parts c: c^.ecklist. STA};DARD :?Z?-ATI:IG ??.OCZZ'JT.Z Date: Jinuary 13 32 Revisicn: £ YZS .SO hVA * ' *• " •< < • - ' n r r n ^ A M a M • » ••0 T r a f f i c ?oT?r*—••? J''-' T ,K^.-.« <-.-.—. vi,.^.,-,.--i..p 1.1 Are the Traffic Report For=s presenr fcr 1_1 A L a l l samples? ACTIG^I: If no. ccnticc lab fcr rsolaceaenr of nissinc or i l l e g i b l e copies. 1.2 Do the Traffic Repcrts or Lab Narrative indicate any prcblens with sample receipt, conditicn of samples, analytical problems or special circucis-ances affecting the > quality of t.he data? rXl ACTIG::: if any sample analyzed as a soil, other than TCL?, contains 50\-90* water, all data should ba flagged as estinated (J) . if a s o i l sample other than TCL? contains more than 90% varer, all data snouid be qualified as unusable (R). ACTIG:r: If samples vere not iced upcn receipt ar t.*:e laboratory," flag all positive results *'J"' and a l l Non- Detects "L'J". ACTICN: If both VOA vials fcr a sample have a i r bubbles .-or the VOA vial analyzed had air bubbles, flag a l l positive results "J" and a l l non-detects "R". 304559 - 2 - STAKDARD 0?Z?JvTi:iG ?ROCZZU:iZ D a t e : Januar-/ 1S92 R e v i s i c n : s YES h'O N/A 2-0 H Q l d i r - ' - ^ - « ^ 2 . 1 Have any VOA t e c h n i c a l holding t i n e s , d e t e m i n e d f r c n d a t e of c o l l e c t i c n t c d a t e of a n a l y s i s , b e e n exceeded? If u n p r e s e r v e d , aqueous samcies m a i n t a i n e d a t 4'C vhich a r e t c be analyzed f c r a r o m a t i c .Vr'drccarccns must be analyzed v i t h i n 7 days of c o l l e c t i c n . If preserved v i t h .HCl (?.".<2i a.nd s t o r e d a t 4*C, t h e n aqueous samples must be a n a l y z e d v i t h i n 14 days cf c o l l e c t i c n . If u n c e r t a i n a b o u t p r s s e r v a t i c n , c c n t a c t sampler t c d e t e r m i n e whether cr not s a m p l e s v e r e p r e s e r v e d . The h o l d i n g t i m e fcr s o i l s i s 10 d a y s . Table of " o l d i r r "-^r.e V< cl ?.t-: orr^ (See T r a f f i c Report; Sample Sample Date Date Lab Cate ID Matrix ? r e s e r \ ' e d ? Samcied Received Analyzed o tn o ACTIc:;: If technical holding times are exceeded, flag all positive results as estimated ("J") and sampie quantitation limits as estimated ("UJ"5, and document in the narrative that holding times were exceeded. If analyses vere dene more than 14 days beyond holding t i n e , either cn the first analysis or upon re-analysis, the reviewer r.ust use professional judgement tc determine t.^.e reliability of the data and t.^e effects of additicnal storage on t.^e samoie r e s u l t s . At a minimum, a l l r e s u l t s must te qualified'"J", but.the reviewer may determine chat non-de*tecr data are unusable (R). If holding times are exceeded by ••mere than 2S days, a l l ncn detecr data are unusable (R) . STAh'DARD C?Z?JvTIKG ??.0CZZ*J7^ Date: J a n u a r y 1S32 R e v i s i c n : 8 YZS .HO N/A a. b. c. Low Low Med Water Soil Soil 2 . 0 SVSter " — ' - - ~ - r—..........4 (cvtny -Sa^-rvc-V ^'^'^T" "^Tl 3.1 Are the VCA SMC Reccvery Summaries (For= II) present for each cf the following r a t r i c e s : • . i A L k 3.2 Are all the VOA samples listed on the apprcpriate Sysren Monitoring Compound Reccvery summary fcr each of t.'-.e following r.atrices: r>i £?i i l l ACTIc:;: call lab for expianarion/ resubmittals. If missing deliveracles are unavailable, document effect i.n data assessments. 3.3 Were outliers marked correctly vith an asterisk? ACTIc::: Circle a l l outliers in red. 3.4 Was one or more VOA system monitoring compound recovery outside of ccntract specificatic.ns fcr any sampie or method blank? If yes, vere samples re-analyzed? Were method blanks re-analyzed? a. b. c. Low Low Med Water Soil Soil )S J L LIL ^ JA XXL — X ^ 304561 A - Date: J a n u a r y 12 92 Revision: s YZS NO N/A ACTION: If r e c o v e r i e s a r e > 101 b u t 1 cr more compounds f a i l t o meet: SOW s p e c i f i c a t i o n s : 1. All positiva r e s u l t s are qualified as estimated ( J ) . 2. Flag all .-.on-detects as estimated detecticn limits ("UJ") where reccvery is less t.han t.'-.e lover acceptance l i n i t . 3. If SMC recoveries are above allcvable levels, do not qualify non-detects. If any system monitoring compound reccvery is <10\ : 1. Flag all positive r e s u l t s as estimated ("J") . 2. Flao a l l ncn-detects as unusable ("R"). Professional judgement should be used to q-jalify data that only have method blank SHC raccveries cut of specifioaiicn in both criginal and re-analyses. Checx r.^.a i.-.rar.nal scandard areas. 3.5 Are there a.^.y transcripticn/calculaticn errors berveen raw data and Form IT? ACTION: If large errors e x i s t , call lab fcr expianaticn/resubmittal, .make any necessary corrections and nore errors in t.*:e data assessment. X .0 Matrix Sr-v°c (^orr. TTT1 4.1 Is the Matrix Spike/Matrix Spike Duplicate Recovery Form (Form III) present? , % 304562 STANDARD C?ZRATI^'3 PROCZZL'RZ Date: January 1292 Revisicn: 8 YES NO N/A 4.2 Were matrix spikes analyzed at t h e required frequency fcr eacc of t.he fcllcving matrices: a . Low Water r i V" b. Lov Soil jJL c. Med Scil _r_2 >( ACTIc::: If any matrix spike data are missing, take the acticn specified in 3.2 above. 4.3 Hov many VOA spike recoveries are outside QC limits? out of 10 O out cf 10 4.4 Kow many RPD's fcr matrix spike and matrix spike duplicate recoveries are cutside QC limits? our of £ I out 01 5 ACTICN: No acticn is taken based cn MS/MSD data alone. However, using informed professional judgement, the MS/MSD results may be used in conjunction wit.h other QC criteria tc determine the need forT-qualificaticn of the data. 5.0 Blanks ^-orm ^V^ 5.1 I s t h e Method Blank Summary (Form IV) , p r e s e n t ? r^i ' ; CJJ o (^ 5.2 Frequency of Analysis: for the analysis ui of VOA T C L compounds, has a reagent/method ^ blank been analyzed for each SDG or every 20 samples of similar matrix (lev water, lov soil, medium soil), whichever is.more freouent? OJ ck STAKDARD CPZRATIMG PROCZZL'RZ Date: J a n u a r y 1292 R e v i s i o n : a YES HO N/A 5.3 Has a VOA method/instrument blank been analyzed at least once every tvelve hours for eacn ccncentraticn level and CZ/liS system usad? I K^ ACTICN: If any method blank data are nissing, call lab for explanaricn/ resubmittal. If method blank data are not available, reject (R) all associated positive data. Hovever, using professional judgement, the data reviewer may subszitute field blank or trip blank data fcr missing method blank data. 5.4 Chrcmarcgrap.ny: review the blank rav data - chrcmarcgrams (RICs), quant reports or data system printouts and spectra. Is the c.hrcm.atcgraphic perfcrmance (baseline stacilitv) for each instrument acceotable y for VOAs? * i£l _ ACTIC:**: Use profassional judcament tc deterr.ine t.ne effect on the data. 6.0 contar.i--''^ ••'"- i;OTZ; "Water blanks", "drill blanks", and distilled varer blanks" are validated like any other sampie, and are not used tc cjualify data. Co not confuse them with the cr.her QC blanks ttiscussed below. 6.1 Do any method/instrument/reagent blanks have positive results (TCL and/or TIC) for VOAs? When applied as described balov, the contaminant ccncentraticn in these blanks are multiplied- by the sample dilution factor and ^Z corracred fcr t moisture vnen necessary. : _. f 1 6.2 Do any field/trip/rinse blanks have positive ^ VOA results (TCL and/or TIC)? JL H- ACTICN: Prepare a list of the samples associated wit.h each or the contam.inared blanks. (Attacn a 304564 seoarate sheet.) STANDARD CPZRATING PROCZZJR.Z Date: J a n u a r y 1292 R e v i s i c n : 8 YZS NO N/A NOTZ: All field blank results associated to a part:.cular group of samoles (may exceed one per case) must ba used tc qualify data. Trip blanks are used to qualify only those samples vith vhich they vere shipped and are not required for non-aqueous matricas. clanks may not be c-jalified because of contamination in another blank. Field Blanks i Trip Blanks must be qualified for system monitoring compound, i.nstrument perfcrmance criteria, spectral or calibration QC problems. ACTIO:;: FOIIOV Che directions in the table belov- to qualify TCL results due to contaminaticn. Use the largest value from all the associated blanks. If any blanks are grossly contaminated, all associated data should be qualified as unusable (R). Sannle cone > CRQL Samoie cone < CRQL Sample cone > CRQL but < lOx blank & <iox blank value i >10x bla.nk value value y.zzr.yl ene Chloride Flag samnle result Report C.~QL i Acetcne with a "U; qualify "U" Toluene 2-Butanone No crualificaticn is needed Saaole cone > CRQL Sample cone < CRQL i Sample cone > CRQL but' < 5x blank is < 5x blank value value & > 5x blank value Other Flag samole result Report CRQL i Ccntam- with a "U" qualify "U" inants NO crual if icaticn is needed NOTZ: Analvtes cjalified "U" for blank contamination are s t i l i oonsidered as "hits" vhen q-uallfying fcr calibration c r i t e r i a . 304565 7 . 3 STANDARD OPZRATIKG PROCZCL-RZ Date: J a n u a r y 1992 Revision: a YES NO N/A ACTION: For TIC compounds, i f t h e c c n c c n r r a t i c n i n t h e sampie i s l e s s than f i v e t i m e s t h e c o n c e n t r a t i c n i n t h e most c e n t a n i n a t e d a s s o c i a t e d blank, f l a g t h e - sample data "R" (unusable) . 6.3 Are t h e r e f i a l d / r i n s e / e o r u i m m e n t blanks Y~ a s s o c i a t e d v i t h every sampie? r ^ A C T I O : : : .-©r l e v l e v e l samples, n o t e i n d a t a assessment t h a t t h e r e i s no a s s o c i a t e d f i e l d / r i n s e / e q u i p m e n t b l a n k . Z x c e p t i c n : samples t a k e n from a dri.nking w a t e r t a p do n o t have a s s o c i a t e d f i e l d b l a n k s . - r u i l i i r . i r » » . n i , . V - . • w - , ^ - - . , . . 7.1 Are the GC/MS Instrument Performance Check Forms (Form V) present fcr Bromofluorobenzene ^, (BFB)? X}k 7.2 Are the enhanced bar gramh snectrum and mass/charge (m/z) listinc for the £73 . provided for eacn tvelve hcur shift? ^A Has an instrum.ent perfcrmance compound been analyzed for every tvelve hours of sample y analysis per instrument? ' r n 304566 STAaNDARD C?Z?J^Ti:iG PROCZZ'JRZ Date: January 1392 Revisicn: S YZS NO H/A ACTICN; List date, time, instrument ID, and sample analysis for vhich no associated GC/KS timing data, are available.- DATZ TI>£Z INSTR'J>CZ:irT SAHPLZ KUHBZRS ACTICN: If lab cannot provide missing data, reject ("R") all data generated cutside an acceptable twelve hour calibration interval. 7.4 Have the icn abundances been norm.aiizad tc m/z 9 5? f y? __ ACTIC::: If mass assicnm.ent is in errcr, qualify all associated data as unusable (H) . 7.5 Have t.he icn abundance criteria been net for , each i.-.strum.ent used? f~-^ _ • ACTICN: List all data which do not m.eet icn abundance criteria (attach a separate sheet). ACTIO:;: if ion abundance criteria are not met, the Regicn II TPO r.ust be notified. 7.6 Are there any transcripticn/calculaticn errers between r.ass lists and Fora Vs? (Check at least two values tut if errors are fcund, check nore.) X 304567 STA};DARD cpz?j.Ti:rG PHOCZZLTJ: Date: January 12 32 Revision: S YES NO N/A 7.7 Have the apprcpriate number cf sianificant . figures (tvo) been, reported? ' f/N ACTICN: If large errors exist, call lab for explanation/resucmittal, make • necessary corrections and document effect in data assessments. 7.S Are the spectra of the mass calibraticn ^ compound acceptable? f'^i ACTICN: Use professional judgement to determ.ine vhether associated data should be accepted, qualified, or rejected. 8.0 Tarcet Commcun-* ''' ^t crrry »n?ivroc 8.1 Are the organic Analysis Data Sheets (Form I VOA) present v i t h required header infcrmaticn cn each page, fcr eacn cf the folloving: a. Samples and/cr fractions as appropriate f ^' b. Matrix spikes and matrix spike . duplicates " rHi c. Blanks J l l 8.2 Are the VOA Reconstructed Icn C.hrom.atograms, the mass spectra for the identified compounds, and the data system printouts (Quant Reports) included in the sample package for each of the following? a. Samples and/or fracticns as apprcpriate LJl b. Matrix spikes and matrix spike \l duplicates (Mass spectra not required) j j l c. Blanks Xhl ACTICN'; If any data are missing, take acticn specifiad in 3.2 above. 304568 STANDARD CPZRATIKG PROCZZ'JRZ Date: January 1392 Revision: s ~~" YES NO N/A 8.3 Are the response factors shovn in the Quant Repcrt? r ^ 8.4 Is Chromatographic performance acceptable vith resoect tc: 5aseii.-,e stability? Resolution? Peak shape? Full-scale graph (attenuation)? Other: X lit X X r T Y ACrrc:;: use professional judgement tc determine the acceptability of the data. 5.5 Are the lab-generated standard mass spectra of tha Identified vcA cor.pcunc3 present fcr each sampie? ACTICN: If any r.ass spectra are missing, take acticn specified in 3.2 above. If lab does not generate their own standard spectra, make note in "Contract Froblems/Non-com.pliance". 8.6 Is the RRT of each reported compound vithin 0.05 RRT units of the standard RRT in the continuing calibration? 8.7 Are all ions present i.n the standard r.ass spectrum, at a" relative intensity greater than 12\ also present in t.he sample mass spectrum? Yl r XI ^ sX - 304569 Date: J a n u a r y 1S92 Revisicn: 8 YZi NO N/A 8,8 Do sample and s t a n d a r d r e l a t i v e i o n N, i n t e n s i t i e s agree v i t h i n 201? r n ACTICN: Use p r o f e s s i o n a l judgement t c datermine a c c e p t a b i l i t y of d a t a . If i t i s d e t e r m i n e d t h a t i n c o r r e c t i d e n t i f i c a t i o n s v e r e made, a i l such data snouid be r e - j e c t e d (R) , flagged "N" (presumptive e v i d e n c e of t h e presence cf t-he compound) c r changed t o not d e t e c t e d (U) a t t h e c a l c u l a t e d d e t e c t i c n l i m i t . In order t o be p o s i t i v e l y i d e n t i f i e d , the data must comply v i t h the c r i t a r i a l i s t e d i n 8 . 6 , 8 . 7 , and 8 . 8 . ACTICN: When sample c a r r - / - o v e r i s a p o s s i b i l i t y , p r o f e s s i o n a l judgenent should be used t c d e t e r m i n e if instrument c r o s s - c o n t a m i n a t i c n has affected any p o s i t i v e cempeund i d e n t i f i c a t i o n . T e n t 5 t i v 9 l v Tdgntified commcunds CTZZ'. 9 . 1 Are a l l T e n t a t i v e l y I d e n t i f i e d Ccmpound Forms (Form I Part 5) p r e s e n t ; and do l i s t e d TICs i n c l u d e scan number o r r e t e n t i o n t i m e , •</ e s t i m a t e d c c i c e n t r a t i o n and "JN" q u a l i f i e r ? L t l - 9.2 Are t h e mass s p e c t r a f c r t h e t e n t a t i v e l y i d e n t i f i e d compounds and a s s o c i a t e d " b e s t match" s p e c t r a i n c l u d e d in the sample p a c k a g e f c r each of t h e f o l l o v i n g : a . Samples and/or f r a c t i o n s a s a p p r o p r i a t e LfJ. - b . Blanks i—1 ACTION: If any TIC data are missing, take acticn specified i.n 3.2 above. ACTION: Add "JN" q-.:alifier if missing. 304570 STANDARD CPZRATING PROCZZ'JRZ Date: January 1292 R e v i s i o n : a YES NO N/A 9.3 Are any TCL cempou.nds (from any fraction) listed as TIC compounds (examnie: 1,2- dinetnylbenzene is xvlene- a VOA TCL analyte - -nd should not ba reported as a TIC)? rVi ACTIC:;: Flag vith "?." any TCL ccmpound listed as a TIC. 9.4 Are all icns present in the reference mass spectrum vith a relative intensity greater than 101 also present in the samcie mass spectrum? 9.5 Do TIC and "bast match" standard relative ion intensities agree vithin 20%? ACTICN: Use professional judgement to determine accaptability of TIC identifications. If it is determ.ined that an incorrect identification vas made, chance identification tc "unknown" or tc some less specific identification (example: "C3 substituted benzene") as apprcpriate. Also, vhen a ccmpound is not fcund in any blank, but is detected in a sample and i-s_ a suspected artifact of a common laboratory contaminant, the result should be cnialified as • unusable (R) . (i.e. Common Lab Contaminants: CO, (M/E 44), Siloxanes (M/E 73) Hexane, Aldol Condensation Products, Solvent Preservatives, and related by products - see Functicnal Guidelines for more guidance). 304571 STA};DAR.D c?z?jiTi:;c ?ROCZZL-?.Z D a t e : J a n u a r y 1292 R e v i s i o n : 8 YES NO N/A L i m i t " 10.1 Are there any transcripticn/calculaticn errors in Form I results? Check at l e a s t tvo positive values. Verify that the correct internal stancard, quantitation icn, a.nd RRF vere used tc calculate Form I r e s u l t . Ware any errors fcund? ty^ 10.2 Are the CRQLs adjusted tc reflect sample diluticns and, fcr soils, sample moisture? fAi ACTIc:i: If errors are large, call lab for expianaticn/resubmittal, m.ake any necessary corrections and note errors under "Conclusions". ACTICN: When a sampie is analyzed at more than one d i l u t i c n , t.he lovest CRQLs are used (unless a QC exceedanca dictates t.he use of the higher CRQL data from the diluted sample analysis). Replace ccncentraticns that exceed the calibraticn range in t.he original analysis by crossing out t.he "Z" and i t s associated value on the original Fom I and substituting the data from t.he analysis of the diluted sample. Specify vhich Form I is to be used, then drav a red "X" acrcss 'S^^e entire page of a l l Form I ' s t h a t should not be used, including any in t.he sumnary package. 11.0 " Star.dsrds Data iGC/ys) 11.1 Are the Reconstructed Ion Chromatograms, and data system printouts (Quant. Reports) present fcr i n i t i a l and ccnti.huing / calibration? I l l ^—• ACTICN: If any calibraticn standard data are nissing, take action specified i.n ' 3.2 above. 304572 STANDARD OPZPJ^TING PROCZZ'JRZ Date: J a n u a r y 1392 R e v i s i o n : S YZS NO N/A 12.0- GC/'"'^ r _ < - - , i / - , i ; v-,...; „„ (-r^— trri 12.1 Are the I.nitial Calibration Forms (Form VI) present and complete for tha volatile fraction at concentrations of ID, 20, 50, 100, 200 ug/1? Are there separate calibraticns fcr lov vater/med soils y and low soil samoles? i J l any calibraticn standard forms are missing, take action specified in 3.2 above. 12.2 Were all lov level soil standards, blanks and samples analyzed by heated purge? i j ^ . —^ ACTICN: If lov level s o i l samoles were not heated during purge, qualify positive h i t s "J" and non-detects "R". 12.3 Are response factors stable for VGA's over the concentration range of the calibraticn (^Relative Standard Deviation , (IRSD) <30.01 )? I—1 - ^ ACTICN: Circia a l l c u t l i e r s in red. NOTZ: Althougn 11 VOA com-pcuncs have a minimum RRF ana no maximum iRSD, the technical c r i t a r i a are the same fcr all analytes. ACTICN: If \RSD > 3 0.01, qualify associated positive results for t.hat analyte "J" and non-detects usinc professional judcement. When RSD > 901, f l a g ' a l l non-detects fcr t.hat analyte R (unusable). NOTZ: Analytes previously qualified "U" for blank^^ contam.inaticn are s t i l l considered as " h i t s " when q-ualifying for i n i t i a l calibraticn c r i t a r i a . 12.4 Are the RRFs above 0.05? -U^ Action: Circle a l l outliers in red. Action: If any RRF are < 0.05, qualify associated^^ non-detects (R) and flag associated posi^-.e data as estim.ated (J). - 16 - STANDARD OPERATING PROCZZ'JRZ Date: J a n u a r y 1392 Revision: 8 YZS NO N/A 1 2 . 5 Are t h e r e any t r a n s c r i p t i c n / c a l c u l a t i c n e r r o r s in t h e r e p o r t i n g of a v e r a g e response f a c t o r s (RRT) or 1RSD7 (Check a t l e a s t 2 v a l u e s , b u t v, i f e r r o r s are fcund, check more.) . L L I . 13.0 G C / y C—---•.•:-~ '-,i/u-,.-.<— ^T^— ,f"'^ 13.1 Are the Continuing Calibraticn Forms (Form VII) present and complete for the \. v o l a t i l e fraction? " r /^ 1 3 . 2 Has a c o n t i n u i n g c a l i b r a t i o n s t a n d a r d baen analyzed for every t v e l v e hours of V sample a n a l y s i s per i n s t r u m e n t ? r "t A C T I O : ; : L i s t balow a l l sample a n a l y s e s t h a t ware not v i t h i n t w e l v e hours of t h e p r e v i c u s c o n t i n u i n g c a l i b r a t i c n a n a l v s i s . ACTICN: I f any forms are m i s s i n g o r no c o n t i n u i n g c a l i b r a t i o n standard h a s been analyzed v i t h i n t v e l v e h o u r s of every samnle a n a l y s i s , c a l l lab f o r e x p i a n a t i o n / r e s u b m i t t a l . I f c o n t i n u i n g c a l i b r a t i o n d a t a a r e not a v a i l a b l e , f l a g a l l a s s o c i a t e d s a m p l e d a t a a s u.nusable ("R"). 1 3 . 3 Do any v o l a t i l e compounds have a 1 Diffarence (1 D) betveen t h e i n i t i a l and c o n t i n u i n g v/ RRF v h i c h exceeds t h e + 251 c r i t e r i a ? A,., I—1 ^ ACTION: C i r c l e a l l o u t l i e r s i n r e d . ACTION: Qualify both p o s i t i v e r e s u l t s and n o n - d e t e c t s f c r t.he o u t l i a r compound (s) as e s t i m a t e d . When % D i s above 901, r e j e c t a l l n o n - d e t e c t s f o r t h a t a n a l v t e (R) u . n u s a b l e . o tn -J O X^viiDi^jVij w.-i.-J\Ta.:iu r-.-.Oi-Z--.--:. Date: January 1992 Revisicn: S YES NO N/A 13.4 Do any v o l a t i l e compounds have a RKF <0.057 ." t V ACTICN: Circle all cutliers in red. ACTICN: If the F-RF <0.05, cjualify associated non-detects as unusable (R) and "J" associated positive values. 13.5 Are t.here any transcripticn/calculaticn errors in the reporting of average response factors (RRF) or ^difference (ID) betveen i n i t i a l and continuing RRFs? (Check at least tvo values but if errors are found, check r.ore.) ACTIO:;: circle errors in red. ACTIO:;: if errors are large, c a l l lab for expianation/resubmittal, .make any necessary corrections and note errors under "Conclusions". ' J . , I - . . - . ... V . 14.1 Are the i.nternal standard areas (Form VIII) of every sample and blank v i t h i n the upper and l e v e r limits (-501 to + 1001) for each continuing calibraticn? X _ f % ACTIO:;: List all t.he outliers belov. Samole » I.nternal Std Area Lover Limit Upper Limit o •J Ul (Attach additional sheets if necessary.) STA:;DARD cPZRATirro PROCZZ'JRZ Date: January 1292 R e v i s i o n : s YES NO N/A ACTICN: 1. I f t h e i n t e m a l s t a n d a r d a r e a c o u n t i s o u t s i d e t h e upper o r l o v e r l i m i t , f l a g v i t h " j " a l l p o s i t i v e r e s u l t s q u a n t i t a t e d v i t h t h i s i n t e m a l s t a n d a r d . 2. .S'on-detects associated vith IS area counts > IQOl should not be q-ualified. 3. If IS area is belov the lover limit (< 501), qualify all associated non- detects (U values) "J". If extremely lov area counts are reported, (< 251) or if performance exhibits a major abrupt drop off, flag a l l associated non-detects as u.nusable ("R"). 14.2 Are the retention times of the internal standards vit.hin 3 0 seconds of the associated calibraticn standard? ACTIc:;: Professional judgement should be used t c q-jalify data if the retention times diffar by more than 30 seconds. 15.0 Field r^-mlioates 15.1 Were any field duplicates submittad fcr VOA analysis? _ ACTICN: Compare the reported results for field duplicates and calculate the r e l a t i v e percent difference. ACTIC:;: Any cross variaticn betveen duplicate results must be addressed in t.he reviever narrative. Hovever, if large differences exist, identification of field duplicates should be confirmed by contacting the samoler. ik ik 304576 STA:;DARD CPZRATI::G PROCZZ'JRZ Date: January 12 32 Revision: 8 — ^ ^ NO N/A pzr~ -. T;^J^ ivjiTv^-r; 1 . 0 Tri"*''"'" - a - •»•«'* '•-.v. , - vj«. ...--i.'O * * * * * * • - ' . r w . - - . - • • - - ' - 1.1 Are tha Traffic Report Forms present for all sanples? r ,i J J ACnCN: If no, contact lab for replacement cf missing cr illegible ccpies. 1.2 Co the Traffic Reports or Lab Narrative i.-.dicate any proeiems vith cample receipt, ocnciticn of samples, analytical prcmiems cr soecial notations affactinc the cuality cf v t.he data? ' " 1_1 ACTIc:;: If any sampie analyzed as a soil, other t.han TCL?,'contains 501-901 vater, all data should be flaaged as estinated ("J"). If a soil sampie, other than TCL?, contains more than 9 01 vater, all data should be qualified as unusaole (R) . ACTICN: If samples vere not iced upcn receipt at the laboratcr-,-, flaa all positive results "J" anc ail ncn-detects "UJ". ' • - a It a r I •-; i i • - - 2.1 Have any ENA technical holding times, determined from date cf collecticn tc date of -w- extraction, been exceeded? A X L Continuous extraction of vater samples fcr ENA analysis r.ust ba started vithin seven days of the date of collecticn. Soil/ sediment samples must be extractad vithin 7 days of ccilecticn. Zxtracts r.ust be analyzed vithin 4 0 days of the date of extraction. 304577 STANDARD CPZHATINZ rROCZ--.-w Date: J a n u a r y 1232 Revision: Z YZS .NO N7A sammle £2^031 1 xo. « a « a T T « i i i » a a i M i i - i • J I I I T , ' i T a a a a a - i i M Sampia Cate Matrix: Sanoied j _ G//6/"/7 so; I r;//i./vn (See Traffic Repcrt) Date f.Ab Date Received Zrtracted G/A..A7 ^/2y/99 'S/ ^? Date Analyzed O 7///97 ACTIO::: if technical holding times are exceeded flag a l l positive r e s u l t s as estimated ("J") and sample q-uantitaticn limits as estimated ("UJ"), and document in the narrative t.hat holding times vare exceeded. If analvses vere cone more than 14 days fcayonc holding"tima. either cn tha f i r s t analysis cr upon raanalysis, the reviewer must use prcfessicnai judgement t c determine tha r e l i a b i l i t y o: t.he data and the effacts cf additional'storage cn t.he sample results. At a minimum, a l l results should be q".:alified "J", but the reviewer r.av determine that non-oetect data are unusable (;:R").'lf holdi.ng times are exceeaed by more t.han 2S days, ail non detect data are unusaole (K) . 3.0 Surrccatp co^gyerv ^'^^rrt ZZ\ 3.1 Are the ENA surrogate Reccvery Summaries (Form II) prssent fcr each cf the folloving matrices: a. Low Water b. Low Soil c. Med Soil i-l r 1 STA:;DARD :?ZR.\TI::G P.ROCZZ'JRZ Date: Januar-,- 12 92 Revision: 3 vre: iS NO N/A 3.2 .\TB a l l the B.KA tacpies l i s t e d cn t.he apprcmricte Surrogate Recc-erv S'ummaries for eacn of the fcllcving matrimas: a. Lov Water 3 . 3 111 b- Lov Soil fVi c. Lov soil j_j_ X ACTIO::: call lab for explanaticn/resucmittals. If missing caliveraoies are unavailable, document effect i.n data assessments.. Ware c-otiiars marked correctly with an w' asterisk? r i A ACTION: Circia all outliers in red. 3.4 Were t---o or more tase-neutrai C^ acid surrogate recoveries cut cf scecif icaticn fcr a.ny sand a .. or mathed bla.nk? ' LX. X - If yes, vere samples reanalyzed? 1 1 X Were matncd blanxs r=analyzec? XX )^ ACTIC:;: if all B.NA surrcgate recoveries are > 101 hut tvo vit.hin t.he base-neutral or acid fraction do not r.eet SOW = p e l - ^ « . _ • . — u » _ . . 5 , . w . . C - . fraction c-^v M.e. oHse-^eutrsl or aqi^ compcu—g) : 1. Flao all positive results as estimated ("J"). 2. Flag all non-cetects as estimated detecticn limits ("UJ") vhen recc-eries are less than the lover acceptance limit. 3. If recoveries are greater than the upper acceptance limit, do not qualify non-detects. 304579 STA:;DARD C?ZRATI::C PROCZZ'JRZ Date: Januar-.- 12 92 Revisicn: £ YZS NC N/A If any t a a e - r e u t r i l ^^ acid s u r r c c a t e has a recovery cf <101: 1. P o s i t i v e r e s u l t s fcr the f r a c t i o n vit.h <101 surrogate reccverv a r e c u a l i f i a d wit.h "J**. 2. Non-detects for t.hat f r a c t i o n should ba q u a l i f i e d as unusacle (R) . Prcfessional judcament should ba used t c qualify cata t.hat have method blank s u r r c g a t e r e c c / e r i a s out cf s p e c i f i c a t i o n in bot.h c r a g i n a i and r s a n a i y s e s . Checx the i.-.temal s t a n c a r c a r e a s . 3.5 Are t h e r e a.ny t r a n s c r i p t i c n / c a l c u l a t i c n e r r o r s between raw data and Form IZ? _ « ^^"^ ACTIO:;: if l a r g e errors e x i s t , c a l l lab fcr e x p l a n a t i c n / r e s u t m i t t a l , make any necessary corrections and dccument effect in data assessments. 4 . 0 M i t ' - - ' - ' ' ^ ' ' ' V o e f T^,.-m T - - ^ " f t Y . . . - . - , . . . . . . . . 4.1 Is the Matrix Scike/Matrix Spike Duplicate Recovery Fort: (Form III) present? 4.2 '-'dre r.atrix spikes analyzed a t t.he r e q u i r e d frequency fcr" eacn cf t.he f c l l c v i n g m a t r i c e s : a. Low Water b. Lov S c i l c. Med S c i l rY, LX. JL J^_ r 1 X ACTION: If a.ny matrix spike data a r e missing, take the acticn" soecified in 3.2 above. 304580 STAaiDARD CPi.-iATIIIC PROCZZL.--i Date: J a n u a r v 1232 R e v i s i o n : s """""^ YZS NO N/A 4.3 How many E.N'A spike raccverias are cutside 2 r •••- — .--•> Wa+'o- SQllS ^-t of 22 O out cf 22 4.4 Hov many RPD's fcr matrix spike a.nd matrix spike cuplicate racc-^eries are outside QC limits? C/>'« 1 <; Z , out o: t-4 % ACTION: No action is taken cn MS/MSD data a).png. Hovever, using informed professional judgement, t.he data reviever may usa the matrix spike an: natrix spike duplicate rasults in conju.ncticn -with other QZ c r i t e r i a and determine t.he need fcr some qualification of tha data. £.1 Is the .hsthoc Blank s--.mm.ary (Form IV) present? 5.2 ."requency of Analysis: Has a raagent/mathod blank analysis teen reportad per 2 0 samples of similar matrix. or ccncentraticn level, and for each extraction batch? LL. £.3 Has a ENA method blank baen analyzed fcr each GC/MS system usad? i-S. (See SOW p. b - 59/SV, Secticn S.7) ACTIO:;: if any method blank data are missing, call lab for explanaticn/resucmittal. If not available, use profassional judgement tc determine*if the associatad sample data should ba qualified. 304581 STANDARD CPZFJVTI::C PROCZD'JRZ Date: January 12 92 Revision: 3 YZS NO N/A 5.4 C.hrcmatcgrcp.-.y: review the blank rav data - chromatograms (RICs^, , quant raports or data system printc'.:ts and s p e c t r a . Is t.ha c.hrcmatogratnic perfcrmance (baseline s t a b i l i t y ) fcr eacn instr-cmsnt accsotabie for B:yis? JL, ACTIO:;: use professional judgenent tc datermtna the effact on the cata. Note: "Water blanks", "drill blanks" a.nd "distilled vater blanks" are validated like any other sample and are not used to c-.:alify the data. Co not confuse them vit.h the cthar QC blanks discussed belov. 6.1 Co anv method/instrument/reaaenr blanks have positive results (TCZ and/or TIC) fcr ENAs? When applied as describad balov, t.he contaminant ccncentraticn in these blanks are r.uitipliad by the sampie diluticn fictcr and ^ corractad fcr \ mcistura vnere necessary. — . 6.2 Co anv fiaid/rinsa/ blanks nive positive 52;A rasults (TCL and/cr TIC)? ACTIC:;: prepare a list cf the sanples associated with each of t.he contaminated blanks. (Attach a separate sneet.) Note: All field tlank results associated tc a particular group cf samples (may exceed one per case) must ba used tc qualify data. Blanks may not be qualified because of contaminaticn in another blank . Field Blanks must be qualified fcr surrcgate. spectral, i.nstrument performance or calibration QC prcmiems. 304582 :i.i-i - i irt.nw.r>-.->_. w~;.i--ATZ:rO PROCZZL.--.-c. Cate: Januar-/ 1 = 32 Revision: 3 iZS N'O N/A A C T I O : : ; FOIIOV tha d i r a c t i c n s i n t h a t a b l e balcv t c - l a l i f y T C I . r a s u l t s dua to contamination. Use t.he l a r g e s t v a l u e from a i l the a s s o c i a t e d b l a n k s . If gross c o n t a m i n a t i o n e x i s t s , a l l data i n tha a s s o c i a t e d sammles should ba q-calified as unusacla (R). Sampia cone ^ CRQL Sample cone <CRQL i but c i c x blank is< ::x b l a n k v a l u e Sample cenc ? CRQL value & >lGx b l a n x r.ht.haiata E s t e r s Flag s a m p l e r e s u l t v i t h a "U"; Repcrt CRQL u qualifv "U" No q u a l i f i c a t i o n i s needed Sample c e n c 5 CRQL Sampia cenc < CRQL i but < 5x b l a n k i s < 5x b l a n k v a l u e Sample cone > CRQL value & >5 b l a n k v a l u e Othar C o n t a m i n a n t s .'.ag sar.mla r a s u l t Report CRQL a c u a l i f v "U" No c - . i a l i f i c a t i c n i s naeaed Analytas c u a l i f i a a "U" f c r c l a n x c o n t a m i n a t i o n a r e s t i l l ' c o n s i d e r e d a s " h i t s " when q u a l i f y i n g f o r c a l i b r a t i c n c r i t a r i a . Ac: • ^ * . r~ «wa ^ «M \ concentration in the sample is less than five times t.he ccncentraticn in the most contaminated associated blank, flag tha sample data "H" (unusable). 5.3 Are there fiald/rinse/ecuipm.ant blanks associatad vith every sampie? ACTIC:;: For lov level samples, note in data assessment that t.here i s no associated field/rinse/equipm.ent blank. Zxcepticn: samples taken from a drinking vater tap do not have associated f i e l d blanks. JLL — - 304583 SrA;;DARD CPZR-^TINC PROCZZ'JRZ Date: Ja.-.uar-y 1 = 92 R e v i s i o n : «- iZZ NO N/A * * • r T a • • • Ml M > iir M Tl I I M V i"l 7.1 Are t h e GZ/y.z I.-.str-imant P e r f o r m a n c e Checx Forms (Form V) p r e s e n t for C-ecaflucrotraphanvlphosonina ^ (DFTPP)? ' • r>^3 7.2 Are t h e enhanced bar craph s m e c t r u n and mass/ c h a r g e (m/z) l i s t i n c for t.hB'DFTP? p r o v i d e d f c r . eacn t-velve hcur s n i f t ? i i i 3 'r.2.s a.n i.nstrumant parfcrmanca c h e c k s o l u t i o n been a n a l y z e c for everv f v e i v e h o u r s cf sample a n a l y s i s c e r i.-.str.imant? 1x1 A C T I O : ; : L i s t d a t a , time, i.-.str-umant IZ, and sampie analyses f c r ---hich no a s s o c i a t e d GC/MS t u n i n g d a t a a r e a v a i l a b l e . DATZ T I K Z INSTR'J:-'.ZNT SAMPLZ .VJHEZF.Z ACTIO:;: if lab cannot provide missing data. re-^ect ("R") ail data generated outside an acceptable tvalve hour calibraticn intern-'ai. ACTIO:?: If mass assignment is in error, flag all associated sampia data as unusable (R). 7.4 .Have t.he icn abundances teen normalized tc m./z isa? m 304584 Date: Januar*/ 12 32 Revisicn: s YZS NO N/A 7.5 Have t.ha icn abuncanca c r i t a r i a been met f c r eacn instrurcant usad? f>^ ^ _ ACTION: List a l l data vhich do not maet i c n abuncanca c r i t a r i a (attacn a s e p a r a t e s h e e t ) . ACTIO:;: if ion abundance c r i t e r i a are not met. t.he Region I I TPO must ba n o t i f i e d . 7.6 .-.re thare any t r a n s c r i p t i c n / c a l c u l a t i c n e r r o r s betveen m a s s ' l i s t s and'Form Vs? (Checx a t l e a s t tvo values but if errors are found, check more.) ^2-1 7.7 Have tha a p p r c p r i a t e number of s i g n i f i c a n t ^ figures (t-vo) been reportad? ' i2j ACTIO:;: if l a r g e errors exist, c a l l l a b f o r expianation/resubmittal, make necessary corrections and document e f f e c t in data assessments. 7.a .-.re tha s p e c t r a cf the r.ass c a l i b r a t i c n cor.peund accaotabla? i J l . — _je p r c f e s s i c n a i judgement t c determine vhetnar associated data should be accepted, qualified, or r e j e c t e d . U . W , - - - ! - . • . . — _ - — - . , . . . S » Y - w — 8.1 Are the organic Analysis Data sheets (Form I BNA) present vith required header information cn each page, fcr each cf tha fcllcving: a. Samples and/or fracticns as appropriate H i b. Matrix spikes and m.atrix spike duplicates _iJ. c. Blanks ^^ 304585 STANDARD CPi..r.ATZ:'0 PROCZZURZ Date: Januar.- 12 32 n e v i s i c n _ . . . o V T C i S NO N/A 0.2 Has GPC Cleanup been p e r f o r m e d on a i l s o i l / seaimant -ample e x t r a c t s ? rX"* Acnc:;: l I d a t a s u g g e s t s t h a t CPC vas not performed, u s e p r o f e s s i o n a l judgement. Make n o t e i n " C o n t r a c t Prcblems/Non-Compiiance*'. 8.3 Are t h e EHA R e c c n s t r c c t a d I c n c.hrcmatcgrcms.. the mass s p e c t r a f c r t h a i d e n t i f i a d compounds, and t.ha data Eystem p r i n t o u t s (Quant Reports) includad in t.he samoie o a c k a a e f c r each of t.he Hi a. Sampiss a n d / o r f r a c t i o n s as a p p r c p r i a t e i Jk Blanxs UX b . .Matrix s p i k e s and m a t r i x s p i k e d u p l i c a t e s (Mass s p e c t r a n o t r e q u i r e d ) ACTIO:;: if any d a t a a r e n i s s i n g , take a c t i o n s p e c i f i e d i n 3 . 2 above. 8.4 Are t h e r a s p c n s e f a c t o r s shovn in t h e Quant Repcrt? c . 5 Is chrcm2tocrap.".ic p a r f c r m a n c a a c c s p t a c l a v i t i r e s o e c t t o : E a s e l i n s s t a b i l i t y ? r_i. i l _ , ^ R e s o l u t i o n ; Peak shape? Full-scale-"graph (attenuation)? Other: ACTIc::: Use prcfessicnai judgement tc determine the acceptability of the data. i l l rYi Y 304586 STANDARD CPZPJiTINC PROCZZURZ Data: January 1392 Revision: 3 V T C ZS NO N/A 3 . 6 Are t h e lab-generated s t a n c a r d mass s o e c t r a of I d e n t i f i a c E.NA comcounds presenm for eacn sample? rKi A C T I O : ; : i f any mass s p e c t r a a r e missing, t a k e a c t i c n s p e c i f i e d i n 3 . 2 a b o v a . ' i f l a b does n o t g e n e r a t e r h a i r cvn standard s p e c t r a , make n o t e i n "Contract Problems/ Non-ccmplianca**. I f s p e c t r a are m i s s i n g , r e j e c t a l l pcsiti-.-e d a t a . 8.7 I s t h e RRT of aacn r a p c r t a d compound v i t h i n 0.06 RRT u n i t s cf t h a s t a n c a r c RRT i n t h e c c n t i n u i n c c a l i b r a t i o n ? r/^J 3.8 Are a l l ions p r e s e n t i n t h e s t a n d a r d mass s p e c t r u m a t a. relati-,-e i n t e n s i t y g r e a t e r than 101 a l s o t r a s e n t in t.he sammle mass soectrcm? X. 8.9 Do sample and standard relative ion intensities agree vithin 201? ACTIO:;: use professional judgement tc determina acceptability cf data. If it is determined that incerract identifications vera made, ail such data should be renectad (R) , flagged ">T" (Presumptiva evidence cf tha presence cf tha cempeund) or cnangec tc net datectad (U) at the calculated detecticn limit. In order to te positively identified, the data must ccmply vith the critaria listed in 8.7, S.B, and 8.9. ACTTO:;: when sample carry-cver is a pcssitility, prcfassic.-:al judgement should be usad to determine if instr-mant cross-contaminatio: has affectad any positive ccmpound identification. 5.0 Tentat-vPiv -:!5ntifi3d . — ...>, — . i ~ . a • • — . 9.1 Are ail Tentatively Identified Ccmpound Forms (Form I, Part S) present: and do listed TICs include scan numJcer or retention time, estimated sr concentraticn and "JN" qualifier? iii 3 04587 STA:;DARD cpzpjiZiNo PROCZZ'JRZ Date: Januar,- 1 = 32 Revision: s YZS NO .\7A » ' '^f^ t n e mass spectra fcr tha t a n t a t i v e l v I d e n t i f i e d ccmpcunes and a s s o c i a t e d "best match" spectra i.ncludad ir. tha sammla packace fcr eac-. of t h e f c l l c v i n g : . ^ - ^^ a. samples and/cr fracticns as appropriate ^A^ b. Blanks Ay ^ ^ ACTION: If any TIC data are missing, take action specified in 3.2 "above. ACTICN: Add.'-J::" q-.:alifier if missing. ^'^ ^^^^Jx3r ^-- ^—"=-r.ds (from any fraction) listed as TIC ccmpeunds (examoie: 1,2-dimBthylbenzene is xylene a voA TCL - -nd should not ba reocrtad as .^ a TIC;? • j ^ ACTICN: Flag vith "R" any Td. compound listed as a TIC. 9.4 Are all ions present in the reference mass spectr-um vith a relative intensity greater than 101 also prasent in t.ha sample mass Epcctr.:m? ^ 9.5 Co TIO and "bast r.atch" standard relative icn ^ I.ntansitias agrae vithin 201? iLl. ACTIC::: Use profassional judgement tc determine accaptability of TIC identifications. If it is determined that an i.-.corract identification vas made, change idantificaticn to "unknovn" or to some less specific identification (example: "C3 substifutad benzene") as appropriate. Also, vhen a ccmpo-uind is not fcund in any blank, but is a suspected artifact of a commen laboratory contaminant, t.ha result snouid ba cualified as u.nusaole (R). 304588 STANDARD CPZRATinC PROCZrJRZ Date: January 1392 Revisicn: a YZS NO N/A 10.0 Commour.d C'j:»r.tIt?.--'— ••r,.* oa^r.-^—e^ not-p,----- rv-i«_ 10.1 Are there any transcription/calculation errors in rorm I results? Chacx at least fvo positiva values. Verify t.hat the correct i.htemai standard, quantitation ion, and RRF vere used to calculate . . Form I result. Were any errors found? JN, 10.2 Are the CRQLs adjusted to reflect sampie diluticns and, fcr soils, sample moisture? rYi ACTICN: If errors are large, call lab fcr expianaticn/resubmittal. make any necessary corractions and document effect in data assessments. ACTIC:;: When a sample is analyzed at more than one dilution, the lovest CRQLs are used (unless a QC exceedance dictates the usa of the higher CRQL data from the diluted sample analysis). Replace concentraticns that exceed t.he calibraticn range in the original analysis by crossing out the "Z" and it's associated value on the original Form I and substituting the data from the analysis of t.he diluted sample. Specify which Form I is tc be used, then drav a red " X" acrcss the entire page of ail Form I ' s that should not be used, including any i.n t.he surciary package. ii-2 Stand?.--^'^ Cata ^GC/Vg> 11.1 Are the Reconstructed Icn Chromatograms. ^ and data system printouts (Quant, Reports) present y for initial and continuing calibration? rAv") ACTIc:;: If any calibraticn standard data are missing, take acticn specified in 3.2 above. 304589 STANDARD OPZRATINO PROCZZ'JRZ Date: January 12 9 2 Revision: a YZS NO .N7A 12.0 GC/y^ 12.1 Are the I.-.itial Calibration Forms (Form VI) present and complete for the E.NA fraction? J L , ACTION: If any calibraticn standard foms are missing, take action specified in 3.2 above. 12.2 Are response factors stable for S.HAs over tha concentraticn ranae of the calibration? (1 Relative standard deviation (IRSD) < 30.01) rAi _ ACTIc:;: Circia all outliers in red. NOTZ: Althougn 2 0 BNA compounds have a minimun RRF a.nd no r.aximuc: "iRSD, the technical criteria are t.he same fcr all analytes. ACTICN: If the * RSD is > 3 0.01, qualify positive results for that analyte ''J" and non-detects using professional judgement. When RSD > 901, flag all non- detect results fcr t.hat a.nalyte R (unusable). NOTZ: Analytes previously qualified "U" (2ue to blank contamination are still considered as "hits" vhen qualifying for calibration critaria. 12.3 Are a l l BNA cempeund RRFs > 0.05? LL,.. ACTIC:;: circle a i l o u t l i e r s in red. ACTICN: If any RRF < 0.05 1. "R" a l l non-detects. 2. "J-° a l l positive results. 12.4 Are t.here any transcripticn/calculaticn errors in- the reporting of average response factors (RRF) or 1 RSD? (Check at l e a s t fvo values but if errors are fcund, check more.) l ^ ACTICN: Circle Errors in red. 304590 STANDARD CPZRATING PROCZZ'JRZ Date: Januar,- 1992 Revision: s VZS )IZ N/A ACTICN: If errors are large, call lab fcr expianaticn/resiibmattal, make any necessary corrections and note errors in data assessments. 13.0 GC/M? Conr-—*-- '^^i < v.-,...^ ««, /T^-^— trrr^ 13.1 Are the continuing-calibration Forms (Form VII) present and complete for tha BNA fraction? r XT 13.2 Has a continuing calibration standard- been analyzed fcr every t--aive hours of sampie y' analysis, per instrument? " ' ' ^ ACTICN: List balov all sampie analyses that vere not vithin tvalve hours of a continuing calibraticn analysis for each instrument usad. ACTICN: If any forms are missing or no continuing calibration stancard has been analyzed vit.hin tvelve hours cf every sampie analysis. call lab fcr explanation/ resubmittal. If continuing calibraticn data are not available, flag all associated sampie data as unusable ("R"). 13.3 Do any semivolatile compounds have a 1 Difference (1 D) betveen the Tnitial and conti.nuing RRF w- vhic.h exceeds the t- 25.01 criteria? _L^ i-J. ACTIO:;: circle all outliers in red. ACTICN: Qualify both positive results and non-detects for t.he outlier compound(s) as estimated (J). When ID is above 901, reject all non-detects fcr that analyte (R) unusable. 304591 STANDARD C?ZrJ%Ti:r3 PROCZZ'JRZ Date: January 1392 i\ 6V X s ^ c r« * s YZS NO N/A 13.4 Co any semivoiatila compounds have a RRF <0.05? rY? _ ACTION; Circle all outliers in red. ACTION: If PJIF <o.05, qualify as unusable (R) associated non-detects and "J" associated positive values. 13.5 Are there any transcription/calculation errors in the reporting of average response factors (RRF) or 1 diffarence (ID) betveen initial and continuing RRFs? (Check at least fvo values ^ but if errors are found, checx more). '^^ _ ACTION: Circle errors in red. ACTION: If errors are large, call lab for expianaticn/resubmittal, make any necessary corrections and document effect in data assessments. 1 4 . 0 T».*o-»—-»•> c f » ., r* ^ •.-.*.? / r « * ~ «T"rT—1 - • ' ' • — • - — . . — ' . — . . . . - — . 14.1 Are the i.nternal standard areas (Form VIII) of every sample and blank vithin the upper and lover limits (-501 tc + 1001) fcr each continuing . calibration? 1X1 - ACTIO:;: List all tha outliers balov. Sa.tcia = Internal Std Area Lover Limit Upper Limi: (Attach additicnal sheets if necessary.) ACTION: 1. If the i.-.ternal standard area count is outside the uoper or lover limit, flag vith "J" a l l positive results and non-detects (U values) q-uantitated vith this internal standard. 304592 STA},'DARD OPZRATi:iG PROCZZ'JRZ Date: Januar/ 1392 Revision: a YES NO N/A Non-detects associated v i t h IS areas > 1001 should not be q u a l i f i e d . If tha IS area i s balov t h e lover l i s i t (<S01), qualify a l l a s s o c i a t e d non-detacts • (U-valuas) "J«. If extremaiy lov araa counts are reported (<2S1) or i f performanca e x h i b i t s a major abrupt drop off, flag a l l associated non-detects as unusable (R). % 14.2 Are the r e t e n t i o n times of the i.nternal s t a n d a r d s vithin 3 0 seconds of the associated c a l i b r a t i o n standard? ACTICN: Professional judgement should be used tc qualify data if the retention times diffar by more t.han 3 0 seconds. 1 5 . 0 F ' e " ' ' ^ P"—1 >• -T«-a«; • ^ • - ' ^ f aSaai—Uai>ra • » » ^ ^ 5 15.1 Were any field duolicates submittad fsr BNA analysis? X—1 K ACTIC:;: Compare the reported rasults fcr fieid duplicates and calculate the relative percent diffarence. ACTIc:;: Any gross variaticn betveen field duplicate results must be addressed in -the reviever narrative. However, if large differences exist, identification of field duplicates should.-ie confirmed by contacting tha samoler. 304593 # SDG No. 98004 VOC, SVOC, and Metals Checklist 1 -5^^ ^ k l ^ C Review of Low Concentration Volatile Data For Pace Analytical SDG: 98004 ISLAND CHEMICAL Revie-wer: Uma Parasar February 19, 1998 Holding Times: All samples -were analyzed within seven days, the holding time for unpreserved aqueous samples. GC/MS Tuning and Mass Calibration: All BFB tuning criteria were within control limits. Initial Calibration: The percent relative standard deviations (%RSD) for methylene chloride (65.3%) and acetone (37.7%) exceeded the criteria of 30%i in the initial calibration run on January 6 1998. Positive detects for methylene chloride and acetone in all samples included in this sample delivery group (SDG) were qualified as estimated (J). All other compounds had %RSDs below 30 % and all relative response factors (RRF) were above 0.05 units. Continuing Calibration: The following compounds had percent differences (%oDs) that were greater than 30% in the continuing calibration run on January 15, 1998: Chloromethane 33.8% Vinyl Chloride 30.4% Non detect results for chloromethane and vinyl chloride in associated samples FB109, TB109, FBOllO, MW-4, MW-1, and P-1 were qualified as estimated (UJ). The following compounds had %Ds that were greater than 30% in the continuing calibration run on January 16, 1998: Carbon tetrachloride 31.3% Bromoform 30.3% Non detect results for carbon tetrachloride and bromoform in associated samples PW-2, MW-10, MW-3, MW-2, FB013, MW-2D, TB0113, MW-7, FBOlll, MW-5, TB0112, MW-9, FBOl 12, MW-8, FBOl 14, TB0114, and MW-6 were qualified as estimated (TJJ). All other compounds had %Ds below 30% and all RRFs were above 0.05 units. 3 0 4 5 9 5 Blanks: All method blanks, trip blanks and field blanks associated with aqueous analyses reported concentrations ofmethylene chloride and acetone. Methylene chloride and acetone data in samples MW-4, P-1, MW-3, MW-5, MW-8, MW-9, MW-7, MW-10, and P-2, were qualified as not detected based on method blank contamination. Six field blanks were collected along with the aqueous samples. One or more field blanks reported concentrations ofmethylene chloride, acetone, 2-butanone, ethylbenzene, toluene, and total xylenes. Sample data for acetone and methylene chloride were qualified based on method blanks. Total xylene results in samples P-1, MW-10, and MW-5 were qualified as not detected based on the associated field blanks. Four trip blanks were collected along with the aqueous samples. All trip blanks reported low concentrations of methylene chloride and acetone. No data were qualified based on the trip blanks. Intemal Standard Area Summary: Intemal standard area counts were within acceptable limits in all the analyses. Surrogate Recovery: All surrogate recoveries were acceptable. Matrix Spike/Matrix Spike Duplicate: The spike/spike duplicate recoveries and relative percent differences were evaluated in conjunction with other QC parameters. No matrix effect is reported in the analyses. Compound ID: All reported compounds were correctly identified and quantitated accurately. Field Duplicates: One field duplicate was collected in this data set. The data were compared and the relative percent differences calculated. All percent differences were within 20%. Sample Receipt: Samples MW-2, MW-2D, MW-7 and MW-8 were received with air bubbles in all 3 VOC vials. The VOC data for these samples were qualified as estimated (J) if detected and (UJ) if not detected. Samples collected on January 10*, 11*'', and 12'*^ were received by the laboratory on January 14'*'. No data were qualified as estimated since all analyses were performed within holding time and the sample coolers were received sealed with the samples stored at 4° centigrade. G\staff\uparai\DVMEMO\98004IC_VOCg 304596 QA/QC Review of Low Concentration TCL Semivolatile and Pyridine Data For Pace Analytical SDG: 98004 ISLAND CHEMICAL Reviewer: Uma Parasar February 23, 1997 Holding Times: All samples were extracted and analyzed within the holding time. GC/MS Tuning and Mass Calibration: All DFTPP tuning criteria were within control limits. Initial Calibration: All compounds had percent relative standard deviations (%RSD) below 30 % and all relative response factors (RRF) were above 0.05 units. Continuing Calibration: All compounds had percent differences (%)D) below 25%) and all RRFs were above 0.05 units. Blanks: One method blank was analyzed with the samples in this SDG. The method blank was reported to contain 2 micrograms per liter of bis(2-ethylhexyl)phthalate. Bis(2-ethylhexyl)phthalate detected in samples MW-2, MW-3, MW-4, MW-7, MW-8, MW-9, MW-2D, PI, and P2 were qualified as not detected based on the method blank. Six field blanks were collected along with the samples in this SDG. Bis(2-ethylhexyl)phthalate was detected in all six blanks at low concentrations. Bis(2-ethylhexyl)phthalate concentrations in samples MW-10 and MW-5 were qualified as not detected based on the associated field blanks FBOl 11 and FBOl 12. Ethylbenzene and dimethylbenzene (xylene) which are part of the TCL VOC list were reported as tentatively identified compounds (TICs) in samples M^-1, MW-6, and field blank FBOl 13. These results were rejected as unusable. Intemal Standard Area Summary: Samples MW-1 and MW-6 exhibited low area counts associated with one or more intemal standards. The area counts for l,4-dichlorobenzene-d4 associated with samples MW-1 and MW-6 were 10%) and 6%o, respectively of the area lower limit for the compound. Therefore, the results for compounds in MW-1 and MW-6 quantitated using this intemal standard were qualified as estimated (J) if detected and rejected as unusable if not detected. 3 0 4 5 9 7 The area counts for naphthalene-dg associated with samples MW-1 and MW-6 were 44% and 27%, respectively. The positive results for compounds in MW-1 quantitated using this intemal standard were qualified as estimated (J). The results for compounds in MW-6 quantitated using this intemal standard were qualified as estimated (J) if detected and rejected as unusable if not detected. The area count for phenanthrene-dio associated with sample MW-6 was below the acceptable limit. The positive results for compounds in MW-6 quantitated using this intemal standard were qualified as estimated (J). All other intemal standard retention times and area counts were within acceptable limits. Surrogate Recovery: All surrogate recoveries were within acceptable limits. Surrogates in samples MW-1 and MW-6 were diluted out Based on the intemal standard area counts, no data were qualified. Matrix Spike/Matrix Spike Duplicate: MS/MSD samples had all percent recoveries and percent differences within control limits. Compound ID: All reported compounds were correctly identified and quantitated accurately. Laboratory Control Sample: The laboratory control sample recovery (32%)) was below acceptable limits (35 - 98%) for 4-chloroaniline. 4-Chloroaniline data in all samples were qualified as estimated (J) if detected and rejected as unusable if not detected. Sample Receipt: Samples collected on January 10*', 11*, and 12"^ were received by the laboratory on January 14"*. No data were qualified as estimated since the samples were analyzed within holding time and the samples were received in sealed coolers stored at a temperature of 4° centigrade. Pyridine Analyses: All samples were analyzed for pyridine using SW-846 Method 8270. Samples were analyzed in conformance with the method. The only deviation noted was the area counts for the intemal standard compound l,4-dichlorobenzene-d4, which was used to quantitate pyridine, associated with samples MW-1 and MW-6. The area counts were 10% and 6.2%), respectively and required the rejection of pyridine data in these samples. G:\staff\uparas\D VMEMO\98004IC_SVg.doc 304598 SOP NO. HW-13 Revision 1 Superfund Analytical Methods For Low Concentration Water for Organics June 19^1 Prepared by the Pegion II Organic ESAT Team By: Wr- George Ka^as, Organic Task Monitor/Chemist Toxic ana Hazardous Waste Section By: r-^C-^/---^ /, ^ .- LeonLaza'i^s/^nvironmental Scientist Toxic and Hazardous Waste Section By: U n ^ . ^ Z ^ ^ ' Stelios Gera2ouni,2-';^^heniist Toxic and Hazardous Waste Section CONCURRED BY: APPROVED. BY: RoBeft Runyon, Chie^ Monitoring Management Branch Date: ^M £r^ 0.te: M f ^ Date : AAZ Date Date: 304599 LOW CONCEhTTRATION WATER STANDAJ^D OPERATING PROCEDURE P a g e : 1 of 51 D a t e : A u g u s t , 1992 F e v i s i o n : 1 ef?9E NUMBER: ^ ' ^ Q O H- SITE: J6L/\^;-I> C H e / n i C A / YES NO N/A LAB. PPiCe P^f\)AL>lTf C A i _ 1.0 Data Completeness and Deliverables 1.1 Have any missing deliverables been received and added to the data package? sJL ACTION: Call lab for expianation/resubmittal of any missing deliverables. If lab cannot provide them, note the effect on reviev of the package under the "Contract Problems/Non- Compliance" section of reviewer narrative. 1.2 Was SAS-request included with package? X I If no, a SAS-request can be retrieved from RSCC- X 2.0 Cover Letter SPG Narrative 2.1 Is the Narrative or Cover Letter Present? [Ki 2.2 Are Case Number and/or SAS number contained in the Narrative or Cover letter? JL 3.0 Data Validation Checklist The following checklist is divided into three parts. Part A is filled out if the data package contains any Low Concentration Volatile analyses, Part B for any Low Concentration Semivolatile analyses and Part C for Low Concentration Pesticide/Aroclors. Does this package contain: Low Concentration Volatile Data? Low Concentration Semivolatile Data? Low Concentration Pesticide/Aroclor data? Action: Complete corresponding parts of checklist. 2L X 304600 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 2 of 51 Date: August, Revision: 1 1992 YES NO N/A PART A: VOA ANALYSES 1.0 Traffic Reports and Laboratory Narrative 1.1 Are Traffic Report Forms present for all samples? ACTION: If no, contact lab for replacement of missing or illegible copies. iXi 1.2 Do Traffic Reports or Lab Narrative indicate any problems with sample receipt, condition of samples, analytical problems or special circumstances affecting the quality of the data? ACTION: If samples were not iced upon receipt at the laboratory, flag all positive results "J" and all non-detects "UJ". ACTION: If both VOA vials for a sample have air bubbles or the VOA vial analyzed had air bubbles, flag all positive results "J" and non-detects using professional judgement. 1.3 Does Lab narrative contain a list of pH determinations for all samples? J ACTION: If I^b narrative does not contain a list of sample pH determinations, contact the lab for explanation/resubmittals. 2. 0 Holding Times 2.1 Have any VOA technical holding times, determined from date of collection to date of analysis, been exceeded? X j _ i ^ _ ^ If unpreserved, samples maintained at 4'C and are to be analyzed for aromatic hydrocarbons must be analyzed within 7 days of collection. If preserved with HCl (pH<2) and stored at 4*C, then samples must be analyzed within 14 days of collection. If uncer" tain about preservation, contact sampler to determine whether or not samples were preserved. 304601 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 3 of 51 Date: August, 1992 Revision: 1 YES NO N/A Table of Holding Time Violations Sample ID Preserved? (See Traffic Report) Date Date Lab Date Sampled Received Analyzed ACTION: If technical holding times are exceeded, flag all positive results as estimated ("J") and sample quantitation limits as estimated ("UJ"), and document in the narrative that holding tiroes were exceeded. If analyses were done more than 14 days beyond holding time, either on the first analysis or upon re-analysis, the reviewer must use profes- sional judgement to determine the reliability of the data and the effects of additional storage on the sample results. At a minimum, all results must be qualified "J", but the reviewer may determine that non-detect data are unusable (R) . If holding times are exceeded by more than 28 days, all non- detect data are unusable (R) . 3 . 0 Surrogate Recovery (Form II LCV) 3.1 Are the VOA Surrogate Recovery Summaries (Form II LCV) present? ACTION: Call lab for explanation/resubmittals. If missing deliverables are unavailable, document effect in data assessments. 3.2 Were outliers marked correctly with an asterisk? ACTION: Circle all outliers in red. 3.3 Was the surrogate (p-bromofluorobenzene) recovery outside of contract specifications for any sample or method blank? IXL I - l l ) < l 2L 304602 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 4 of 51 Date: August, 1992 Revision: 1 YES NO N/A If yes, were samples re-analyzed? _[ ]_ Were method blanks re-analyzed? _[ ]_ ACTION: If bromofluorobenzene recovery is >10%, but fails to meet SOW specifications: 1. All positive results are qualified as estimated (J). 2. Flag all non-detects as estimated detection limits ("UJ") where recovery is less than the lower acceptance limit. 3. If surrogate recovery is above allowable levels, do not qualify non-detects. If surrogate recovery is < 10% : 1. Flag all positive results as estimated ("J") 2. Flag all non-detects as unusable ("R"). Professional judgement should be used to qualify data that only have the method blank's surrogate recovery out of speci- fication in both original and reanalyses. Check the internal standard areas. 3.4 Are there any transcription/calculation errors between raw data and Form II? ACTION: If large errors exist, call lab for expianation/resubmittal, make any necessary corrections and note errors in the data assessment. M 4.0 Laboratory Control Sample (Form III LCV) 4.1 Is the Laboratory Control Sample Recovery Form (Form III LCV) present? • ii_ 304603 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE P a g e : 5 of 51 D a t e : A u g u s t , 1992 R e v i s i o n : 1 YES NO N/A 4.2 Was the Laboratory Control Sample (LCS) analyzed at the required frequency (once per SDG or every 20 samples, whichever is more frequent) for the Low Concentration VOA method? [X] ACTION: If any LCS data are missing, take the action specified in 3.2 above. 4.3 How many VOA LCS recoveries are outside QC limits of 60-140%? Low Cone. Water 0 out of 12 ACTION: If the LCS recovery is greater than 140%, positive results should be flagged "J" for the affected compound. If the mass spectral criteria are met but the LCS recovery is less than 60%, then the associated detected target compounds should be flagged "J". Associated non- detected target compounds should be flagged "R", If 25 % of the analyte recoveries are below QC-limits qualify all associated positive sample data as "J" and non-detects "R". If two or more analytes show recoveries of < 10% all associated positive sample data as "J" and non-detects "R". It should be noted for TPO action if a laboratory fails to analyze an LCS vith each SDG, or if a laboratory consistently fails to generate acceptable LCS recoveries. 5.0 Method Blanks (Form IV-LCV) 5.1 Is the Method Blank Summary (Form IV LCV) present? iXi 304604 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE P a g e : 6 of 51 D a t e : A u g u s t , 1992 R e v i s i o n : 1 YES NO N/A 5.2 Frequency of A n a l y s i s : For the analysis of Low Concentration VOA TCL compounds, has a method blank been analyzed for each SDG or every 20 samples, . whichever is more frequent? J^Q 5.3 Has a VOA method blank been analyzed at least once every twelve hours for each GC/MS system used? (X] ACTION: If any method blank data are missing, call lab for expianation/resubmittal. If method blank data are not available, reject (R) all associated positive data. However, using professional judgement, the data reviewer may substitute field blank or trip blank data for missing method blank data. 5.4 Chromatography: review the method blank raw data - chromatograms (RICs), quant reports or data system printouts and spectra. Is the chromatographic performance (baseline stability) for each instrument acceptable for Low Concentration VOAs? (A) ACTION: Use professional judgement to determine the effect on the data. 5.0.1 Storage Blank 5.0.1a Has a storage blank been analyzed at the required frequency (once per SDG) for VOAs? [X.1 5.0.1b Chromatography: Compare the storage blank raw data with the associated method blank data in order to determine if the contamination is also present in the method blank. ACTION: If the storage blank contains target compounds at a concentration greater than the CRQL, positive results for that compound(s) should be flagged "J". If gross contamination occurred positive sample results may require rejection for that compound. 304605 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 7 of 51 Date: August, Revision: 1 1992 YES NO N/A 5.0.1c Is the chromatographic performance (baseline stability) for the storage blank acceptable for Low Cone. VOAs? fX] ACTION: Use professional judgement to determine the effect on the data. 6.0 Contamination NOTE: "Water blanks", "drill blanks", and distilled water blanks" are validated like any other sample, and are not used to qualify data. Do not confuse them with the other QC blanks discussed below. 6.1 Has an instrument blank been analyzed following a sample analysis which contained an analyte(s) at high concentration(s). j)<i ACTION: Sample analysis results after the high concentration sample must be evaluated for carryover. Instrument cross contamination should be noted for TPO action if an effect on the data is suspected. 6.2 Do any method/storage blanks have positive results (TCL and/or TIC) for Low Cone. VOAs? When applied as described below, the contaminant concentration in these blanks ^^ are multiplied by the sample dilution factor. A i 1 6.3 Do any field/trip/rinse blanks have positive ^ Low Cone. VOA results (TCL and/or TIC)? A r 1 ACTION: Prepare a list of the samples associated with each of the contaminated blanks. (Attach a separate sheet.) 304606 (VlefhodL ai>.^*;s V^^ -2- l/feLKiAil A^oacJe4 p.^.^^q p/2>£)/((9 mtoooo/ rvi^oooo^, T^ooo/^ \/PiLKl'\!'?^ fkiAomoMA 3 0 - V^feLKiA/3 /vii/vooo3 rY\i/\iooo^ /VXIAJOOOG. miAjoooi fv\iA)mo^ miAyOOO^ /V\iAJ0(D(O AAlA/a0C3^ ?0C'O0/2iL.^ 7 o o o o a ^ X/3)(9/(3L^ TfiO 113^ TT^Oi i (4 . F/^0 iio A A4>9u.'co(xpi ^owwy^ttt : I J" / M'iAJi miAJh) P-I , AI^ 304607 (Xal^yyu. 3 ^-^ P6011X ; /^^dO(U^iU:b2l Ti^uyv^tti: nni/v-5' A/niA/-^ (XULCAXZ 3/^1 (Atti^y^JL ^ ^ ^ 0.33- 'VKX- P(^€ili4 : A ^ ^ O U o J - ^ A ^^r^f>^^-- fy\lAJ-%- Qca3Ay^Ji oi'l^ut(Xj\AAA^\JL { 106 Q (3 OAlf o>(or 304608 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 8 of 51 Date: August, 1992 Revision: 1 YES NO N/A NOTE: All field blank results associated with a particular group of samples (may exceed one per case) must be used to qualify data. Trip blanks are used to qualify only those samples with which they were shipped. Blanks may not be qualified because of contamination in another blank. Field blanks i trip blanks must be qualified for system monitoring compound, instrument performance criteria, spectral or calibration QC problems. ACTION: Follow the directions in the table below to qualify TCL results due to contamination. Use the largest value from all the associated blanks. If any blanks are grossly contaminated, all associated data should be qualified as unusable (R). Sample cone > CRQL Sample cone < CRQL but < lOx blank & <10x blank value value Sample cone > CRQL & >10x blank value Methylene Chloride Flag sample result Report CRQL & Acetone with a "U" qualify "U" 2-Butanone No qualification is needed Sample cone > CRQL Sample cone < CRQL & Sample cone > CRQL but < 5x blank is < 5x blank value value & > 5x blank value Other Contam- inants Flag sample result with a "U" Report CRQL i qualify "U" No qualification is needed NOTE: Analytes qualified "U" for blank contamination are still considered as "hits" when qualifying for calibration criteria.. 304609 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 9 of 51 Date: August, 1992 Revision: 1 ACTION: For TIC compounds, if the concentration in the sample is less than five times the concentration in the most contaminated associated blank, flag the sample data "R" (unusable). 6.3 Are there field/rinse/equipment blanks associated with every sample? YES NO N/A iX ACTION: Note in data assessment that there is no associated field/rinse/equipment blank* Exception: samples taken from a drinking water tap do not have associated field blanks. 7.0 GC/MS Instrument Performance Check (Form V-LCV1 7.1 Are the GC/MS Instrument Performance Check Forms (Form V-LCV) present for ^, Bromofluorobenzene (BFB)? fX] 7.2 Are the enhanced bar graph spectrum and mass/charge (m/z) listing for the BFB provided for each twelve hour shift? cXi 7.3 Has an instrument performance compound been analyzed for every twelve hours of sample analysis per instrument? [Xj ACTION: List date, time, instrument ID, and sample analysis for which no associated GC/MS tuning data are available. DATE TIME INSTRUMENT SAMPLE NUMBERS ACTION: If lab cannot provide missing data, reject ("R") all data generated outside an accep- table twelve hour calibration interval. 304610 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 10 of 51 Date: August, 1992 Revision: 1 YES NO N/A X 7.4 Have the ion abundances been normalized to m/z 95? f/M ACTION: If mass assigronent is in error, qualify all associated data as unusable (R). 7.5 Have the ion abundance criteria been met for ^ each instrument used? [/\] ACTION: List all data which do not meet ion abundance criteria (attach a separate sheet). ACTION: If ion abundance criteria are not met, the Region II TPO must be notified. 7.6 Are there any transcription/calculation errors between mass lists and Form Vs? (Check at least two values but if errors are found, check more.) 7.7 Have the appropriate number of significant figures (two) been reported? ACTION: If large errors exist, call lab for expianation/resubmittal, make necessary corrections and document effect in data assessments. 7.8 Is the spectrum of the mass calibration compound acceptable? fXl ACTION: Use professional judgement to determine whether associated data should be accepted, qualified, or rejected. 8.0 Target Compound List (TCL) Analytes (Form I LCV) 8.1 Are the Organic Analysis Data Sheets (Form I LCV) present with required header information on each page, for each of the following: a. Samples and/or fractions as appropriate? (Xj b. Laboratory Control Samples? fXl c. Blanks? {Aj 304611 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 11 of 51 Date: August, 1992 Revision: 1 YES NO N/A 8.2 Are the VOA Reconstructed Ion Chromatograms, the mass spectra for the identified compounds, and the data system printouts (Quant Reports) included in the sample package for each of the following: a. Samples and/or fractions as appropriate? f )(l b. Laboratory Control Samples? [ ^ c. Blanks? fXl ACTION: If any data are missing, take action specified in 3.2 above. 8.3 Are the response factors shown in the Quant Report? 8.4 Is chromatographic performance acceptable with respect to: Baseline stability? Resolution? Peak shape? Full-scale graph (attenuation)? Other: ACTION: Use professional judgement to determine the acceptability of the data. 8.5 Are the lab-generated standard mass spectra of the identified VOA compounds present for each sample? J_JL_X iXi JCi -D<;i j _ ^ m ACTION: If any mass spectra are missing, take action specified in 3.2 above. If lab does not generate their own standard spectra, make note in data assessment - "Contract Problems/Non-Compliance". 304612 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 12 of 51 Date: August, 1992 Revision: 1 8.6 8.7 Is the RRT of each reported compound within 0.06 RRT units of the standard RRT in the continuing calibration? YES NO N/A iXi Are all ions present in the standard mass spectrum at a relative intensity greater than < 25% also present in the sample mass spectrum? iX} 8.8 Do sample and standard relative ion intensities agree within 20%? JL ACTION: Use professional judgement to determine acceptability of data. If it is determined that incorrect identifications were made, all such data should be rejected (R), flagged "N" (presumptive evidence of the presence of the compound) or changed to not detected (U) at the calculated detection limit. In order to be positively identified, the data must comply with the criteria listed in the SOW page VOA D-32, section 21. ACTION: When sample carry-over is a possibility, pro- fessional judgement should be used to determine if instrument cross-contamination has affected any positive compound identification. 9.0 Tentatively Identified Compounds (TIC) 9.1 Are all Tentatively Identified Compound.Forms (Form I LCV-TIC) present? Do listed TICs include scan number or retention time, estimated concentration and "JN" qualifier? xKl 9.2 Are the mass spectra for the tentatively identified compounds and associated "best match" spectra included in the sample package for each of the following: a. Samples and/or fractions as appropriate? [ X] b. Blanks? jjL ACTION: If any TIC data are missing, take action specified in 3.2 above. 304613 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 13 of 51 Date: August, 1992 Revision: 1 YES NO N/A ACTION: Add "JN" qualifier if missing. 9.3 Are any TCL compounds (from any fraction) listed as TIC compounds (example: 1,2-dimethyl- benzene is xylene- a VOA TCL analyte - and should not be reported as a TIC)? m ACTION: Flag with "R" any TCL compound listed as a TIC. 9.4 Are all ions present in the reference mass spectrum with a relative intensity greater than 25% also present in the sample mass spectrum? fXl 9.5 Do TIC and "best match" standard relative ion intensities agree within 20%? fXl ACTION: Use professional judgement to determine acceptability of TIC identifications. If it is determined that an incorrect iden- tification was made, change its identifica- tion to "unknovn" or to some less specific identification (example: "C3 substituted benzene") as appropriate. Also, when a compound is not found in any blank, but is detected in a sample and is a suspected arti- fact of a common laboratory contaminant, the result should be qualified as unusable (R). (i.e. Common Lab Contaminants: COj (M/E 44), Siloxanes (M/E 73) Hexane, Aldol Condensation Products, Solvent Preservatives, and related by products - see Functional Guidelines for more guidance). 10.0 Compound Quantitation and Reported Detection Limits 10.1 Are there any transcription/calculation errors in Form I results? Check at least two positive values. Verify that the correct internal standard, quantitation ion, and RRF were used to calculate Form I result. Were any errors found? [X 304614 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 14 of 51 Date: August, 1992 Revision: 1 YES NO N/A 10.2 Are the CRQLs adjusted to reflect sample dilutions? sX ACTION: If errors are large, call lab for expianation/resubmittal, make any necessary corrections and note errors under "Conclusions". ACTION: When a sample is analyzed at more than one dilution, the lowest CRQLs are used (unless a QC exceedance dictates the use of the higher CRQL data from the diluted sample analysis). Replace concentrations that exceed the calibration range in the original analysis by crossing out the "E" and its associated value on the original Form I and substituting the data from the analysis of the diluted sample. Specify which Form I is to be used, then draw a red "X" across the entire page of all Form I's that should not be used, including any in the summary package. 11.0 Standards Data (GC/MS) 11.1 Are the Reconstructed Ion Chromatograms, and data system printouts (Quant. Reports) present for initial and continuing calibration? ^ ACTION: If any calibration standard data are missing, take action specified in 3.2 above. 12.0 GC/MS Initial Calibration (Form VI) 12.1 Are the Initial Calibration Forms (Form VI LCV) present and complete for the volatile fraction at concentrations of 1, 2, 5, 10, and 25 ug/1? ACTION: If any calibration standard forms are missing, take action specified in 3.2 above. M — 304615 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 15 of 51 Date: August, 1992 Revision: 1 YES NO N/A 12.2 Are response factors stable for VOA's over the concentration range of the calibration (%Relative Standard Deviation (%RSD) <30.0%)? ACTION: Circle all outliers in red. X NOTE; ACTION: NOTE: Although 12 Low Cone. VOA compounds have a minimum RRF and no maximum %RSD, the technical criteria are the same for all analytes. If %RSD > 30.0%, qualify associated positive results for that analyte "J" and non-detects using professional judgement. When RSD > 90%, flag all non-detects for that analyte R (unusable). Analytes previously qualified "U" for blank contamination are still considered as "hits" when qualifying for initial calibration criteria. 12.3 Are the RRFs above 0.05? Action: Circle all outliers in red. sX Action: If any KRF values are < 0.05, qualify associated non-detects (R) and flag associated positive data as estimated (J). 12.4 Are there any transcription/calculation errors in the reporting of average response factors (RRF) or %RSD? (Check at least 2 values, but if errors are found, check more.) _ i ) i _ 13.0 GC/MS Continuing Calibration (Form VII LCV) 13.1 Are the Continuing Calibration Forms (Form VII LCV) present and complete for the volatile fraction? fX] 13.2 Has a continuing calibration standard been analyzed for every twelve hours of sample analysis per instrument? ^ 1 304616 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 16 of 51 Date: August, 1992 Revision: 1 ACTION: List below all sample analyses that were not within twelve hours of the previous continuing calibration analysis. YES NO N/A ACTION: If any forms are missing or no continuing calibration standard has been analyzed within twelve hours of every sample analysis, call lab for explanation/ resubmittal. If continuing calibration data are not available, flag all associated sample data as unusable ("R"). 13.3 Do any volatile compounds have a % Difference (% D) between the initial and continuing RRF which exceeds the + 30% criteria? A. i 1 ACTION: Circle all outliers in red. ACTION: Qualify both positive results and non-detects for the outlier compound(s) as estimated "J". When % D is above 90%, reject all non-detects for that analyte (R) as unusable. 13.4 Do any volatile compounds have a RRF <0.05? I ]_ X ACTION:Circle all outliers in red. ACTION: If the RRF <0.05, qualify associated non- detects as unusable (R) and associated positive values as estimated "J". 13.5 Are there any transcription/calculation errors in the reporting of average response factors (RRF) or %difference (%D) between initial and continuing RRFs? (Cheek at least two values but if errors are found, check more.) _ ACTION: If errors are large, call lab for expianation/resubmittal, make any necessary corrections and note errors under "Conclusions". JL 304617 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 17 of 51 Date: August, 1992 Revision: 1 YES NO N/A 14.0 Internal Standard (Form VIII LCV) 14.1 Are the internal standard areas (Form VIII LCV) of every sample and blank within the upper and lower limits (±40%) for each continuing calibration? ACTION: List all the outliers below. Sample f Internal Std Area Lower Limit sX Upper Limit ACTION: 1. 2. If the internal standard area count is outside the upper or lower limit, flag with "J" all positive results quantitated with this internal standard. Non-detects associated with IS area counts > 40% should not be qualified. If IS area is below the lower limit (< 40%), qualify all associated non- detects (U values) "J". If extremely low area counts are reported, (< 20%) or if performance exhibits a major, abrupt drop off, flag all associated non-detects as unusable ("R"). 14.2 Are the retention times of the internal standards within 20 seconds of the associated calibration standard? ^ - ACTION: Professional judgement should be used to qualify data if the retention times differ by more than 20 seconds. 304618 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 18 of 51 Date: August, 1992 Revision: 1 YES NO N/A 15.0 Field Duplicates 15.1 Were any field duplicates submitted for Low Cone. VOA analysis? ACTION: Compare the reported results for field duplicates and calculate the relative percent difference. ACTION: Any gross variation between duplicate results must be addressed in the reviewer narrative. However, if large differences exist, identification of field duplicates should be confirmed by contacting the sampler. i > ( i _ 304619 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 19 of 51 Date: August, 1992 Revision: 1 PART B: BNA ANALYSES YES NO N/A 1.0 Traffic Reports and Laboratory Narrative 1.1 Are the Traffic Report Forms present for all samples? ACTION: If no, contact lab for replacement of missing or illegible copies. 1.2 Do the Traffic Reports or Lab Narrative indicate any problems with sample receipt, condition of samples, analytical problems or special notations affecting the quality of the data? ACTION: If samples were not iced upon receipt at the laboratory, flag all positive results "J" and all non-detects "UJ". i ^ _ x > i 2.0 Holding Times 2.1 _Have any BNA technical holding times, determined from date of collection to date of extraction, been exceeded? Continuous liquid-liquid extraction of samples for BNA analysis must be started within seven days of the date of collection, Extracts must be analyzed within 40 days of the date of extraction. • ^ Table of Holding Time Violations Sample ID (See Traffic Report) Date Date Lab Date Date Sampled Received Extracted Analyzed 304620 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 20 of 51 Date: August, 1992 Revision: 1 YES NO N/A ACTION: If technical holding times are exceeded, flag all positive results as estimated ("J") and sample quantitation limits as estimated ("UJ"), and document in the narrative that holding times were exceeded. If analyses were done more than 14 days beyond holding time, either on the first analysis or upon reanalysis, the reviewer must use profes- sional judgement to determine the reliability of the data and the effects of additional storage on the sample results. At a minimum, all results should be qualified "J", but the reviewer may determine that non-detect data are unusable ("R"). If holding times are exceeded by more than 28 days, all non-detect data are unusable (R) . xXi iXi 3.0 Surrogate Recovery (Form II LCSV) 3.1 Are the Low Cone. Semivolatile Surrogate Recovery Summaries (Form II LCSV) present? 3.2 Are all the semivolatile samples in each SDG listed on the proper Surrogate Recovery Form(s)? ACTION: Call lab for explanation/resubmittals. If missing deliverables are unavailable, document effect in data assessments. 3.3 Were outliers marked correctly with an asterisk? I 1 ACTION: Circle all outliers in red. 3.4 Were two or more base-neutral OR acid surrogate recoveries out of specification for any sample or method blank? If yes, were samples reanalyzed? i 1 Were method blanks reanalyzed? i 1 X IXI 2< X 304621 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 21 of 51 Date: August, 1992 Revision: 1 YES NO N/A ACTION: If all BNA surrogate recoveries are >10% but two within the base-neutral or acid fraction do not meet SOW specifications for the affected fraction only (i.e. base-neutral or acid compounds) : 1. Flag all positive results as estimated ("J"). 2. Flag all non-detects as estimated detection limits ("UJ") when recoveries are less than the lower acceptance limit. 3. If recoveries are greater than the upper acceptance limit, do not qualify non-detects, If any base-neutral gjz acid surrogate has a recovery of <10%: 1. Positive results for the fraction with <10% surrogate recovery are qualified with "J". 2. Non-detects for that fraction should be - qualified as unusable (R) . Professional judgement should be used to qualify data that have method blank surrogate recoveries out of specification in both original and reanalyses. Check the internal standard areas. 3.5 Are there any transcription/calculation errors between raw data and Form II? ACTION: If large errors exist, call lab for expianation/resubmittal, make any necessary corrections and document effect in data assessments. _ i 2 S _ 4.0 Laboratory Control Sample (Form III LCSV) 4.1 Is the Semivolatile Laboratory Control Sample (LCS) Recovery Form (Form III LCSV) present? f^T •Xl 304622 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 22 of 51 Date: August, 1992 Revision: 1 YES NO N/A i(i__ 4.2 Was the LCS analyzed at the required fre- quency (once per SEX;, or every 20 samples)? ACTION: If any LCS data are missing, take the action specified in 3.2 above. 4.3 How many Low Cone. Semivolatile LCS recoveries are outside QC limits? Low Cone. Water / out of 15 ACTION: If the LCS recovery is greater than the QC-limit, provided on Form III LCSV (140%), positive results should be flagged "J" for the affected compound(s). If the mass spectral criteria are met but the LCS recovery is less than 60%, then the associated detected target compounds should be flagged "J". Associated non-detected target compounds should be flagged "R". If 25 % of the analyte recoveries are below QC-limits qualify all associated positive sample data as "J" and non-detects "R". If two or more analytes show recoveries of < 10% all associated positive sample data as "J" and non-detects "R". It should be noted for TPO action if a laboratory fails to analyze an LCS with each SDG, or if a laboratory consistently fails to generate acceptable LCS recoveries. 5.0 Blanks (Form IV LCSV) 5.1 Is the Method Blank Summary Form (Form IV LCSV) present? iXi 304623 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 23 of 51 Date: August, 1992 Revision: 1 YES NO N/A 5.2 Frequency of Analysis: For the analysis of Low Cone. Semivolatile TCL compounds, has a method blank been reported per 20 samples and for each extraction batch? 5.3 Has a Low Cone. Semivolatile method blank been analyzed for each GC/MS system used? (See SOW page SV D-34, section 26.2.2) sX ACTION: If any method blank data are missing, call lab for expianation/resubmittal. If method blank data are not available, reject (R) all associated positive data. However, using professional judgement, the data reviewer may substitute field blank data for missing method blank data. 5.4 Chromatography: review the blank rav data - chromatograms (RICs), quant reports or data system printouts and spectra. Is the chromatographic performance (baseline _stability) for each instrument acceptable for "BNAs? J ^ ACTION: Use professional judgement to determine the effect on the data. 6.0 Contamination Note: "Water blanks", "drill blanks" and "distilled vater blanks" are validated like any other sample and are not used to qualify the data. Do not confuse.them vith the other QC blanks discussed belov. 6.1 Do any method blanks have positive results (TCL and/or TIC) for Lov Cone, semivolatiles? When applied as described belov, the contaminant concentration in these blanks are multiplied by^ the sample dilution factor. X J_L 304624 SfcL^Wl O^cdj^-^l ^ l l ^ l ^ r : A^^OuaUA A < ^ ^ i ^ : M L AOMUf F60H3 • 6 ^ (a-^x^Yt^^u/)/)/nrKiLX^4:c ^ 304625 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 24 of 51 Date: August, 1992 Revision: 1 YES NO N/A X 6.2 Do any field/rinse blanks have positive Lov Cone. Semivolatile results (TCL and/or TIC)? ACTION: Prepare a list of the samples associated vith each of the contaminated blanks. (Attach a separate sheet.) Note: All field blank results associated vith a particular group of samples (may exceed one per case) must be used to qualify data. Blanks may not be qualified because of contamination in another blank. Field blanks must be qualified for surrogate, spectral, instrument performance or calibration QC problems. ACTION: Follov the directions in the table belov to qualify TCL results due to contamination. Use the largest value from all the associated blanks. If gross contamination exists, all data in the associated samples should be qualified as unusable (R). 1 _ L Sample cpnc > CRQL but < lOx blank Sample cone <CRQL & is < lOx blank value Sample cone > CRQL value & > lOx blank Common Phthalate Esters Flag sample result with a "U"; Report CRQL & qualify "U" No qualification is needed Sample cone > CRQL but < 5x blank Sample cone < CRQL & is < 5x blank value Sample cone > CRQL value & >5 blank value Other Contaminants Flag sample result with a "U"; Report CRQL & qualify "U" No qualification is needed NOTE: Analytes qualified "U" for blank contamination are still considered as "hits" when qualifying for calibration criteria. 304626 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 25 of 51 Date: August, 1992 Revision: 1 YES NO N/A ACTION: For TIC compounds, if the concentration in the sample is less than five times the concentration in the most contaminated associated blank, flag the sample data "R" (unusable). 6.3 Are there field/rinse/equipment blanks associated with every sample? ACTION: Note in data assessment that there is no associated field/rinse/equipment blank. Exception: samples taken from a drinking water tap do not have associated field blanks. JL 7.0 GC/MS Instrument Performance Check (Form V LCSV) 7.1 Are the GC/MS Instrument Performance Check Forms (Form V LCSV) present for Decafluorotriphenylphosphine (DFTPP)? 7.2 Are the enhanced bar graph spectrum and mass/charge (m/z) listing for the DFTPP provided for each twelve hour shift? 7.3 Has an instrument performance check solution been analyzed for every tvelve hours of sample analysis per instrument? ACTION: List date, time, instrument ID and sample analyses for which no associated GC/MS tuning data are available. iXi — M iii DATE TIME INSTRUMENT SAMPLE NUMBERS ACTION: If lab cannot provide missing data, reject ("R") all data generated outside an acceptable twelve hour calibration interval. 304627 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 26 of 51 Date: August, 1992 Revision: 1 YES NO N/A 7.4 Have the ion abundances been normalized to m/z 198? ACTION: If mass assignment is in error, flag all associated sample data as unusable (R). 7.5 Have the ion abundance criteria been met for each instrTJunent used? ACTION: If ion abundance criteria are not met, the Region II TPO must be notified. 7.6 Are there any transcription/calculation errors between mass lists and Form Vs? (Check at least two values but if errors are found, check more.) 7.7 Have the appropriate number of significant figures (two) been reported? ACTION: If large errors exist, call lab for expianation/resubmittal, make necessary corrections and document effect in data assessments. 7.8 Is the spectrum of the mass calibration compound acceptable? ACTION: Use professional judgement to determine whether associated data should be accepted, qualified, or rejected. ^ _ JL i)i__ IXL lAi 8.0 Target Compound List (TCL) Analytes (Form I LCSV) 8.1 Are the Organic Analysis Data Sheets (Form I LCSV-1,2) present vith required header information on each page, for each of the following: a. Samples and/or fractions as appropriate? y \ ] b. Laboratory Control Sample(s)? [X] c. Blanks? D^ 304628 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 27 of 51 Date: August, 1992 Revision: 1 YES NO N/A 8.2 Are the Low Cone. Semivolatile Reconstructed Ion Chromatograms, the mass spectra for the identified compounds, and the data system printouts (Quant Reports) included in the sample package for each of the following: a. Samples and/or fractions as appropriate? fA] b. Laboratory Control Sample(s)? fX] e. Blanks fXo ACTION: If any data are missing, take action specified in 3.2 above. 8.3 Are the response factors shown in the Quant Report? J_l _X- 8.4 Is chromatographic performance acceptable with respect to: Baseline stability? Resolution? Peak shape? Full-scale graph (attenuation)? Other: iL i><i DL 'LX X ACTION: Use professional judgement to determine the acceptability of the data. 8.5 Are the lab-generated standard mass spectra of identified Low Cone. Semivolatile compounds present for each sample? |X^ ACTION: If any mass spectra are missing, take action specified in 3.2 above. If lab does not generate their own standard spectra, make note in "Contract Problems/ Non-Compliance". If spectra are missing, reject all positive data. 304629 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 28 of 51 Date: August, 1992 Revision: 1 8.6 8.7 8.8 Is the RRT of each reported compound within 0.06 RRT units of the standard RRT in the continuing calibration? YES NO N/A iXi Are all ions present in the standard mass spectrvim at a relative intensity greater than 25% also present in the sample mass spectrum? fX) Do sample and standard relative ion intensities agree within 20%? iL ACTION: Use professional judgement to determine acceptability of data. If it is determined that incorrect identifications were made, all such data should be rejected (R), flagged "N" (Presumptive evidence of the presence of the compound) or changed to not detected (U) at the calculated detection limit. In order to be positively identified, the data must comply with the criteria listed in SOW page SV D-27, section 20. ACTION: When sample carry-over is a possibility, professional judgement should be used to _ determine if instrument cross-contamination has affected any positive compound identification. 9.0 Tentatively Identified Compounds (TIC) 9.1 Are all Tentatively Identified Compound Forms (Form I, Part B) present; and do listed TICs include scan number or retention time, estimated concentration and "JN" qualifier? 9.2 Are the mass spectra for the tentatively identified compounds and associated "best match" spectra included in the sample package for each of the folloving: a. Samples and/or fractions as appropriate? b. Blanks? lA s3L D3L 304630 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 29 of 51 Date: August, 1992 Revision: 1 YES NO N/A ACTION: If any TIC data are missing, take action specified in 3.2 above. ACTION: Add "JN" qualifier if missing. 9.3 Are any TCL compounds (from any fraction) listed as TIC compounds (example: 1,2- dimethylbenzene is xylene a VOA TCL and should not be reported as a TIC)? X x_i ACTION: Flag vith "R" any TCL compound listed as a TIC. 9.4 Are all ions present in the reference mass spectrum vith a relative intensity greater than 25% also present in the sample mass spectrum? 9.5 Do TIC and "best match" standard relative ion intensities agree vithin 20%? ACTION: Use professional judgement to determine acceptability of TIC identifications. If it is determined that an incorrect ~ identification vas made, change identification td "un)cnovn" or to some less specific identification (example: "C3 substituted benzene") as appropriate. Also, vhen a compound" is not found in any blank, but is a suspected artifact of a common laboratory contaminant, the result should be qualified as unusable (R). iXl ixi 10.0 Compound Quantitation and Reported Detection Limits 10.1 Are there any transcription/calculation errors in Form I results? Cheek at least tvo positive values. Verify that the correct internal standard, quantitation ion, and RRF vere used to calculate Form I result. Were any errors found? [/^^ 304631 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 30 of 51 Date: August, 1992 Revision: 1 YES NO N/A 10.2 Are the CRQLs adjusted to reflect sample dilutions? iH ACTION: If errors are large, call lab for expianation/resubmittal, make any necessary corrections and document effect in data assessments. ACTION: When a sample is analyzed at more than one dilution, the lowest CRQLs are used (unless a QC exceedance dictates the use of the higher CRQL data from the diluted sample analysis) . Replace concentrations that exceed the calibration range in the original analysis by crossing out the "E" and it's associated value on the original Form I and substituting the data from the analysis of the diluted sample. Specify which Form I is to be used, then draw a red " X" across the entire page of all Form I's that should not be used, including any in the summary package. 11.0 -Standards Data (GC/MS) 11.1 Are the Reconstructed Ion Chromatograms, and data system printouts (Quant, Reports) present for initial and continuing calibration? [Xl ACTION: If any calibration standard data are missing, take action specified in 3.2 above. 12.0 GC/MS Initial Calibration (Form VI LCSV) 12.1 Are the Initial Calibration Forms (Form VI LCSV-1,2) present and complete for the Lov Cone. Semivolatile fraction at concentrations of 5, 10, 20, 50 and 80 ug/1? [X] ACTION: If any calibration standard forms are missing, take action specified in 3.2 above. 304632 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 31 of 51 Date: AugTJst, 1992 Revision: 1 YES NO N/A 12.2 Are response factors stable for semivolatiles over the concentration range of the calibration (% Relative standard deviation (%RSD) < 30.0%)? ACTION: Circle all outliers in red. s ^ NOTE; ACTION: NOTE: Although 22 Lov Cone. Semivolatile compounds have a minimum RRF and no maximum %RSD, the technical criteria are the same for all analytes. If the % RSD is > 30.0%, qualify positive results for that analyte "J" and non- detects using professional judgement. When RSD > 90%, flag all non-detect results for that analyte R (unusable). Analytes previously qualified "U" due to blank contamination are still considered as "hits" when qualifying for calibration criteria. 12.3 Are all Semivolatile compound RRFs > 0.05? ACTION: Circle all outliers in red. iXi ACTION: If any RRF < 0.05: 1. "R" all non-detects. 2. "J" all positive results. 12.4 Are there any transcription/calculation errors in the reporting of average response factors (RRF) or % RSD? (Cheek at least tvo values but if errors are found, check more.) ACTION: If errors are large, call lab for expianation/resubmittal, make any necessary corrections and note errors in data assessments. iH 304633 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 32 of 51 Date: August, 1992 Revision: 1 YES NO N/A 13.0 GC/MS Continuing Calibration (Form VII LCSV) 13.1 Are the Continuing Calibration Forms (Form VII LCSV-1,2) present and complete for the semivolatile fraction? 13.2 Has a continuing calibration standard been analyzed for every tvelve hours of sample analysis per instrument? ACTION: List belov all sample analyses that were not within twelve hours of a continuing calibration analysis for each instrument used. ACTION: If any forms are missing or no continuing calibration standard has been analyzed within twelve hours of every sample analysis, call lab for explanation/ - resubmittal. If continuing calibration data are not available, flag all associated sample data as unusable ("R"). 13.3 Do any semivolatile compounds have a % Difference (% D) between the initial and continuing RRF which exceeds the + 25.0%" criteria? ACTION: Circle all outliers in red. ACTION: Qualify both positive results and non- detects for the outlier compound(s) as estimated (J). When %D is > 90%, reject all non-detects for that analyte (R) unusable. 13.4 Do any semivolatile compounds have a RRF <0.05? ACTION: Circle all outliers in red. S ^ lA — 304634 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 33 of 51 Date: August, 1992 Revision: 1 YES NO N/A ACTION: If RRF <0.05, qualify as unusable (R) associated non-detects and "J" associated positive values. 13.5 Are there any transcription/calculation errors in the reporting of average response factors (RRF) or % difference (%D) between initial and continuing RRFs? (ChecJc at least tvo values but if errors are found, check more). ACTION: If errors are large, call lab for expianation/resubmittal, make any necessary corrections and document the effect in data assessments. ixi 14.0 Internal Standards (Form VIII LCSV) 14.1 Are the Internal Standard Area and RT Summary Forms (Form VIII LCSV-1,2) present and complete for the semivolatile fraction? 14.2 Are the internal standard areas for every sample and blank vithin the upper and lover limits (-50% to +100%) for each continuing -calibration? ACTION: List all the outliers belov. Sample i Internal Std Area Lower Limit iXi i ) < i _ Upper Limit ACTION: 1. If the internal standard area count is outside the upper or lover limit, flag vith "J" all positive results and non-detects (U values) quantitated with this internal standard. 2. Non-detects associated vith IS areas > 100% should not be qualified. 304635 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 34 of 51 Date: August, 1992 Revision: 1 YES NO N/A 3. If the IS area is belov the lover limit (<50%), qualify all associated non- detects (U-values) "J". If extremely lov area counts are reported (<25%) or if performance exhibits a major abrupt drop off, flag all associated non-deteets as unusable (R). 14.3 Are the retention times of the internal standards vithin 20 seconds of the associated calibration standard? ACTION: Professional judgement should be used to qualify data if the retention times differ by more than 20 seconds. sX 15.0 • Field Duplicates ^ 15.1 Were any field duplicates submitted for Lov Cone. Semivolatile analysis? f^j ACTION: Compare the reported results for field duplicates and calculate the relative percent difference. ACTION: Any gross variation betveen field duplicate results must be addressed in the reviever narrative. Hovever, if large differences exist, identification of field duplicates should be confirmed by contacting the sampler. 304636 • QA/QC Review of Target Analyte List Metals Data For Pace Analytical SDG: 98004 ISLAND CHEMICAL January 19, 1998 Reviewer: Uma Parasar Holding Times: Samples were analyzed within holding times. Initial and Continuing Calibration Verification: All percent recoveries were within control limits except for cyanide. The percent recoveries associated with the continuing calibration verifications for cyanide were 120.6%, 117.4%, 118.2%, and 115.8%. No data were qualified since cyanide was not detected in any of the samples. Blank Contamination: No metals were detected in the calibration and preparation blanks at concentrations above the contract required detection limit (CRDL). Field blanks reported concentrations of iron, lead, and zinc above the CRDL. Iron results in samples MW-1, MW-4, MW-2, MW-2D, and MW-7 were qualified as not detected based on the field blanks. Lead results in samples MW-1, MW-4, MW-10, MW-3, MW-5, and MW-9 were qualified as not detected based on the field blanks. Zinc results in samples MW-2, MW-2D, MW-5, MW-9, and MW-7 were qualified as not detected based on the field blanks. CRDL Standard: The percent recoveries for the CRDL standard were outside acceptable limits (80-120%) for selenium (78.6%>) and zinc (69.8% and 66.6%i). All selenium and zinc data were qualified as estimated (J) if detected and (UJ) if not detected. ICP Interference Check Sample: The percent recoveries were outside acceptable control limits (80-120%) for calcium (70.8%, 69.8%) and cobalt (79.6%, 77.9%). All associated calcium and cobalt data were qualified as estimated (J) if detected and (UJ) if not detected. Spike Sample Recovery: All spike recoveries were within control limits with the following exceptions: lead (-56.9%), manganese (-20.1%), and cyanide (26.2%i). Based on these recoveries, the cyanide data for all samples is rejected as unusable. Duplicates: The RPDs exceeded 50%i or the difference between replicate results exceeded the CRDL for the following metals: aluminum, calcium, iron, magnesium, manganese, and zinc. The associated data for these metals in all samples were qualified as estimated (J) if detected and (UJ) if not detected. 3 0 4 6 3 7 Laboratory Control Sample: All recoveries were within control limits. ICP Serial Dilution: All %Ds were below the allowable maximum (10%) with the exception of calcium (11.1%). Calcium data in all samples were qualified as estimated (J) if detected and (UJ) if not detected. Field Replicate: One field replicate was collected and the data were compared and the RPDs calculated. The RPD for zinc (69.6%) was greater than 50%). Zinc data were qualified as not detected based on field blank contamination; therefore, no additional qualifiers were applied. ICP Linear Ranges: The following results in the respective samples were qualified as estimated since the results exceeded the linear range and were not re-analyzed at a dilution. Sample MW-1 MW-3 MW-5 MW-6 MW-10 Metal (s) Manganese, Potassium Manganese Potassium Manganese Manganese Qualifier J J J J J G\stafi\uparas\DVMEMOS\98004IC_rNg 3 0 4 6 3 8 Evaliiation of Metals Data for tha Contract Laboratory Program (CLP) based on SCK7. 3/90 (SOP Revision XT) PREPARED BY: Th\y^-^l ^-:.-k-Cc(A DATE: Hahif Sheikh, Quality Assurance Chemist Toxic and Hazardous Waste Section --^-- '?2 APPROVED BY APPROVED BY Ruhyon, Monitoring Managi DATE: \ ' ^ ^ ' ~ \ Z Kevin Kubik, Qiief Toxic and Hazardous Waste Section DATE: //?^7<?' 3 0 4 6 3 9 # STANDARD "^^rPJC^l'C tnXZDQRE Title: Evaluation of hfetals Data'xor c^ia Date: Jan. 1992 Contract laboratory Program Number: HW-2 Revision: 11 •' 1.0 Soope 1.1 This procedure is applicable to inorganic data obt^dned frrxn oorrtractor laboratxiries working for Hazardous Waste Site Contract laboratory Program (OP). 1.2 The data validation is based upon cinalytical and quality assurance requirements specified in Statement of Work (SOW) 3/90 . 2.0 Reaponaibilities - Data reviewers vill ccnplete the follcwing tasks as cissigned by tl Data Review Coondinator: 2.1. For a total reviev; 2.1.1 Data Assessnent - "Total Review-Inorganics*' Chetdclist Appendix (A.l). The reviewer must answer every question on the checklist. 2.1.2 Data Assessment - Data Assesymfint Kzucrative (Appendix A.2) The answer on the checklist must mat:ch the action in the nsurrative (appendix A.2) cind on Form I's. IDo not vise pencil to write the riarrative. 2.1.3 Contract tfon-Ccc^liance - ShP Report (Ai:pent1ix A.3) This report is to be completed only when a serious contract violation is encountered, or upon the request of the Data Validation Task Monitor, or Technical Project Officer (TPO). Forward 5 copies: one each for intemal files, appropriate Regionail TPO, Sample Management Office (SMD) and last two addresses of Mailing List for Data Reviewers (Appendix A.4). In other cases, all contract violations should be appended to the end of the Data Assessment Narrative (Sec. A.2.2). 2.1.4 CLP Data A3se35aTipnt sutmary Fona 2.1.4.1 Appendix A.5 Fill in the total number of analytes analyzed by different aneilyses and the number of Einalytes rejected or flagged as estimated due to corresponding quality control criteria. Place an "X" in boxes where cuialyses were not performed, or criteria do not apply. 2.1.4.2 Appendix A.6 Data reviewer is also required to fill out Inorganic Regional Data Assessment form (Appendix A.7) provided by EPA Headquarters. Codes listed on the form will be used to describe t:he Data Assessment Summary; 304640 STANDARD OPERATING PROCEDURE Title: Evaluation of Metzals Dat:a for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Revision: 11 2.1.5 Data Review Lxr; It is reacninended that each data reviewer should maintain a log c the reviews caipleted to include: a. date of staurt of case revie b. dat^ of oonpleticn of case review c. site d. case romtoer e. contract laboratory f. number of samples g. matrix h. hours warked i. reviewer's initials 2.1.5 Telephone Reoord leg - the data reviewer should enter the beure facts of inquiry, before initiating any phone conversation with CLP laboratory. After the case review has been caipleted, mail white ccpy of Telephone Record Log to the laboratuary and pink copy to SWD. File yellow copy in tzhe Telephone Record Log folder, and attach a xerox copy of the Telephone Record Log to the ccrpleted Data Assessment Narrative (Appendix A.2). 2.1.7 Forvarded Paperwork .•' 2.1.7.1 Upon conpletion of review, the follcwing are to be forwarded to the Regional Saitple Control Centier (RSCC) located in the Surveillcince and Monitoring Brar£h: a. data package b. completed data assessment checklist (Appendix A.l,original) c. SMO Contract Ccmpliance Screening (CCS) d. Record of Ccmtiunication (copy) e. CLP Reanalysis Request/Approval Record (originail + 3 ccpies) f. Appendix A.6 (original). 2.1.7.2 Forward 2 copies of ccrpleted Data Assessment Narrative (Appendix A.2) along with Z copies of the Irxjnganic Data Assessment Form (Appendix A. 6) and Telephone Record log , if any,: ene each for appropriate Regional TPO, and the other one to EEA EMSL office in Las Vegas. The addresses of TPOs and EPA office in Las Vegas are given in Appendix A-^. '" 2.1.8 Filed Papervorjc - Upon ccnpletiion of review, the follcwing are to be filed within MMB files: a. Two copies of ccrpleted Cata Assessment Narrative (Appendix A.2) each carrying Appendix A.6. b. Telefiior^ Raoord Leg (copy) c. SMD Report (copy Appendix A-3) d. CLP Reanalysis Recjiest/Approval Record (copy) 304641 STANDARD OPERATING fRDCEDURE Title: Evaluation of Metals Data for the Data: Jan. 1992 Contract Laboratory Program Number: HW-2 Revision: 11 3.0 Data Occplet.PTtfW3 Each data package is checked by a Ragicnal Sanple Ocaitrol Coordinator (RSSC) for ccnpleteness. A data package is ag;.<?^7Tnpr^ to be ccnplete when' all the deliverables required under the contract are present. If a data package is inoaiplete,the RSSC would call the laboratory for nissing document(s). If the laboratory does not respon within a week, SMD and MMB coordinator of Regicn H will be notified. 4.0 Rejection of Data - All values determined to be unacceptable on the Inorganic Analysi Cata Sheet (Form I) must be lined over with a red pencil. As soon as any review criteria causes data to be rejected, that dal:a can be eliminated fran any further revie or consideration. 5.0 Acceptance Criteria - In order that reviews be consistent among reviewers, accept:anc criteria as stated in /^pendix A.l (pages 4-25) should be used. Additioral guidanc can be found in the National Inorganic Functimal Guidelines of October 1, 1989. 6.0 SMD Contract Ccnpiiance Screening (CCS) - This is intended to aid reviewer in locatin any problems, both corrected and uncorrected. However, the validation should be carrie out even if CCS is not present. Resutnittals received fran laboratory in response t CCS must be used by the reviewer. 7.0 Repueat for Rftnnfllysis - Data reviewers must rxjte all items of contract non-complianc wit:hin Data Assessment Narratu.ve.If holding times and sample storage times have not bee exceeded, TPO may request reancilysis if items of non-ocnpliance are critical to dat assessment. Requests aure to be made on "CLP Re-Analysis Request/Approval Record". 8.0 Record of CrtTiTn.mication - Provided by the Regional Sanple Control Center (RSCC) to indicate wtiich data packages have been received and are ready to be reviewed. 9.0 Roundino off nunbers - The data reviewer will follow the standard practice. 304642 STANDARD OPSHKnUG raOCEHIRE •^os 4 of 34 Title: Eval\jation of Metals Data for the Contract Laboratory Program Appendix A.l: Datia Assessment - Contract Ccnpiiance (Total Review) i^ate: Jan. 1992 Number: HWT2 Revision: 11 A. 1.1 Contract Cmplianoe Screening Report (CCS) - Present? ACTION; If no, contact RSOC. A. 1.2 Reoord of nmrrimieation (fran R8CC) - Present? ACTION: If no, request fran RSOC. A. 1.3 Trip Report - Present and ccnplete? ACTION; If no, contact RSOC for trip report. A. 1.4 Sample Traffic Report - Present? Legible? ACTION; If no, request fran Regional Sample Control Center (RSOC). A. 1,5 Cover Page - Present? Is cover page properly filled in and signed by the lab manager or the manciger's designee? ACTION: If no, prepare Telephone Record leg, and contact laboratory. Do numbers of sanples correspond to numbers on Record of Cammunicat:icn? Do sanple nuniacrs on cover page agree vith sanple numbers on: (a) Traffic Ri^xart Sheet? (b) Form I's? ACTION; If no for einy of the above, ccntact RSOC for clarification. YES IW NZ^ [ ] [ ] [JL K X [ X j _ ^ _ C.X] _ _ 304643 STANCftRD OPERATING PROCEDURE Title: Evaluation of Metals Data for the Contract labaratcry PtDgran ;^pendix A-1: Data Assessaent - Contract ccnpiiance (Tbtal Review) Date: Jan. 1992 Number: Hy-2 Revision: li A.1.6 Form I to IX i ^ No M A. 1.6.1 Are all t:he Ptorm I through Form IX labeled with: laboratory name? Case/SAS nuntser? EPA sanple No.? SDG No.? Contract No.? Correct units? Matrix? ACTION; If rx3 for ciny of the above, note under Contract Problenv^on-Ocrpliance section of the "Data Assessment Narratu.ve". A. 1.5.2 Do any ccnputation/transcription errors exceed 10% of reported values on Forms I-DC for: (NOTE: Check all forms against raw data.) (a) all analytes analyzed by ICP? (b) all analytics analyzed by GFAA? (c) all analytes analyzed by AA Flame? (d) Ifercury? (e) Cyanide? ACTION; If yes, pr^aare Telephone leg, contact laboratory for corrected data and correct errors vith red perxdJ. and initial. t 1 (il: 1 1 (il) (AI K X X «^»*-* x x; X X 304644 STANDARD OPERATING IWXEDURE Title: Evaluation of Hetals Data for the Contract Laboratory Program i^^pendix A.l: nat:a Assessment - Contract Ccrnpliance (Total Review) Date: Jan. 1992 Nuntser: HW^2 Revision: 11 A.1.7 Raw Data A. 1.7.1 Digestion Log* for flame AA/ICP (Form XUI) present? Digestiicn Log for furraoe AA Fom x m present? Distillation Log for mercury Form x m present? Distillation Log for cyanides Form x m present? Are pH values (pH<2 for all metals, pH>12 for cyanide) present? *Weights, dilutions and volumes .used to cbtaiin values. Percent solids calculation present for soils/sediments? iX J - iX — ^ ( _ ] _ ^ A.1.7.2 A.1.7.3 in sectu.ons A.l.7.1 through A.l.7.3, v r i t e Tel^Jhone Record log and contact laboratory for resubmittals. logs/berch sheets? Measurement read art reoord present? ICP Flame AA Furnace AA Mercury Cyanides Are aill raw data to support a l l sanple analyses and QC operations present? Tftjible? Pmopprly TflbplPd? ACTION: If no for any of the above questions tX3 iJL [ . ] r .1 [JL [2L] iJL iJL iJSJ '. j C A X 304645 STANDARD OPERATING FRDCEDURE Title: Evaluation of Metals for the Contract Date: Jan. 1992 Laboratory Program Nuntaer: HW-2 Appendix A.l: Data Assessment - Contract Revision: 11-- Compliance (Total Review) YES NO N/A A. 1.8 Holding Timaa - (euqueous amd soil sanples ) (Examine sanple traffic reports and digesticaVdistillation logs.) Mercury analysis (28 days) exceeded? [_LSJ Cyanide distillation (14 days) exceeded? [JL Other htetals. analysis (6 months). . . . exceeded? [JL NOTE: Prepare a list of all sanples and analytes for which holding times have been exceeded- Specify the number of days f m n date of collection to the date of preparation (from raw data). Attach to checklist. ACTION; If yes, reject (red-line) values less than Instrument Detection Limit (IDL) and flag cis estimated (J) the values above IDL even though sample(s) was preserved properly. A. 1.8.2 Is pH of aqueous Scinples for; w Metals Analysis >2? J L C ] Cyanides Analysis <12? Vs [ ] Action: If yes, flag the associated metals and cyanides data as estimated. A.1.9 Fonn I (Final Data) A. 1.9.1 Are ciU Form I's present and ccnplete? [_SJ ACTION; If no, prepare telephone record log arxi contact laboratory for sufcciittal. A. 1.9.2 Are correct units (ug/1 for waters and mg/kg for soils) -^ indicated on Form I's? r '^l Are soil sanple results for each parameter corrected for w percent solids? [ ] "^ Are 2LL1 "less than IDL" values properly coded with "U"? r X 1 304646 STANDARD OFERATING PROCEDURE Title: Evaluation of Metals Data for the Contract Laboratory Program Appendix A.l; Data Assessment - Contract Ccnpiiance (Total Review) Date: Jan. 1992 Number: HW-2 Revision: 11 A.1.9.3 A.1.10 A.1.10.1 Are the correct ccncentraticn qualifiers used with . final data? L _ J ACTION; If no for any of the above, prepare Telephone Record Log, and contact laboratory for corrected data. m NZA Are EPA sanple # s and corre^xsxUng laboratory sanple ID # s the same as on the Cover Page, Form I's and in the raw data? Was a brief physical description of sanples given on Form I's? Was the dilution of any sanple diluted beycxxi the requirementis of the contract noted on Form I or Form XIV? ACTION; If no for any of the above, note under Ccntract-Problem/Non-Ccnplianoe of the"Data Assessment Nsurratrive". Calibration Is record of at least 2 point calibraticn present for ICP analysis? Is record of 5 point calibration present for Hg analysis? Is record of 4 point calibration present for: - Flame AA? Rimaoe AA? cyanides? Is one calibration standard at the CRDL level for all AA (exoept Hg) and cyanides analyses? [ ] K _ •X [_X] [ ] [JL — — ACTION: If no for any of the above, write in the Ccntract Prohleny/Non-Carpliance section of the "Data Assessment Narrative". 304647 STANDARD OPERATING PROCEDURE Title: Eval\:iation of Metals Dat:a for the Contract Laboratory Program Appendix A.l; Data Assessment - Ccntract Ccnpiiance (Total Review) Date; Jan. 1992 Number: HW-2 Revisiai: ll A.1.10.2 Is oorrelatiicn coefficient less than 0.995 for: Mercury Anadysis? cyanide Analysis? Atcndc Absorption Analysis? ACTION: If yes, flag the associated data as estimated. NOTE: The data validator shall calculate t:he correlation coefficient using ccrcentrations of the standards and the corresponding instrument response ( e.g. absorbance, peak area., peak height, e t c . ) . A.1.10.3 In the instance where less than 4 standards are measured in absorbance (or peak eunea, peak hei^t,etc.) mode, cu?e the remaining standcurds analyzed in concentration mode immediately after calibration within ±10% of the true values? [ ] ACTION; If no, flcig the associated data as estimated if standards are not within +10% of true values. Do not flag the data as estimated in linear range indicat:ed by good reoovery of standard(s). YES NO _ [JL] _ [JL U/A X K A.1.11 Fonn II A (Initial and Qontinuing calibration Verification)- A. 1.11.1 Present and ccnpletie for every metal and cyanide? [^ ] Present and caiplet:e for AA cind ICP when both are used for the sane analyte? [ ] AgnON; If no for any of tha above, prepare Telephone Reoord Log and contact laboratory. A.1.11.2 Circle on each Form IIA all percent reooveries that are outside the contract windows. Are all calibratiion standards (init:ial and continuing) within cont:rcl limits: ^, Metals- 90-110%R? f \ ] Bg - 80-120%R? r K i Cyanides- 85-115%R? [ ] X - 304648 STANDARD OPERATING PROCEDURE Page 10 of . 34 Title: Evaluation of Metzals Data for the Date: Jan. 1992 Contract Laboratory Program Number; HW-2 Appendix A.l: Data Assesanent - Ccntract Revision: 11 Ccnpiiance (Total Review) ~^ ^ ^ " ^ N/A ACTION; Flag as estimated (J) all positive data (not flawed with a "U") analyzed between a calibration standard vith %R between 75-89% (65-79% for Hg; 70-84% for CN) or 111-125% (121-135% for Hg; 116-130% for CN) recxrvery and rvearest good calibratJ.cn standard. Qualify results <IDL as estimated (UJ) if the ICV or CCV %R is 75-89% ( d i , 70-84% ; HG, 65-79%). Reject (red-line) as unacceptable data if reoovery of the ICV or CCV is outside the range 75-125% (CN, 70-130%; Hg, 65-135%). Qualify five sanples cai either side of verification standard out of control limit:s. A. 1.11.3 Was continuing calibration performed every 10 sanples , or every 2 hours? [___] Was ICV for cyanides distilled? [JL] ACTION; If no for ciny of the above, vrite in the Contract-Problenv/Non-Ccnpliance secticn of the "Data Assessment Narrative". A.1.12 Form II B (CRDL St.nnrt;>rd3 for AA and ICP) - ^• A. 1.12.1 Was a CRDL standard (CRA) aralyzed after initial y calibration for all AA metals (except Hg)? [ ] A Wais a mid-range calib. verification standard distilled and cinalyzed for cyanide analysis? f X 1 Was a 2XCRDL ( or 2xIDL when IDL>CRDL) analyzed (CRI) for each ICP run? f A] (Note: CRI for AL,Ba,Ca,Fe,Mg,Na,or K is not required.) ACTION: If no for any of tha above, flag as estimated all data falling within the affected ranges. Tha affectad ranges are: AA AnzLlysis - **True Value ± CRDL ICP Analysis - **True Value + 2CRDL CN Analysis - **True Value ± 0.5 x True Value. **True value of CRA, CRI or mid-range standard. Substitute IDL for CRDL when IDL > CRDL. Compute the concentration of the missing mid-range standard from the calibratd.on range. 304649 STANDARD OPERATING FRDCEDURE Title: Evaluation of Metals Data for the Cate: Jan. 1992 Contract Laboratory Program Nunfcer: HW-2 Appendix A.l: Data Assesanent - Ccntract Revisicn: 11 Ccnpiiance (Totial Review) _ _ _ _ A.1.12.2 Was CRI analyzed after ICV/ICB arxi before the final OCV/CCB, and twice every e i ( ^ hours of ICP rtm? f X 1 ACTTON: If no, write in Contract Problem/Non-Ocnpliance Section of the "Data Assessment Narrative". A. 1.12.3 Circle on each Form IIB all tha percent reooveries that eure outside the acceptzinoe windows. X Are CRA cmd CRI standards within control limits: Metals 80 - 120%R? [ ] Is mid-rsinge standard within control limits: Cyanide 80 - 120%R? r X ] . ACTION; Flag as estimated all sanple resultis within tha affected range if the recovery of the standard is between 50-79%; flag only positive data within the aiffected range if the recovery is between 121-150%; reject all dat:a within the affected range if the recovery is less than 50%; reject only positive data within the affected range if the reoovery is greater than 150%. Qualify 50% of tha samples on either side of CRI standard outside the control limits. Note: Flag or reject the final results cnly vhen sanple raw data are within the affected ranges and the CRDL standards are outside the acceptsnnp windcws. A.1.13 Form I H (Initial and Continuing Calibration Blanks) A. 1.13.1 Present and ccnplete? [JL For both AA and ICP when both a r e usad for tha ^ same analyte? [ ] A Was an initial calibratiion blank aralyzed? [JL Wcis a continuing calibraticn blank aralyzed after every 10 sanples or every 2 hours (which ever is more frequent)? _ [JL 304650 STANDARD OPERATING PROCEDURE Title: Evaluation of iCsitzJ-s Data for the Data: Jan. 1992 Contract Latoratiii/ i-rcgram Number: HW-2 Appendix A.l; Data Assessment - Contract Revision: 11 Corpliance (Totial Review) ACTICN; If no, prepare Tel^ixyie Reoord Log, ccntact laboratory and write in the Contract-Problems/ Non-Ccnplianoe secticn of the "Data Assessment Narrative". A. 1.13.2 Circle on each Form I H all calibration blamk values that are above CRDL (or 2 x IDL when IDL > CBLKJ) . Are all calibratJ.cn blanks (when IDLcCRDL) less than or . equal to the Contract Required Detection Limits (CRDLs)? [ J L Are all calibratiion blanks less than two tJmes .^ Instrument Detection Limit {\A)en IDL>CRDL)? [ ] X ACTTON; If no for any of the eibove, flag as estimated (J) positive sanple results when raw sample value is less than or equal to calibration blank value einalyzed between calibration bleink with vsilue over CRDL (or 2xIDL) and r^earest good, calibration blank. Flaig five samples on either side of the calibration blank outside t h e control limits. A.1.14 FORM III (Preparation Blank) - (Note; The preparation blcink for mercury is tihe same as the calibratiion blank.) A. 1.14.1 Was one prep, blank anedyzed for: each Sanple Delivery Group (SDG)? [ ^ 1 each batch of digested sanples? [JL each matrix type? [ ] A both AA and ICP when both are used for the same analyte? [ ] A ACTION; If no for any of the above, flag as estimatied (J) all tha associati?d positive data <10 X IDLs for which prep, blank was not analyzed. NOTE: If only one blank was analyzed for more than 20 sanples, then first 20 sanples analyzed do not have to be flagged as estimated (J). 304651 K .STANTARD 'OPERATING FRDCEDURE Title: Evaluation of Netcils Data for the Date; Jan. 1992 Contract Laboratory Program Nuniser; HW-2 Appendix A.l: Cata Assessment - Contract Revisicai: 11 cinpliaixae (Ttjtaa Review) _ — . _ - A. 1.14.2 Is concentration of prep, blank value greater -w than tha CRDL vA^en IDL is less than or equal to CRDL? t^—ij If yes, is the concentration of tha sanple with the least concentrated analyte less thcin 10 times N/ the prep.blank? [ ] Jx ACTION: If yes, reject (red-lina) all assoriatfsi data greater than CRDL ocnoentration but less than ten times the prep, blsmk value. A. 1.14.3 Is conoentration of prep, blank Vcilxie (Form III) less than two times IDL, when IDL is greatier than CRDL? [ ] ACTTON; If no, reject (red-line) edl positive sanple resultis when sanple raw data are less tihan 10 times the prep, bleink valvie. A. 1.14.4 Is concentratiion of prep, blaink below ^ the negative CRDL? [JL ACTT(3N; If yes, reject (red-line) all associated sanple results less than lOxCRDL. A. 1.15 Fonn TV (ICP Interference Check Sjcnple) A. 1.15.1 Present and ccnplete? f Y ] (NOTE: Not required for furr^ce AA, flame AA, mercury, cyanide and Ca, Mg, K arxl Na.) Was ICS analyzed at beginning and end of run (or at least twice every 8 hours)? f X ] ACTTON; If no, flag as estimated (J) all tha sanples for which AL, Ca, Fe, or Mg is higher than in ICS. A.1.15.2 Circle all values cm each Form IV that are more than + 20% of true or established mean vadue. Are all Interference Check Sanple results inside tha control limits (+ 20%)? [ ] If no, is ccncentration of Al, Ca, Fe, or Mg lower thsn the respectiive concentration in ICS? r ^ ] K 304652 STANDARD CPE9ATING HKXECURE Title: Evaluation of Metals Data for tbe Data: Jan. 1992 Contract Laboratory Program Number: HW-2 Afpendix A.l: Data Assessment - Ccntract Revision: 11 Ccmpliance (Ttotad Review) " ^ ^^ N/A ACTTCM; If rx), flag as estimated (J) those positiive results for v*aich ICS recovery is between 121-150%; flag all sanpia results as estimated if ICS recovery falls wilihin 50-79%; reject (red-line) those sanple results for which ICS reoovery is less than 50%; if ICS reoovery is above 150%, reject positive results only (not flagged with a "U"). A. 1.16 Form V A (Spiked Sample Reoovery - Pre-Diae3tion/Pr&"Distillation)- ( Note; Not required for Ca, Mg, K, and Na (both matrices), Al, and Fe (soil only.) A. 1.16.1 Present and coipletie for: each SDG? f X 1 each matrix type? [ ] X • each cone, range (i.e. low, mad., high)? [ ] X For both AA and ICP when both are used for y,- the same analyte? [ ] ', X ACTION: If no for any of tihe eibove, flag as ^-. estimatied (J) a l l the positive data less than four times the spiking levels specified in SCW for v^ch spiked sanple was not analyzed. NOTE: If one spiked sanple was aralyzed for more than 20 sanples, then first,20 sanples analyzed do r>ot have to be flagged as estimated (J). A. 1.16,2 Was field blank used for spiked sanple? [_Sj ACTTON; If yes, flag all positive data less them 4 X spike added as estimaliad (J) for which field blank was vised as ^iked sanple. A. 1.16,3 Circle on each Form VA all spike recoveries that cire outside ccntrol limits (75^ to 125%). Are all recoveries within ccntrol limits? [ ] A J - 304653 If rxD, is sanple oorx:entiration greater than or equal to four times spike concentration? STANDARD OPERATING i«DCEaiP£ Title: Evaluation of Metals Datia for the Contract laboratory Program Appendix A.l; Data Assessment - Contract Corpliance (Total Review) Data; Jan. 1992 Number: HW-2 Revisicn; 11 A.1.16.4 YES AcncM; If yes, disregard ^ i k e reooveries for analytes whose conoei 1 trat icns are greater than or equal to four times spike added. If no, circle those analytes on Form V for which sanple concentration is less than four tiimas tha ^iJos ocTx^entration. Are results outside the control limits (75-125%) flagged with "N" cn Form I's and Form VA? X ACTION; If no, write in the Contract - Problenv/Non - Ccnpliarce section of "IData Assessment Narrative". Aqueous Are any spike recoveries; ACTTON; (a) less than 30%? (b) between 30-74%? (c) between 126-150%? (d) greater than 150%? If less than 30%, reject all associated aqueous data; if between 30-74%, flag edl associated aqueous data as estimated (J); if between 126-150%, flag as estimated (J) all assoniatPd aqueous data n o t flagged with a "U"; if greatier than 150%, reject (red-line) all associated aqueous data rxrt flcigged with a "U". X m [JL] iJL [JL N/A CZN] A.1.16.5 Soll/Sftd-immt Are ciny spika reooveries; (a) less than 10%? (b) between 10-74%? (c) between 126-200%? (d) greater than 200%? [ . ] f ] f ] [ ,] X X X X 304654 STANDARD OPERATING FRDCEDURE Title: Evaluation of Metals Data for the Date; Jan. 1992 Contract laboratory Program Nunter: HW-2 Appendix A.l; Datia Assesanent - Ccntract Revision; 11 Ccmpliance (Total Review) _ _ _ _ ACTION: If less than 10%, reject all associated data; if between 10-74%, flag all accot^i:^t**i data as estimated; if between 126-200%, flag as estimated all associated data was not flagged with a "U"; if greater than 200%, reject all associated data ix3t flagged with a "U". A. 1.17 Fonn VI (Lwb Duplicates) A. 1.17.1 Present and ccnplete for; each SDG? f X ] each matrrix type? f X ) each concentratiion range (i.e. low, med., high)? [ ] X both AA eind ICP when both are used for tha same analyte? [ ] ACTTON: If ro for any tihe above, flag eis estimated (J) all the data >CRDL* for which duplicate sanple was r>ot analyzed. Note; 1. If one duplicate sanple was cinalyzed for more than 20 samples, then first 20 sanples do not have to be flagged as estimated. 2. If percent solids for soil sanple and its duplicate differ by more than 1%, pr^aare a Form VI for each duplicate peiir, report ccnoentrations in xjg/L on wet wei^t basis and calculate RPD or Difference for each aneilyte. A. 1.17.2 Was field blar^ vsed for duplicate euialysis? f X ] ACTION; If yes, flag all data >a^DL* as estimated (J) for which field blank was used as duplicate. A. 1.17.3 Are all values within cantrol limits (RPD 20% or ^ differerx» < 4CRDL)? [ ] JL If rx3, cure all results outside tha cantrol limits v^ flagged with an * on Form I's and VI? [JL ACTTON: If r>o, write in the Contract - Problems/Non- Ocnpliarxsa section of "Data Assessment Narrative". * Substitutie IDL for CRDL when IDL > CRDL. 304655 >< STANDARD OPERATING IRDCEDURE Title: Evaluaticn of Metals Data for the Data: Jan. 1992 • Contract Labocatory Program Nunfcer: HW-2 Appendix A-1: Data Assessaent - Ccntract Revision: 11 Ccnpiiance (Ttital Review) f NOTE: 1. RPD is not calculable for an anadyta of the sasple - duplicate pair when both values are less than IDL. 2. If the result of lab duplicate aralyzed by GFAA is rejectable dua to coefficient of oorrelatiion of MSA, analytical ^ika reoovery, or duplicate injections criteria, do not apply precisicsi criteria t o ^nt^^^ig euiedyzed by GFAA. A.1.17.4 Aqueous Circle on each Form VI edl values that are; RPD > 50%, or Dif f ererx» > CRDL* Is any RPD greater than 50% where sanple and duplicate ^ eure both greater than or equed. to 5 times *CRDL? [ X 1 Is any difference** between sanple and duplicate greater than *CRDL where sanple and/or duplicate is less them ^ 5 tines *CRDL? 2_:i. C ] ACTTON; If yes, fleig tihe associated data as estimated. A.1.17.5 Soil/Sert-impnt Circle on each Form VI all values that are; RPD > 100%, or Difference > 2 X CRDL* Is any RPD (vA^ere sanple and duplicate are both greatier than or equal to 5 times *CRDL) : > 100%? [ ] J L Is any **differehce between sanple arxi duplicate (where sanple and/or duplicate is less tihan 5x*CRDL) > 2X*CRDL? * Substitute IDL for CRDL whan IDL > CRDL. ** Use absolute values of sanple and duplicate to cedculata the difference. X 304656 STANDARD OPERATING I«DCEDURE Title: Evaluation of Metals Data for the Cate: Jan. 1992 Contract Laboratory Program Number; HW-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 Ccmpliarvce (Total Reviev) YES NO N/A AcnoW: If yes, flag the associated data as estimated. A.1.18 Field Duplicates A. 1.18.1 Were field dupiicatas analyzed? f X^ 1 ACTTON; If yes, pr^jare a Form VI for each aqueous field duplicate pair. Prepare a Form VI for each soil duplicate pair, if percent solids for sanple arxi its duplicate differ by more than 1%; report ooncentratiions of soils in ug/1 on wet weight basis and calculate RPDs or Differerx3e for each analyte. NOTE: 1. Do r a t calculate RPD when both values are less than IDL. 2. Flag all associated data only for field duplicate pair. A.1.18.2 ?>queou3 Circle all values on self prepared Form VI for field duplicates that eirc; RFD > 50%, or Difference > CRDL* Is any RPD greater than 50% where sanple and duplicate are both greatier than or equal to 5 tunes *a?DL? Is any **differenoe between sanple arxi duplicate greater than *CRDL where sanple and/or duplicate is less than > 5 times *CRDL? A^ ACTTON: If yes, flag the as-snciated data as estimated. . ^ • - ciG * Substitute IDL for CRDL when IDL > CRDL. ** Use absolute values of sanple and duplicate to calculate tha difference. 304657 STANDARD OPERATING PROCEDURE Title; Evaluatiion of Metads Data for the Contract Laboratory Program Appendix A.l: Data Assessment - Ocntract Ccnpiiance (Total Review) Data: Jan. 1992 Number: HW-2 Revisicn: 11 YES A.l.18.3 Soil/SfxHmpnt m. N/A Circle all valvies cn self prepared Form VI for field duplicates that are: RPD >100%, or Difference > 2 x CRDL* Is amy RPD (vrtiere sanple aind duplicate are both greater than 5 times *CRDL) : >100%? Is amy **differerx3e between sanple and diplicate (where sanple and/or duplicate is less than 5x *CRDL ); >2x *CRDL? [. ACnCN; If yes, flag the associated data as estimated. [ ] L K A. 1.19 Fonn V U (laboratory Control Sanple) (Note: ICS - not required for aqueous Hg aind cyanide airalyses.) A. 1.19.1 Was one ICS prepared and anadyzed for: each SDG? each batch sanples digested/distilled? both AA and ICP vhen both are used for tha same analyte? iX (21] ( ] X ACTTON: If no for any of tha above, pr^jare Tel^iione Reoord Log and contact laboratory for sutmittal of results of LCS. Flag as estiimatad (J) all the data for which ICS was not analyzed. NOTE; If oriLy ana U S was analyzed for more than 20 sanples, then first 20 sanples close to LCS do not have to be flagged as estimated. * Substitute IDL for CRDL when H ^ > CRDL. ** Use absolute values of sanple and dtplicate to calculate the difference. 304658 STANDARD OPERATING FRDCEDURE Title: Evaluation of Metals Data for the Contract Laboratory Program Afpendix A.l: Data Assessment - Ccntract Conpliarxse (Total Review) Data; Jan. 1992 NuEber; HW-2 Revision; 11 YES A. 1.19.2 Aqueous U S Circle on each Form V U the LCS peroent reooveries outside control limits (80 - 120%) exoept for aqueous Ag and Sb. Is any LCS reoovery: less than 50%? between 50% arxi 79%? between 121% and 150%? greater than 150%? ACTTON; Less than 50%, reject (red-line) all data; between 50% and 79%, flag adl associated data as estimated (J); between 121% and 150%, flag all positive (not flagged with a "U") results as estimated; greatier than 150%, reject all positive results. NO n/A _ (A] _ _ ( ^ _ _ iX _ _ (il! _ A.1.19.3 Solid LCS lOJE; 1. 2. ACTION: If "Found" value of LCS is rejectable dua to duplicate injections or aralvticad spite recovery criteria, regardless of LCS recovery, flag the associated data as estimated (J). If IDL of am analyte is equal tio or greatier than true vadua of LCS, disregard the "Actiion" belcw even though LCS is out of ccntrol limits. Is LCS "Found" value hi^ier than the ccntrol limits cn Form VU? If yes, qualify all as estimated. positiive data X ACTION; Is LCS "Found" value lower than the Oontrol limits on Form VIT? If yes, quadify a l l associatPri datia as estimated. t ] _ _ K ,04659 STANDARD OPERATING FRDCEDURE Title: Evaluation of Metads Data for tha Contract laboratory Program Appertiix A.l; Data Assesanent - Ocntract Cotpliaince (Ttotad Review) Date: Jan. 1992 Nunber: HW-2 Revisicn: 11 YES A.l.20 Fom^_tISLSedlfil_DilHtisal.- NOTE; Serial diluticn aralysis i s required cnly for i n i t i a l ccnoentratiicns equad t o or greater than 10 x IDI.. A. 1.20.1 Was Serial Diluticn analysis perfonnad for: each SDG? each matrix type? each concentration range (i.e. lew, med.)? [ 3 ACTION; If rxj for any of the above, flag as estiimated all the positive data >. lOxIDLs or >. CRDL when lOxIDL <. CRDL for which Serial Dilutioi Analysis was rot performed. NO NZA C ] >< X A. 1.20.2 Was field blank(s) xosed for Serial Dilution Analysis? ACTTON; If yes, flag all associated data > 10 x IDL as estimated (J). If lOxIDL < CRDL, flag adl data > CRDL. X A. 1.20.3 Are results outiside cantrol limit flagged with an "E" on Form I's and Form IX when initial ccnoentratiion on Form IX is equad to 50 times IDL or greater. ACTION; If no, write in the Oontract-Problenv/Ndn- CcnplianoR secticn of the "Data Assessment Narrative". (Xl _ A. 1.20.4 Circle on each Form IX all peroerrt: difference that are outside the cantrol limitis for initial corx:entiratiions equal tio or greater than 10 x IDLs only. Are any % difference values: > 10%? > 100%? A [ ] iJL 304660 • STANDARD OPERATING FRDCEDURE Title: Evaluation of Metals Data for the Date: . Jan. 1992 Contract Laboratory Program Nun±3er: HW-2 Appendix A.l: Data Assessment - Contract Revision: 11 Conpliarx^ (Total Review) ^ m N/A ACTION; Flag as estimated (J) all the associated sanple data > lOxIDLs (or > CRDL when lOxIDL < CRDL) for which percent differerx^e is greater than 10% but less than 100%. Reject (red-lir>e) all the associated sanple results equad to or greater tihan lOxIDIs (or >; CRDL whan lOxIDL < CRDL) for which PD is greater than or equad to 100%. Note; Flag or reject on Form I's only the sanple resultis vAose associatied raw data are >. lOxIDL (or >. CRDL when 10xIDL< CRDL) A.1.21 Furnace Atcndc Absorbtion (AA) OC Analysis A. 1.21.1 Are duplicate injectiicns present in furnace raw data (except during full Method of Standard Addition) for \/ each sanple cinalyzed by GFAA? [ ] JJ ACTION; If no, reject the data on Form I's for which .•' duplicate injections were rxJt performed. A. 1.21.2 Do the duplicate injection readings agree within 20% ^' Relative Standard Deviation (RSD) or Coefficient of y^ Variation (CV) for ccncerTtration greater than CRDL? [ ] Was a dilutiion analyzed for sanple with analytical \v spike recovery less than 40%? [ ] j J ACTION: If TX3 for any of the above, flag all tihe associated data as estiimated. A. 1.21.3 Is *analytical spike reoovery outside tha cantrol limits (85-115%) for any sanple? ACTION; If yes, flag as estimatied tha adffacted sanple results if tha reoovery is between 10-84%; if tha recovery is between 115-200%, flag tha associated positiive sanple results as estimated; reject the associated sanple results if the reoovery is less than 10%; reject positiive sanple results if the reoovery is greater than 200%. * Analytical spike is not required on the pre-digesticn spiked sanple. K 304661 STANDARD OFERATING PROCEDURE Title: Evaluaticn of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Nunber: HW-2 Appendix A.l: Data Assessment - Contract Revision: 11 C o m p l i a n c e ( T o t a l R e v i e w ) -^^ _ _ . HJTE: Reject or flag the data cnly when the affected sanple (s) was rxjt subsequently analyzed by Method of Standard Addition. A.1.22 Form v m (Method d ' M-nn^n-rj Additiom Rasults) A.1.22.1 Present? [ ] . If rxD, is any Form I result coded with "S" or a "+"? [ ] A ACTION; If yes, write request on Telephcne Record Log and contact laboratory for submittal of Form VIII. A. 1.22.2 Is coefficient of correlation for MSA less tihan 0.990 for any sanple? [ ] ACTTON; If yes, reject (red-lirve) tha affected data. A. 1.22.3 Was *MSA required for any sanple but rxrt performed? -.[ ] Is coefficient of correlation for MSA less than 0.995? [ ] * MSA is not required on LCS and prep, blank. X X X >< Are MSA ccdculatiians cutside the linear range of the calibration curve generated at tha beginning of the y;^ anedytical run? [ ] ACTTON; If yes for any of the above, flag a l l the associatied data as estimated (J). A. 1.22.4 Was proper quantitatiion procedure followed correctly '^ as outilinad in the SCW cyv page E-23? [ ] ACTT(3N: If no, note exo^jticn vmder Oontract Problenv/ Non-ocnplianne section of tha "Data Assessment Narrative", and prepare a separatia l i s t . 304662 STANDARD OFH»TING FRDCEDURE Title: Evaluation n;.; riatals Data for tha Data: Jan. 1992 Contract Li-barratLory Program Nunber: HW-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 Compliance (Ttotal Review) _ _ _ _ _ A.1.23 Dissolved/Ttotal or Inoraanic/Total Analvtes - A.1.23.1 Were any analyses performed for dissolved as well as y^ totad analytes on tha same sample (s). [ ] ^ Were any analyses performed for inorganic as well as total \ . (organic + inorganic) analytes on tha same sanple(s)? [ ] XN NPTE: 1. If yes, pr^sare a list ocnparing differenoes between all dissolved (or inorganic) and total ainadytes. Ccnpute the differenoes as a percent of the total analyte only when dissolved corxxntration is greater than CRDL as well as total concentration. 2. Apply the following questions only if in- organic (or dissolved ) results are (i) above CRDL, arxi (ii) greater than total constituents. 3. At least one preparatiion blank, ICS, and LCS should be analyzed in each ainadytical run. A. 1.23.2 Is the concentratiian of any dissolved (or inorganic) analyte greater tham its total conoentration by mare than 10%? [ ] _}£ A. 1.23.3 Is the carx3entratiion of any dissolved (or inorganic) analyte greater than itis tiotal ccncentraticn by "y more than 50%? [ ] X\ ACTTON; If more than 10%, flag both dissolved (or inorganic) and totad values as estimated (J); if more than 50%, reject (red-line) the data for both values. A.l.24 F9CT I {rtrt«a BlQBX) - (Notai Desicmata "Field Blank" as such em Form I.) A. 1.24.1 Circle all field blank values on Form I that are greater than CRDL, (or 2 x IDL .when IDL > CRDL). Is field blank corjoentration less than CRDL (or 2 X IDL when IDL > CRDL) for all parameters > of associated aqueous and soil sanples? [ ] -X 304663 STANa^^RD OPERATING PROCEDURE Page 25 . of 34 Title: Evaluation of Itetals "Eata for the Data: Jan. 1992 Contract Laboratory Program Nunber; HW-2 Appendix A.l; Data Assessment - Ccntract Revision; ll Ccnpliarx^e (Total Review) _ _ _ _ If 1X3, was field blank vadue adieady rejected due to otiher QC criteria? [ ] -X ACncN; If no, reject (except field blank results) all cLssociatied positiive sanple data less than or equal to five times the field blank value. Reject cn Form I's tha soil sanple results that ;^ien converted to ug/L on wet baisis are less than or equad to five times the field blank value in ug/L. A.1.25 Form X, XI. xn (Verification of Instnmp^^'*"' ^>><r;mv»t.«'T3). A. 1.25.1 Is verification r^xsrt present for: Instrument Detection Limitis (quarterly)? [ J j 3 ICP Interelement Correction Factors (annually)? fA 1 ICP T.inpar Ranges (quarterly)? [ J L ACTTON; If rx5, contact TPO of the lab. A.l.25.2 Fom X (Instrrmwrnt Detection ^.-t.pj^jg) - (Note: IDL is not required for Cyanide.) A.l.25.2.1 Are IDLs present for: all the analytes? [ J J ] all the instiruments used? [ J L For both AA and ICP when both are used for tha same Y' analyte? [ ] JJ ACTICN: If rx3 for any of tha above, prepare Telesphcne Reoord Log arxi ccntact laboratory. A.1.25.2.2 Is IDL greater than CRDL for any analyte? . [JL If yes, is the conoentration on Form I of the sanple analyzed on the instrument whose IDL exceeds CRDL, ^ greater than 5 x IDL. [ ] X 304664 STANDARD QPERAITr-'G I5?DCEDURE Title: Evaluation of Metals Data rrr-'va Date: Jan. 1992 Contract Laboratory Progron Number: HW-2 Aipendix A.l: Data Assessment - Ccntract Revision: 11 Ccnpliarx^e (Total Review) YES ^ N/A Action : If no, flag as estimated adl values less than five times IDL of the instrument whose IDL exceeds CRDL. A.1.25.3 Form XI (X-^-npjtr Ranges) . A. 1.25.3.1 Was any .sanple result hi^ier than hic^ linear range of ICP. Was any sample result hic^ier than the highest calibration standard for non-ICP parameters? If yes for any of the above, wais the sanple diluted to cbtain the result on Form I? ACTTON; If rx3, flag the result reported cn Form I as estimatBd(J). A. 1.26 Percent Solids of Sadimffnts ^• A.1.26.1 Are percent solids in sediment(s): < 50%? [ ] JL X >^ [Ji.] r ] r 1 < 10%? [ ] X ACTION; If yes, quadify as estimated all the results of a sanple that has per oent solids between 10%-50% (i.e. moisture oontent between 50%-90%). Reject all the results of a sanpia that has per cent pf>lidq less than 10% (i.e. moisture ccntant greater than 90%). NOTE; Reject or flag (J) only the sanple results that were not previously rejected or flaged dua tio other QC criteria. 304665 STANDARD OPERATING PROCEDURE Title: Evaluation of Metals Data for the Date: Jan. 1992 Contract laboratory Program Nuniaer: HW-2 Appendix A.2: Datia Assesanent Narrative Revision: 11 Case# ;2I Sit* 3ALf\NT> CnfrYiiCA L. Matrix: Soil ; SDG# ^ " ^ O O H Lab P/^CC Af\}f\L^-ncA L watar X Contraurtor — Raviewer lAlYlf] f'^fiKA'^nlK. Othar Up/\f\ 'i^/\MMl3. A.2.1 Validation Flags- The follcwing flags have been applied in red by the data vadidator and must be considered by the data user. J- This flag indicates the result qualified as estimatad Red- Line- A red-line drawn through a sanple result indicates unusable vadue. The red-lined data aire kncwn to contain significani errors based on documented inf ormatiion and must not be used by the data user. Fully Dsable Data- The results that do rxjt carry "J" or "red-line" are fully iisabl Contractual Oualiflera- The legend of contractual qualifiers applied by the lab on Form I's is found on page B-20 of SOW IIMOl.O. A.2.2 The data assessment is given below and cn the attached sheets. ^Uy aHoiCkel ncxxxaJxirO 304666 I > STANDARD OFERATING PROCEDURE Title: Evaluation of Metals Data for the Date; Jan. 1992 Contract laboratary Program i'Junber; HW-2 ^^pendix A.2: Data Assesanent Neunirative Revisicn: 11 A.2.2 (continuation) • 304667 STANDARD OFERATING FRDCEDURE Title: Evaluation of Metals Datia for the r:at£: Jan. 1992 Contract laboratory F>rogram IJiimixar: HW-2 hpperdxx. A.2: Data Assessment Narrative Revisicn; 11 A.2.2 (contirxaticn) 304668 STANDARD OPERATING TODCEDURE Title: Evaluaticn of Metads Data for the Data: Jan. 1992 Contract Laboratary Rxgram Number; HW-2 Appendix A.2: Efeta Aseesaaent Nairrative Revisicn: 11 A.2.3 Contract-Prcblsiv/Ncn-Ciccplianoe M<B/ESAT Rviewer: [ Date:_ Signature Contractor Reviewer: . Date:_ Signature Verified by: Date:_ 304669 *\ STANDARD OPEKAIING PROCEDURE T i t l e : Evaduation of Metads Data for t h e Date: Jan. 1992 Contract Laboratory Program Nunter: HW-2 Appendix A. 3 : Ccntract Non-Ocnpliarioe Revision: 11 (SMD Report) aCNTRACT NON-OCWPLIANCE (SMO REPOPT) Regionad Review of UrcontroUed Hazardous Waste S i t e Ccntract laboratory Data Package CASE NO. The hardcopied (laboratory name)___ Inorganic data package received at Region II has been reviewed aind the quality assurance ar performance data summarized. The data reviewed included: SI-30 Sample No.: Cone. & Matrix: Contract No. ( )_ requires that specific anadytical work be done and that associated reports be provided ty the contractor to the Regions, IMSL-LV, and SMO. Th general criteria used to determine the performance were based cn an examination of: - Data Ccnpleteness - Duplicate Analysis Results - Matirix SpiJoe Results - Blank Analysis Results - calibration Standards Results - MSA Results Items of non-ccnpliance with the above contract aire described belcw. Coitr^entis: Reviewer's I n i t i a l - Date 304670 STANDARD OPERATING H^DCHURE itle; Evaluaticn of Ifetals Data for the Oontract Laboratary Program Appendix A.4: Mailing List for Data Reviewers Date: Jan. 1992 Number: HM-2 Revision: 11 ar?r>an.nr. U J ? «=• rmn. a. x s z n »»«jjan J (rso) IjUUJiqrun. t9k 02173 IMt SZATO (617) K i - ^ s a : c r . KE. » . »«. M . v r OkX, n—njTM Ar*iy«t*, Yortc, £32. SlunnBT. "09, 3 . VSn>A »«jjon I i : [OC) a3> tejrt^U te«5 A.-n«pcia8. t o 2UZi (3C1) 26t-9:i3 CE. >o. yjk. \7k. v : . DC C«.rt*c. Hitr*.-.. JTC, KkO;. V D S « , S^jtjatn Tacr... K*/ PA 5. •unrx Tutjicr. V (xsz) 534 SoJV. C : v k Sxr«»t T«.-nft riocr, OC Q-.aca7C, I I 6D6:5 Pit Oi-.:ri:i» 312-3«3-J5Z"r I t . D.-. K : . K ; . CK. vt V5I?A R«;ian Nil lASontary 25 r.rtft£n Re«d KA.-«AS City, ys 6€ii5 Ifcin «3rry ($13) 236-3BU 10. ys. K5, » Viltor., XjL-tfAk Cir>' SciKTiilic VSD'X lt«9ion IX (tSS) Ok KA.'M9«-«m s«eticn 215 Trtrcm. S t r w r S*n r r v c u i a o , CX 94105 («15) «74-0«2« A2. » . KI, Ki?, Krmrian SA.rc*. OuA.-: Trust TuTitxiriM oi P»eUie Itla-Tlx, w^.« Xftlimd M J . a a w « « t m . S-Cubid. n - c \ , V«}U l&tKA taqian ZI (ZSO) Woo&rickT* Av«ru« Xdiaon, N M J«rMy 0»t37 (301) a21-M7« KJ. Ky. W, VI OvRiay, OMBCaeH. t S Ttat, N4.n3o, CC, GtOten, IKS, CiiUon, 2 « tSCPX taqisn TV ( S ? ) AnaJytieal Su;T"rt B.I.U. CDll«9« r u t i c n Rati Kxt»r», » 30613 ttjr. BBrtirrt. J r . (4M) 546-3112 XL, n . . « , IQf, «S. HC, SC, IS orpxTMR, IPS, zsi, nsfcr, TfiAnjlt Labs tSITX Itejion VI (153) HTKMXny Krtc P l k u , a i d ; . C 6606 HSZTMQOd CETivt HMKcn. TX 77074 CBvid Staoocr. (713) 953-3435 Ml, IA, m , TX. OK M9oas, MOiwi, sn=s, CS, Cl r — i n u i . Z / s . , SK. I n c . , 5WRI, Alliad, Xff>- TX. C3U XStTX taqion VIH U J x n x o r y KX 25366 D w « r r a d t n l Ovxur Uk^wcod, 03 •0225 (303) 236-7371 03, >0, SO, m , W . KT Aca*. CSCU. I M a , rkt« OMC, cannf T»tTTr»tory 9I3S3 10. USZPX Hi^ien X r.O. BOX 549 Caz^ld njth (30<) 443-0370 AX, ZO. Ok, tA lAudv TMtirq tkbt, CvT&sy Ttstirq Ufa* {Tor vox Cray). UtyvTMUMr CD. Colurfeia l^Bctin;, Silv«r Valley 33. Curia Dt-pM/ - (C6-230) 4c; n r s-j-»r:, s.w. V•*».^i^7^o^., OC 2U60 r r s 3£2-5746 13. S*.-?2« KA.-vs?«.-«rr: OJJjc* V.k.- JL-d Car^jcry P.O. BCX eiE x:»xa.Tc.-:a. '.^ : : : : ? 12. ia.%n x&.-»or USEPA DSlrlV 944 £. K&man AV«.<XM BOX «347a L*k V«gu. K-.' 69119 3 0 4 6 7 1 4 •' \ STANDARD OPERAIING PRDCEEURE tie; Evaluation of Metals Data for the Contract Laboratary Program Aperdix A.5: CLP Data Assessment Suittnary Fona (Inorganics) Pzige 33 of 34 Date: Jan. 1992 Number: HW-2 Revision: ii t « ! _ _ ^ 6«cai U»t I: U k M J M I ri»wt'» Inltlalt: KyMk«r cf S u i f l a t t *nilyt»« I t j t c t t f Out to t i c f d l n t >»»!«» C f l t t t H ! * c? 'll*» AA 'urnact AA Tlaft ItTCurr 1 : e t * l )th*T 1 1 C a ^ b r t t l o n l l i n k 1 n t i 4 t l i n k I n t t T - f t r t n r c f »teo*»r» Du^llcati* L i b l f l t l d &«t*etl*a L l a i t i tCSIBllutien i nik Total -. l e ^ t e t l o n Aaolytti T}ttt*4 11 t t t l M t t d (J) Pvjt te t i t u d l a t C r l t t r l i for; :cf ' U » * A> ''grntct iu^ MtTturr Total OtMr 1 ' ; -' I Hota: A a i t r i a a (•} l a d l c a t t a a44itlanal atcttaoacaa a( ravia* a r l t a r l a . 304672 t STANDARD OPERATING PRDCHJURE Title: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Appendix A.6: CtP Data Assesaaent Checklist Revisicn: 11 Irxarganic Analysis INC»GANIC RB3I0NAL DATA ASSESSI^Sif Region CASE NO. ' SITE NO. OF SAMPLES/ LABORATORY MASRIX SDG# REVIEWER (IF NOT ESD)_ ^a,^!! KLVliWIR'S NAME DPO: 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. ACTION 1 HOIDING TIMES rAT,TPRATTnN<> BIANKS ICS LCS DUPIZCATE ANALYSIS MAIRIX SPIKE MSA SIRIAL DHUnCN SAMPLE Vi:imiCAI'iaN UiUtK QC OVERALL ASSESaiEOT TH. OCMPLETICN DATE DATA ASSESSMENT SIJWARY ICP AA Hg CYANIDE 0 = Data has no problems/or qualified due to minor problems. M = Data qualified due to major problems. Z = Data unacceptable. X = Problems, but do rxrti affect data. AdioN irms; / : • • tSdIS OF CONCERN: NOTABLE PERH2RMANCE: 3 0 4 6 7 3 SDG No. 98037 VOCs, SVOCs, and Metals Checklist m 304674 Pau^C&'.'^S^^? SOP NO. HW-13 Revision 1 Superfund Analytical Methods For Low Concentration Water for Organics June 19^1 Prepared by the Pegion II Organic ESAT Team By: W f > 7 ^ x ^ /A:-^L.^t^fO^ George Ka.^as, Organic Task Monitor/Chemist Toxic ana Hazardous Waste Section ieon Lazd^ds/TjEnvironmental Scientist Toxic and Hazardous Waste Section By; U : ^ y ^ ^ l Stelios Gerazouni.s'^^hemist Toxic and Hazard6us Waste Section (^l^}nyC^^ CONCURRED BY APPROVED BY: Robert Runyon, Chi^ Monitoring Management Branch Date Date; A2A7- Date: ^ "3^ 9'Z. Date: /nU^7- 304675 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 1 of 51 Date: August, 1992 Revision: 1 3D(r BASE }RJli&ER;. SITE: "^^o^n I<,/e\A ohcAt^^' I YES NO N/A LAB: I aC(z. 1.0 Data Completeness and Deliverables 1.1 Have any missing deliveraUales been received and added to the data package? LILJL ACTION; Call lab for expianation/resubmittal of any missing deliverables. If lab cannot provide them, note the effect on review of the package under the "Contract Problems/Non- Compliance" section of reviewer narrative. 1.2 Was SAS-request included with package? .[ ]_ ^ If no, a SAS-request can be retrieved from RSCC. 2.0 Cover Letter SDG Narrative 2.1 Is the Narrative or Cover Letter Present? T/S 2.2 Are Case Number and/or SAS number contained in the Narrative or Cover letter? J ]_ }^ 3.0 Data Validation Checklist The following checklist is divided into three parts. Part A is filled out if the data package contains any Low Concentration Volatile analyses, Part B for any Low Concentration Semivolatile analyses and Part C for Low Concentration Pesticide/Aroclors. Does this package contain: Low Concentration Volatile Data? Low Concentration Semivolatile Data? Low Concentration Pesticide/Aroclor data? Action: Complete corresponding parts of checklist. y: 304676 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 2 of 51 Date: August, 1992 Revision: 1 YES NO N/A 1.0 1.1 PART A: VOA ANALYSES Traffic Reports and Laboratorv Narrative Are Traffic Report Forms present for all samples? J__L Y ACTION: If no, contact lab for replacement of missing or illegible copies. 1.2 Do Traffic Reports or Lab Narrative indicate any problems with sample receipt, condition of samples, analytical problems or special circumstances affecting the quality of the data? ACTION; If samples were not iced upon receipt at the laboratory, flag all positive results "J" and all non-detects "UJ". ACTION; If both VOA vials for a sample have air bubbles or the VOA vial analyzed had air bubbles, flag all positive results "J" and non-detects using professional judgement. 1.3 Does Lab narrative contain a list of pH determinations for all samples? ACTION: If Lab narrative does not contain a list of sample pH determinations, contact the lab for explanation/resubmittals. 2.0 Holding Times 2.1 Have any VOA technical holding times, determined from date of collection to date of analysis, been exceeded? JL x_i JL JL LU If unpreserved, samples maintained at 4*C and are to be analyzed for aromatic hydrocarbons must be analyzed within 7 days of collection. If preserved with HCl (pH<2) and stored at 4*C, then samples must be analyzed within 14 days of collection. If uncer^ tain about preservation, contact sampler to determine whether or not samples were preserved. 304677 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 3 of 51 Date: August, 1992 Revision: 1 YES NO N/A Table of Holding Time Violations Sample ID rBo3Z2RE FBo.-i2Hi^i fi\UJocOHRc ACTION; Preserved? V€) Date Sampled ?>/:i-i / i 0 X/ii!li^_ TWfW (See Traffic Report) Date Lab Date Received lege ive Analyzed H/nm If technical holding times are exceeded, flag all positive results as estimated ("J") and sample quantitation limits as estimated ("UJ"), and document in the narrative that holding times were exceeded. If analyses were done more than 14 days beyond holding time, either on the first analysis or upon re-analysis, the reviewer must use profes- sional judgement to determine the reliability of the data and the effects of additional storage on the sample results. At a minimum, all results must be qualified "J", but the reviewer may determine that non-detect data are unusable (R) . If holding times are exceeded by more than 28 days, all non- detect data are unusable (R) . 3.0 Surrogate Recovery (Form II LCV) 3.1 Are the VOA Surrogate Recovery Summaries (Form II LCV) present? Hi ACTION: Call lab for explanation/resubmittals. If missing deliverables are unavailable, document effect in data assessments. 3.2 Were outliers marked correctly with an asterisk? f Al ACTION: Circle all outliers in red. 3.3 Was the surrogate (p-bromofluorobenzene) recovery outside of contract specifications for any sample or method blank? ih. 304678 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE P a g e : 4 of 51 D a t e : August, 1992 R e v i s i o n : 1 YES NO N/A If yes, were samples re-analyzed? i 1 Were method blanks re-analyzed? i 1 ACTION: If bromofluorobenzene recovery is >10%, but fails to meet SOW specifications: 1. All positive results are qualified as estimated (J). 2. Flag all non-detects as estimated detection limits ("UJ") where recovery is less than the lower acceptance limit. 3. If surrogate recovery is above allowable levels, do not qualify non-detects. If surrogate recovery is < 10% : 1.. Flag all positive results as estimated ("J"). 2. Flag all non-detects as unusable ("R"). Professional judgement should be used to qualify data that only have the method blank's surrogate recovery out of speci- fication in both original and reanalyses. Check the internal standard areas. 3.4 Are there any transcription/calculation errors between raw data and Form II? ACTION: If large errors exist, call leib for expianation/resubmittal, make any necessary corrections and note errors in the data assessment. ih. 4.0 Laboratory Control Sample (Form III LCV> 4.1 Is the Laboratory Control Sample Recovery Form (Form III LCV) present? nk 304679 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 5 of 51 Date: August, 1992 Revision: 1 YES NO N/A 4.2 Was the Laboratory Control Sample (LCS) analyzed at the required frequency (once per SDG or every 20 samples, whichever is more frequent) for the Low Concentration VOA method? r^ ACTION: If any LCS data are missing, take the action specified in 3.2 above. 4.3 How many VOA LCS recoveries are outside QC limits of 60-140%? Low Cone. Water O o u t o f 1 2 0"^ r e 'OM^*, Is^M ACTION: If the LCS recovery is greater than 140%, positive results should be flagged "J" for the affected compound. If the mass spectral criteria are met but the LCS recovery is less than 60%, then the associated detected target compounds should be flagged "J". Associated non- detected target compounds should be flagged "R". If 25 % of the analyte recoveries are below QC-limits qualify all associated positive sample data as "J" and non-detects "R". If two or more analytes show recoveries of < 10% all associated positive sample data as "J" and non-detects "R". It should be noted for TPO action if a laboratory fails to analyze an LCS with each SDG, or if a laboratory consistently fails to generate acceptable LCS recoveries. • 5.0 Method Blanks (Form IV-LCV) 5.1 Is the Method Blank Summary (Form IV LCV) present? JL 304680 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 6 of 51 Date: August, 1992 Revision: 1 YES NO N/A 5.2 Frequency of Analysis: For the analysis of Low Concentration VOA TCL compounds, has a method blank been analyzed for each SDG or every 2 0 samples, whichever is more frequent? 5.3 Has a VOA method blank been analyzed at least once every twelve hours for each GC/HS system used? Lk £ii ACTION: If any method blank data are missing, call lab for expianation/resubmittal. If method blank data are not availaible, reject (R) all associated positive data. However, using professional judgement, tihe data reviewer may substitute field blank or trip blank data for missing method blank data. 5.4 Chromatography; review the method blank raw data - chromatograms (RICs) , quant repoirts or data system printouts and spectra. Is the chromatographic performance (baseline stability) for each instrument acceptable for Low Concentration VOAs? A] ACTION: Use professional judgement to determine the effect on the data. 5.0.1 Storage Blank 5.0.1a Has a storage blank been analyzed at the required frequency (once per SDG) for VOAs? f 1 Y^ 5.0.1b Chromatography: Compare the storage blank raw data with the associated method blank data in order to determine if the contamination is also present in the method blank. ACTION: If the storage blank contains target compounds at a concentration greater than the CRQL, positive results for that compound(s) should be flagged "J". If gross contamination occurred positive sample results may require rejection for that compound. 304681 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 7 of 51 Date: August, 1992 Revision: 1 YES NO N/A 5.0.1c Is the chromatographic performance (baseline stability) for the storage blank acceptable for Low Cone. VOAs? i 1 ACTION: Use professional judgement to determine the effect on the data. y 6.0 Contamination NOTE; "Water blanks", "drill blanks", and | distilled water blanks" are validated like j any other sample, and are not used to i qualify data. Do not confuse them with the other QC blanks discussed below. 6.1 Has an instrument blank been analyzed following a sample analysis which contained an analyte(s) at high concentration(s) . A _[ -^ ACTION; Sample analysis results after the high concentration sample must be evaluated for carryover. Instrument cross contamination should be noted for TPO action if an effect on the data is suspected. 6.2 Do any method/storage blanks have positive results (TCL and/or TIC) for Low Cone. VOAs? When applied as described below, the contaminant concentration in these blanks y. are multiplied by the sample dilution factor. ^ J _ l 6.3 Do any field/trip/rinse blanks have positive Low Cone. VOA results (TCL and/or TIC)? ACTION: Prepare a list of the samples associated with each of the contaminated blanks. (Attach a separate sheet.) Xi^ 304682 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 8 of 51 Date: August, 1992 Revision: 1 YES NO N/A NOTE: All field blank results associated with a particular group of samples (may exceed one per case) must be used to qualify data. Trip blanks are used to qualify only those samples with which they were shipped. Blanks may not be qualified because of contamination in another blank. Field blanks & trip blanks must be qualified for system monitoring compound, instrument performance criteria, spectral or calibration QC problems. ACTION; Follow the directions in the table below to qualify TCL results due to contamination. Use the largest value from all the associated blanks. If any blanks are grossly contaminated, all associated data should be qualified as unusable (R). Sample cone > CRQL Sample cone < CRQL but < lOx blank & <10x blank value value Sample cone > CRQL & >10x blank value Methylene Chloride Flag sample result Acetone with a "U" 2-Butanone Report CRQL & qualify "U" No qualification is needed Sample cone > CRQL but < 5x blank Sample cone < CRQL & is < 5x blank value Sample cone > CRQL value & > 5x blank value Other Contam- inants Flag sample result with a "U" Report CRQL 6 qualify "U" No qualification is needed NOTE: Analytes qualified "U" for blank contamination are still considered as "hits" when qualifying for calibration criteria. 304683 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 9 of 51 Date: August, 1992 Revision: 1 YES NO N/A ACTION: For TIC compounds, if the concentration in the sample is less than five times the concentration in the most contaminated associated blank, flag the sample data "R" (unusable). 6.3 Are there field/rinse/equipment blanks associated with every sample? i^ ACTION: Note in data assessment that there is no associated field/rinse/equipment blank. Exception: samples taken from a drinking water tap do not have associated field blanks. 7.0 GC/MS Instrument Performance Check (Form V-LCV) 7.1 7.2 7.3 Are the GC/MS Instimment Performance Check Forms (Form V-LCV) present for Bromofluorobenzene (BFB)? Are the enhanced bar graph spectrum and mass/charge (m/z) listing for the BFB provided for each twelve hour shift? Iii X Has an instrument performance compound been analyzed for every twelve hours of sample ^ analysis per instrument? i r ] ACTION: List date, time, instrument ID, and sample analysis for which no associated GC/MS tuning data are available. DATE TIME INSTRUMENT SAMPLE NUMBERS ACTION: If lab cannot provide missing data, reject ("R") all data generated outside an accep- table twelve hour calibration interval. 304684 V LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 10 of 51 Date: August, 1992 Revision: 1 YES NO N/A r^ — 7.4 Have the ion abundances been normalized to m/z 95? ACTION: If mass assigrunent is in error, qualify all associated data as unusable (R). 7.5 Have the ion abundance criteria been met for each instrument used? f ^ ACTION: List all data which do not meet ion abundance criteria (attach a separate sheet). ACTION: If ion abundance criteria are not met, the Region II TPO must be notified. 7.6 Are there any transcription/calculation errors between mass lists and Form Vs? (Check at least two values but if errors are found, check more.) Ijk i^ Ll 8.0 7.7 Have the appropriate nuiaber of significant figures (two) been reported? ACTION: If large errors exist, call lab for expianation/resubmittal, make necessary corrections and document effect in data assessments. 7.8 Is the spectrum of the mass calibration compound acceptable? ACTION: Use professional judgement to determine whether associated data should be accepted, qualified, or rejected. Target Compound List (TCL) Analvtes (Form I LCV) 8.1 Are the Organic Analysis Data Sheets (Form I LCV) present with required header information on each page, for each of the following: a. Samples and/or fractions as appropriate? r'^ b. Laboratory Control Samples? f^.") e. Blanks? i ^ 304685 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 11 of 51 Date: August, 1992 Revision: 1 YES NO N/A 8.2 Are the VOA Reconstructed Ion Chromatograms, the mass spectra for the identified compounds, and the data system printouts (Quant Reports) included in the sample package for each of the following: a. Samples and/or fractions as appropriate? r f^ b. Laboratory Control Samples? \H^ e. Blanks? fYl ACTION; If any data are missing, take action specified in 3.2 above. 8.3 Are the response factors shown in the Quant Reporrt? L-lJL 8.4 Is chromatographic performance acceptable with respect to: Baseline s t a b i l i t y ? Resolution? Peak shape? Full-scale graph (attenuation)? Other: ££i x:^ x:k d l r 1 ACTION: Use professional judgement to determine the acceptability of the data. 8.5 Are the lab-generated standard mass spectra of the identified VOA compounds present for each sample? iX ACTION; If any mass spectra are missing, take action specified in 3.2 above. If lab does not generate their own standard spectra, make note in data assessment - "Contract Problems/Non-Compliance". 304686 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 12 of 51 D a t e : August, 1992 R e v i s i o n : 1 8.6 8.7 8.8 Is the RRT of each reported compound within 0.06 RRT units of the standard RRT in the continuing calibration? YES NO N/A Lb. Are all ions present in the standard mass spectrum at a relative intensity greater than , 25% also present in the sample mass spectrum? f r) Do sample and standard relative ion intensities agree within 20%? ii_ ACTION: Use professional judgement to determine acceptability of data. If it is determined that incorrect identifications were made, all such data should be rejected (R), flagged "N" (presumptive evidence of the presence of the compound) or changed to not detected (U) at the calculated detection limit. In order to be positively identified, the data must comply with the criteria listed in the SOW page VOA D-32, section 21. ACTION: When sample carry-over is a possibility, pro- fessional judgement should be used to determine if instrument cross-contamination has affected any positive compound identification. 9.0 Tentatively Identified Compounds (TIC) 9.1 Are all Tentatively Identified Compound Forms (Form I LCV-TIC) present? Do listed TICs include scan number or retention time, estimated concentration and "JN" qualifier? r^] 9.2 Are the mass spectra for the tentatively identified compounds and associated "best match" spectra included in the sample package for each of the following: a. Samples and/or fractions as appropriate? [^1 b. Blanks? rYh ACTION: If any TIC data are missing, take action specified in 3.2 above. 304687 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 13 of 51 Date: August, 1992 Revision: 1 YES NO N/A ACTION: Add "JN" qualifier if missing. 9.3 Are any TCL compounds (from any fraction) listed as TIC compounds (example: 1,2-dimethyl- benzene is xylene- a VOA TCL analyte - and should not be reported as a TIC)? ACTION: Flag with "R" any TCL compound listed as a TIC. 9.4 Are all ions present in the reference mass spectrum with a relative intensity greater than 25% also present in the sample mass spectmm? rY-1 9.5 Do TIC and "best match" standard relative . ion intensities agree within 20%? f r-1 LR — ACTION; Use professional judgement to determine acceptability of TIC identifications. If it is determined that an incorrect iden- tification was made, change its identifica- tion to "unknown" or to some less specific identification (example: "03 substituted benzene") as appropriate. Also, when a compound is not found in any blank, but is detected in a sample and is a suspected arti- fact of a common laboratory contaminant, the result should be qualified as unusable (R). (i.e. Common Lab Contaminants: COj (M/E 4 4 ) , Siloxanes (M/E 73) Hexane, Aldol Condensation Products, Solvent Preservatives, and related by products - see Functional Guidelines for more guidance). 10.0 Compound Quantitation and Reported Detection Limits 10.1 Are there any transcription/calculation errors in Form I results? Check at least two positive values. Verify that the correct internal standard, quantitation ion, and RRF were used to calculate Form I result. Were any errors found? _ A 304688 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 14 of 51 Date: August, 1992 Revision: 1 10.2 Are the CRQLs adjusted to reflect sample dilutions? YES NO N/A i B _ ACTION: If errors are large, call lab for expianation/resubmittal, make any necessary corrections and note errors under "Conclusions". ACTION: When a sample is analyzed at more than one dilution, the lowest CRQLs are used (unless a QC exceedance dietates tihe use of the higher CRQL data from the diluted sample analysis). Replace concentrations that exceed the calibration range in the original analysis by crossing out the "E" and its associated value on the original Fonn I and substituting the data from the analysis of the diluted sample. Specify which Form I is to be used, then draw a red "X" across the entire page of all Form I's that should not be used, including any in the summary package. 11.0 Standards Data (GC/MS) 11.1 Are the Reconstructed Ion Chromatograms, and data system printouts (Quant. Reports) present for initial and continuing calibration? sX ACTION: If any calibration standard data are missing, take action specified in 3.2 above. 12.0 GC/MS Initial Calibration (Form VI) 12.1 Are the Initial Calibration Forms (Form VI LCV) present and complete for the volatile fraction at concentrations of 1, 2, 5, 10, and 25 ug/1? ACTION: If any calibration standard foirms are missing, take action specified in 3.2 above. Lk 304689 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 15 of 51 Date: August, 1992 Revision: 1 YES NO N/A 12.2 Are response factors stable for VOA's over the concentration range of the calibration (%Relative Standard Deviation (%RSD) <30.0%)? ACTION: Circle all outliers in red. NOTE: Although 12 Low Cone. VOA compounds have a minimum RRF and no maximum %RSD, the technical criteria are the same for all analytes. ACTION: If %RSD > 30.Ot, qualify associated positive results for that analyte "J" and non-detects using professional judgement. When RSD > 90%, flag all non-detects for that analyte R (unusable). NOTE: Analytes previously gualified "U" for blank contamination are still considered as "hits" vhen qualifying for initial calibration criteria. 12.3 Are the RRFs above 0.05? Action: Circle all outliers in red. Action: If any RRF values are < 0.05, qualify associated non-detects (R) and flag associated positive data as estimated (J). 12.4 Are there any transcription/calculation errors in the repoirting of average response factors (RRF) or %RSD? (Check at least 2 values, but if errors are found, check more.). 7^ f^ lk 13.0 GC/MS Continuing Calibration (Form VII LCV) 13.1 Are the Continuing Calibration Forms (Form VII LCV) present and complete ,. for the volatile fraction? FN 13.2 Has a continuing calibration standard been analyzed for every twelve hours of y. sample analysis per instrument? [f^ 304690 ^ LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 16 of 51 Date: August, 1992 Revision: 1 ACTION: List below all sample analyses that were not within twelve hours of the previous continuing calibration analysis. YES NO N/A ACTION: If any forms are missing or no continuing calibration standard has been analyzed within twelve hours of every sample analysis, call lab for explanation/ resubmittal. If continuing calibration data are not available, flag all associated sample data as unusable ("R"). 13.3 Do any volatile compounds have a % Difference (% D) between the initial and continuing RRF which exceeds the + 30% criteria? Dk ACTION: Circle all outliers in red. ACTION: Qualify both positive results and non-detects for the outlier compound(s) as estimated "J". When % D is above 90%, reject all non-detects for that analyte (R) as unusable. 13.4 Do any volatile compounds have a RRF <0.05? f^] ACTTION: Circle a l l o u t l i e r s in r e d . ACTION: If the RRF <0.05, qualify associated non- detects as unusable (R) and associated positive values as estimated "J". 13.5 Are there any transcription/calculation errors in the reporting of average response factors (RRF) or %difference (%D) between initial and continuing RRFs? (Cheek at least two values but if errors are found, check more.) _ ACTION: If errors are large, call lab for expianation/resubmittal, make any necessary corrections and note errors under "Conclusions". X * 304691 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 17 of 51 Date: August, 1992 Revision: 1 YES NO N/A 14.0 Internal Standard (Form VIII LCV) 14.1 Are the internal standard areas (Form VIII LCV) of every sample and blank within the upper and lower limits (±40%) for each continuing calibration? ACTION: List all the outliers below. Sample I Internal Std Area Lower Limit lE Upper Limit ACTION: 1. 2. 3. 14.2 ACTION; If the internal standard area count is outside the upper or lower limit, flag with "J" all positive results quantitated with this internal standard. Non-detects associated with IS area counts > 40% should not be qualified. If IS area is below the lower limit (< 40%), qualify all associated non- detects (U values) "J". If extremely, low area counts are reported, (< 20%) or if perfonnance exhibits a major, abrupt drop off, flag all associated non-detects as unusable ("R"). Are the retention times of the internal standards within 2 0 seconds of the • associated calibration standard? f^ Professional judgement should be used to qualify data if the retention times differ by more than 20 seconds. 304692 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 18 of 51 Date: August, 1992 Revision: 1 YES NO N/A 15.0 Field Duplicates 15.1 Were any field duplicates submitted for Low Cone. VOA analysis? 1 1 ACTION: Compare the reported results for field duplicates and calculate the relative percent difference. ACTTION: Any gross variation between duplicate results must be addressed in the reviewer narrative. However, if large differences exist, identification of field duplicates should be confirmed by contacting the sampler. J£- 304693 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 19 of 51 Date: August, 1992 Revision: 1 PART B: BNA ANALYSES YES NO N/A 1.0 Traffic Reports and Laboratorv Narrative 1.1 Are the Traffic Report Forms present for all samples? ACTION: If no, contact lab for replacement of missing or illegible copies. 1.2 Do the Traffic Reports or Lab Narrative indicate any problems with sample receipt, condition of samples, analytical problems or special notations affecting the quality of the data? ACTION: If samples were not iced upon receipt at the laboratory, flag all positive results "J" and all non-detects "UJ". — 4- m 2.0 Holding Times 2.1 Have any BNA technical holding times, detennined from date of collection to date of extraction, been exceeded? Continuous liquid-liquid extraction of samples for BNA analysis must be started within seven days of the date of collection. Extracts must be analyzed within 40 days of the date of extraction. iL. Table of Holding Time Violations Sample ID (See Traffic Report) Date Date Lab Date Date Sampled Received Extracted Analyzed 304694 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 20 of 51 Date: August, 1992 Revision: 1 YES NO N/A ACTION: If technical holding times are exceeded, flag all positive results as estimated ("J") and sample quantitation limits as estimated ("UJ"), and document in the narrative that holding times were exceeded. If analyses were done more than 14 days beyond holding time, either on the first analysis or upon reanalysis, the reviewer must use profes- sional judgement to determine the reliability of the data and the effects of additional storage on the sample results. At a minimum, all results should be qualified "J", but the reviewer may determine that non-detect data are unusable ("R"). If holding times are exceeded by more than 28 days, all non-detect data are unusable (R). 3.0 Surrogate Recovery (Form II LCSV) 3.1 Are the Low Cone. Semivolatile Surrogate Recovery Summaries (Form II LCSV) present? 3.2 Are all the semivolatile samples in each SDG listed on the proper Surrogate Recovery Form(s)? ACTION: Call lab for explanation/resubmittals. If missing deliverables are unavailable, document effect in data assessments. 3.3 Were outliers marked correctly with an asterisk? ACTION: Circle all outliers in red. 3.4 Were two or more base-neutral Ofi acid surrogate recoveries out of specification for any sample or method blank? If yes, were samples reanalyzed? Were method blanks reanalyzed? Ik m Ltl LU LX. — J L 304695 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 21 of 51 Date: August, 1992 Revision: 1 YES NO N/A ACTION: If all BNA surrogate recoveries are >10% but two within the base-neutral or acid fraction do not meet SOW specifications for the affected fraction only (i.e. base-neutral or acid compounds); 1. Flag all positive results as estimated ("J"). 2. Flag all non-detects as estimated detection limits ("UJ") when recoveries are less than the lower acceptance limit. 3. If recoveries are greater than the upper acceptance limit, do not qualify non-detects. If any base-neutral QX. acid surrogate has a recovery of <10%: 1. Positive results for the fraction with <10% surrogate recovery are qualified with "J". 2. Non-detects for that fraction should be qualified as unusable (R) . Professional judgement should be used to qualify data that have method blank surrogate reeoveries out of specification in both original and reanalyses. Check tihe intemal standard areas. 3.5 Are there any transcription/calculation errors between raw data and Form II? (Tl ACTION: If large errors exist, call lah for expianation/resubmittal, make any necessary corrections and document effect in data assessments. 4.0 Laboratory Control Sample (Form III LCSV) 4.1 Is the Semivolatile Laboratory Control Sample (LCS) Recovery Form (Form III LCSV) present? [>] 304696 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 22 of 51 Date: August, 1992 Revision: 1 YES NO N/A 4.2 Was the LCS analyzed at the recjuired fre- quency (once per SDG, or every 20 samples)? T")^ ACTIOH: If any LCS data are missing, take tihe action specified in 3.2 above. 4.3 How many Low Cone. Semivolatile LCS recoveries are outside QC limits? Low Cone. Wate;- D out of 15 ACTION; If the LCS recovery is greater than the QC-limit, provided on Form III LCSV (140%), positive results should be flagged "J" for the affected eompound(s). If the mass spectral criteria are met but the LCS recovery is less than 60%, then the associated detected target compounds should be flagged "J". Associated non-detected target compounds should be flagged "R". If 25 % of the analyte reeoveries are below QC-limits qualify all associated positive sample data as "J" and non-detects "R". If two or more analytes show recoveries of < "10% all associated positive sample data as "J" and non-detects "R". It should be noted for TPO action if a laboratory fails to analyze an LCS with each SDG, or if a laboratory consistently fails to generate acceptable LCS recoveries. 5.0 5.1 Blanks (Form IV LCSV) Is the Method Blank Summary Form (Form IV LCSV) present? JL 304697 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 23 of 51 Date: August, 1992 Revision: 1 YES NO N/A 5.2 Frequency of Analysis: For the analysis of Low Cone. Semivolatile TCL compounds, has a method blank been reported per 20 samples and for each . extraction batch? 5.3 Has a Low Cone. Semivolatile method blank been analyzed for each GC/MS system used? (See SOW page SV D-34, section 26.2.2) i:a m ACTION: If any method blank data are missing, call lab for expianation/resubmittal. If method blank data are not availeOsle, reject (R) all associated positive data. However, using professional judgement, the data reviewer may substitute field blank data for missing method blank data. 5.4 Chromatography: review the blank raw data - chromatograms (RICs) , c[uant reports or data system printouts and spectra. Is the chromatographic performance (baseline stability) for each instrument acceptable for ^ BNAs? r^l ACTION: Use professional judgement to determine the effect on the data. 6.0 Contamination Note: "Water blanks", "drill blanks" and "distilled water blanks" are validated like any other sample and are not used to qualify the data. Do not confuse them with the other QC blanks discussed below. 6.1 Do any method blanks have positive results (TCL and/or TIC) for Low Cone, semivolatiles? When applied as described below, the contaminant concentration in these blanks are multiplied by . the sample dilution factor. "% 304698 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 24 of 51 Date: August, 1992 Revision: 1 YES NO N/A 6.2 Do any field/rinse blanks have positive Low Cone. Semivolatile results (TCL and/or TIC)? Y^ ACTION: Prepare a list of the sauoples associated with each of the contaminated blanks. (Attach a separate sheet.) Note: All field blank results associated with a particular group of samples (may exceed one per case) must be used to qualify data. Blanks may not be qualified because of contamination in another blank. Field blanks must be qualified for surrogate, spectral, instrument performance or calibration QC problems. ACTION: Follow the directions in the table below to qualify TCL results due to contamination. Use the largest value from all the associated blanks. If gross contamination exists, all data in the associated samples should be qualified as unusable (R) . Sample cone > CRQL but < lOx blank Sample cone <CRQL & is < lOx blank value Sample cone > CRQL value & > lOx blank Common Phthalate Esters Flag sample result with a "U"; Report CRQL & qualify "U" No qualification is needed Sample cone > CRQL but < 5x blank Sample cone < CRQL & is < 5x blank value Sample cone > CRQL value 4 >5 blank value Other Contaminants Flag sample result with a "U"; Report CRQL & qualify "U" No qualification is needed NOTE: Analytes qualified "U" for blank contamination are still considered as "hits" when qualifying for calibration criteria. 304699 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 25 of 51 Date: August, 1992 Revision: l YES NO N/A ACTION: For TIC compounds, if the conoentration in the sample is less than five times the concentration in the most contaminated associated blank, flag the sample data "R" (unusable). 6.3 Are there field/rinse/equipment blanks associated with every sample? ACTION: Note in data assessment that tihere is no associated field/rinse/equipment blank. Exception; samples taken from a drinking water tap do not have associated field blanks. ill 7.0 GC/MS Instrument Performance Cheek (Form V LCSV) 7.1 Are the GC/MS Instrument Performance Check Forms (Form V LCSV) present for Decafluorotriphenylphosphine (DFTPP)? f^ 7.2 Are the enhanced bar graph spectrum and mass/charge (m/z) listing for the DFTPP provided for each twelve hour shift? r r) 7.3 Has an instrument performance check solution been analyzed for every twelve w hours of sample analysis per instrument? r/I ACTION: List date, time, instrument ID and sample analyses for which no associated GC/MS tuning data are available. DATE TIME INSTRUMENT SAMPLE NUMBERS ACTION: If lab cannot provide missing data, reject ("R") all data generated outside an acceptable twelve hour calibration inteirval. 304700 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 26 of 51 Date: August, 1992 Revision: 1 YES NO N/A 7.4 Have the ion abundances been normalized to m/z 198? ACTION: If mass assignment is in error, flag all associated sample data as unusable (R). 7.5 Have the ion abundance criteria been net for each instrument used? ACTION: If ion abundance criteria are not met, the Region II TPO must be notified. 7.6 Are there any transcription/calculation errors between mass lists and Form Vs? (Check at least two values but if errors are found, check more.) 7.7 Have the appropriate number of significant figures (two) been reported? A(rriON: If large errors exist, call lab for expianation/resubmittal, make necessary corrections and document effect in data assessments. 7.8 Is the spectrum of the mass calibration compound acceptable? ACTION: Use professional judgement to determine whether associated data should be accepted, qualified, or rejected. Lk 4i i : ^ m i^_ 8.0 Target Compound List (TCL) Analvtes (Form I LCSV) 8.1 Are the Organic Analysis Data Sheets (Form I LCSV-1,2) present with required header information on each page, for each of the following: a. Samples and/or fractions as appropriate? f\3 b. Laboratory Control Sample(s)? f^l e. Blanks? f^^l 304701 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 27 of 51 Date: August, 1992 Revision: 1 YES NO N/A 8.2 Are the Low Cone. Semivolatile Reconstructed Ion Chromatograms, the mass spectra for the identified compounds, and the data system printouts (Quant Reports) included in the sample package for each of the following: a. b. c. Samples and/or fractions as appropriate? f r^ Laboratory Control Sample(s)? r ^ Blanks S3k ACTION: If any data are missing, take action specified in 3.2 above. 8.3 8.4 Are the response factors shown in the Quant Report? Is chromatographic performance acceptable with respect to: Baseline stability? Resolution? Peak shape? Full-scale graph (attenuation)? Other; l^A^ sxk LHl M l m ACTION; Use professional judgement to determine the acceptability of the data. 8.5 Are the lab-generated standard mass spectra of identified Low Cone. Semivolatile compounds present for each sample? ACTION: If any mass spectra are missing, take action specified in 3.2 above. If lab does not generate their own standard spectra, make note in "Contract Problems/ Non-Compliance". If spectra are missing, reject all positive data. Ck 304702 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 28 of 51 D a t e : August, 1992 R e v i s i o n : 1 8.6 8.7 8.8 Is the RRT of each reported compound within 0.06 RRT units of the standard RRT in the continuing calibration? YES NO N/A JLL Are all ions present in the standard mass spectrum at a relative intensity greater than 25% also present in the sample mass spectrxim? f^ Do sample and standard relative ion intensities agree within 20%? 1^1 ACTION: Use professional judgement to determine acceptability of data. If it is determined that incorrect identifications were made, all such data should be rejected (R), flagged "N" (Presumptive evidence of the presence of the compound) or changed to not detected (U) at the calculated detection limit. In order to be positively identified, the data must comply with the criteria listed in SOW page SV D-27, section 20. ACTION; When sample carry-over is a possibility, professional judgement should be used to determine if instrtiment cross-contamination has affected any positive compound identification. 9.0 Tentatively Identified Compounds (TIC) 9.1 Are all Tentatively Identified Compound Forms (Form I, Part B) present; and do listed TICs include scan number or retention time, estimated concentration and "JN" qualifier? (p 9.2 Are the mass spectra for the tentatively identified compounds and associated "best match" spectra included in the sample package for each of the following: a. b. Samples and/or fractions as appropriate? r^l Blanks? X ^ 304703 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 29 of 51 Date: August, 1992 Revision: 1 YES NO N/A ACTION: If any TIC data are missing, take action specified in 3.2 above. ACTION: Add "JN" qualifier if missing. 9.3 Are any TCL compounds (from any fraction) listed as TIC compounds (exajnple: 1,2- dimethylbenzene is xylene a VOA TCL and should not be reported as a TIC)? ua ACTION; Flag with "R" any TCL compound listed as a TIC. 9.4 Are all ions present in the reference mass spectrum with a relative intensity greater than 25% also present in the sample mass spectrum? 9.5 Do TIC and "best match" standard relative ion intensities agree within 20%? ACTION; Use professional judgement to determine acceptability of TIC identifications. If it is determined that an incorrect identification was made, change identification to "unknown" or to some less specific identification (example: "C3 substituted benzene") as appropriate. Also, when a compound is not found in any blank, but is a suspected artifact of a common laboratoiry contaminant, the result should be qualified as vmusable (R) . JH 111 — 10.0 Compound Quantitation and Reported Detection Limits 10.1 Are there any transcription/calculation errors in Form I results? Check at least two positive values. Verify that the correct internal standard, quantitation ion, and RRF were used to calculate Form I result. Were amy errors found? (j^ 304704 LOW CONCENTRATION WATER STT^DARD OPERATING PROCEDURE Page: 30 of 51 Date: August, 1992 Revision: 1 YES NO N/A 10.2 Are the CRQLs adjusted to reflect sample dilutions? I ^ _ ACTION: If errors are large, call lada for ejcplanation/resubmittal, make any necessary corrections and document effect in data assessments. ACTION: When a sample is analyzed at more than one dilution, the lowest CRQLs are used (unless a QC exceedance dietates the use of the higher CRQL data from the diluted sample analysis). Replace concentrations that exceed the calibration range in the original analysis by crossing out the "E" and it's associated value on the original Form I and substituting the data from the analysis of the diluted sample. Specify which Form I is to be used, then draw a red " X" across the entire page of all Form I's that should not be used, including any in the summary package. 11.0 Standards Data (GC/MS) 11.1 Are the Reconstructed Ion Chromatograms, and data system printouts (Quant, Reporrts) present for initial and continuing calibration? fY.] ACTION: If any calibration standard data are missing, take action specified in 3.2 above. 12.0 GC/MS Initial Calibration (Form VI LCSV) 12.1 Are the Initial Calibration Forms (Form VI LCSV-1,2) present and complete for the Low Cone. Semivolatile fraction at concentrations of 5, 10, 20, 50 and 80 ug/1? fA] ACTION: If any calibration standard forms are missing, take action specified in 3.2 above. 304705 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 31 of 51 Date: August, 1992 Revision: 1 YES NO N/A 12.2 Are response factors stable for semivolatiles over the concentration range of the calibration (% Relative standard deviation (%RSD) < 30.0%)? ACTION: Circle all outliers in red. j - ^ ^ NOTE: ACTION; NOTE; Although 22 Low Cone. Semivolatile compounds have a minimum RRF and no maximum %RSD, the technical criteria are the same for all analytes. If the % RSD is > 30.0%, qualify positive results for that analyte "J" and non- detects using professional judgement. When RSD > 90%, flag all non-detect results for that analyte R (unusable). Analytes previously qualified "U" due to blank contamination are still considered as "hits" when qualifying for calibration criteria. 12.3 Are all Semivolatile compound RRFs > 0.05? Pf\} ACTION: Circle all outliers in red. ACTION; If any RRF < 0.05: 1. "R" all non-deteets. 2. "J" all positive results. 12.4 Are there any transcription/calculation errors in the reporting of average response factors (RRF) or % RSD? (Check at least two values but if errors are found, check more.) ACTION; If errors are large, call lab for expianation/resubmittal, make any necessary corrections and note errors in data assessments. £& — 304706 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 32 of 51 Date: August, 1992 Revision: 1 YES NO N/A 13.0 GC/MS Continuing Calibration ^Form VIT LCSV) 13.1 Are the Continuing Calibration Foimis (Form VII LCSV-1,2) present and complete for the semivolatile fraction? f r) 13.2 Has a continuing calibration standard been analyzed for every twelve hours of sample analysis per instrument? r'jvl ACTION: List below all sample analyses that were not within twelve hours of a continuing calibration analysis for each instrument used. ACTION; If any forms are missing or no continuing calibration standard, has been analyzed within twelve hours of every sample analysis, call lab for explanation/ resubmittal. If continuing calibration data are not available, flag all associated sample data as unusable ("R"). 13.3 Do any semivolatile compounds have a % Difference (% D) between the initial and continuing RRF which exceeds the + 2 5 . 0 % criteria? ^ 1 1 ACTION: Circle all outliers in red. ACTION: Qualify both positive results and non- deteets for the outlier compound(s) as estimated (J). When %D is > 90%, reject all non-detects for that analyte (R) unusable. 13.4 Do any semivolatile compounds have a RRF <0.05? ACTION: Circle all outliers in red. — sX 304707 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 33 of 51 Date: August, 1992 Revision: 1 YES NO N/A ACTION: If RRF <0.05, qualify as unusable (R) associated non-deteets and "J" associated positive values. 13.5 Are there any transcription/calculation errors in the reporting of average response factors (RRF) or % difference (%D) between initial and continuing RRFs? (Check at least two values but if errors are found, check more). f^ hCTlOU: If errors are large, call lab for expianation/resubmittal, make any necessary corrections and document the effect in data assessments. 14.0 Internal Standards (Form VIII LCSV) 14.1 Are the Internal Standard Area and RT Summary Forms (Form VIII LCSV-1,2) present and , complete for the semivolatile fraction? r rl 14.2 Are the internal standard areas for every sample and blank within the upper and lower limits (-50% to +100%) for each continuing calibration? ACTION; List all the outliers below. Sample # Internal Std Area i^b : Lower Limit Upper Limit ACTION: 1. If the internal standard area count is outside the upper or lower limit, flag with "J" all positive results and non-detects (U values) quantitated with this internal standard. 2. Non-detects associated with IS areas > 100% should not be qualified. 304708 LOW CONCENTRATION WATER STANDARD OPERATING PROCEDURE Page: 34 of 51 Date: August, 1992 Revision: 1 YES NO N/A 3. If the IS area is below the lower limit (<50%), qualify all associated non- detects (U-values) "J". If extremely low area counts are reported (<2!5%) or if performance exhibits a major abrupt drop off, flag all associated non-detects as unusable (R). 14.3 Are the retention times of the internal standards within 20 seconds of the . associated calibration standard? f r^ ACTION: Professional judgement should be used to qualify data if the retention times differ by more than 20 seconds. 15.0 Field Duplicates 15.1 Were any field duplicates submitted for Low Cone. Semivolatile analysis? 1 1 ACTION; Compare the reported results for field duplicates and calculate the relative percent difference. ACTION; Any gross variation between field duplicate results must be addressed in the reviewer narrative. However, if large differences exist, identification of field duplicates should be confirmed by contacting the sampler. : : ! 304709 QA/QC Review of Volatiles Data for Pace Analytical SDG: 98037 May 4, 1998 Holding Times: Samples FB0323RE, FB0324RE2, MW0004RE, TB0323RE, and TB0324RE were re-analyzed outside Region II holding times. Results for samples FB0323RE, FB0324RE2, MW0004RE, TB0323RE, and TB0324RE should be considered estimates. GC/MS Tuning and Mass Calibration: All BFB tuning criteria were within control limits. Initial Calibration: All compounds with contract criteria for %RSDs met those requirements. Vinyl chloride (0.097) had an RRF below the contractual minimum (0.100) 04-01-98. No action is taken on two or fewer compounds outside contract requirements as long as no %RSD is above 40% and no RRF is below 0.010. 2-Hexanone (0.041) had an average RRF below the allowable minimum (0.050) on 04-01- 98. 2-Hexanone (0.040) had an average RRF belouw the allowable minimum (0.050) on 04- 06-98. Positive results for 2-hexanone should be considered estimates (J) and negative results unusable (R). Methylene chloride (36.2%) and acetone (51.1%)) had %)RSDs above the allowable maximum (30%o) on 04-01-98. Results for these compounds should be considered estimates (J) in associated samples. Continuing Calibration: All compounds with contractual requirements for RRFs and %RSDs met those criteria. 2-Hexanone (0.037) had an RRFS below the allowable minimum (0.050) on 04-02-98 (0402M02). 2-Hexanone (0.039) had an RRF5 below the allowable minimum (0.050) on 04- 03-98 (0403M02). 2-Hexanone (0.041) had an RRF5 below the allowable minimum (0.050) on 04-06-98 (0406M04). 2-Hexanone (0.040) had an RRFS below the allowable minimum (0.050) on 04-07-98 (0407M02). 2-Hexanone (0.039) had an RRFS below the allowable minimum (0.050) on 04-08-98 (0408M02). Positive results for 2-hexanone should be considered estimates (J) and negative results unusable (R). All target compounds had %oRSDs below the allowable maximum {25%) as required. Blanks: Method blank VBLKWl contained traces ofmethylene chloride (1 ug/L) and acetone (4 ug/L). Method blank VBLKW2containedtraces ofmethylene chloride (1 ug/L) and acetone (4 ug/L). Method blank VBLKW3 contained traces ofmethylene chloride (1 ug/kg) and acetone (4 ug/L). Method blank VBLKW4containedtracesofmethylenechloride(0.5 ug/L) and acetone (4 ug/L). Method blank VBLKWS contained traces ofmethylene chloride (0.5 ug/L) and acetone (3 ug/L). Instrument blank VIBLK02 contained a trace of xylene (0.2 3 0 4 7 1 0 Ug/L). Instrument blank VIBLK06 contained a trace of chloroform (0.4 ug/L). Instrument blank VIBLK09 contained a trace of chloroform (O.S ug/L). Instrument blank VIBLKIO contained traces of ethyl benzene (0.6 ug/L) and xylene (1 ug/L). Trip blank TB0323RE contained a trace of carbon disulfide (0.2 ug/L). Trip blank TB0324 contained a trace of carbon disulfide (0.3 ug/L). Trip blank TB0324RE contained a trace of carbon disulfide (0.2 ug/L). Trip blank TB0326 contained a trace of carbon disulfide (0.1 ug/L). Trip blank TB0327 contained a trace of carbon disulfide (0.1 ug/L). Field blank FB0323 contained traces of acetone (930 ug/L) and 2-butanone (4 ug/L). Field blank FB0324RE2 contained trace of chloromethane (0.8 ug/L), acetone (400 ug/L) and toluene (0.1 ug/L). Field blank FB0325 contained a trace of toluene (0.1 ug/L). Field blank FB0326 contained traces of acetone (160 ug/L), toluene (0.5 ug/L), ethyl benzene (0.2 ug/L), and xylene (0.8 ug/L). Field blank FB0326DL contained a trace of toluene (0.6 ug/L). Field blank FB0326RE contained a trace of toluene (0.6 ug/L). Field blank FB0327 contained traces ofmethylene chloride (7 ug/L), toluene (0.5 ug/L), ethyl benzene (0.5 ug/L), and xylene (2 ug/L). Field blank FB0329 contained traces of acetone (140 ug/L), ethyl benzene (0.7 ug/L), and xylene (3 ug/L).FieldblankFB0329DLcontainedtracesof acetone (150 ug/L), toluene (0.3 ug/L), ethyl benzene (0.7 ug/L), and xylene (3 ug/L). Results for acetone, methylene chloride, 2- butanone, and toluene less than ten times the highest associated blar\k should be considered not detected (U) in samples. Results for chloromethane, carbon disulfide, chloroform, ethyl benzene, and xylene less than five times the highest associated blank should be considered not detected (U) in samples. Field blanks FB0323 (930 ug/L), FB0324RE2 (400 ug/L), FB0326 (160 ug/L), FB0329 (140 ug/L), and FB0329DL (150 ug/L) contained unacceptable levels of acetone. Results for acetone less than ten times the highest blank level should be considered unusable (R) in associated samples. The following are listed the contaminated blanks and associated samples: Method blank VBLKWl: FB0323, FB0326, MW0003, MW0004, MWOOOS, MW0008 Method blank VBLKW2: FB0323DL, FB0324, FB0326DL, MW0002, TB0323, TB0324 Method blank VBLKW3: FB0325, FB0326RE, MWOOOl, MW0006, MW0007, MW0008RE, MW0009, MW002D, TB0326 Method blank VBLKW4: FB0323RE, FB0324RE, FB0327, FB0329DL, MW0002RE, MW0003RE, MW0004RE, MW0005RE, MWOOlO, P00002, TB0323RE, TB0324RE, TB0327 Method blank VBLKWS: FB0324RE2, FB0329, MWOOO 1 RE, MW0002RE2, MW0006RE, MW002DRE, POOOOl Instrument blank VIBLK02: No samples Instrument blank VIBLK06: FB0329 Instalment blank VIBLK09: MWOOOIRE Instrument blank VIBLKIO: MW0006RE Trip blank TB0323RE: MW0004 Trip blank TB0324: MW0003, MWOOOS Trip blank TB0324RE: MW0003, MWOOOS Trip blank TB0326: MWOOOl, MW0006, MW0008 Trip blank TB0327: P00002, MWOOlO Field blank FB0323: MW0004 304711 Field blank FB0324RE2: MW0003, MWOOOS Field blank FB0325: MW0002, MW002D, MW0007, MW0009 Field blank FB0326: MWOOOl, MW0006, MW0008 Field blank FB0326DL: MWOOOl, MW0006, MW0008 Field blank FB0326RE: MWOOOl, MW0006, MW0008 Field blank FB0327: P00002, MWOOlO Field blank FB0329: POOOOl Field blank FB0329DL: POOOOl Intemal Standard Area Summary: All intemal standard areas and retention times were within control limits. Surrogate Recovery: All surrogate recoveries were within control limits. Matrix Spike/Matrix Spike Duplicate: MS/MSD samples were analyzed but the data was not reported as per the SOW. Laboratory Control Sample: VLCSOl had 2 of 12 percent recoveries outside control limits on the initial analysis but VLCSOl RE had all percent recoveries within control limits on the re- analysis. Compound ID: Checked compounds were within GC/MS quantitation and qualitation limits. All positive hit compounds had the primary and secondary ions in their mass spectra as outlined in the SOW. G:\STAFF\DANNE\Island\98037.VOL 304712 Cone, of Intemal Standard: ID; M Date: 4/1/98 RRF Cone, of Compound 1,4-Difluorobenzene Vinyl Chloride RRF Chlorobenzene-d5 Triehloroethene RRF 1,4-Dichlorobenzene-d4 1,2-Dichlorobenzene RRF 0401M06 Sample 1 1 2903861 76172 0.131 3056446 280439 0.459 2351023 567596 1.207 0401M07 Sample 2 2 2558135 128774 0.126 2894671 512926 0.443 2292894 1116090 1.217 0401M08 Sample 3 5 2804841 272515 0.097 3136479 1216022 0.388 2451916 2655128 1.083 0401M09 Sample 4 10 2444456 553762 0.113 2818903 2342764 0.416 2165967 5310170 1.226 0401M10 Sampie 5 25 2208571 1419265 0.129 2519352 5638387 0.448 1979383 12199960 1.233 Average 0.119 0.431 1.193 % RSD 11.8% 6.7% 5.2% Continuing Calibrations Gone, of Compound 1,4-Difluorobenzene Vinyl Chloride RRF Chlorobenzene-d5 Triehloroethene RRF 1,4-Dichlorobenzene-ci4 1,2-Dichlorobenzene RRF 0402M02 Sample 5 2705284 288265 0.107 3118716 1189689 0.381 2396935 2773541 1.157 %D 10.6% 11.4% 3.0% 0403M02 Sample 5 2583795 260859 0.101 3032991 1274871 0.420 2166044 2493966 1.151 %D 15.3% 2.4% 3.5% Sample #DIV/0! #DIV/0! #DIV/0! %D #DIV/OI #DIV/0! #DIV/0! Sample #DIV/0! #DIV/0! #DIV/0! %D #DIV/0! #DIV/0! #DIV/0! Sample #DIV/0! #DIV/0! #DIV/0! %D #DIV/OI #DIV/0! #DIV/0! 304713 Cone, of Internal Standard: ID: M Date: 4/6/98 RRF Cone, of Compound 1,4-Difluorobenzene Vinyl Chloride RRF Chlorobenzene-d5 Triehloroethene RRF 1,4-Dichlorobenzene-d4 1,2-Dichlorobenzene RRF 0406M02 Sample 1 1 1993501 192538 0.483 2526273 238680 0.472 1969133 549026 1.394 0406 M03 Sample 2 2 2032503 379866 0.467 2501909 492947 0.493 2025749 1061008 1.309 0406M04 Sample 3 5 2166252 932464 0.430 2641183 1250227 0.473 2196270 2764167 1.259 0406M05 Sample 4 10 2037184 1862540 0.457 2475506 2560991 0.517 2085271 5394959 1.294 0406M06 Sample 5 25 1956675 4383896 0.448 2393981 5858705 0.489 1976144 12203450 1.235 Average 0.457 0.489 1.298 % RSD 4.3% 3.7% 4.7% Continuing Calibrations Cone, of Compound 1,4-Difluorobenzene Vinyl Chloride RRF Chlorobenzene-d5 Triehloroethene RRF 1,4-Dichlorobenzene-d4 1,2-Dichlorobenzene RRF 0406M04 Sample 5 2166252 932464 0.430 2641183 1250227 0.473 2196270 2764167 1.259 %D 5.8% 3.2% 3.0% 0407 M02 Sample 5 1720851 864319 0.502 2102412 1102473 0.524 1672942 2249814 1.345 %D 9.9% 7.2% 3.5% 0408M02 . Sample 5 1493406 689330 0.462 1917947 848067 0.442 1571980 2051431 1.305 %D 1.0% 9.6% 0.5% Sample #DIV/0! #DIV/OI #DIV/0! %D #DIV/0! #DIV/0! #DIV/0! Sampie #DIV/0! #DIV/OI #DIV/0! %D #DIV/0! #DIV/0! #DIV/0! 304714 QA/QC Review of Semivolatiles Data for Pace Analytical SDG: 98037 May 5, 1998 Holding Times: All samples were extracted and analyzed within Region II holding times. GC/MS Tuning and Mass Calibration: All DFTPP tuning criteria were within control limits. Initial Calibrafion: All compounds with contract criteria for RRFs and %)RSDs met those requirements. All target compounds had average RRFs above the allowable minimum (0.050) and %RSDs below the allowable maximum (30%)) as required. Continuing Calibration: All compounds with contract criteria for RRF20s met those requirements. 2,4-Dinitrotoluene (31.2%)) had a %D above the contractual maximum (25%o) on 03-31-98 (0331 HOI). 2,4-Dinitrotoluene (31.5%)) had a %oD above the contractual maximum (2S%o) on 04-01-98 (0401 HOI). No action is taken on two or fewer compounds per calibrafion outside contract limits as long as %oDs are below 40% and RRFSOs are above 0.010. All target compounds had RRFSOs above the allowable minimum (0.050) as required. Hexachlorocyclopentadiene (S3.0%o), 2,4-dinitrotoluene (31.2%), and bis(2- ethylhexyl)phthalate (25.4%)) had %)Ds above the allowable maximum (25%)) on 03-31-98 (0331H01). Hexachlorocyclopentadiene (49.7%)) and 2,4-dinitrotoluene (31.5%) had %Ds above the allowable maximum (25%o) on 04-01-98 (0401 HOI). Hexachlorocyclopentadiene (37.2%), hexachlorobenzene (27.9%), and bis(2-ethylhexyl)phthalate (26.1%) had %Ds above the allowable maximum (25%)) on 04-06-98 (0406H02). Results for these compounds should be considered estimates (J) in associated samples. Blanks: Method blank SBLKB2 contained a trace of bis(2-ethylhexyl)phthalate (3 ug/L). Field blank FB0323 contained a trace of bis(2-ethylhexyl)phthalate(6 ug/L). Field blank FB0324 contained traces of diethylphthalate(3 ug/L) and bis(2-ethylhexyl)phthalate(93 ug/L). Field blank FB0324DL contained traces of diethylphthalate (3 ug/L) and bis(2- ethylhexyl)phthalate(100 ug/L). Field blank FB0325 contained a trace of diethylphthalate (2 ug/L). Field blank FB0326 contained a trace of diethylphthalate (5 ug/L). Field blank FB0327 contained a trace of diethylphthalate(S ug/L). Field blank FB0329 contained a trace of diethylphthalate (14 ug/L). Results for diethylphthalate and bis(2-ethylhexyl)phthalate less than ten fimes the highest associated blank level should be reported as not detected (U) in samples. The following are contaminated blanks and their associated samples: 304715 Method blank SBLKB2: FB0325, FB0326, FB0327, FB0329, MWOOOl, MW0002, MW0006, MW0007, MWOOOS, MW0009, MWOOlO, MW002D, POOOOl, P00002 Field blank FB0323: MW0004 Field blank FB0324: MW0003, MWOOOS Field blank FB0324DL: MW0003, MWOOOS Field blank FB0325: MW0002, MW002D, MW0007, MW0009 Field blank FB0326: MWOOOl, MW0006, MW0008 Field blank FB0327: MWOOlO, P00002 Field blank FB0329: POOOOl Intemal Standard Area Summary: All intemal standard areas and retention times were within control limits. Surrogate Recovery: Sample MW0002 had 1 of 3 acid extractable surrogate recoveries outside control limits but not below 10%. Sample MW0006 had 1 of 3 acid extractable and 1 of 3 base/neutral surrogates diluted beyond detection limits. No action is taken on 1 of 3 surrogates per fraction outside control limits as long as no recovery is below 10%. Sample MW002D had 1 of 3 acid extractable surrogate recoveries outside control limits and below 10%). Posifive results should be considered esfimates (J) and negative results unusable for the acid extractable fraction of sample MW002D. Matrix Spike/Matrix Spike Duplicate: MS/MSD samples were analyzed but the data was not reported. Laboratory Control Sample: All percent recoveries were within control limits for sample SLCSl. Compound ID: Checked compounds were within GC/MS quantitafion and qualitation limits. All positive hit compounds had the primary and secondary ions in their mass spectra as outlined in the SOW. G:\STAFF\DANNE\Island\98037.SVL 304716 Cone, of Intemal Standard; 20 ID: H Date: 2/11/98 RRF Cone, of Compound 1,4-Dichlorobenzene-d4 Phenol RRF Naphthalene-d8 Naphthalene RRF Acenaphthene-dIO Aeenaphthylene RRF Phenanthrene-dlO Phenanthrene RRF Chrysene-d12 Pyrene RRF Perylene-d12 Benzo(g,h,i)perylene RRF 0211H05 Sample 1 5 251347 92952 1.479 880326 226543 1.029 400005 217601 2.176 706344 187432 1.061 529508 195496 1.477 605760 145503 0.961 0211H06 Sample 2 10 250325 180181 1.440 918271 423029 0.921 388620 401037 2.064 678133 329665 0.972 515973 370200 1.435 584393 254634 0.871 0211H04 Sample 3 20 268652 370497 1.379 955926 847831 0.887 404776 796645 1.968 697452 624541 0.895 516476 701925 1.359 624222 548967 0.879 0211H07 Sample 4 50 250886 790541 1.260 838528 1685200 0.804 330227 1529307 1.852 583210 1196836 0.821 392560 1343044 1.368 476428 1048678 0.880 0211H08 Samples 80 230685 1096505 1.188 703126 2246680 0.799 276304 1943686 1.759 468554 1511052 0.806 295370 1838252 1.556 363077 1431081 0.985 Average 1.349 0.888 1.964 0.911 1.439 0.916 % RSD 9.1% 10.7% 8.4% 11.7% 5.7% 5.8% Continuing Calibrations Cone, of Compound 1,4-Dichlorobenzene-d4 Phenol RRF Naphthalene-d8 Naphthalene RRF Acenaphthene-dIO Acenaphthylene RRF Phenanthrene-dlO Phenanthrene RRF Chrysene-d12 Pyrene RRF Perylene-d12 Benzo(g,h,i)perylene RRF 0331 HOI Sample 20 267601 392231 1.466 927546 824497 0.889 376190 779608 2.072 731823 646023 0.883 544850 802105 1.472 640317 562899 0.879 %D 8.6% 0.1% 5.5% 3.1% 2.3% 4.0% 0401 HOI Sample 20 215299 305278 1.418 727988 651917 0.896 287533 599365 2.085 567348 511699 0.902 410505 580134 1.413 455261 409370 0.899 %D 5.1% 0.8% 6.1% 1.0% 1.8% 1.8% 0406H02 Sample 20 295132 403290 1.366 919426 795948 0.866 369738 758173 2.051 690777 605571 0.877 524003 738070 1.409 605722 546897 0.903 %D 1.3% 2.5% 4.4% 3.8% 2.1% 1.4% Sample #DIV/0! #DlV/0! #DlV/0! #DIV/0! #DIV/0! #DIV/0! %D #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! Sample #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DIV/0! %D #DIV/0! #DIV/0! #DIV/0! #DIV/0! #DlV/0! #DIV/0! 304717 QA/QC Review of 8270 Pyridine Data for Pace Analytical SDG: 98037 Mays, 1998 Holding Times: All samples were extracted and analyzed within Region II holding times. GC/MS Tuning and Mass Calibration: All DFTPP tuning criteria were within control limits. Initial Calibration: All SPCCs and CCCs were within control limits. Pyridine had average RRFs above the allowable minimum (0.050) and %)RSDs below the allowable maximum (30%) as required. Continuing Calibration: All SPCCs and CCCs were within control limits. Pyridine had RRFSOs above the allowable minimum (0.050) and %Ds below the allowable maximum (25%) as required. Blanks: Method and field blanks reported pyridine as not detected. Intemal Standard Area Summary: All intemal standard areas and retention times were within control limits for reported data. Surrogate Recovery: Samples FB0323, MW0002, FB0325, MWOOOl, and FB0326 had 1 of 3 base/neutral surrogate percent recoveries outside control limits but above 10%). No action is taken on 1 surrogate per fraction outside control limits as long as no recovery is below 10%. Matrix Spike/Matrix Spike Duplicate: MS/MSD sample MWOOOS had the relative percent difference and percent recoveries within QC limits. Laboratory Control Sample: Pyridine had a percent recovery within QC limits for the LCS. Compound ID: All samples reported pyridine as not detected. G:\STAFF\DANNE\Island\98037.PYR 304718 ^b&: %o37 Evaluation of Metals Data for the Contract Laboratory Program (CII>) based on BOa. 3/90 (SOP Revision XI) PREPARED BY: . pffx^L LA.^~U.|\ DATE: | — 3 O — % HanifSheiJui, Quality Assurance Chemist Toxic and kazardous Waste Section k..^-^ U J V ^ ^ A D«rE: l-^J-^2 APPROVED BY: KevTJi Kubik, Qiief Toxic cind Hazardous Waste Section \rPRDVED EY:\ AWf^IjfftAl^ ^ -^ DATE: //^^Yf' RoBert^unyonTo^^L Monitoring Management Branch 304719 STANEftRD OFERATING FRDCEDURE Title: Evaluation of Metals Data for the Date: J a n . 1992 Contract Laboratory Program Number: HW-2 Pevisicai: 11 1.0 Scope 1.1 Tliis procedure is applicable to irwrganic data obtained fran cantrac±or laboratories working for Hazardous Waste Site Ccntract laboratory Program (CLP). 1.2 1i\e data validation is based \spcn ar^alytical and quality assurance requirements specified in Statement of Work (SCW) 3/90 . 2.0 Responsibilities - Data reviewers will ccnplete the following tasks as assigned by the Data Review Coordinator: 2.1. For a total rerview: 2.1.1 Data P.s3es'=me^f - "Total Rgviev-Inorganics" Checklist Appendix (A.l). Ihe reviewer must answer every question on the checklist. fl.2 Data Assesaaent - Data Assessment Kaurrative (Appendix A.2) Ihe answer on the c±iecklist must match the action in the narrative (appendix A-2) and on Form I's. Do not use perx:il to write the narrative. 2.1.3 Contract Non-Cctnpliance - S^P Report (Appendix A.3) This report is to be caipleted only when a serious contract violation is encountered, or upon the request of the Data Validation Task Monitor, or Technical Project Officer (TPO). Forward 5 copies: one each for intemal files, appropriate Regional TPO, Sample Management Office (SMD) and last two addresses of Mailing List for Data Reviewers (Appendix A.4). In other cases, all contract violations should be appended to the end of the Data Assessment Narrative (Sec. A.2.2).- 2.1.4 CLP Data Assesqrtf'nt SlgTrnary Form«^ 2.1.4.1 Appendix A.5 Fill in the tctal number of.analytes analyzed by different analyses and the number of ansdytes rejected or flagged eis estimated due to corresponding quality control criteria. Place an "X" in boxes vhere analyses were not performed, or criteria do not apply. 2.1.4.2 Appendix A.6 Data reviewer is also required to fill out Inorganic Regional Data Assessment form (Appendix A.7) provided by EPA Headquarters. Codes listed on the form will be used to describe t:he Data Assessment Summary. 304720 # STANDARD OFERATING PROCEDURE PEkge 2 of 34 e: Evaluation of Metals Data for the Date: Jan. 1992 Ccntract Laboratory Program Nunber: HW-2 Revisicn: 11 2.1.5 Data Reviev lixr; It is reootmended that each data reviewer should maintain a log of the reviews caipleted to include: a. date of start of case review b. date of ocicpletion of case review c. site d. case ramber e. contract laboratory f. ruimher of sanples g. matrix h. hours worked i. reviewer's initials 2.1.6 Telephone Reoord Log - the data reviewer should enter the bare facts of inquiry, before initiating any phone conversation with CLP laboratory. After t±ie case review has been caipleted, mail white copy of Telephone Record Log to the laboratory and pink copy to SMD. File yellow copy in the Telephone Record Log folder, and attach a xerox ccpy of the Telephone Record Log to the caipleted Data Assessment Narrative (;^pendix A.2). 1.7 Forwarded Paperwsrk 2.1.7.1 Upon ccsipletiOTi of .review, the followir^ are to be forwarded to the Regional Sanple Control Center (RSOC) located in the Surveillance and Monitoring Branch: a. data package b. conpleted data assessment checklist (Appendix A.l,origii^al) c. syo Contract Ccnpiiance Screenirxg (CCS) d. Record of Canmunication (copy) e. CLP Reanalysis Request/Approval Reoord (original + 3 ccpies) f. .?^3per>dix A.6 (original). 2.1.7.2 Forward 2 ccpies of caipleted Data Assessment Narrative (Apperdix A.2) along with 2 ccpies of the Inorganic Data Assessment Form (Appendix A.6) and Tele{±ione Record Leg , if any,: one each for appropriate Regional TPO, and the other one t o EPA EMSL office in Las Vegas. The addresses of TPOs and EPA office in Las Vegas cire given in Apperdix A-4. 2-1.8 Filed Paiaerwork - Upon ccnpletion of review, the followir»g are to be filed within MMB f i l e s : a. Two copies of conpletied Data Assessment Narrative (Apperxiix A.2) each carrying Appendix A.6. b. Telef^one Record Log (copy) c. ShSD Report (copy ;^:pendix A-3) d. CLP Reanedysis Request/;^rnval Record (copy) 304721 # : STANDARD OPERATING FRXEDQRE Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Revisicn: 11 3.0 Data Occipleteness Each data package is checked by a Regional Sample Oontrol Coordinator (RSSC) for ccnpleteness. A data package is af>s>myyi to be oonplete vhen a l l the deliverables required under the contract are present. If a data package is incomplete,the RSSC would call the laboratory for missing document(s), If the laboratory does not respond within a week, SMD arxi m s coordinator of Region n will be notified. 4.0 Rejection of Data - All values determined to be ur^oceptable on the Inorganic Analysis Data Sheet (Form I) must be lined over with a red pencil. As soon as any review criteria causes data to be rejected, that data can be eliminated fran ciny further review or consideration. 5.0 Acceptance Criteria - In order that reviews be consistent among reviewers, acceptance criteria as stated in /^jpendix A.l (pages 4-25) should be used. Additior^al guidarK:e can be found in the National Inorganic Functicnal Guidelines of October 1, 1989. EH3 Contract Ccmpliance Scrpipninq (PCS) - This is intended to aid reviewer in locating any problems, both corrected and ur>corrected. However, the validation should be carried out even if CCS is not present. Resutnittals received fran laboratory in response to CCS must be used by the reviewer. 7.0 Recruest for Rearmlysis - Data reviewers must note all items of ccntract non-caipliance within Data Assessment Narrative. If holding tiines and sample stoirage times have not been exceeded, TPO may request reanalysis if items of non-ccrpliarx:e are critical to data assessment. Requests a r e to be made on "CLP Re-Anailysis Request/Approval Record". 8.0 Record of CVTrmmication - Provided by the Regional Sanple Control Center (RSCC) to indicate which data packages have been received eoxi cu:e ready to be reviewed. 9.0 Rounding off numbers - The data reviewer will follcw the standard practice. 304722 STANEARD OPERATING FRDCEDURE Ttle: Evaluation of Metals Data for the Contract laboratory Program ;^:3peniix A.l: Data Assessment - Ccntract Ccnpiiance (Total Review) Date: Jan. 1992 Number: HW-2 Revision: 11 A, 1.1 Contract OmDlianoe Scrpionina Report (OCS) - Present? ACTION: If no, contact RSOC. ySS. m HZA [ ] — J L A. 1.2 Reoord of nommmication (fran RSOC) - Present? ACTION: If no, request fran RSOC. [ ] JL A. 1.3 Trip Report - Present and ccnplete? ACTTON: If no, ccntact RSOC for trip report. A. 1.4 Sample Traffic Report - Present? Legible? ACTION: If no, request fran ftegional Sanple Control Center (RSOC). [ ] [ ] ,1.5 Cover Page - Present? Is cover page prcperly filled in and signed by the lab manager or the manager's designee? ACTTON: If r>o, prepare Telephone Record Log, and contact laboratory. Do numbers of samples correspond to numbers on Record of Communication? Do sanple numbers on cover page agree with sanple numbers on: (a) Traffic Report Sheet? (b) Form I's? ACTTON: If no for any of the above, contact RSOC for clarification. [JL] _ [JL] _ [ ] [ ] [JL] _ ^C 304723 STANDARD OFH^ATING FROCEJTHE 'tie: Evaluation of Mstals Data for the Contract laboratory Program Appendix A.l: Data Assessment - Ccntract Caipliance (Total Review) Date: Jan. 1992 NuiEber: HW-2 Revisicn: 11 A.1.6 Form I to r s Yes Ho N^A A. 1.6.1 Are all the Form I throu^ Form IX labeled with: laboratory name? Case/SAS number? EPA sanple No.? SDG No.? Ocntract No.? Correct units? • Matrix? ACTTON: If no for any of the above, note under Contract Problem/Non-Ccnplianoe section of the "Data Assessment Narrative". A. 1.6.2 Do any ccnputation/transcription errors exceed 10% of reported values on Forms I-IX for: (NDTE: Check all forms against raw data.) (a) all analytes anadyzed by ICP? (b) all analytes analyzed by GFAA? (c) all analytes analyzed by AA Flame? (d) Mercury? (e) Cyanide? ACTTON: If yes, prepare Telephone Log, contact laboratory for corrected data and correct errors with red pencil and irutial. [ ] [JLi [ X J JL] [ ^ ] J ] ] _ JL _ ^ Jk X ^ ^ JL 304724 STANTARD OFERATING FRDCmiRE Title: Evaluaticn of Metals Data for the Contract laboratory Program Appendix A.l: Data Assessment - Ccntract Corpliance (Total Review) Date: Jan. 1992 Nuntaer: HW-2 Revisicn: 11 A.1.7 Raw Data A. 1.7.1 Digestion Log* for flame AA/ICP (Form XUI) present? Digestioi Log for fumaoe AA Form XIU present? Distillation Log for mercury Form XUI present? Distillation Log for cyanides Form X U I present? Are pH values (pH<2 for all met:als, pH>12 for cyanide) present? *Weights, dilutions cind volumes used to obtain values. Peroent solids calculaticn present for soils/sediments? ^ ^ Are preparation datfy; preserrt ai sanple pn^saration logs/bench sheets? A. 1.7.2 Measurement read out record present? A. 1.7.3 Are all raw data to support all sanple cinalyses and QC opaerations present? Legible? Properly Labeled? ACTTON: If no for any of the above questioTS in sections A.1.7.1 through A.1.7.3, write Telephone Record Log and contact laboratory for resutmitrtals. YES CXJ CJCJ [Xx [JL] [ ] [ ] ICP Flame AA Fumaoe AA Mercury Cyanides cinalyses and [ ] [ ^ ] [ 3 rYi [ X ] [X-] [X£J [3^] r Y i m N/A X NC 304725 STANDARD OPERATING FRDCEDURE l e : Evaluation of Metals for the Ccntract Date: Jan. 1992 laboratory Program Nunber: HW-2 Apperxiix A.l: Data Assesanent - Ocntract Revisicn: U CanpliarKze (Total Review) YES NO N/A ^.1.8 Holding Timfta - (aqueous and soil samples ) (Examine sanple traffic reports and digesticr\/distillaticn logs.) Mercury analysis (28 days) exceeded? [JL cyanide distillation (14 days) exoeeded? [ X 1 Other Metcils analysis (6 m o n t h s ) . . . . exceeded? [JL] NOTE: Prepare a list of all sanples and analytes for vAiich holding times have been exoeeded. Specify the number of days fran date of collection to the date of prepeiraticn (from raw data). Attach to checklist. ACTTCN: If yes, reject (red-line) values less than Instrument Detection Limit (IDL) and flag as estimated (J) the values above IDL even t:hough sanple(s) was preserved properly. ^.1.8.2 Is pH of aqueous sanples for: Metals Analysis >2? [IL] Cyanides Analysis <12? [JL\ Action: If yes, flag the associated metals and cyanides data as estimated. \.1.9 Form I (Final Data) '^.1.9.1 Are all Form I's present and ccnplete? [ /\ ] ACTTCgT: If no, prepare tel^iior^ record log and contact laboratory for sutndttal. \.1.9.2 Are correct units (ug/1 for waters and mg/kg for soils) indicated on Form I's? [JL Are soil sanple results for each parameter corrected for percent solids? [ ] K Are all "less than IDL" values properly coded with "U"? [_Y] 304726 STANDARD OFERATING FRDCHtlRE Evaluation of Metals Data for the Date: Jan. 1992 Contract laboratory Program Number: HW-2 Apperdix A.l: Data Assessment - Contract Revision: 11 coiplianoe (Total Review) US HO HZA Are the correct concentration quzdifiers used with final data? F X l ACTTON: If rx3 for any of the above, prepare Tel^iicne Reoord Log, ard ccntact laboratory for ourxectai data. A. 1.9.3 Are EPA sanple # s ard oorre^xyding laboratory semple ID # s the same as on the Cover Page, Form I's and ., in the raw data? f Nl Was a brief physical description of sanples given on Form I's? [ ] j;^ Wcis the dilution of any sanple diluted beyond the requirements of the contract noted on Form I or Form XIV? [ j ^ ] ACTTON; If no for any of the above, note under Contract-Ftoblem/Non-Ocnplianoe of the"DQta Assessment Naurrative". A.1.10 Calibration A. 1.10.1 Is record of at least 2 point calibration present for ICP analysis? [JX] Is record of 5 point calibration present for -v, Hg ancdysis? [__] Is record of 4 point calibration present for: Flame AA? [ ] Furnace AA? f X l Cyanides? [JLj Is one calibration standard at the CMDL level for all AA (exo^Tt Hg) ard cyanides analyses? f Ys 1 ACTION: If no for any of the above, write in the Contract Problem/Non-Caipliance section of the "Data Assessment Narrative". 304727 ^i^e: SIANEARD OPERATING IRXEDURE Evaluation of Metals Data for the Contract Laboratory Program Appendix A.l: Data Assesaaent - Ccntract Ccrtplianoe (Total Review) Date: Jan. 1992 Number: HW-2 Revision: H YES A. 1.10.2 Is correlaticn coefficient less than 0.995 for: Mercury Analysis? Cyarude Analysis? Atcndc Absorption Analysis? T^CTTON; If yes, flag the associated data as estimated. NDTE: The data validator shall calculate the correlaticn coefficient using concentrations of the standards ard the corre^xsTding instrunent response ( e.g. absorbance, peak eirea, peak height, etc.). A.1.10.3 In the instance where less tham 4 standards are measured in cibsorbance (or peak area, peak height,etc.) mode, cire the remairung standards cinalyzed in conoentration mode immediately after calibration within +10% of the true values? [ ] ACTTON; If no, flag the associated data as estimated if standards are not within +10% of true values. Do not flag the data as estimated in linear range indicated by good reoovery of stardatd(s). [ ^ N/A K A. 1.11 A.1.11. Form II A (Initial and Contirminq Calibration Verification)- Present and ccnplete for every metal and cyarude? A.1.11.2 Present ard ccnplete for AA ard ICP when both are used for the same analyte? ACTION: If r» for any of the above, pr^>are Telephone Reoord Log ard contact laboratory. Circle on each Form IIA a l l percerrt recoveries that are outside the contract windows. Are a l l calibration standards (initial ard continuing) within control limits: Metals- 90-110%R? Hg - 8C>-120%R? cyanides- 85-115%R? I J X J^ 304728 STANEftRD OPEIIATING HCCECURE Title: Evaluation of Metals Data for the - Date: Jan. 1992 Contract laboratory Program Number: HW-2 Apperdix A.l: Data Assessment - Contract Revisicn: 11 Corpliance (Toteil Review) iss. m N/A ACTTCN; Flag as estimated (J) all positive data (r>ot flagged with a '"U") analyzed between a ccilibraticn stardard with %R between 75-89% (65-79% for B3; 70-84% for Qi) or 111-125% (121-135% for Hg; n6-130% for CN) reoovery and rgarest good calibration standard. Qualify results <IDL as estimated (UJ) if the ICV or CCV %R is 75-89% (CN, 70-84% ; HG, 65-79%). Reject (red-line) as unacceptable data if reoovery of the ICV or CCV is outside the range 75-125% (CN, 70-130%; Hg, 65-135%). Qualify five sanples on either side of verification standard out of control limits. A. 1.11.3 Was continuing calibration performed every 10 sanples V or every 2 hours? f / 1 Was ICV for cyanides distilled? O L I ACTION; If no for any of the above, write in the Cantract-Ftoblenv/Non-Ccnpliance section of the "Data Assessment Narrative". A.1.12 Form II B (CRDL Standards for AA and ICP) - A. 1.12.1 Was a CRDL standard (CRA) analyzed after initial calibration for all AA metals (exoept Hg)? [XX Was a mid-range calib. verification standard distilled and ar^alyzed for cyarude analysis? [ ] X Was a 2XCRDL ( or 2xIDL when IDI>CRDL) ar^alyzed (CRI)- y for each ICP run? [JX] (Note; CRI for AL,Ba,Ca,Fe,Mg,Na,or K is not required.) ACTTON: If no for any of the above, flag as estimated all data feilling within the affected ranges. The affected ranges eire: AA Ar^alysis - **True Value + CRDL ICP Analysis - **True Value + 2CRDL CN Analysis - **True Value + 0.5 x True Value. |*True value of CRA, CRI or mid-range stardard. Substitute IDL for CRDL vAien IDL > CRDL. rompute the concentration of the missing mid-range stardard fran the calibration range. 304729 STANEftRD OFERATING FRDCEDURE ^ 'le: Evaluation of Metals Data for the Date: Jan. 1992 Contract laboratory Program Nuniaer: HW-2 Apperdix A.l: Data Assessment - Ccntract Revision: 11 CaipliarxDe (Total Review) ^ m N/A A. 1.12.2 Was CRI analyzed after ICV/ICB and before the final OCV/CCB, ard twice every eight hours of ICP run? [_ijj ACTTCN; If no, write in Contract Problenv/Non-Ocnpliance Section of the "Data Assessment Nairrative". A. 1.12.3 Circle on each Form U B all the peroent reooveries that are outside the aoceptarjoe windows. Are CRA ard CRI standards within oontrol limits: Metals 80 - 120%R? [ ] _ X Is mid-range standard within ccntrol limits: cyanide 80 - 120%R? [Jl] ACTTCN; Flag cis estimated a l l sample results within the affected range if the reoovery of the standard is between 50-79%; flag cnly positive data within the affected range if the recovery is between 121-150%; reject all data within the aiffected range if the recovery is less than 50%; reject only positive data within the affected range if the recovery is greater than 150%. Qualify 50% of the sanples on either side of CRI stardard outside the control limits. Note; Flag or reject the finail results only vhen sample raw data are within the affected ranges and the CRDL standards aire outside the acceptance windows. A.1.13 Form III (Initial and ContirTuing Calibration Blanks) A.1.13.1 Preserrt ard ccnplete? [JX] For both AA ard ICP when both are irsed for the same anailyte? [ ] No Was an initial calibration blank analyzed? [JL] Was a continuing calibration blank analyzed after every 10 samples or every 2 hours (which ever is more ^ frequent)? [JL] 304730 STANDARD OPERATING FRDCEDURE Evaluation of Metals Data for the Date: Jam. 1992 Contract laboratory Program Number: HW-2 Apperdix A.l: Data Assessment - Ccntract Revisicn: U Corpliarjoe (Total Review) YES NO N/A ACTTON: If no, prepare Telephcne Reoord log, ccntact laboratory and write in the Contract-Prcblems/ Non-Coiplianoe secticn of the "Data Assessment Narrative". , 1.13.2 Circle CXI each Form l U all calibration blank values that are above CKDL (or 2 x IDL vAien IDL > CRDL). Are cill calibration blanks (when IDLcCRDL) less than or ^ equal to the Contract Required Detection Limits (CRDLs)? [_J_^] Are all calibration blanks less than two times "Y Instrument Detection Limit (when IDI>CRDL)? [ ] /^ ACTTON; If no for any of the above, flag eis estimated (J) positive sanple results when raw sample value is less than or equal to calibraticn blank value anadyzed between calibration blank with value over CRDL (or 2xIDL) and nearest good calibraticn blamk. Flag five sanples on either side of the .calibration blank outside the oontrol limits. 1.14 FORM III (Preparation Blank) - (Note: The preparation blank for mercury is the same as the calibration blank.) ,1.14.1 Wcis one prep, blank analyzed for: each Sanple Delivery Gro^) (SDG)? [ Y Q each batch of digested sanples? [JL.] each matrix type? [ ] >< both AA ard ICP when both aure used for W N the same analyte? [ ] r^ ACTTON: If no for any of the above, flag ais estimated (J) all the associated positive data <10 X IDLs for which p r ^ . blank was not anadyzed. NOTE: If only one blank was analyzed for more than 20 sanples, then first 20 sanples analyzed do not have to be flagged as estimated (J). 304731 STANEftRD OFERATING FRDCEDURE Title: Evaluation of Mstals Data for the "" Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Apperdix A.l: Data Assessment - Oontract Revisicn: 11 Osipliarxse (Total Review) " ^ m N/A A.1.14.2 Is concentration of prep, blank value greater . than the CRDL v*>en IDL is less than or equal to CRDL? iLL If yes, is the ocnoentration of the sample with the least ccncentrated analyte less than 10 times ^• the prep.blank? [ ] _/\ ACTTCN: If yes, reject (red-line) a l l associated data greater than CRDL conoentraticn but less than ten times the prep, blank value. A. 1.14.3 Is concentration of prep, blank veilue (Form l U ) less ^ than two times IDL, vAien IDL is greater than CRDL? [ ] y^ ACTION; If no, reject (red-line) all positive sanple results when sample raw data are less than 10 timRs the pr^. blank valiie. A. 1.14.4 Is concentration of prep, blank belcw the negative CRDL? [XX] ACTTCN; If yes, reject (red-line) aill associated sanple results less than lOxCRDL. A. 1.15 Form IV (ICP Interference Check Sannple) A. 1.15.1 Present aind ccnplete? [JL] '. (NDTE: Not required for furnace AA, flame AA, mercury, cyanide ard Ca, Mg, K and Na.) Was ICS analyzed at beginning ard end of run (or at least twice every 8 hours)? [JL] ACTTON; If no, flag as estimated (J) aill the sanples for which AL, Ca, Fe, or Mg is hii^ier than in ICS. A. 1.15.2 Circle all values on each Form IV that are more than + 20% of tnie or established mean value. Are all Interference Check Sanple results inside the control limits (+ 20%)? F NCI If no, is concentration of Al, Ca, Fe, or Mg lower than the respective concentration in ICS? [ ] K. 304732 # : STANEftRD OFEyOT2«3 PROCEDURE Evaluation of Metals Data for the Date: Jan. 1992 Contract laboratory Program Number: HW-2 J!^:3perdix A.l: Data Assessment - Cortract Revisicn: U Caipliance (Total Review) ~~ ' ~~ ^ . m NTA" ACTTON: If no, flag as estimated (J) those positive results for which ICS reoovery is between 121-150%; flag all sample results as estimated if ICS reoovery falls within 50-79%; reject (red-line) those sanple results for which ICS recovery is less than 50%; if ICS reoovery is above 150%, reject positive results cnly (not flagged with a "U"). A. 1.16 Form V A (SpiJced Sample Reoovery - Pre-Diqestion/Pre-Distillation)- ( Note; Not required for Ca, Mg, K, ard Na (both matrices), Al, ard Fe (soil only.) A. 1.16.1 Present and ccnplete for: each SDG? Cj^] . each matrix type? [Xj each cenc. range (i.e. low, med., hi^)? [ \C. 1 For both AA ard ICP v*ien both are used for the same anailyte? [ ] A ACTTON: If no for any of the above, flag as estimated (J) all the positive data less than fcur times the spiking levels specified in SCW for v^ch spiked sanple was rx3t anadyzed. NDTE: If one spiked sanple was anadyzed for more than 20 sanples, then first 20 sanples anadyzed do not have to be flagged as estimated (J). .^.1.16.2 Was field blank used for spiked sanple? [JL] ACTTON; If yes, flag all positive data less than 4 X spike added as estimated (J) for vrtiich field blaink was used as spiked sanple. A. 1.16.3 Circle on each Form VA adl spike reooveries that are outside control limits (75% to 125%). Are all reooveries within ccntrol limits? [ K i If no, is sanple concentration greater than or equal ^^ to four times spike concentration? [ ] /V- 304733 STANEftRD OFERATING FRDCEDURE Evaluation of Metals Data for the Oontract laboratory Program Apperxiix A.l: Data Assessment - Ccntract Ccnpiiance (Total Review) Date: Jan. 1992 Number: HW-2 Revision: 11" US. ACTTON: If yes, disregard spiJoe recoveries for analytes vtvxe oonoentraticns are greater than or equal to four times spike added. If no, circle those anadytes on Ftarm V for which sanple conoentration is less than four times the ^ike conoentration. Are results cutside the control limits (75-125%) flagged with "N" cn Form I's ard Form VA? A.1.16.4 ACTTCN; If no, write in the Oontract - Problenv/Non - Coiplianoe secticn of "Data Assessmerrt Narrative". Aqueous Are any spike reooveries; (a) less than 30%? (b) between 30-74%? (c) between 126-150%? (d) greater than 150%? ACTTON; If less tham 30%, reject adl aissociated aqueous data; if between 30-74%, flag adl associated aqueous data as estimated (J); if between 126-150%, flag as estimated (J) all associated aqueous data not flagged with a "U"; if greater than 150%, reject (red-line) all associated aqueous data not flagged with a "U". HO N/A [_] _ J^ iJJ] — [xL] [JL] _ [JL] _ A.1.16.5 Soil/Sediment Are any spike reooveries: (a) less than 10%? (b) between 10-74%? (c) between 126-200%? (d) greater than 200%? [ ] [ ] [ ] [ ] 304734 0tle: STANDARD OFERATING FRDCEDURE Evaluation of Metals Data for the Contract laboratory Pxogi'am Appendix A.l: Data Assessment - Ccntract Coiplianoe (Total Review) Date: Jan. 1992 Number: HW-2 Revisicn: 11 YES ACTTCN: If less than 10%, reject all associatPd data; if between 10-74%, flag all associated data as estimated; if between 126-200%, flag as estimated all associated data was not flagged with a "U"; if greater than 200%, reject all aissociated data not flagged with a •TT'. HS N/A A.l.17 A.1.17.1 A.1.17.2 A.1.17.3 Form VI (Tfth Duplicates) Present ard ccnplete for; each SDG? each matrix type? each concentration range (i.e. lew, med., hi^)? both AA and ICP when both are used for the same analyte? [J^] [XLJ [JL] [ ] ACTTON; If no for any the above, flag as estimated (J) all the data >CRDL* for vAiich duplicate sanple was not analyzed. Note;" 1. If one duplicate sanple was analyzed for more than 20 sanples, then first 20 sanples do not have to be flagged as estimated. 2. If percent solids for soil sanple and its duplicate differ by more than 1%, prepare a Form VI for each duplicate padr, report ccncentraticns in ug/L on wet wei^t basis and calculate RFD or Differer>ce for each analyte. Was field blank used for duplicate analysis? ACTTON; If yes, flag all data >CRDL* as estimated (J) for which field blank was used as duplicate. Are adl values within control limits (RPD 20% or dif f ererx:e < +CRDL) ? If no, aire all results outside the control limits flacked with an * on Form I's ard VI? [ ] ACTTON; If no, write in the Contract - Prcblems/Non- Caipliance section of "Data Assessment Narrative". * Substitute IDL for CRDL when IDL > CRDL. _ X i X X 304735 STANTARD OFERATING FRDCEDURE . ^ P b : Evaluation of Metals Data for the Date: Jan. 1992 Contract laboratory Program Nunber: HW-2 Apperdix A.l: Data Assessment - Cm tract Revision: U Caipliance (Ttrtal Review) " ^ m NTA" NOTE: 1. RPD is not calculable for an analyte of the sanple - diylicate pair \Aen both values are less than IDL. 2. If the result of lab duplicate einedyzed by GFAA is rejectable due to coefficient of oorrelaticxi of MSA, analytical ^ike reoovery, or diplicate injections criteria, do not apply precision criteria to metads anadyzed by GFAA. \. 1.17.4 Aqueous Circle on each Form VI adl values that aire: RFD > 50%, or DiffererxDe > CRDL* Is any RPV greater than 50% where sanple ard duplicate are both greater than or equal to 5 times *CRDL? A [ ] Is any difference** between sanple ard di^jlicate greater than *CRDL where sanple and/or duplicate i s less than y. 5 times *CRDL? [/^] ACTTON; If yes, flag the associated data as estimated. ..1.17.5 Soil/Sediment Circle on each Form VI all values that are: RPD > 100%, or Difference > 2 x CRDL* Is cUTy RFD (where sanple aind duplicate aure both greater than or equad to 5 times *CKDL) : > 100%? [ ] Is any **difference between sanple and duplicate (where sanple and/or duplicate is less than 5x*CRDL) : > 2x*CRDL? [ ] ^Substitute IDL for CRDL v^ien IDL > CRDL. 'use absolute values of sanple ard duplicate to cadculate the difference. 3 0 4 7 3 6 STANDARD OFERATING FRDCEDURE e: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Apperdix A.l: Data Assessment - Qjntiact Revision: 11 Ccnpiiance (Total Review) ACTTON: If yes, flaig the associa1:ed data as estimated. YES HQ HZA A.l.18 Field IXplicates A. 1.18.1 Were field duplicates analyzed? [ ] ACTTON; If yes, prepare a Form VI for each aqueous field duplicate pair. Prepare a Form VI for each soil di^slicate pair, if percent solids for sanple ard its duplicate differ by more than 1%; report concentraticns of soils in ug/1 cn wet wei^t basis ard calculate RPDs or Dif ferenoe for each analyte. NOTE; 1. Do not calculate FJFD when both values aire less than IDL. 2. Flag all associated data cnly for field duplicate pair. /l.l.18.2 Aqueous Circle all values on self prepared Form VI for field duplicates that are: RPD > 50%, or Differerx3e > CRDL* Is any RPD greater than 50% where sanple ard duplicate are both greater than or equal to 5 times *CRDL? , [ ] Is any **difference between sanple aid duplicate greater than *CRDL where sanple and/or duplicate is less than 5 times *CRDL? [ ] ACTION; If yes, flag the associated data as estimated. * Substitute IDL for CRDL when IDL > CRDL. ** Use absolute values of sanple and duplicate to calculate the difference. 304737 m^^ STANEftRD OFERATING FRDCEDURE Evaluation of Metals Data for the Contract laboratory Program Apperdix A.l: Data Assessnent - Ocntract Ccnpiiance (Total Review) Date: Jan. 1992 Number: HW-2 Revision: U YES A.1.18.3 Soil/sediment Circle all values cn self prepeired Ptxnn VI for field duplicates that are: RFD >100%, or Difference > 2 x CRDL* Is any RPD (v*iere sanple aind duplicate are both greater than 5 times *CRDL) : >100%? Is any **differenoe between sanple and duplicate (where sanple ard/or duplicate is less than 5x *CRDL ): >2x *CRDL? ACTICN; If yes, flag the associated data ais estimated. HQ HZA [ ] A. 1.19 Form VU (Laboratorv Control Sample) (Note: LCS - rvot required for aqueous Hg aind cyarude analyses.) A.l. 19.1 Was one LCS prepared ard ar^alyzed for: each SDG? f X l each batch sanples digested/distilled? [ J L ] both AA cind ICP when both are used for the same anadyte? [ ] ACnON: If no for amy of the above, prepare Telephone Reoord Log ard contact laboratory for sutndttal of results of LCS. Flag as estimated (J) adl the data for v^iich LCS was rx3t analyzed. NDTE; If only one LCS was anadyzed for more than 20 sanples, then first 20 sanples close to ICS do not have to be flagged as estimated. X. * Substitute IDL for CRDL vA>en IDL > CRDL. * Use absolute values of sanple and duplicate to calculate the differer>ce. 304738 STANEftRD OFERATING FKXZEDURE le: Evaluaticm of Metads Data for the Contract laboratory Program Apperdix A.l: Data Assessment - Oontract cinplianoe (Total Review) Date: Jan. 1992 Number: HW-2 Revisicn: 11 A.1.19.2 YES Aqueous LCS Circle cn each Form V U the ICS peroent reooveries outside ccntrol limits (80 - 120%) except for aqueous Ag ard Sb. Is any LCS recovery: less than 50%? between 50% aid 79%? between 121% and 150%? greater than 150%? ACTTCN; Less than 50%, reject (red-lir>e) all data; between 50% ard 79%, flag all associated data as estimated (J); between 121% ard 150%, flag all positive (not flagged with a "U") results as estimated; greater than 150%, reject all positive results. HQ [JL] [JL] [JL] HZ4 A.1.19.3 solid LOS NDTE; 1. If "Found" value of LCS is rejectable due to duplicate injections or analytical spike reoovery criteria, regardless of LCS reoovery, flag the aissociated data as estimated (J). 2. If IDL of an analyte is equal to or greater tham true vadue of LCS, disregaird the "Action" below even thouK^ LCS is out of control limits. ACTTON: I s LCS "Found" value hi^ier than the control limits on Form VII? If yes, qualify a l l associated positive data as estimated. [ ] I s LCS "Found" value lower than the Control limits on Form VU? ACTION; If yes, qualify a l l associated data as estimated. [ ] 304739 m. STANEftRD OFERATING PROCEDURE Evaluaticai of Metals Data for the Contract laboratory Program Appendix A.l: Data Assessment - Ocntract Ctcpliance (Itotal Review) Date: Jan. 1992 Nunber: HW-2 Revisicn: 11 A.1.20 Form rg (ICP serial Dilution) - NDTE; Serial diluticn anadysis is required cnly for initial ccnoentraticns equal to or greater than 10 x IDL. A. 1.20.1 Was Serial Diluticn anadysis performed for: each SDG? each matrix type? each concentration range (i.e. low, med.)? X [ X J [3L] ACTTCN; If no for amy of the aibove, flag ais estimated a l l the positive data >. lOxTDTfi or >. CRDL vhen lOxIDL <. CRDL for vMch Serial Dilution Arvdysis vas not performed. HQ HZA 1.20.2 Was field blank(s) used for Serial Diluticn Analysis? ACTTCN; If yes, flag all aissociated data >. 10 x IDL as estimated (J). If lOxJDL <. CRDL, flag all data >. CRDL. A. 1.20.3 Are results outside control limit flagged with an "E" on Form I's and Form IX v^en irutial coTcentration on Form IX is equal to 50 times IDL or greater. ACTTON; If no, write in the Contract-Problen\/Non- Ccnpliance section of the "Data Assessment Narrative". i X ] [JS] A. 1.20.4 Circle on each Form IX adl percent differervce that are outside the control limits for initial concentraticns equal to or greater than 10 x IDLs only. Are any % differer>ce values: > 10%? > 100%? JL [ ] [XJ 304740 STANEftRD OFERATING PROCEDURE e: Evaluation of htetals Data for the Contract Laboratory Program Afperdix A.l: Data Assessment - Ccntract corpliance (Totad Review) Datie: Jan. 1992 Number: HW-2 Revisicn: U YES ACTTCN: Flag as estimated (J) all the associated sanple data > lOxIDIs (or > CRDL when lOxIDL < CRDL) for vSiich peroent difference is greater than 10% but less tham 100%. Reject (red-line) all the aissociated sample results equal to or greater than lOxIDLs (or > CRDL when lOxIDL < CRDL) for vAiich FD is greater tham or equal to 100%. Note: Flag or reject on Form I's only the sanple results whose aissociated raw data are >. lOxIDL (or >. CRDL vAien 10xIDL< CRDL) HQ N/A A.1.21 Furnace Atcndc Absorbtion (AA) OC Anadysis A. 1.21.1 Are duplicate injections present in furnace raw data (exc^3t during full Method of Standard Addition) for each sanple anadyzed by GFAA? ACTTON: If rx3, reject the data on Form I's for which duplicate injections were not performed. A. 1.21.2 Do the duplicate injection readings agree within 20% Relative Standard Deviation (RSD) or Coefficient of Variation (CV) for concentration greater than CRDL? Was a dilution ar^alyzed for sanple with analytical spike reoovery less than 40%? ACTION; If no for any of the above, flag all the associated data as estimated. A. 1.21.3 Is *analytical spike recovery outside the control limits (85-115%) for any sanple? [i] iX X t_] ACTTON; If yes, flag as estimated the affected sanple results if the recovery is between 10-84%; if the recovery is between 115-200%, flag the associated positive sanple results as estimated; reject the associated sample results if the reoovery is less than 10%; reject positive sanple results if the recovery is greater than 200%. .Analytical spike is not required on the pre-digestion spiked sanple. 304741 • ^ STANI»RD OFERATING FROCEEURE .- e: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HH-2 Appendix A.l: Data Assessment - Ccntract Revision: 11 C o m p l i a n c e ( T o t a l R e v i e w ) _ — - _ NOTE; Reject or flag the data cnly v*ien the affected sanple (s) was not subsequently analyzed by Method of Standard Addition. A.1.22 F o m v n i (Method of BtJtndard Addition Results) A.1.22.1 Present? [^X] ''jL. If no, is any Form I resudt coded with "S" or a "+"? [JL] ACTTCN: If yes, write request cn Telephcne Record Log ard contact laboratory for sutndttal of Form VIII. A. 1.22.2 Is coefficient of correlaticn for hKA less than 0.990 for .^ any sanple? [ ] j N ACTTCN; If yes, reject (red-line) the affected data. A. 1.22.3 Was *MSA required for any sanple but not performed? [ ] X- Is coefficient of correlation for MSA less than 0.995? [ ] NC Are MSA calculatior^ outside the linear range of the calibration curve generated at the beginning of the anadytical run? ( ] JQ_ ACTTON; If yes for any of the above, flag all the associated data as estimated (J). A. 1.22.4 Was prcper quantitation procedure followed correctly as outlined in the SCW on page E-23? [JLJ ACTTiON: If no, note exception under Contract Prcblera/ Ncn-Ccnplicinoe section of the "Data Assessmerrt Narrative", ard prepare a separate list. MSA is not required on LCS and prep, blank. 3 0 4 7 4 2 m^^ STANIftRD OPERATING FROnTTTRE .. Evaluation of Metals Data for the Date: Jan. 1992 Contract laboratory Program Number: HW-2 Apperdix A.l: Data Assessment - Contract Revision: H Ctnplianoe (Total Review) ^ m NTA" A.1.23 Dissolved/Total or iporqaT^i r/Tntai fT>ji]Y*'**^ - A. 1.23.1 Were any anadyses performed for dissolved eis well as total analytes cn the sane sample(s). [ ] ^ Were any analyses performed for inorgaruc as well as total (orgcinic + inorgardc) analytes on the same sanple(s)? [ ] ^ NDTE: 1. If yes, prepeupe a list ocnparing differenoes between all dissolved (or inorganic) ard total analytes. Ccnpute the differenoes as a percent of the total analyte only when dissolved ccncentraticn is greater than CRDL as well as total ccxjoentraticn. 2. Apply the following questions only if in- organic (or dissolved ) results aire (i) aibove CRDL, aird (ii) greater tham totad constituents. 3. At least one preparation blank, ICS, and LCS should be analyzed in each ainalytical run. A. 1.23.2 Is the concentration of any dissolved (or inorganic) anadyte greater than its total conoentration by nore than 10%? [ ] j2_ A. 1.23.3 Is the concentration of any dissolved (or inorgaruc) analyte greater than its total concentration by more than 50%? [ ] \ ACTTON; If more than 10%, flag both dissolved (or irxarganic) ard total values as estimated (J); if more than 50%, reject (red-line) the data for both values. A.l.24 Form I (Field Blank) - (Note: Designate "Field BlarA" as mvrh on Fonn I.) A. 1.24.1 Circle all field blank values on Form I that are greater than CRDL, (or 2 x IDL when IDL > CRDL). Is field blank concentration less than CRDL (or 2 X IDL v^en IDL > CRDL) for all paraneters . ^ of associated aqueous and soil sanples? [ ] /\ 304743 STANEftRD DISRATING FRDCHURE ^ le: Evaluation of Metals Data for the Date: Jan. 1992 Contract Laboratory Piugram Number: HW-2 ;^perdix A.l: Data Assesanent - Contract Revision: 11 Corpliance (Total Review) m. m HZA If no, was field blank value edieedy rejected due to other QC criteria? [ ] X ACTTON; If no, reject (exo^jt field blamk results) all associated positive sample data less than or equal to five times the field blank vadue. Reject on Form I's the soil sanple resudts that vhsn converted to ug/L on wet beisis aire less than or equal to five timps the field blank value in ug/L. A.1.25 Form X, XI, X U (Verification of Instniwntal Pzimmflt/srs). A. 1.25.1 Is verification report present for: Instrument Detecticn Limits (quiairterly) ? [JX] .ICP Interelement Correction Factors (annually)? [_JLL] ICP Linear Ranges (quarterly)? [ J L ] ACTTON; If no, contact TPO of the lab. A.1.25.2 Form X (Instrument Detecting T.-lmii-«^) - (Note: IDL is not required for Cyarude.) A. 1.25.2.1 Are IDLs present for: all the analytes? [_^] adl the instruments used? f ^ 1 For both AA and ICP when both are used for the same ... analyte? [JX] ACTTON; If no for any of the above, prepare Telephone Record Log ard cartact laboratory. A. 1.25.2.2 Is IDL greater than CRDL for any analyte? [JX] If yes, is the concentration on Form I of the sanple analyzed on the instrument v^ose IDL exceeds CRDL, .- greater tham 5 x IDL. [ ] r- 304744 m, STANI»RD OFERATING FRDCEDURE Evaluation of Metals Data for the Contract Laboratory Program Appendix A.l: Data Assessment - Ocntract Coiplianoe (Total Review) Date: Jan. 1992 Number: HW-2 Revision: 11 IE£ HQ N/A Action : If no, flag as estimated adl values less than five times IDL of the instrument vhose IDL exceeds CRDL. A.1.25.3 Form XI (Linear Ranges) A. 1.25.3.1 Was any sanple result hi^ier tham high linear range of ICP. ^ . Was any sanple result hi(^ier tham the hi^vest calibration standard for rcn-ICP parameters? If yes for any of the above, was the sanple diluted to obtain the result on Form I? [ ] [2f] _ ACTTCN; If no, flag the result reported on Form I as estimated(J). A.1.26 Percent Solids of Sediments A. 1.26.1 Are percent solids in sediment(s): < 50%? < 10%? ACTTCN; If yes, qualify as estimated all the results of a sanple that has per cent solids between 10%-50% (i.e. moisture content between 50%-90%). Reject all the results of a sanple that has per cent solids less than 10% (i.e. moisture content greater than 90%). NDTE: Reject or flag (J) only the sample results that were not previously rejected or flaged . due to other QC criteria. [ ] [ ] 304745 STANEftRD OFERATING PROCEDURE Evaluation of Metals Data for the Contract laboratory Program Appendix A.2: Data Assesaaent Naurrative Date: Jan. 1992 Number: HW-2 Revision: 11 :^e# 3DG# Dontractor "^8 031 site ~J<.lcir\cl Cl\.CtY\irc Lab K<ice Beviower Uor\ nt\/\i Matrix: Soil MtXBrLiL Other .\.2.1 Vadidation Flags- The following flags haive been applied in red by the data validator and nust be considered by the data user. J- This flag indicates the result quadified as estimated Red- Line- A red-line drawn throu^ a sanple resudt indicates imusable value. The red-lined data are Jcncwn to contain significant errors based cn document ed information ard must rx3t be used by the data user. Fully Usable teta- Ihe results that do not carry "J" or "red-line" are fully usable. Contractual Oualifiers- The legend of contractual qualifiers applied by the lab on Form I's is fourd cn page B-20 of SCW IIMOl.O. A.2.2 The data aissessment is given below ard on the attached sheets. Pon AAc. q(,u<<r^tA ^V.,e. Qf^/Oc /^otAgK/ o ^ J R L 3Cnar^c,^/cf PA L PO^ Pc<c<L f^n^/w /. A I 0 & : "190^0 304746 STANDARD OFERATING FRDCEDURE lie: Evaluation of Mstals Data for the Date: Jan. 1992 Contract laboratory I>rogram Number: HW-2 ;!^perdix A.2: Data Assessment Narrative Revision: 11 A.2.2 (continuation) 3 04747 # STANEftRD OFERATING FRDCEDURE e: Evaluatics^ of Metals Data for the Date: Jan. 1992 Contract laboratory Program Number; HW-2 Appendix A.2: Data Assessment Narrative Revision: 11 A.2.2 (continuation) 304748 # ^ STANIARD OPERATING IRXEDURE Evaluation of Mstals Data for the Date: Jan. 1992 Contract Laboratory Program Number: HW-2 Appendix A.2: Data Assessment Narrative Revision: U A.2.3 Contract-Problenv/Non-Ocnplianoe MMB/ESAT Rviewer; Date: Signature Contractor Reviewer: ii)frr^/clA / / 7IA.P Date: Sigr^Uire Signature XXl ' / / / l / \ i / (_ ' Verified by; Date 3 0 4 7 4 9 STANDRTO CPSyOTNG FRDCUXJRE tig: Evaluation of Metals Data for the Ccntract Laboratary Program i^pperdix A.4: Mailing List for Data Reviewers Date: Jan. 1992 Number: HW-2 Revisicn: 11 I.TfT TtF '^^ "t^TTV a. VSXPX haqion Z (XSD) «0 Wwrvisw- Strmet C*b Srtro (617) »61-4312 cx, KE. >ft, w . ju, vr 3. t S C X Rjqion I i : (OC) B39 ternTiu fOAi A.-napcli». KO 2KC1 OucX SA.-tls (3C1) 26t-9iE0 rc, KD. PA, vx, v:, rc C*.-.':*=, Hitra.-., JTC. KKO;. VDS», JTW. w*n=r., M^rs. IA En;ir»«eriJTj S-jt3«r: T«cr.., K«>- PA 5. VSTPA R«;icr. V fES?) 53fc Sa--V. Ciirk Sxr»et T*.-nh rjocr, OC C-.ic«9:, I I fcOtrs P«*. C?j-.:ri:i« 31J-3S3-90ST I I . u.-. ^C. K.-, CH. v- KUL. I A I / T K : Ka.-&u City. KS 6£li5 Deir* Jtorry (S:3) 236-3Bn 3C, KS, NB, yo Wilsor., K^-v&u City Scit-it:lic ryr^trprifcfci, ts^le Pit£?>er USIJ'A Reqion CC (ESO) 10. O"* Ha.i*9«.~e-it S*cticr 215 rreront Sir*et &Ar\ TThrciico, CA »*105 K t i t KJtxMnynan (<15) 974-092* AJ, CA, KI. K.', A.rerica.1 S*.'x». OJA-T. Trust T t r T : t . s r i « cl Pacific Js^eLnds, W&V.c ItlAnd AU. CAL WcTLor., S-Cub«S, XT-CA. V«g&s tSCA taqion I I (ISO) UacdbridTC AWOJC tai»an, Hmj JcrMy « 8 3 7 (201) 321-M76 KJ, W . » , VI CVTCury, OMBRA:^, 15 T«rt, Mano:, r r c , CKteA. 0 £ . CAlsen, I W USEPA tagion TV (ZSO) An&lyticsii fr^^rut B:fc;*Jt CDll«9* S u t i e ^ Ra*:! AUw», CA 30613 Tar. B«."Tnm, J r . (4M) &46-3112 AL, n , , CA, Ki, H5, WC, K , I S CaTpjtfier., EPS, ESE, WBk:, TriAn;It ULx USI^A R«jicr VI (ESD) Hrrjtrry p*rt Piaz*, aiA;. C 660C Horrvood Qrivi HojEicr. TX 77074 (713) f53-3425 AR, IA, W.. !:<, OK W0^3=K, WOIAH, SPECS, EIS, Clocher. J^ftsAAra-., iTc., E P I l n c . , SWPI, X : : i « i , Ury TX, EIRA tSUA Raqjcn VIII lAbor»tary BOX 25366 OvT^cr PadenJ Otrnjtx lAXfwocd. CD 80225 Ev> K3JirA.-i (303) 236-7371 CD. KD. SD, m , W, KT AOr. CSMSI. fKU.. Cat* Cher.. O t i r t l USH'A RflQion X lahnratory P.O. K3X S49 K&n:hest£r, VO. 98353 CftTxld HJth (206) 442-0370 AX, ID, OR. KA Liuctis 7*stijxj L&bK, CfcTtury Tfestm; LiLb* (For VO>> CrUy), Weyerr^eufcer CD. CDl;rtija Testing, £Uv«r Valley 11. Cirlfc Oe.-ps*y - (C6-230) USIFA <C: " t r Street. S.V. WasJ-.ingtor., DC 2W60 r r s 3£2-57^t V.I.- a-t: Ccr:pA.-.y F.C. Br>: £:£ 12. t i . - i r t Ki.ntor UStJA DSL-LV 9*4 E. Karrcn Avt-ue BOX 93478 L(LS Vag&s. N".' 89119 304750 ; ' / V • STANDARD OPERATING ERDCEEtKE Evaluation of Metals Data for the Contract Laboratary Program Apendix A.5: CLP Data Assessment Sunsnary Form (Inorganics) Date: Jan. 1992 Number: HW-2 Revision: 11 Cir P/kTA ASSIStKtVT tUWUjT TOtK (lW0tCA>7CS) OL^? rpt • ! B«rl«v: Uk IUM: P^C-^ • v i t w c r ' * l s l t l « l * : P6pl HusMr • ( t*Mpl»»: n. Anilyt»« >«1«ctt< Put te t»c«»dlnt ltt»l»> C r l t t r l n * c? • 1 » » » *>. ' U f f l t t * *-t uMj^rv W^M t h»r Heldlci O 0 r> n :r : • » * «jk UTTVlCf *-«. n 0 (rturjf 1 O o t t l t h t f ( ) C « l l b r * T l o n 0 o o o f f t p l l i n k 0 0 0 o Kr\t) vt t ^ n 0 t^ l l i n k !,^ 0 Q 0 t r i i K f t d • ! 0 0 0 0 0 0 0 0 I n t t r - f t r t r c t i o A A A, [ i t i K J t l 0 X v^ /^ t p l k t t » C O V » t-» o p? 0 0 &upllcat«i L i b l r i i i d o o 0 0 K Y ) ^ T i ( J ) Pw» to t t c t t i 0 0 Q c) C) 0 q d K ^ ^ X 0 « t t e t l e e L l a i t i o o o o Of e n t e r ) 0 0 0 d U l 0 0' 0 0 »«ri«l CUutlon o KSl X X X Y 1 F o r : * 0 o 0 0 16 / ^ ^ y K >^ r T e t t l A n i l y t t l 3^9 / ^ / ^ n X ) ^ / X 3^9 /? /I /f UtAtetlofl 13 0 H • 0 BshmJfr af 6 0 0 o t t : A i t c r l t k . (•} I n d l c j c t i « d d l t l o n i l c t c f t d i B c t i • ( r t v l * « c r l t i r l * . 3 0 4 7 5 1 SIANDARD (3Pn?ATINj FTOCEDCIRE Evaluation of Metals Data for the Contract Laboratory Program Appendix A.6: CLP Data Assessment Checklist Irxnnganic Analysis Date: Jan. 1992 Number: HW-2 Revision: 11 INCRGANIC RHUONAL DATA ASSESSMENT Region 2.. ••SE NO. SITE J-S(^f\cj Chcn\uc,( •iBORATORY 2an NO. OF SAMPLES/ MAIRIX I'f A,.hr yz^ ^^^37 •J^f' iLfnoz.o REJmJER ( I F NOT ESD) KLVltWER'S NAME K): ACTICK rn. ). HOLDING TIMES CMZBRATIONS BLANKS ICS LCS DUPLICATE ANALYSIS MATRIX SPIKE MSA SERIAL DTLUnOt^ SAMPLE VERIFICATia^ OTHER QC OVERALL ASSESS-HlTr x; CCMPLEIKa^ DATE DATA ASSESSMEOT SUMMARY ICP O IX AA o "TT -II. XX IL JX XX IL An JL ± H. IL o IX JL 6 SL IX JL IL IX. 0 = Data has no problents/or qualified due to mirxDr problems. M = Data qualified due to major problems. Z = Data unacceptable. X = Problems, but do not affect data. 'Q>2^ A nne /^«v r,/f^^ 7^ CYANIDE O o a O TL D n. .TION ITEMS; U'S OF CONCERN; TABLE PERFOK-IANCE: 304752 QA/QC Review of TAL Inorganic Data for Pace Analytical SDG: 98037 May 5, 1998 Holding Times: Samples were analyzed within EPA Region II CLP holding times. Initial and Continuing Calibration VeriFication: Aluminum (124.0% and 117.3%), calcium (110.8%), magnesium (113.5%), potassium (88.1%), sodium (113.2%), and thallium (89.6%) had percent recoveries outside control limits (90-110%). Results for aluminum, calcium, magnesium, potassium, sodium, and thallium should be considered estimates (J) in associated samples. CRDL Standard for AA and ICP: Lead (73.5%) and silver (63.2% and 59.8%), and zinc (134.6%) had percent recoveries outside Region II control limits (80-120%). Results for these metals in associated samples within effected ranges should be considered estimates (J). Blanks: Initial and continuing calibration, and preparation blanks had analyte levels less than the CRDLs as required by Region II. Field blank FB0323 contained aluminum (559 ug/L) and zinc (61.8 ug/L) above their CRDLs. Field blank FB0324 contained zinc (46.9 ug/L) above its CRDL. Field blank FB0325 contained mercury (0.27 ug/L) and zinc (24.2 ug/L) above their CRDLs. Field blank FB0326 contained zinc (58.2 ug/L) above its CRDL. Field blank FB0327 contained aluminum (233 ug/L) and zinc (71.2 ug/L) above their CRDLs. Field blank FB0329 contained calcium (5650 ug/L) and zinc (132 ug/L) above their CRDLs. Results for these metals less than five times the associated blank level should be considered unusable (R) in samples. ICP Interference Check Sample: All applicable percent recoveries were within control limits (80- 120%). Spike Sample Recovery: All percent recoveries were within control limits (75-125%) for spike samples MW0005S and MW0003S Duplicates: Zinc (83%) had a relative percent difference above the CLP maximum (20%) and the allowable maximum (50%) for duplicate sample MW0005D. Results for should be considered estimates (J) in water samples Laboratory Control Sample: All percent recoveries were within control limits (80-120%) for the water LCSs. Standard Addition Results: No results were quantitated by MSA in this LP. ICP Serial Dilution: Aluminum (16.4%), potassium (24.9%), and zinc (15.2%) had %Ds above the allowable maximum (10%) for serial dilution sample MW0005L. Results for aluminum, potassium, and zinc should be considered estimates (J) in water samples. Instrument Detection Limits: All IDLs were at or below the CRDLs as required. G:\STAFF\DANNE\Island\98037.INO 304753 Thallium Date: 4/20/98 X range y range 10 25 50 100 0 0.012 0.034 0.068 0.13 0 Slope: Intercept: Cor. Coef.: 0.001308 0.000422 0.999568 304754 Thallium Date: 4/20/98 X range 0 10 25 50 100 y range 0 0.016 0.04 0.077 0.142 Slope: Intercept: Cor. Coef.: 0.001416 0.002603 0.998863 304755 Mercury Date: 4/15/98 X range 0 0.2 0.5 1 5 10 y range -1916 1603 6124 13727 83837 171008 Slope: Intercept: Cor. Coef.: 17324.95 -2490.61 0.999956 304756 Cyanide Date: 4/6/98 X range 0 0.01 0.05 0.1 0.5 1 y range 0.0004 0.0031 0.0129 0.0246 0.1057 0.2026 Slope: Intercept: Cor. Coef.: 0.201593 0.002443 0.99972 304757 Cyanide Date: 4/7/98 X range 0 0.01 0.05 0.1 0.5 1 y range 0.0004 0.0036 0.0155 0.03 0.1311 0.2511 Slope: Intercept: Cor. Coef.: 0.250237 0.002718 0.999729 304758 X range 0 0.01 0.05 0.1 0.5 1 y range 0.0005 0.0029 0.0148 0.0289 0.1285 0.245 Slope Intercept Cor. Coef. Cyanide 0.244659 0.002411 0.999688 Date: 4/9/98 304759 SDG No. 98045 VOC Checklist 304760 QA/QC Review of Volatiles Data for Pace Analytical SDG: 98045 May 19, 1998 Holding Times: Samples were analyzed within Region II holding times. GC/MS Tuning and Mass Calibration: All BFB tuning criteria were within control limits. Initial Calibration: All SPCCs andCCCs were within control limits. Acetone (0.030) and 2-butanone (0.031) had an average RRF below the allowable minimum (0.050) on 01-27-98. Positive results for acetone and 2-butanone should be considered estimates (J) and negative results unusable (R). Methylene chloride (55.94%) had a %RSD above the allowable maximum (30%) on 01-27-98. Methylene chloride (50.72%) and acetone (50.72%) had %RSDs above the allowable maximum (30%) on 03-25-98. Results for these compounds should be considered estimates (J) in associated samples. Continuing Calibration: All SPCCs and CCCs were within control limits. 2-Butanone had an RRF50 (0.040) below the allowable minimum (0.050) and %D (30.6%) above the allowable maximum (25%) on 04-06-98 (0406A02). Acetone (191.8%) had an unacceptable (>100%) %D on 04-06-98 (0406A02). Acetone (0.023) and 2-butanone (0.039) had an RRF50 below the allowable minimum (0.050) on 04-07-98 (0407A02). Positive results for these compounds should be considered estimates (J) and negative results unusable (R). Methylene chloride (48.5%), 1,2-dichloroethane (40.5%), 4-methyl-2- pentanone (56.5%)), and 2-hexanone (66.8%) had %Ds above the allowable maximum (25%) on 04-06-98 (0406A02). Methylene chloride (52.3%), 2-butanone (25.8%), 1,2-' dichloroethane (32.2%), carbon tetrachloride (35.1%), and 2-hexanone (41.9%) had %Ds above the allowable maximum (25%) on 04-07-98 (0407A02). Methylene chloride (42.5%) and 4-methyl-2-pentanone(29.6%) had %Ds above the allowable maximum (25%) on 04-07- 98 (0407K02). Methylene chloride (34.3%) and chloroethane (31.3%) had %Ds above the allowable maximum (25%) on 04-08-98 (0408K02). Results for these compounds should be considered estimates (J). Blanks: Method blank 25900B1A06 contained a trace of acetone (23.5 ug/kg). Method blank 25900B1A07 contained a trace of acetone (20.1 ug/kg). Results for acetone less than ten times the highest associated blank should be considered not detected (U) in samples. The following are listed the contaminated blanks and associated samples: Method blank 25900B1A06: LSF-001, LSF-002 3 0 4 7 6 1 Method blank 25900B1A07: LTC-001, LTC-003, LTC-004 Intemal Standard Area Summary: All intemal standard areas and retention times were within control limits. Surrogate Recovery: All surrogate recoveries were within control limits. Matrix Spike/Matrix Spike Duplicate: The water MS/MSD sample had all relative percent differences and percent recoveries within QC limits. The soil MS/MSD sample had all percent recoveries within QC limits but had 1 of 33 relative percent differences outside QC limits. No action is taken on MS/MSD data alone to qualify or reject an entire set of samples. Laboratory Control Sample: Soil and water LCSs had all percent recoveries within QC limits. Compound ID: Checked compounds were within GC/MS quantitation and qualitation limits. All positive hit compounds had the primary and secondary ions in their mass spectra as outlined in the method. G:\STAFFADANNE\Island\98045.VOL 304762 Cone, of Intemal Standard: 50 ID; K Date: 3/25/98 RRF Cone, of Compound Pentafluorobenzene Vinyl chloride RRF 1,4-Difluorobenzene Triehloroethene RRF Chlorobenzene-d5 Tetrachloroethene RRF 1,4-Dichlorobenzene-d4 Isoprpopylbenzene RRF 0325K02 Sample 1 10 1161895 90048 0.388 1945587 197375 0.507 1578693 207031 0.656 1078045 511138 2.371 0325K03 Sample 2 20 1153870 173418 0.376 1994395 392549 0.492 1592610 412916 0.643 1100783 1043476 2.370 0325K04 Sample 3 50 1191064 455000 0.382 1983344 985329 0.497 1666983 1051865 0.631 1167975 2711490 2.322 0325K07 Sample 4 100 1218328 892510 0.366 2034306 2094578 0.515 1721541 2272730 0.660 1198770 5860096 2.444 0325K09 Sample 5 200 1238466 1906038 0.385 2160979 4432082 0.513 1816447 4550831 0.626 1254927 12871861 2.564 Sample 6 Average 0.379 0.505 0.644 2.414 % RSD 2.2% 2.0% 2.3% 3.9% Continuing Calibrations Cone, of Compound Pentafluorobenzene Vinyl chloride RRF 1.4-Dinuorobenzene Triehloroethene RRF Chlorobenzene-d5 Tetrachlorobenzene RRF 1.4-Dichlorobenzene-d4 Isopropylbenzene RRF 0407K02 Sample 50 1346916 460665 0.342 2361331 1152030 0.488 2000626 1178926 0.589 1348498 2902472 2.152 %D 9.8% 3.3% 8.5% 10.8% 0408K02 Sample 50 1272025 486711 0.383 2222677 1154393 0.519 1938338 1219903 0.629 1320538 3080404 2.333 %D 0.9% 2.9% 2.3% 3.4% Sample #DlV/0! #DIV/0! #DlV/0! #DIV/0! %D #DIV/0! #DlV/0! #DlV/0! #DIV/0! Sample #DIV/0! #DIV/0! #DlV/0! #DIV/0! %D #DIV/0! #DIV/0! #DlV/0! #DIV/0! Sample •»DlV/0! #DlV/0! #DlV/0! #DlV/0! %D #DIV/0! #DIV/0! #DIV/0! #DIV/0! 304763 Cone, of Internal Standard: 50 ID: A Date: 1/27/98 RRF Cone, of Compound Pentafluorobenzene Vinyl chloride RRF 1,4-Difluorobenzene Triehloroethene RRF Chlorobenzene-d5 Tetrachloroethene RRF 1,4-Dichlorobenzene-d4 Isoprpopylbenzene RRF 0127A03 Sample 1 10 1375565 84700 0.308 1607921 163329 0.508 1178812 164034 0.696 650886 551876 4.239 0127A04 Sample 2 20 1405270 205540 0.366 1639526 319293 0.487 1189086 327777 0.689 700574 1159863 4.139 0127A05 Sample 3 50 1520249 554889 0.365 1706759 791891 0.464 1200720 826851 0.689 737177 2904208 3.940 0127A07 Sample 4 100 1578624 1284856 0.407 1732702 1662193 0.480 1233289 1849468 0.750 925306 7492985 4.049 0127A09 Sample 5 200 1821357 3324900 0.456 2088927 4150200 0.497 1549981 4898829 0.790 1128744 17604839 3.899 Sample 6 Average 0.380 0.487 0.723 4.053 % RSD 14.5% 3.4% 6.3% 3.5% Continuing Calibrations Cone, of Compound Pentafluorobenzene Vinyl chloride RRF 1,4-Difluorobenzene Triehloroethene RRF Chlorobenzene-d5 Tetrachlorobenzene RRF 1.4-Dichlorobenzene-d4 Isopropylbenzene RRF 0406A02 Sample 50 2596376 1029488 0.397 2798758 1306086 0.467 2010408 1361457 0.677 1324110 5034327 3.802 V.D 4.2% 4.2% 6.3% 6.2% 0407A02 Sample 50 2101897 839416 0.399 2043558 971347 0.475 1428422 1010550 0.707 1085821 3816266 3.515 %D 5.0% 2.4% 2.1% 13.3% Sample #DlV/0! #DIV/0! #DIV/0! #DlV/0! %D #DlV/0! #D!VfO! #DlV/0! #DIV/0! Sample #DIV/0! #DIV/0! #DIV/OI #DIV/0! %D #DlV/0! #0IVm! #DIV/0! #DIV/0! Sample #DIV/0! #DIV/0! #DlV/0! #DIV/0! %D #DIV/0! #D1V/Q! «DIV/0! #DlV/0! 304764 MEMORANDUM ^imw K ChemRisk A S«<VH:« ol Mt±mforvUArt To: Anuj Gulati; M/H-Warren v A From: John Samuelian; M/H-Portland i ^ ^ Date: 16 July 1998 (j Re: Island Chemical Corporation-Validation of Method 8260 Analytical Data M/H Project No. 12.0805380.001.004 Soil samples, groundwater samples, and aqueous field blanks were analyzed for up to 17 volatile organic componds (VOCs) following EPA Method 8260. The analyses were performed by a mobile laboratory operated by McLaren/Hart. The analytical results were validated using relevant criteria fi:om EPA Region U guidance (USEPA, 1996). The EPA Region II checklists were tised to review the data but were not completed as part of this assessment. The following information was used to validate the analytical results: Sample Hold Time before Analysis Initial and Continuing Calibration Surrogate Recoveries Intemal Standards Matrix Spike/Matrix Spike Duplicate (MS/MSD) analyses Laboratory Control Sample PE Sample Results Method Blank Contamination Rinsate Blank Contamination Compound Identification Chromatogram quaUty Calculations. A holding time simimary table (Table 1) is attached to this memorandum. 304765 McLaren/Hart - ChemRisk 1685 Congress Street Portland, ME 04102 Phone:(207)774-0012 Fax: (207) 774-8263 1. Sample Holding Time Before Extraction and Analysis: The technical holding times for VOC analyses by Method 8260 is 14 days fi"om sample collection to analysis. Review of Table 1 shows that all holding times were met. 2. Initial and Continuing Calibrations: The instrument was initially calibrated using a five point calibration standard. The relative standard deviations (RSDs) of each analyte in the multi-concentration calibration are assessed. In the continuing calibration, the percent difference (%D) of the continuing calibration concentration and the average of the initial multipoint calibration is assessed. RRF values must be greater than 0.05, RSD values less than 30%, and %D values less than 25%, for the analytes to be in compliance. The RRFs, RSDs and %D values were within controls, except for the following: • Initial Calibration, 4/1/98, aqueous: acetone (63%), methylene chloride (41%), and 1122- tetrachloroethane (38%). • Liitial Calibration, 4/15/98, soil: bromoform (41%). • Continuing Calibration, 4/1/98, aqueous and soil: vinyl chloride (27%) • Continuing Calibration, 4/7/98, aqueous: chloromethane (32%) No qualifications were required for either initial or continuing calibrations. 3. Surrogate Recoveries: Surrogates measure the ability of the laboratory to extract the targeted analytes by evaluating the recovery of indicator compounds which are stmcturally similar to the targeted analytes as indicators for all of the analytes. For these analyses, three surrogates were used (l,2-dichloroethane-d4, toluene-d8, and bromofluorobenzene). Control limits were 75-125% for the water samples, and 70-130% for the soil samples. AH surrogate recoveries were within the control limits, except for the following samples: • Drainage Pit-1 SW: l,2-dichloroethane-d4(74%) • SB-PP-8/4-6: bromoflurobenzene (68%) • SB-PP-10/4-6: bromoflurobenzene (67%) • SB-PP-32/16-18: bromoflurobenzene (66%) • SB-PP-32/24-26: bromoflurobenzene (68%) • SB-PP-13/16-18: bromoflurobenzene (68%) • GW31 DL: l,2-dichloroethane-d4 (134%) Qualifjcation.';: a) All positive VOCs were qualified with a "J," and all non-detects with a "UJ" in 6 samples (Drainage Pit-1 SW, SB-PP-8/4-6, SB-PP-10/4-6, SB-PP-32/16-18, SB-PP-32/24-26, and SB-PP-13/16-18) due to one SMC below the lower control Umit. b) All positive VOCs were qualified with a "J" in sample GW31 DL due to one SMC above the upper contol Umit. No action was required for the non-detect results in this sample. • Page 2 3 0 4 7 6 6 4. Internal Standards: Intemal standards are added to all sample, blank and calibrations and are used to quantify the analytes. For these analyses, 3 intemal standards (bromochloromethane, 1,4- difluorobenzene, and chlorobenzene-d5) were used. All intemal standard retention times and areas were within the control limits. 5. MS/MSD Analyses: An MS/MSD was performed for the soil samples only. The samples were spiked v^dth a mixture of 4 VOCs (11-dichIoroethene, benzene, toluene, and chlorobenzene), with acctiracy measured by the spike recovery and precision measured by the relative percent difference between the MS and MSD results. All recoveries and RPDs were within the control limits. MS/MSD frequency is typically one per batch or one per 20 samples. This was not the frequency used by the mobile laboratory. 6. LCS Analysis: An LCS (blank spike) was also performed with a mixture of 4 VOCs (11- dichloroethene, benzene, toluene, and chlorobenzene). The spike recoveries were within the confrol limits. 7. PE Results: A PE sample was analyzed with these samples. The results are summarized in Table 2. All observed results were within the acceptance limits. 8. Analysis Sequence: The laboratory properly performed an initial calibration, sample analyses, and continuing calibration as described by the method. 9. Method Blank Contamination: A method blank measures the potential for false-positive results infroduced by intemal laboratory contamination. A total of 11 aqueous method blanks and 8 soil method blanks were prepared. All of these contained no detectable analytes, with the exception of the following blank: • WB040898A, aqueous blank (Corresponding samples: GWPP28 and GWPP29): acetone (8 J lig/L). Qual{fication.s: a) Acetone was qualified with a "U" in sample GWPP29 due to method blank contamination. 10. Field Blank Contamination: The field blank (FB) measures the potential for false-positive results infroduced by improper field decontamination procedures of sampling equipment. A total of two field blaiiks were included with this package, and neither contained any detectable VOCs. 11. Trip Blank Contamination: The Trip Blank measures the potential for cross-contamination during sample storage and shipment. Since these samples were hand-delivered to the mobile laboratory, trip blanks were not reqtiired. 3 0 4 7 6 7 12. Compound Identification: Verification of identification of VOC analyte analuzed using a GC/MS is based upon the relative retention time compared to the intemal standard and ion spectra match. All positive results met RRT and ion spectia criteria. 13. Chromatogram Quality: The quality of the VOC chromatograms is evaluated to determine whether there are any interfering unknowns present which prevent the identification of the targeted analytes. All chromatograms were of acceptable quality. 14. Calculations: The reported analyte concentrations and any intemal QC calculations were verified for their accuracy. All checked calculations were acceptable within rounding errors. 15. Other OC: • Reporting limits and VOC concentrations in the soil samples were calculated and reported based on a wet weight basis. • Meditim level soil extractions were performed on all soil samples using purge and trap grade methanol. • Chlorobenzene and bromoform were incorporated into the target parameter list during the initial cahbration acquired on 4/3/98, and were not originally analytes of concem at.this Site. According to the laboratory narrative, they were added to round out qtiality controF procedures. • The following samples required dilutions due to high concentrations of chloroform: • GW-PP-15(8'-10')-10X; • GW-PP-19(8'12')-10X; • GW-PP-23 (22'-27') - 20X; • GW-PP-28 (26'-31') - 5X; and • GW-PP-31(22'-27')-25X. The laboratory reflected these dilutions by adjusting the sample volumes on the Form I's, instead of reporting them in the dilution factor field. The appropriate non-detects and positive results to report were identified by the Reviewer on the affected Form Is. Data Limitation Overview The VOC analysis of the soil and groundwater samples from the Island Chemical site showed compliance with the QC requirements of the method and all data are valid and acceptable, with quaUfications applied and other actions as summarized below: Drainage Pit-1 SW: All results were qualified with a "UJ" due to SMC recovery below the lower confrol limit. There were no positive results in this sample. 3 0 4 7 6 8 • Page 4 GW-PP-15 and GW-PP-15DL: Report the non-detect results from tire undiluted analysis, and the chloroform result from the undiluted analysis as the sample result. GW-PP-19 and GW-PP-19DL: Report the non-detect results from tiie undiluted analysis, and tiie chloroform result from the undiluted analysis as the sample result. GW-PP-23 and GW-PP-23DL: Report the non-detect results from the undiluted analysis, and tiie chloroform result from the imdiluted analysis as the sample result. GW-PP-28 and GW-PP-28DL: Report the non-detect results from tiie undiluted analysis, and tiie chloroform result from the undiluted analysis as tiie sample result. GWPP29: Acetone was qualified witii a "U" due to metiiod blank contamination. The result was raised to the sample quantitation limit. GW-PP-31 and GW-PP-31 DL: Report tiie non-detect results from the imdiluted analysis, and the chloroform result from the undiluted analysis as the sample result. Chloroform was qualified with a "J" in sample GW31 DL due SMC recovery above the upper control limit. SB-PP-8/4-6: All results were qualified witii a "UJ" due to SMC recovery below the lower confrol limit. There were no positive results in this sample. SB-PP-10/4-6: All results were qualified witii a "UJ" due to SMC recovery below the lower confrol limit There were no positive results in this sample. SB-PP-13/16-18: All results were qualified with a "UJ" due to SMC recovery below the lower confrol limit. There were no positive results in this sample. SB-PP-32/16-18: All results were quaUfied witii a "UJ" due to SMC recovery below the lower confrol limit. There were no positive results in tiiis sample. SB-PP-32/24-26: The 16 non -detect results were qualified with a "UJ," and the single positive result (chloroform) was qualified witii a "J," due to SMC recovery below the lower confrol limit. There were no positive results in this sample. .Pages 3 047 6 9 Table 1. Table of Holding Times Field Sample ID Drainage Pit 1-SW FB033098 FB(M0498 GW-OR-1 GW-PP-10 GW-PP-11 GW-PP-12 iGW-PP-13 GW-PP-14 GW-PP-15 GW-PP-15 DL GW-PP-16 GW-PP-17 GW-PP-19 GW-PP-19 DL GW-PP-20 ,GW-PP-21 :GW-PP-23 GW-PP-23 DL ,GW-PP-24 :GW-PP-25 ,GW-PP-26 GW-PP-27 DL GW-PP-28 GW-PP-28 DL GW-PP-29 GW-PP-30 GW-PP-31 GW-PP-31 DL GW-PP-32 GW-PP-33 GW-PP-34 GW-PP-35 GW-PP-7 GW-PP-8 GW-PP-9 GW-PP-9 RE PE, Lot No. 577 SB-OR-1/10-12 SB-OR-1/14-16 SB-OR-1/20-22 SB-OR-1/22-24 SB-OR-1/2^ SB-OR-1/24-26 SB-OR-1/26-28 SB-OR-1/4-6 Matrix aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous aqueous soil soil soil soil soil soil soil soil Parameter VOCs VOCs VOCs VOCs VOCs VOCs VOCs VOCs VOCs VOCs VOCs VOCs VOCs VOCs VOCs voa VOCs VOCs voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa Date Collected 3/30/98 3/30/98 4/4/98 4/1/98 3/31/98 3/29/98 3/30/98 3/31/98 4/1/98 4/2/98 4/2/98 4/3/98 4/3/98 4/3/98 4/3/98 4/3/98 4/5/98 4/4/98 4/4/98 4/5/98 4/5/98 4/5/98 4/5/98 4/8/98 4/8/98 4/8/98 4/9/98 4/8/98 4/8/98 4/7/98 4/9/98 4/9/98 4/10/98 3/27/98 3/27/98 3/29/98 3/29/98 4/1/98 4/1/98 4/1/98 4/1/98 4/1/98 4/1/98 4/1/98 4/1/98 Date Lab Received 3/30/98 3/30/98 4/4/98 4/1/98 3/31/98 3/29/98 3/30/98 3/31/98 4/1/98 4/2/98 4/2/98 4/3/98 4/3/98 4/3/98 4/3/98 4/3/98 4/5/98 4/4/98 4/4/98 4/5/98 4/5/98 4/5/98 4/5/98 4/8/98 4/8/98 4/8/98 4/9/98 4/8/98 4/8/98 4/7/98 4/9/98 4/9/98 4/10/98 3/27/98 3/27/98 3/29/98 3/29/98 4/6/98 4/1/98 4/1/98 4/1/98 4/1/98 4/1/98 4/1/98 4/1/98 4/1/98 Date Lab Analyzed 4/2/98 4/7/98 4/7/98 4/1/98 4/1/98 4/1/98 4/2/98 4/1/98 4/2/98 4/3/98 4/4/98 4/4/98 4/3/98 4/3/98 4/3/98 4/4/98 4/6/98 4/5/98 4/5/98 4/6/98 4/6/98 4/7/98 4^/98 4/8/98 4/9/98 4/8/98 4/9/98 4/9/98 4/9/98 4/8/98 4/9/98 4/9/98 4/10/98 4/1/98 4/1/98 4/1/98 4/2/98 4/10/98 4/4/98 4/4/98 4/4/98 4/4/98 4/4/98 4/4/98 4/4/98 4/4/98 Holding Times C-»R 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 R-^A 3 8 3 0 1 3 3 1 1 1 2 1 0 0 0 1 1 1 1 1 1 2 2 0 1 0 0 1 1 1 0 0 0 5 5 3 4 4 3 3 3 3 3 3 3 3 • Page 6 304770 Table 1 (Continued) Field Sample ID SB-PP-10/10-12 SB-PP-10/16-18 SB-PP-10/20-22 SB-PP-10/22-24 SB-PP-10/24-26 SB-PP-10/26-28 SB-PP-10/28-30 SB-PP-10/30-32 SB-PP-10/4-6 SB-PP-13/10-12 SB-PP-13/16-18 SB-PP-13/16-18 Dup SB-PP-13/20-22 SB-PP-13/22-24 SB-PP-13/24-26 SB-PP-13/26-28 SB-PP-13/28-30 SB-PP-13/4-6 SB-PP-15/10-12 SB-PP-15/5-7 SB-PP-22/10-12 SB-PP-22/12-14 SB-PP-22/1-3 SB-PP-22/5-7 SB-PP-22/7.5-9.5 SB-PP-23/10-12 SB-PP-23/16-18 SB-PP-23/20-22 SB-PP-23/22-24 SB-PP-23/24-26 SB-PP-23/26-28 SB-PP-23/28-30 SB-PP-23/6-8 SB-PP-23/8-10 SB-PP-26/10-12 SB-PP-26/6-8 SB-PP-26/8 SB-PP-26/8-10 SB-PP-27/10-12 SB-PP-27/16-18 SB-PP-27/4-6 SB-PP-32/10-12 SB-PP-32/16-18 SB-PP-32/24-26 SB-PP-32/26 SB-PP-32/27-28 SB-PP-32/4-6 Matrix soil soil soil soil soil soil soil soil soil soil soO soil soil soil soil soil soil soil soil soO soil soil soil soil soil soil soil soil soil soil soil soil soil soil soil soil soil soil soil soil soil soil soil soil soil soil soil Parameter voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa Date Date Lab Collected Received 3/30/98 3/30/98 3/30/98 3/30/98 3/30/98 3/30/98 3/30/98 3/30/98 3/30/98 3/31/98 3/31/98 3/31/98 3/31/98 3/31/98 3/31/98 3/31/98 3/31/98 3/31/98 4/2/98 4/2/98 4/3/98 4/3/98 4/3/98 4/3/98 4/3/98 4/4/98 4/4/98 4/4/98 4/4/98 4/4/98 4/4/98 4/4/98 4/4/98 4/4/98 4/5/98 4/5/98 4/5/98 4/5/98 4/5/98 4/5/98 4/5/98 4/7/98 4/7/98 4/7/98 4/7/98 4/7/98 4/7/98 3/30/98 3/30/98 3/30/98 3/30/98 3/30/98 3/30/98 3/30/98 3/30/98 3/30/98 3/31/98 3/31/98 3/31/98 3/31/98 3/31/98 3/31/98 3/31/98 3/31/98 3/31/98 4/2/98 4/2/98 4/3/98 4/3/98 4/3/98 4/3/98 4/3/98 4/4/98 4/4/98 4/4/98 4/4/98 4/4/98 4/4/98 4/4/98 4/4/98 4/4/98 4/5/98 4/5/98 4/5/98 4/5/98 4/5/98 4/5/98 4/5/98 4/8/98 4/8/98 4/8/98 4/8/98 4/8/98 4/8/98 Date Lab Analyzed 4/7/98 4/7/98 4/7/98 4/7/98 4/7/98 4/7/98 4/7/98 4/7/98 4/7/98 4/8/98 4/8/98 4/8/98 4/8/98 4/15/98 4/15/98 4/15/98 4/16/98 4/8/98 4/4/98 4/4/98 4/4/98 4/4/98 4/4/98 4/4/98 4/4/98 4/4/98 4/5/98 4/5/98 4/5/98 4/5/98 4/5/98 4/6/98 4/5/98 4/5/98 4/5/98 4/6/98 4/6/98 4/6/98 4/6/98 4/6/98 4/6/98 4/8/98 4/8/98 4/8/98 4/8/98 4/8/98 4/8/98 Holding C->R 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Times ji R->A 8 8 8 8 8 8 8 8 8 8 8 8 8 15 15 15 16 8 2 2 0 1 2 1 0 1 0 0 0 0 0 0 304771 Table 1 (Continued) Field Sample ID SB-PP-7/12-14 SB-PP-7/15-17 SB-PP-7/20-22 SB-PP-7/22-24 SB-PP-7/24-26 SB-PP-7/4-6 SB-PP-8/10-12 SB-PP-8/16-18 SB-PP-8/20-22 SB-PP-8/22-24 SB-PP-8/4-6 SB-PP-9/10-12 SB-PP-9/16-18 SB-PP-9/20-22 SB-PP-9/22-24 SB-PP-9/4-6 Matrix soil soil soil soil soil soil soil soil soil soil soil soil soil soil soO soil Parameter voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa voa Date Collected 3/27/98 3/27/98 3/27/98 3/27/98 3/27/98 3/27/98 3/27/98 3/27/98 3/27/98 3/27/98 3/27/98 3/29/98 3/29/98 3/29/98 3/29/98 3/29/98 Date Lab Received 3/27/98 3/27/98 3/27/98 3/27/98 3/27/98 3/27/98 3/27/98 3/27/98 3/27/98 3/27/98 3/27/98 3/29/98 3/29/98 3/29/98 3/29/98 3/29/98 Date Lab Analyzed 4/4/98 4/4/98 4/4/98 4/5/98 4/5/98 4/3/98 4/2/98 4/2/98 4/2/98 4/2/98 4/2/98 4/3/98 4/3/98 4/3/98 4/3/98 4/3/98 Holding Times j C-^.R 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 R-^A 8 8 8 9 9 7 6 6 6 6 6 5 5 5 5 5 • Page 8 304772 Table 2. PE Sample' Results Analyte Chlorometiiane Vinyl chloride 1,1-Dichloroetiiene Acetone Methylene chloride 1,1-Dichloroethane Chloroform Benzene 1,2-Dichloropropane Bromoform Toluene Chlorobenzene Ethylbenzene m&p Xylenes o-Xylene Styrene 1,1,2,2-Teti^chloroetiiane Observed Result ([ig/L) ND (10 U) ND(IOU) ND(IOU) ND (25 U) 27 53 100 42 ND (10 U) 67 64 53 51 ND (20 U) ND(IOU) 40 ND (10 U) Certified Value (^lg/L) 28.3 60.1 112 45 73.8 74.4 61.3 64.9 48.4 Acceptance Lirruts (l^g/L) ' 19.6-37.0 42.4 - 77.8 84.4-138 34.6 - 56.4 53.1-95.8 57.2 - 89.8 47.8 - 73.4 48.3-76.1 33.0-59.6 Comment Within confrol Within confrol Within confrol Within confrol Within confrol Within confrol Within confrol Within confrol Within confrol Note: 1. The PE sample was provided by Environmental Research Associates (Arvada, Colorado), Lot No. 577, Catalog No. PP-41. The PE sample included eleven other analytes that were not targeted for analysis. None of the results that were reported as non-detects in this table were present in the PE sample. • Page 9 304773 REFERENCES USEPA 1996. USEPA Region UData Validation (Juidancefor CLP/SOWOLM03.2. SOP HW-6, Rev. 11, June • PagetO 3 0 4 7 7 4 SOP NO. H«-6 Revision 18 Pac^ ^ ^ # ^^'''/^ _ / • _ / - ^ • x \ Leon^l2 2ar'.is. £.-vir=r,r.2nr2i Scientisz Tcxzc and Hazarzcus Wasre Secricr. BY I '^'^ALL'J^X. X^ L-A^^. Caorcs >'-frrcs. c.^.enisr Tcxic a.~.c Hazarccuc Wasre Secricn Datc: J^Cr^. J - h ^ l ^ Date / r -'/f^; / - I — / > ^ ^ . ' ^ . * - • * • > < -i/ 7< '- S r e i i c s Gcrazcur.is/ C.'^.enisr Tcxic 2nd Hazarcrius Wasre Secricr. Kevin .KutJiJi^-STsr Date: / / . ' / / ' « > ' „ ' ' Date: azirrc^iis Waste Secricn I ' Date:, ' / 7 r-7. Rotrerr F.unyo.n, C.'iiet Monircrir.c .".anaqeroenr Srancn 304775 STAltDrtjlD CPZHATT-iG ?HOCZ—-^vl Date: J a n u a r y 1392 R a v i s i c n : s PACKAGE CCMPLZrrrZSS A}JD tZlZ'.-ZRX-ElZZ D X SITZ: J done! Anemic J -•0 Data CCdciereness and Daliveracies 1-1 Have any rissinc daliveracies been received and added rc rr.a data pacXace? 1 1 ACTir:;: Call lab fcr expianaticn/resubsittal of any nissinc daliveracies. If lab cannot provide tham, note t^.e effacr cn review of t^.a package under t^.^ "Ccntract Prcbi£ns/Non-Co=piiance" sacticn cf reviewer narrative- V" 1.2 Was SMO CZZ c.nscXiisr includad -\zh package? : 1 __!. 2 - D C^'^-TP'^ ' ^ - r * * * - C ' ^ ' * . ^ , ' - i«-^-i *- • • • p 2.1 Is r.'-.e Karrcriva or Ccver L-attar Present? ^ ^'' — — 2.2 Are Case Nuiibar and/cr SAS nuzber contained ,• in t.^a Narrative or Ccver letter? r >-i ___ 1 n Data t^ai ;-J.,*.^-- r^^-a^^.t .-«- The fcllcvine checXlisr is divided i.ntc t.^ree parts. Part A is filled cut if tha data pacicaga contains any VOA analyses, .-art 3 fcr any EHA analyses and Fart C fcr PS3ticida/PC2s- Does r.'^is cackaoe conrainr > o VOA Data? V^. . -J BNA Data? L- Pesticiia/PCE data? X Acticn: ctr-clare ccrrssccndinc carts cf c.':ecKiist. SiAixL/AjMj -.-i,P«ATTII2 PP.OCZZimZ Date: Januar"/ 13 32 R e v i s i c n : £ YZS NO .S'/A - ° T r a : : ; ; P.er^r-.z ?.r:! --bcr^t-r-,- M'^ 'Ivg 1.1 Are t.^.a Traffic Report rorrs presenr fcr /^i X all samples? rtC.4...... _i r.c. ccr.ract lab fcr rsDiacesenr of nissinc or illegicie ccpies. 1.2 Do r.^.e Traffic Repcrrs cr Lab Harrrtive indicate any prccleas vith sample receipt, conditicn cf samples, analytical problems or special circursrancas affecting t.':E ., quality of t.^.a data? fA.i ACTTC!.': If any sample analyzed as a soil, other than TCLP, contains S0%-90* water, ail data should be flagged as esti-ated (J) . If a soil sampie other than TCIP contains more than 90\ varer, all data sncuid ba qualified as unusable (R) . ACTIC^r; If samples vere not iced upcn receipt at the laboratcr-/, flag ail posirive rssulrs "J"' and all Non- Detects '"JJ", ACTIC:!: If both VCA vials fcr a sampie have air bv:bbles.-cr the VOA vial analyzed had air bubbles, flag all positive results "J" and all non-detects "R". 304777 2 - STAiiDARD 0?ZPATIir3 PROCZZl.."^ D a t e : Januar-/ 19 92 R e v i s i c n : 8 YES HO N/A 2*0 H o l d i n r _ T i r « « 2.1 Have any VOA t e c h n i c a l holdi.-.g t i m e s . determined from d a t e cf c o l l e c r i c n t c d a t e of . a n a l y s i s , b e e n exceeded? r-^ If u n p r e s e r v e d , aqueous Eamoias m a i n t a i n e d a t 4*C vhich a r e t c be analyzed f c r a r o m a t i c hydrccarcons must be analyzed v i t h i n 7 days cf c o l l e c t i o n . If p r e s e r v e d v i t h .HCl (?.H<2') and s t o r e d a t 4*C, t h e n aqueous samcies must be a n a l y z e d v i r h i n 14 days cf c c l l e c r i c n . " If u n c e r t a i n a b o u t p r e s e r v a t i o n , c c n t a c t sampler t c d e t e r m i n e vnether c r n o t s a m p l e s v e r e p r e s e r v e d . The h o l d i n g t i m e fcr s o i l s i s 10 d a y s . T a b l e c"* U-.1J-:-.-. ' " ' - a vr.-^1 ,1-.; *.-«. (See T r a f f i c Report; Sample Sample Date Date Lab 2ate ID y.atrix ?reser-.*ed? Samcied Received Analyzed w o it* <i 00 ACTIc::: If technical holding times are exceeded, flag all positive results as estimated ("J") and sampie quanritaticn limits as estimated ("UJ")/ and document i: the narrative that holding times were exceeded. If analyses were done more t.han 14 days beyond holding tine, either cn the first analysis or upon rs-anaiysis, t.he reviewer r.ust use prcfessicnai judgement to deterr.ine the reliability of the data and the effects c: additicnal srorace on the sammle results. At a minimum., all results must'be q-ualif ied" "J" , but. the reviewer^may determine that ncn-detecr dara are unusable CR) . If holding times are exceeded by•more than 23 days, ail nc: detecr dara are unusable (R), JTAKDAI^D CPZPATI^IG P?.DCZZ*J?>Z Date: J a n u a r y IS32 R e v i s i c n : a YES NO N/A ^^ ' ' ' ~ r j l i r i i « , i r . .,,-| » ^..Z ':.T'-: -"^C^: . ^ T ^ . - - . 3.1 Are the VCA SMC Reccvery summaries (Form 11^ present for each cf tha folloving matricas: a. Lov Water rYj b. Low Scil r'y^ c. Med Soil X 3.2 Are all the VOA samples listed cn the apprcpriate System Monitoring Ccmpound Recovery summary fcr each ol the fcllcving matricas: a. Low Water b. Low Soil c. Med Scil ACTi:::: call lab fcr explanation/ resucmittals. If missing deliveracles are unavailable, document effect in data assessments, 3.3 Were outliers marked correctly virh an asrerisX? ACTIO": Circle all cutliers in red. ill LL - x^ J i _ X — 3.4 Was one cr more VOA system r.cnitcring comccund recovery outside of ccntract specifications for any sampie or r.ethcd NV^ blank? -^-^ If yes, were samples re-analyzed? Were r.erhcc blanks re-analyzed? 1 — JL 1 — - ^ 304779 - < - STAliuAR.D CPZPJkTI^o PROCZZ'JTLZ Date: Januar*/ 1292 Revision: s YES NO N/A ACTICN: If r e c e v e r i e s a r e > 101 b u t 1 or more compounds f a i l t o meer SOW s p e c i f i c a t i o n s : 1. All positi-.'B r e s u l t s are qualified as estimated (j) . 2. Flag a i l non-cetects as estimated detecticn limits ("UJ") vnere reccvery is less t.han the lever aocaprance limit. 3. If SMC recoveries are above ailcvaole levels, do not qualify non-detects. If any system monitoring compound reccvery is <1GI : 1. Flag a l l pcsiti'/e r e s u l t s as estimated ("J") . 2. Flaa a l l non-detects as unusable ("R"). Professional judgernenr should be used rc qualify data t h a t only have merhod blank SHC raccveries cur of specificaricn in bot.h criginal and re-anaiyses. ChecK rr.a i.-.tarnai standard areas. 3.5 Are there any transcrip-ricn/caicuiaticn errors betveen rav data and Fcrm II? ACTIO::: if large errors e x i s t , call lab fcr expianaticn/iresubmittal, .make any necessary corrections and note errors in the data assessment. A^ Matrix: C'-'Voe fr^.—. TTT^ 4.1 Is tha Matrix Soike/Hatrix Soike Duolicate Recovery form (Form III) presenr? X 304780 STAKDAR:; cpzpj^Ti^'a P R O C Z Z L ^ R Z Date: Januar-/ IS32 Revision: s YZS NO N/A 4.2 Were matrix spikes analyzed at the required frequency for eacc cf the folloving matricas: a. Low Water r'^^'' b. Low Soil rT^i c. Med Scil i_l )C ACTICN: If any matrix spike data are missing, rake the acricn specified i.n 3.2 above. 4.3 Hov many VOA spike recc'eries are outside QC limits?" O out cf >o O out cf ari 4.4 Hov many RPD's fcr matrix spike a.nd matrix spike duplicate recoveries are cutsida QC limits? O cur =f ^ / out c: /' ACTICN: .\'o acticn is taken based cn MS/MSD data alone. Hovever, using informad professional judgement, the MS/MSD results may be used in conjunction wir.h cr.her QC crireria rc determine the need frr~-qual if icaticn of the data. .0 Blanyts ^-crr Z^) 5.1 Is the Method Blank Summary (Form IV) , p r e s e n t ? r/vi o 00 5-2 Frequency of Analysis: fcr t h e a n a l y s i s of VOA TCL ccm.pouncs, has a reagent/r.ethod , H blank been analyzed fcr each SDG c r every 20 samples of similar matrix (lev water, low s o i l . .T.adium s o i l ) , vnichever is,more freouent? ill _ STANDA^vD CPZ?JiTi::C PROCZZL'^iZ Date: January 1=92 Revision: 8 YES NO N/A 5.3 Has a VGA method/instrument blank been analyzed at l e a s t once every tvelve hours for eacn concentraticn level and GC/HS system / usaa? r ri . ACTICN: If any mathed blank data are missinc, call lab fcr explanation/ resucmittal. If ner.hcd blanx data are not available. reject (R) ail associated positi'/e data. However, using professional judgement, t.he data reviewer may substituta field blank or trip blank data fcr missing method blank data. 5.4 Chrcmarograpn-y: review r.he blank raw data - chrcmarograms (RICs), quanr reports or data system printcuts and spectra. Is the c.hrcm.atcgraphic perfcrmance (baseline statiliry) fcr eacn instrumant accectable / for VOAs? " I£i ACTION': 'Jse professional judgement to determine r.ne erfect cn t.ha data. 5.0 Center;: NOTZ: "Water blanks", "drill blanks", and distilled vater blanks" are validated like any other sample, and are net used to qualify data. Co not confuse t.hem vit.h the ether QC blanks iliscussed below. 6.1 Do any r.erhcd/instrumanr/reagent blanks have positive results (TCL and/or TIC) for VOAs? When applied as describad balov, t.he contaminant concentration in these blanks are multiplied by the sample diluticn factor and w corrected fcr % m.oistura vnen necessary. J x -—^ 6.2 Do anv field/trip/rinse blanks have positive w VOA results (TCL and/or TIC)? -t—- - ^ Prepare a list cf tha samples associated wit.h eacn =: the contaminated blanks. (Attacn a 304782 seoarate s.neet. ) STANDARD OPERATING PROCZZLTJ: Date: J a n u a r y 1332 R e v i s i o n : a YES NO H/A NOTZ: All field blank results associated to a particular group of samcies (may exceed one per case) must be used to qualify data. Trip blanks are used to qualify only those samples with which they were shippad and are not required fcr non-aqueous matricas. Blanks mav not be cualified because of contaminaticn in another blank. Field Blanks i Trip Blanks must be q-ualified fcr system mcnitcrir.g compound, i.nstr-ima.nt performance criteria, spectral or calibration QC probleias. ACTICN: Follcv rhe direcmions in the table belov- to qualify TCL results due tc contaminaticn. Use the largest value from all the associated blanks. If any blanks are crossly contaminated, all associated data should be qualified as unusaole (R). Samcle cenc > CRQL Samoie cone < CRQL Sampie cone :> CRQL but < iQx blank & <iox blank value i >10x bla.nk value value y.etnviene Chloride Flaa sar.mle result Reoort CRQL i No q-uaiificaticn Acetcne virh a "U; qualify "U" is needed Toluene 2-2uranone samole cone > CRQL Sample cone < CRQL i Sample cone > CRQL but" < 5x blank is < 5x blank value value 6 > 5x blank value Other Flag samcle r e s u l t Report CRQL i No q-uaiification Ccntam- wirh a "U" qualify "U" is neeaea ;anrs NOTZ: Analvtes crualified "U" for blank ccnraminaricn are s r i l i ccns'idered as "hirs" vhen q-ual-ifying for caiibraricn c r i r a r i a . 304783 ACTICN. 6.3 ACTICN: 7 . 0 7 . 2 / . 2 STANDARD CPEPJ^TING PROCZZURZ Date: J a n u a r y 1332 R e v i s i c n : a YZS NO N/A s ! L : : ^ T^^''"^^^' - ^ ^ ^ c o n c e n t r a t i o n in t h e t h e ^ ; o . i ^ ^ " ^ ^"'^" - ^ ° ^ — ^ ^ ^"^ c o n c a n r r a t i o n i n ™„ ? 5 t t n t a m i n a t e d a s s o c i a t e d blank, f l a g r h e samoie data "O" '•'•m,•,^..^^ ^^ ^ sample data "R" (unusable). Are rhere fiald/rinse/eouicment blanks associarad virh every sampie? _^^ )<^ For low level samples, note in data assessment t.hat tnere i s no associatad fiald/rinse/eouipment blank. Si^ ! ° ' ~ : " * ^^=P-^s ^aken from a dri.-J:ing water t a p do not have associated f i e l d blanks. Q^/r,^ ' - ^ err ?<>w—r?r-P rv«ck f^-^^^n 7.1 Are tha GC/MS instrument Performance Check ^ ? ? r f , ( ^ ° — '^) present f c r Srcmoflucrccanzene , (BFE)? P ^ ^ Are r.he enhanced bar grap.h specrrum and mass/charce (m/z; l i s t i n c fcr tha EFB . provided f-r eacn rvaive nour snift? J L Has an i.nstrum.enr perfcrmance compound been analyzed fcr every t v e l v e hours cf sampie w a n a l y s i s per instrumant? J x . 304784 STA.NDARD CPZPJ^TING PROCZZUAZ Date: J a n u a r y 1332 R e v i s i o n : a YES NO N/A ACTICN: List date, rima, instrument ID, and sampie analysis for vhich no associated GC/KS tuning data, are available.- DATZ TIHZ INSTT^L'^TZNT SAHPLZ NUHBZRS ACTICN: If lab cannot provide missing data, reject ("R") all data generated curside an acceprable rvaive hour calibration inter%'ai. 7.4 Have rha icn abundances been normalized rc r./z 9 5? JL. ACTICN: If r.ass assicr.m.er.r is in errcr, qualify all associared dara as unusable (R). 7.5 Have r.he icn abundance criteria been met fcr / each i.nstrumenr used? r/^ • ACTICN: Lisr all drta vhich do net r.eet icn abundance criteria (attach a separare sheer). ACTICN: If icn abundance criteria are not met, rhe Regicn II TPO must be notified. 7.5 Are rhere any rranscripricn/caicularicn errors berveen r.ass lists and Form Vs? (Check at least tvo values but if errors are fcund. check ^ more.) Lol 304785 ST^\DAR.u CrZPJi.TING PP.QCZZL.-.Z Date: January 1332 R e v i s i o n : a YES NO N/A 7.7 Have r h e a p p r o p r i a t e number of s i g n i f i c a n t f i g u r e s ( t v o ) been r e p o r t e d ? ' r/^ ACnCN: I f l a r g e e r r o r s e x i s t , c a l l l a b f o r e x p l a n a t i c n / r e s u c m i t t a l , make • n e c e s s a r y c c r r e c r i c n s and document e f f e c t i n data assessmenms. Are t.he s p e c r r a of rhe mass c a l i b r a t i o n compound a c c e p r a b l e ? ACTICN: Use p r o f e s s i o n a l judgement t o d e t e r m i n e v h e t h e r a s s o c i a t e d d a t a s h o u l d be accepred, q u a l i f i e d , o r r e j e c t e d - 8.0 Tares'" '-——-'•--J T .• c- i'^^*^ j___iw.-oe 8.1 Are rhe O r g a n i c Analysis Data S h e e r s (Form I VOA) presenr vir.h r e q u i r e d header i n f c r m a r i c n on each page, t z r eacn cf rha f c l l c v i n g : X a. Sammies and/cr fracricns as acorcmriare X x b. Matrix spikes and matrix spike duplicares I 1 -2L c. Blanks JL a.2 Are rhe voA Reconsrfucrad Icn Chrcmarograms, t.he mass spectra fcr the identified ccmpeunds, and the data system printcuts (Quant Raports) included in t.he saromie cackaae fcr each of' t.he following? a. Samples and/or fracticns as apprcpriate JX b. Matrix spikes and marrix spike -y dumlicares (Mass specrra not required) l H c. Blanks !XL ACTIC:.'; If anv data are missing, rake acticn scecifisd in 3.2 above.' 304786 SZXllZXRu CPZilATING PROCZZL'RZ Date: J a n u a r y 1332 R e v i s i o n : s YES NO N/A X 8.3 Are the resocnse facters shovn in the Quant Repcrt? r i X 8.4 Is Chromatographic performance acceptable with respect t c : Baseline srability? 'V'' Resolution? 1 ^ Peak shape? Full-scale graph (attenuation)? ''X.i Other: r i . ACTIIN: Use professional judgement to determine the acceptability of the data. 3.5 Are tha lab-generated standard mass specrra of tha idenrifiad VOA ccm.pcuncs presenr fcr eacn sampie? ACTICN: If any mass specrra are missing, take acricn specified in 3.2 above. If lab does not generate their own standard spectra, make note in "Contracr Problems/Non-compliance". 3.6 Is the RRT z i each reported compound vithin 0.0 5 FJIT units of tha stahdard RRT in the continuing calibration? B.7 Are ail ions present i.n the standard m.ass specrrur. ar a' reiarive i.nrensiry grearer than i z \ also presenr in t.he sampie mass specrrum? i2i _ . _ rXi J X _ 3047 87 s i.M.^Ljjyj\u OPZ^ATZNG PROCZ-.L."-i Date: J a n u a r y 13 92 Revision: S YZS NO N/A 8.8 Do sample and s t a n d a r d r e l a t i v e i o n i n t e n s i r i a s agree v i r h i n 2 0 t ? rX^ ACTICN: Use p r o f e s s i o n a l judgernenr t o determine a c c c p r a b i l i t y of d a t a . If i t i s determined t h a t i n c o r r e c t i d e n r i f i c a r i c n s w e r e made, a i l suc.n dara snouid be r e i e c r e d (R) , flagged "N" (presumpri'.-e e v i d e n c e of t h e presence cf t h e ccmpound) c r changed to net d e t e c t e d ( U ) " a t t h e c a l c u l a t e d d e t e c t i o n l i m i t . In order ro be p o s i t i v e l y i d e n t i f i e d , the data must ccmply w i r h t h e c r i t e r i a l i s t e d i n 8 . 6 , 8 . 7 , and 8 . 8 . ACTICN: When sampie c a r r y - o v e r i s a p o s s i b i l i t y , p r c f e s s i c n a i judgement should be used t o d e t e r m i n e if instrument c r e s s - c o n t a m i r . a t i c n has affected any p o s i r i v e compound i d e n r i f i c a r i c n . W . W i l ^ . 1 = . . • . . . . . . . . ^ . , 9 . 1 Are a l l T a n r a r i v e l y I d e n t i f i e d Compound Forms niQ (Form I P a r t 5) p r e s e n r : and do l i s r e d TICs i y \ i n c l u d e scan number or r e t e n t i o n t i m e , / ^ e s t i m a t e d c c n c e n t r a t i c n and "JN" c u a l i f i a r ? 'X'' —b_ 9.2 Are t h e m.ass s p e c t r a f c r t h e t e n t a t i v e l y i d e r i t i f i e o compounds and a s s o c i a t e d " b e s r m.arch" s p e c r r a i n c l u d e d ir. t h e sampie p a c k a g e f c r eacn cf t h e f o l l o w i n g : a. Samples a n d / c r f r a c t i o n s as a p p r c p r i a t e rXv _)ti. b . Blanks / m ) L ACTIO.N: If any TIC data arc r.issing, take ^ acticn specified in 3.2 above. -504788 UP- nu.'^ Iff re fuiillJ STANDARD OPERATING PR0CZZU:RZ Date: January' 1 = 32 Revision: s YES NO N/A 9.3 Are any TCL compounds (from any fraction) listed as TIC compounds (example: 1,2- dimerhyibenzene is xviene- a VOA TCL analyte - -nd should'not ba reporrad as a TIC)? I _ l _ ^ lOP ACTIO::: Flag vith "?." any TCL compound listed as a TIC. 9.4 Are a l l icns present i.-. the reference mass specrrum vir.h a reiarive intensify grearer than 101 also present in the samoie mass , spectr-cm? j__T_ A iU'/< 9.5 Do TIC and "besr march" srandard relative ion I.ntensities agree vithin 2 0*? f i )C ^l- ACTICN: Use prcfessicnai judgem.ent to determine acceptabilit*/ cf TIC identificatiens. If i t i s d e t e m n e d that an i.nccrrect idenrificarien vas made, c.nange 1 denrifleaner, tc "unknown" cr tc some less scecifie identificaticn (example: "C3 substitutad benzene") as apprcpriate. Also, vhen a ccmpound i s not fcund in any blank, but is detected in a sample and i-3_ a suspected a r t i f a c t of a com:mcn laboratory contaminant, the result should be q-ualifiad as " unusable (R) . ( i . e . Common Lab Contaminants: 00^ (M/E 44), Siloxanes (M/E 73) Hexane, Aldol Condensatien Products, Solvent Preservatives, and related by produces - see Funcricnal Guidelines for more guidance). 304789 STA2CDAR.D CRZPATINC PROCZZLIIZ D a t e : J a n u a r y 1332 R e v i s i o n : a YES UO :;/A 10.1 Are there any transoripricn/calculaticn errers in Fcrm I results? Check at least f-o positi-.-e values. Verify that the correct internal stancarc, quantitation icn, and RR.F vare used tc calculate Form I result. Were any errers found? ^y^ 10.2 Are the CRQLs adjusted te reflect sample ^ diluticns and, fer soils, sample moisture? r r-i ACTICN: If errers are large, call lab for explanaticn/resutmittal, make any necessary corrections and note errers under "Conclusions". ACTICN: When a sam.ple is analyzed at more than cr.e diluticn, t.he ievest CRQLs are used (unless a QC exceedanca dictates rhe use ef the higher CRQL data from t.ha diluted sampia analysis). Replace ccncenrraricns thar exceed r.he caiibraricn range i.n r.he original analysis by crossing cut t.he "Z" and its associated value on t.he criginal Form I and substituting t.he data from t.he analysis of the diluted sample. Specify which Form I is to be used, then draw a red "X" acrcss ^le entire page cf all Form I's that should not be used, including any in t.he sumj=ary package. 11.0 standards Z2t?. <GC/MS^ li.^ /%re rha Reconsrrucred Ien Chrcmarograms, 1 1 1 ' and dara sysrem prinrcurs (Quanr. Reports) presenr for i n i t i a l and ccnri.nuing . caiibraricn? I ^ ACTION: If any caiibraricn standard dara are ...iss^..-, --.-^e a syec i.. 304790 ' 3 . 2 a b o v e . .SU'i/^u STANDARD 0?Z?J».TING PROCZZL'RZ Date: Januar-/ 1=32 R e v i s i o n : 3 YES NO N/A 12.0 GC/y^T--'---'1 --^T ,'V-,....: rr..,..— »rT-\ 12.1 Are the I.nitial Calibraticn Forms (Form VI) present and complete for tha volatile fraction at concentrations of 10, 20, 50, 100, 200 ug/17 Are thare seoarate calibraticns for low water/med soils ^ and low soil samoles? r>j If any calibration standard forms are missing, rake acticn specifiad in 3.2 above. 12.2 Were ail lew level soil standards, blanks and samoles analvzed bv heated curce? rV3 ACTION: If lev level soil samples were not heated during purga, qualify positive hits "J" and non-detects — <; "TJtt 12.3 Are response factors stable fcr VOA's over the cencantration range of the calibraticn (^Relative standard Deviation (IRSD) <30.0l )? r T X ACTICN: Circia ail cutliars in red. NOTZ: Although 11 VOA ccm.pcunc3 have a minimum RRF and no maximum iRSD, the technical critaria are tha same fcr ail analytes- ACTICN: If \RSD > 3 0.01, qualify associated positive results for that analyte "J" and ncn-detects using professi_onal judgement. When RSD > 901, flag all non-detects fcr that analyte R (unusable) . NOTZ: Analytas previously qualified "U" fcr blank contamination are still considered as "hits" when qualifying fcr initial calibraticn critaria. 12.4 Are the RRFs above 0.05? Acticn: Circia all outliers in red. Acticn: If any FIHF are < 0.05, qualify associated non-detects (R) and- flag associated pcsitivj data as estimated (J). - 16 - 304792 STANDARD CPZRATING PROCZZL'RZ Data: J a n u a r y 13 32 Revision: 8 YEI NO N/A r% 12.5 Are there any transcription/calculaticn errors in tha reporting of averace resocnse factors (RRF) cr IRSD? (Check at least 2 values, but if errors are fcund, check more.) 1 3 . 0 Q Z / y I " - - - • - , 1 / u _ , . i - . i 1^ r - ^ — <»—' T W C I l i r - r - « - i l » » . . - ^ . . - i • - - - « i « r • • • • ' . < • • • - ' 13-1 Are the Continuing Calibraticn Forms (Form VII) present and ccmmlete fcr the volatile fraction? " lA^ 13.2 Has a continuing calibraticn standard baen analyzed fcr every t'-elve hours of sample analysis per i.nstrument? T^^T • ___ ACTICN: List balov all sample analyses that vere not virhin r--alve hours of tha previcus continuing calibration analvsis. ACTICN: If any forms are missing or no continuing calibration standard has been analyzed vir.hin rvaive hours of every sample analysis, call lab fcr expianaticn/resubmittal. If continuing calibraticn data are not available, flag all associated sample data as unusable ("R"). 13.3 Do any volatile compounds have a 1 Difference (1 D) betveen rhe inirial and conti.nuing .. RRF which exceeds the + 251 critaria? /^ i—- ACTICN: Circle ail cutliers in red. ACTION: Qualify both positive results and non-derects fcr t.he outliar cempeund(s) as estimared. When % D is above 901, reject all .-.cn-derecrs fcr rhat analvte (R) unusable. 304793 Date: January 1332 R e v i s i c n : a YES NO N/A 13.4 Do any v o l a t i l e compounds have a RRT <o.05? ' ^ ACTICN: C i r c l e a i l c u t l i e r s i n r e d . ACTICN: I f t h e RPJ" <0.05, q u a l i f y a s s o c i a t e d n o n - d e t e c r s as u n u s a b l e (R) and " J " a s s o c i a r e a p c s i t i ' / e v a l u e s . 13.5 Are t . h e r e any t r a n s c r i p t i c n / c a l c u l a t i c n e r r e r s i n t.he repcrtir.g of a v e r a g e r e s p o n s e f a c t e r s (RRF) e r ' ^ d i f f e r e n c e (ID) b e t v e e n i n i t i a l and continuing RRTs? (Check a t l e a s t t v o v a l u e s b u t i f e r r o r s a r e f c u n d , ^r check r . o r e . ) L f l . ACTICN: Circle errors in red. ACTICN: If errors are large, c a l l lab for explanarien/resubmirtai. .make any necessary ccrrecricns and nore errors under "Conclusions". J . . , • . - — ^ — — . . . . . — ^ p . . 14.1 Are the i.nternal standard areas (Form VIII) of every sample and blank vithin t.he upper and lower limits (-501 to -K 1001) for each ^ continuing calibration? llL. ACTICN: List all t.he cutliers below. Samoie f I.-:ternai Std Area Lower Limit Upper Limit (Attacn addirienai sheers if necessary.) STA:;DARD CPZPJ^TINC PROCZZLTZ D a t e : J a n u a r y 1392 R e v i s i o n : s ~ ~ ~ " ^ ^ ' YES NO N/A ACTICN: 1. If the i.nternal standard area count is outside the upper or lower linit, flag with "J" all positive results quantitated with this internal standard. 2- .Non-detects associated vith IS area counts > 1001 Ehould not be qualified. 3. If IS area is belov the lover limit (< 501), qualify all associated non- detects (U values) "J". If extremely lov area counts are reported, (< 251) or if perfcrrance exhibits a major abrupt drop off, flag all associated non-detects as unusable ("R"). 14.2 Are the retention times of the intemal standards vit.hin 3 0 seconds of the associated calibraticn standard? ACTION': Professional judgement should be used tc qualify data if the retention times differ by r.ore than 30 saccncs. iX _ 15.0 15.1 Were any field duplicates submittad fer VOA anaiysis? _ ACTION: Compare the reported results fcr field duplicates and calculate the reiati-.'e percenr difference. ACTICN: Any c r e s s variaticn betveen duplicate results r.ust be addressed in t.he reviewer narrative. However, if large differences exist, identification of field duplicates should be confirmed by contacting the samoler. 1^ X - 304794 QA/QC Review of Total Organic Carbon (TOC) Data for Pace Analytical SDG: 98045 May 19, 1998 Holding Times: Samples were analyzed within holding times. Initial and Continuing Calibration VeriFication: TOC had percent recoveries within control limits (85-115%). Blanks: The method blank reported TOC as not detected. Spike Sample Recovery: TOC (94%) had a percent recovery within control limits (75-125%) for soil spike sample. Duplicates: TOC (8%) had a relative percent difference below the allowable maximum (35%) for soil duplicate sample. Laboratorv Control Sample: TOC (102%) had a percent recovery within control limits for the soil LCS. 3 0 4 7 9 5 • SDG No. A98287 VOC checklist 304796 /o/is^ MEMORANDUM To: Norma Eichlin From: B.F. Cockcroft Date: January 18, 1999 Re: Island Chemical Corporation - Validation of Method 8260 Analytical Data M/H Project No. 12.0805380.001.004 Fifty-six groundwater samples, trip blanks, and field blanks were analyzed for up to 15 volatile organic compounds (VOCs) following EPA Method 8260B. The analyses were performed by a mobile laboratory operated by McLaren/Hart. The analytical results were validated using relevant criteria from EPA Region II guidance. The EPA Region II checklists were used to review the data but were not completed as part of this assessment. The following information was used to validate the analytical results: Sample Hold Time before Analysis GC/MS Tuning Criteria Initial and Continuing Calibration Surrogate Recoveries Internal Standards Matrix Spike/Matrix Spike Duplicate (MS/MSD) analyses Laboratory Control Sample PE Sample Results Method Blank Contamination Rinsate Blank Contamination Compound Identification Chromatogram Quality Calculations. A holding time summary table (Table 1) is attached to this memorandum. 1.) Sample Holding Time Before Extraction and Analysis: The technical holding times for VOC analyses by Method 8260B is 14 days from sample collection to analysis. Review of Table 1 shows that all holding times were met. 2.) GC/MS Tuning Criteria: Bromofluorobenzene (BFB) was run every 12 hours of sample analysis. The BFB ion abundance criteria were met for all analyses. •— ^mw """ M E M O R A N D U M (Continued) 3.) Initial and Continuing Calibration: The instrument was initially calibrated using a six point calibration standard. The relative standard deviations (RSDs) of each analyte in the multi- concentration calibration are assessed. In the continuing calibration, the percent difference (%D) of the continuing calibration concentration and the average of the initial multipoint calibration is assessed. RRF values must be greater than 0.05, RSD values less than 30%, and %D values less than 25%, for the analytes to be in compliance. The RRFs, RSDs and %D values were within control and for the following: Sample Group A98278 • Initial Calibration, (ISLVOA.M) and • Continuing Calibrations 10/07/98, 10/08/98, 10/09/98, 10/1/98, 10/12/98, and 10/13/98. No qualifications were required for these initial or continuing calibrations. Sample Group A98287 • Initial Calibration (ISLVOA70.M): acetone (58%) and methylene chloride (34%) had %RSD above the allowable maximum (30%). Qualifications: Positive results for these compounds should be considered estimates (J) in associated samples. • Continuing Calibrations: On 10/20/98, chloromethane (27%) and methylene chloride (28%) had %D above the allowable maximum (25%). Acetone (43%) and methylene chloride (26%) had %D above the allowable maximum (25%) on 10/21/98. Qualifications: Positive results for these compounds should be considered estimates (J) in associated samples. 4.) Surrogate Recoveries: Surrogates measure the ability of the laboratory to extract the targeted analytes by evaluatmg the recovery of indicator compounds which are structurally similar to the targeted analytes as indicators for all of the analytes. For these analyses, three surrogates were used (l,2-dichloroethane-d4, toluene-d8, and bromoflourobenzene). Control limits were 75-125% for the water samples. All surrogate recoveries were within the control limits, except for the following sample: • VBLKIO (10/21/98): l,2-dichloroethane-d4 (115%) No qualification was required for the non-detect results of this sample because the one SMC was above the upper control limit. 5.) Internal Standards: Internal standards are added to all sample, blank calibrations and are used to quantify the analytes. For these analyses, 3 internal standards (bromochloromethane, 1,4-difluorobenzene, and chlorobenzene-d5) were used. All internal standard retention times and areas were within the control limits. ESS^a?^ G:\clienu\l 2080S380\Memo 1 -12-99.wpd ., Inc. JX. M E M O R A N D U M (Continued) 6.) MS/MSD Analyses: Three MS/MSD analyses were performed for the water samples (a frequency of one per 20 samples). The samples were spiked with a mixture of three VOCs (1,1-dichloroethane, toluene, and chlorobenzene). Accuracy was measured by the spike recovery, and precision was measured by the relative percent difference between the MS and MSD results. All recoveries and RPDs were within the control limits. 7.) LCS Analysis: An LCS (blank spike) was also performed with a mixture of three VOCs (1,1-dichloroethane, toluene, and chlorobenzene). The spike recoveries were within the control limits. 8.) PE Results: A PE sample was not analyzed with these samples. However, five replicate samples were shipped to an independent laboratory for confirmatory analysis. The results are summarized in Table 2. All observed results correlate well and within acceptable limits. 9.) Analysis Sequence: The laboratory properly performed an initial calibration, sample analyses, and continuing calibration as described by the method. 10.) Method Blank Contamination: A method blank measures the potential for false-positive results introduced by internal laboratory contamination. A total of 10 aqueous method blanks were prepared. None of the method blanks contained detectable analytes. 11.) Field Blank Contamination: The field blank (FB) measures the potendal for false-positive results introduced by improper field decontamination procedures of sampling equipment. One field blank was included with the samples analyzed on 10/12/98. Acetone was detected in the field blank (at a concentration lOX greater than the detected sample concentration) and attributed to the decontamination procedures because acetone was not detected in the method blank and the groundwater samples preceding (3) and following (1) the field blank. Trip Blank Contamination: The trip blank (TB) measures the potential for cross- contamination during sample storage and shipment. Because these samples were hand- delivered to the mobile laboratory, trip blanks were not required. However, three trip blanks were included with this package. Target analytes were not detected in the 10/09/98 and the 10/13/98 trip blanks. Acetone was detected in the 10/12/98 trip blank and attributed to instrument carryover from the 10/12/98 field blank. 13.) Compound Identification: Verification of idendfication of VOC analytes analyzed using a GC/MS is based upon the relative retention time compared to the internal standard and ion spectra match. All positive results met RRT and ion spectra criteria. —"'-^ ESS'^iE' JK M E M O R A N D U M (Continued) 14.) Chromatogram Quality: The quality of VOC chromatograms is evaluated to determine whether there are any interfering unknowns present which prevent the identification of the targeted analytes. All chromatograms were of acceptable quality. 15.) Calculations: The reported analyte concentrations and any internal QC calculations were verified for their accuracy. All checked calculations were acceptable within rounding errors. 16.) Other QC: The following samples required dilutions due to presence of the respective target analytes outside of the initial calibration range: * MW-2 - Chloroform - 5X * FB101198 - Acetone - lOOX * GWPP29A Waste 2 - Acetone - No dilution was completed due to insufficient sample volume. The laboratory reflected these dilutions by adjusting the sample volumes on the respective Form I, instead of reporting them in the dilution factor field. The appropriate non-detects and positive results to report were identified by the reviewer on the affected Form Is. Data Limitation Overview The VOC analysis of the groundwater samples from the Island Chemical site showed compliance with the QC requirements of the method and all data are valid and acceptable, with qualifications applied and other actions as summarized below: MW-2 and MW-2DL: Report the non-detect results from the undiluted analysis, and the chloroform result from the diluted analysis as the sample result. FB101198 and FB101198DL: Report the non-detect results from the undiluted analysis, and the acetone result from the diluted analysis as the sample result. GWPP29A Waste 2: Report the non-detect and estimated (J) detected results from the undiluted analysis. Report the acetone result as estimated (J) and exceeding the initial calibration range (E). ^ , ^ ^ , „ Beth F. Cockcroft Supervising Engineer McLaren/Hart, Inc. Two North Shore Center, Suite 100 Pittsburgh, PA 15212-5838 (412) 395-1400 Fax: (412)395-1410 r u V l Hartr~ 304800 , Inc. JK TABLE 1 SAMPLE PREPARATION AND ANALYSIS SUMMARY VOA ANALYSES - SDG A98287 ISLAND CHEMICAL CORPORATION Client Sample ID CHARLIEtfl CHARUEffZ GWPP37(45-49) VIPA#1 VIPA#2 SOURCE WATER GWPP37 WASTE GWPP37(80-84) GWPP37(35-39) GWPP37(70-74) MW-2 GWPP37(97-107) MW-7 G W P P 2 9 A ( 150-154) G W P P 2 9 A ( 5 0 - 5 4 ) G W P P 2 9 A ( 9 5 - 9 9 ) TBI 00998 GWPP29A W A S T E I GWPP29A WASTE2 GWPP29A WASTE3 GWPP29A(137-147) GWPP27A(84-87) F B 1 0 n 9 8 T B 1 0 n 9 8 GWPP27A(95-991 FB101198DL GWPP27A( 110-120) GWPP27A WASTEI GWPP27A WASTE2 TB101398 Lab Sampia 10 A9827801 A9827802 A9828002 A9828004 A9828005 A9828006 A9828007 A9828008 A9828001 A9828003 A9828101 A9828102 A9828103 A9828104 A9828105 A2821 A9828202 A9828301 A9a28302 A9828303 A9828401 A9828402 A9828403 A9828404 A9828501 28403DL A9828601 A9828602 A9828603 A9828604 Matrix Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Data Coflacted 10/5/98 10/5/98 10/7/98 10/7/98 10/7/98 10/7/98 10/7/98 10/7/98 10/7/98 10/7/98 10/8/98 10/8/98 10/8/98 10/8/98 10/8/98 10/9/98 10/9/98 10/10/98 10/10/98 10/10/98 10/11/98 10/11/98 10/11/98 10/11/98 10/12/98 10/12/98 10/13/98 10/13/98 10/13/98 10/13/98 Data Rec'd a t U b 10/5/98 10/S/98 10/7/98 10/7/98 10/7/98 10/7/98 10/7/98 10/7/98 10/7/98 10/7/98 10/8/98 10/8/98 10/8/98 10/8/98 10/8/98 10/9/98 10/9/98 10/10/98 10/10/98 10/10/98 10/11/98 10/11/98 10/11/98 10/11/98 10/12/98 10/12/98 10/13/98 10/13/98 10/13/98 10/13/98 HoUmg Tima 10/19/98 10/19/98 10/21/98 10/21/98 10/21/98 10/21/98 10/21/98 10/21/98 10/21/98 10/21/98 10/22/98 10/22/98 10/22/98 10/22/98 10/22/98 10/23/98 10/23/98 10/24/98 10/24/98 10/24/98 10/25/98 10/25/98 10/25/98 10/25/98 10/26/98 10/26/98 10/27/98 10/27/98 10/27/98 10/27/98 1 Data Extractad NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA Data Analyzed 10/6/98 10/6/98 10/7/98 10/7/88 10/7/98 10/7/98 10/7/98 10/7/98 10/8/98 10/8/98 10/8/98 10/8/98 10/8/98 10/8/98 10/8/98 10/9/98 10/9/98 10/12/98 10/12/98 10/12/98 10/12/98 10/12/98 10/12/98 10/12/98 10/12/98 10/12/98 10/13/98 10/13/98 10/13/98 10/13/98 C:\cIicnuU20805380\TABLEIPGE.wpd 304801 TABLE 1 (continued) SAMPLE PREPARATION AND ANALYSIS SUMMARY VOA ANALYSES - SDG A98278 ISLAND CHEMICAL CORPORATION CQent Sampia 10 MW-11 PRELIM GWPP36(97-107) MW-14 P-1 ABOVE P-1 BELOW P-1 TOTAL MW-12 WASTEI MW-14 WASTEI MW-14 WASTE2 FAIR PLAINS<(9 GWPP36 WASTE GWPP36(197-207) GWPP36(82-85) MW-3 MW-11 MW-13 MW-11 WASTE MW-13 WASTE MW-2 GWPP37(124-134) GWPP36(20-24) GWPP36(50-54) GWPP36(82-85) GWPP36(75-79) MW-1 2 MW-2DL Lab Sampia ID A9829001 A9829003 A9829304 A9829301 A9829302 A9829303 A9829002 A9828702 A9828703 A9828701 A9828902 A2904 A9828901 A9828801 A9829403 A9829404 A9829401 A9829402 A9829405 A9828802 A9828803 A9828804 A9828805 A2886 A9829406 29405DL Matrix Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Data CoHactad 10/17/98 10/17/98 10/18/98 10/18/98 10/18/98 10/18/98 10/18/98 10/14/98 10/14/98 10/14/98 10/14/98 10/17/98 10/16/98 10/15/98 10/20/98 10/20/98 10/20/98 10/20/98 10/20/98 10/15/98 10/15/98 10/15/98 10/15/98 10/15/98 10/19/98 10/20/98 Data Rec'd at Lab 10/17/98 10/17/98 10/18/98 10/18/98 10/18/98 10/18/98 10/18/98 10/14/98 10/14/98 10/14/98 10/14/98 10/17/98 10/16/98 10/15/98 10/20/98 10/20/98 10/20/98 10/20/98 10/20/98 10/15/98 10/15/98 10/15/98 10/15/98 10/15/98 10/19/98 10/20/98 Holding TIma 10/31/98 10/31/98 11/1/98 11/1/98 11/1/98 11/1/98 11/1/98 10/28/98 10/28/98 10/28/98 10/28/98 10/31/98 10/30/98 10/29/98 11/3/98 11/3/98 11/3/98 11/3/98 11/3/98 10/29/98 10/29/98 10/29/98 10/29/98 10/29/98 11/2/98 11/3/98 Data Extractad NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA Date Analyzad 10/20/98 10/20/98 10/20/98 10/20/98 10/20/98 10/20/98 10/20/98 10/20/98 10/20/98 10/20/98 10/20/98 10/20/98 10/20/98 10/20/98 10/21/98 10/21/98 10/21/98 10/21/98 10/21/98 10/21/98 10/21/98. 10/21/98 10/21/98 10/21/98 10/21/98 10/22/98 G:\clienu\ 1208053SO\TABLE I PGE.wpd 304802 TABLE 2 CONFIRMATORY SAMPLE ANALYSIS SUMMARY (^) SDG A98278 AND A98287 - VOA ANALYSES ISLAND CHEMICAL CORPORATION Client Sample ID MW-2 MW-11 Fairplaines #9 GWPP36 (82-85) GWPP36 (124-134) Trip Blank 102098 Compound'^' Chloroform Acetone Toluene Xylene (totel) Acetone ND ND ND McLaren/Hart Analytical Results 150 10U 5U 5U 10U 5 U - 1 0 U 5 U - 1 0 U ND PACE'''Analytical Results 125 10.3 A11(^' 15.4 A l l 5 U - 1 0 U 5 U - 1 0 U 5 U - 1 0 U NOTES: 1) All concentration are presented in ^g/L or parts per billion. 2) Samples analyzed for 15 target compounds following EPA Method 8620, only compounds detected in the samples at concentrations above the quantitation/reporting limit are listed. ND indicates that none of the 15 compounds were detected. 3) PACE Analytical Services, Inc., St. Rose, Louisiana. ' 4) Compound analyzed, but not detected; value represents the minimum quantitation limit. 5) All indicates analyte is a common solvent. Its presence in field samples may be an artifact of sample collection, transport, lab storage or analysis. G:\clicn ts'.120805380\tablc2.wpd E S S ' ^ ^ " 304803 O recycled paper STANDARD OPERATING PROCEDURE US EPA Region II Datei October 1995 Method: CLP/SOW 0LM03.1 SOP HW-6, Rev. 10 PACKAOE COMPLETENESS AND DELIVERABLES October 1998 CASE NUMBERt Groups A98278 and A98287 LABORATORY! M / H - S2C2 Inc. SITE NAME: Island Chemical SDG Number (a): A98278 and A98287 1.0 Chain of Cufltodv and SnmpllncT Trip Reports 1.1 Are the Traffic Reports/Chain-of-Custody Records present for all samples? ACTION: If no, contact lab for replacement of missing or illegible copies. li^ 1.2 Is the Sampling Trip Report present for all >• samples and all fractions? [ 1 ACTION: If no, contact either RSCC or the prime contractor for this information. 2.0 Data Completeneaa and Deliverables 2.1 Have any missing deliverables been received and added to the data package? NOTE: The lab is required to submit data for only two analyses, for each fraction. (i.e., the original sample and one dilution, or, from the moat concentrated dilution analyzed and one further dilution.) ACTION: Call lab for an explanation or resubmittal of any missing deliverables. If lab cannot provide them, note the effect on review of the package under the Contract Non- compliance section of the Data Assessment and the Organic Regional Data Asseasment summary. y 2.2 Was CLASS CCS checklist included with package? f 1 ^ A y 2.3 Are there any discrepancies between the Traffic Reports/Chain-of-Custody Records, Sampling Report and Sample Tags? ACTION: If yes, contract the laboratory for an explanation or resubmittal of any missing ««>,onA deliverables. 304804 -1 - STANDARD OPERATINQ PROCEDURE ua EPA Region II Mathodj CLP/SOW 0LM03.1 Date: Oatober 199! SOP HW-6, Rev. H 3.0 Cover Latter SDG Narrative 3.1 la the Narrative or Cover Letter Present? 3.2 Are Case Number and/or SAS number contained in the Narrative or Cover letter? 3.3 Does the narrative contain the following information: VOA: description of trap and columns used during sample analyses? BNA: description of columns used during sample analyses? Pest: description of columns used during sample analyses? NOTE: As per section 6.23.3.1 SOW/p. D-Il/Pest, Packed columns are not permitted. 3.4 Does the narrative, VOA and BNA sections, contain a list of all TICs identified as alkanea and their estimated concentrations? 3.5 Does the narrative contain a record of all cooler temperatures? If the temperature of a cooler was exceeded, > 10" C, the lab must list by fraction and sample number, all affected samples. 3.6 Does the narrative contain a list of the pH values determined for each water sample submitted for volatile analysis? 3.7 Does the Case Narrative contain the statement, "verbatim", as required in. Section B of the SOW? ACTION: If "No", to any question in this section, contact the laboratory for all necessary resubmittals. If information is not available, document in the Data Assessment under Problems/Non-Compliance section. YES NO N/i K t< LIL -4^ -2 304805 STANDARD OPERATING PROCEDURE US EPA Region II Data: October 1995 Method! CLP/SOW OLM03.1 . SOP HW-6, Rev. 10 YSi NO N7^ 4.0 Data Validation ChacklJBt 4.1 Check the package for the following discrepancies: a. Ia the package paginated in ascending order ^ starting from the SDG narrative? b. Are all forms and copies legible? G. Is each fraction assembled in the order set forth in the SOW? d. Is a Sample Data Summary Package submitted immediately preceding the Sample Data Package? The following checklist is divided into three parts. Part A is for any VOA analyses. Part B is for BNAs and Part C is Pesticide/PCBa. Does this package contain: VOA Data? BNA Data? Pesticide/PCB data? ACTION: Complete corresponding parts of checklist. A 1^1 A _ -3- 304806 STANDARD OPERATING PROCEDURE US EPA Region II Datet Octobar 1995 Method: CLP/SOW 0LMO3.1 SOP HW-6, Rev. 10 YBS NO N/A PART AI VOA ANALYSES 1.0 Sample Cooditione/Prpblemg 1.1 Do the Traffic Reports/Chain-of-Custody Records, Sampling Report or Lab Narrative indicate any problems with sample receipt, condition of samples, analytical problems or special . circumstances affecting the Y quality of the data? \ \ ACTION: If any sample analyzed as a soil, other than TCLP, contains 50% - 90% water, all data should be flagged as estimated "J". If a soil sample other than TCLP contains more than 90% water, all data should be gualified as unusable "R". ACTION: If samples were not iced or the ice was melted upon arrival at the laboratory and the temperature of the cooler was elevated (> 10" C), then flag all positive results with a "J" and all non-detects "UJ". ACTION: If both VOA vials for a sample have air bubbles or the VOA vial analyzed had air bubbles, flag all positive results "J" and all non-detects "R" . ACTION: The smallest soil size permitted is 0.5g. If any soil sample is smaller than 0.5g, document in the Data Assessment under Contract Probleras/Non-Compliance. 2.0 Holding TimeB 2.1 Have any VOA technical holding times, determined from date of collection to date of analysis, been exceeded? Technical Holding Times: If unpreserved, aqueous samples, maintained at 4"* C for aromatic hydrocarbons analysis must be analyzed within 7 days of collection. If preserved with HCl (pH < 2) and scored at 4° c, then aqueous samples must be analyzed within 14 days of collection. If uncertain about preservation, contact sampler to determine whether or not samples werp. preserved. The holding time for soils is 10 days from date of collection. 304807 -4- A: STANDARD OPERATING PROCEDURE US EPA Region II Mathod: CLP/SOW 0LM03.1 Date: October 1995 SOP RW-6, Rav. 10 YES NO N/A Sanpia ID Table of Holding Time Violations (See Chain-of-Custody Records) Sairple Matrix Was Saaxple Preserved? Data Sampled Date Lab Raceivad Date Analyzed ACTION: If technical holding times are exceeded, flag all positive results as estimated "J" and sample quantitation limits as estimated "UJ", and document in the Data Assessment that holding times were exceeded. If analyses were done more than 14 days beyond holding time, either on the first analysis or upon re-analyais, the reviewer must use professional judgement to determine the reliability of the data and the effects of additional storage on the sample results. At a minimum, all results must be qualified "J", but the reviewer may determine that non-detect data are unusable "R". If holding times are exceeded by more than 2 8 days, all non detect data are unusable "R". NOTE: Contractual Holding Times: Analysis of water and soil/sediment samples must be completed within 10 days of Validated Time of Sample Receipt (VTSR). This requirement does not apply to Performance Evaluation (PE) samples. ACTION: If contractual holding times are exceeded, document in the Data Asseasment and on the Organic Regional Data Assessment Summary form. NOTE: The data reviewer must note in the Data Assessment whether or not tachnical and contractual holding times were met. 304808 5- STANDARD OPERATING PROCEDURE US EPA Region II Data: October 1995 Method: CLP/SOW 0LM03.1 SOP HW-6, Rev. 10 ~~~" YES NO NTA 3.0 Syetem Monitoring Compound (SMC) Recovery (Form II) 3.1 Are the VOA SMC Recovery Summaries (Form II) present for each of the following matrices: a. Low Water? I I. b. Low Soil? i_L c. Med Soil? l_i 3.2 Are all the VOA samples listed on the appropriate System Monitoring Compound Recovery Summary for each of the following matrices: Were method blanks re-analyzed? ACTION: If recoveries are > 10%, but 1 or more compounds fail to meet SOW specifications: 1. All positive results are qualified as estimated "J". 2. Flag all non-detects as estimated detection limits "UJ" where recovery is less than the lower acceptance limit. 3. If SMC recoveries are above allowable levels, do not qualify non-detects. -6- a. Low Water? b. Low Soil? J__L c. Med Soil? ACTION: Call lab for explanation/resubmittals. If missing deliverables are unavailable, document effect in the Data Assessments. 3.3 Were outliers marked correctly with an asterisk? ACTION: Circle all outliers in red. 3.4 Was one or more VOA system monitoring compound recovery outside of contract specifications for any sample or method blank? If yes, were samples re-analyzed? \ ] A - 4 / A ^ _ ^ 304809 STANDARD OPERATING PROCEDURE US EPA Region II Method: CLP/SOW 0LM03 Date: October 1995 SOP HW-6, Rev. 10 YES NO N/A . If any system monitoring compound recovery is < 10%: 1. Flag all positive results as estimated "J". 2. Flag all non-detects as unusable "R" . Professional judgement should be used to qualify data that only have method blank SMC recoveries out of specification in both original and re-analyses. Check the internal standard areas. NOTE: Contractual requirements state that if any SMC fails the acceptance criteria, the sample must be re-analyzed. If the affected sample was not re- analyzed, document in the Data Assessment under Contract Problems/Non-Compliance. NOTE: The laboratory must submit the following data: 1. If SMC recoveries and internal standard responses meet the acceptance criteria in the re- analyzed sample, then the laboratory must submit only the re-analysis. 2. If an SMC recovery and/or intemal standard response fails to meet the acceptance criteria upon re-analyais, then submit data from both analyses. (Refer to section 11.4.3.2, page D-46/VOA of the SOW for more information.) 3.5 Are there any transcription/calculation errors between raw data and Form II? ACTION: If large errors exist, call lab for expianation/resubmittal, make any necessary corrections and note errors in the Data Assessment. 4.0 Matrix Spikea /Porm III) 4.1 Is the Matrix Spike/Matrix Spike Duplicate Recovery Form (Form III) present? j ^ _ i^__ 304810 us EPA Region II Method: CLP/SOW 0LM03.1 STANDARD OPERATING PROCEDURE Date: October 1995 SOP HW-6, Rav. 10 YES NO N/A 4.2 Were matrix spikes analyzed at the required frequency for each of the following matrices: a. Low Water? b. Low Soil? c. Med Soil? ACTION: If any matrix spike data are missing, take the action specified in 3.2 above. 4.3 How many VOA spike recoveries are outside QC limits? Water -o- out of 10 Soils ^ K out of 10 4.4 How many RPDs for matrix spike and matrix spike duplicate recoveries, are outside QC limits? Water "^"^ out of 5 out of 5 ACTION: No action is taken based upon MS/MSD data alone. However, using informed professional judgement, the MS/MSD results may be used in conjunction with other QC criteria to determine the need for qualification of the data. ACTION: Circle all outliers in red. 5.0 Blanks (Porm IV) 5.1 Is the Method Blank Summary (Form IV) present? 5.2 Frequency of Analysis: for the analysis of VOA TCL compounds, has a reagent/method blank been analyzed for each SDG or every 20 samples of similar matrix (low water, low soil or medium soil), whichever is more frequent? 5.3 Has a VOA method blank been analyzed at least once every twelve hours for each concentration level and GC/MS system used? 1 ^ . u. . J_L . V ^ il A / 304811 STANDARD OPERATING PROCEDURE US EPA Region II Date: October 199! Mathod: CLP/SOW 0LMO3.1 SOP HW-6, Rev. K YES NO N/i 5.4 Was a VOA instrument blank analyzed after each ^ sample/dilution which contained a target compound / that exceeded the initial calibration range? IVJ 5.5 Was a VOA storage blank analyzed at the end of / all samples for each SDG in a case? f I ^ ACTION: If any method/instrument blank data are missing, call lab for explanation or resubmittal. If method blank data are not available, reject "R" all associated positive data. However, using professional judgement, the data reviewer may siibstitute field blank or *^trip blank data for missing method blank data. If any instrument blank analyzed after a sample with high concentration is missing, contact the lab for resubmittals. If the instrument blank was not analyzed or not available, inspect the chromatogram of the sample analyzed immediately after this analysis for possible carryover. Use professional judgement to determine if any contamination occurred and qualify analyte(s) accordingly. If storage blank data is missing, contact the lab for the data. If unavailable, note in the Data Assessment under Contract Problems/Non- Compliance. 5.6 The validator should verify that the correct identification scheme for the EPA Blank samples were used. See page B-33, section 3.3.7.3 of the SOW for further information. Was the correct identification scheme used for all VOA blanks? ACTION: Contact the lab for resubmittals or make the required corrections on the forms. Document in the Data Assessment under Contract Problems/ Non-compliance if corrections were made by the validator. J ^ _ _ 5.7 Chromatography: review the blank raw data- chromatograms (RICs), quant reports or data system printouts and spectra. Is the . chromatographic performance (baseline stability) / for each instrument acceptable for VOAs? ^Y[ -9- 304812 STANDARD OPERATING PROCEDURE US EPA Region I I Date: October 199E Method: CLP/SOW 0LM03,1 SOP HW-6, Rev. 10 YES NO N/A ACTION: Use professional judgement to determine the effect on the data. 5.8 Are all detected hits for target compounds in method and instrument blanks less than the CRQL for that analyte? Exception: Acetone and 2-butanone must be less than 5 times the CRQL, and methylene chloride must be less than 2.5 times its CRQL. ACTION: If yes, an explanation and laboratory's corrective actions must be addressed in the case narrative. If the narrative contains no explanation, then make note in the Data Assessment under Contract Problems/Non- Compliance . 6.0 Contamination NOTE: "Water blanks", "drill blanks", and "distilled water blanks" are validated like any other sample, and are not used to qualify data. Do not confuse them with the other QC blanks discussed below. 6.1 Do any method/instrument/reagent/storage blanks have positive results (TCL and/or TIC) for VOAs? NOTE: When applied as directed in the table below, the contaminant concentration in these blanks are multiplied by the sample dilution factor and corrected for %moisture when necessary. NOTE: A contaminated instrument blank is not allowable under this SOW. See page D-48/VOA, section 12.1.2.4 for additional information. Document in the Data Assessment under Contract Problems/Non- Compliance if contaminated instrument blank was submitted. ^ ^ _ i/_ 6.2 Do any field/trip/rinse blanks have positive VOA ^ results (TCL and/or TIC)? V^ -Ll ACTION: Prepare a list of the samples associated with each of the contaminated blanks. (Attach a separate sheet.) One rinse blank not associated vvith any samples, detected acetone (at a concentration more than lOX greater than any detected sample concentration). Acetone in the rinse blank is attributed to the decontamination procedures. -10- 3 0 4 8 1 3 STANDARD OPERATING PROCEDURE US EPA Region II Method: CLP/SOW 0I.M03 Date: October 199E SOP HW-6, Rev. IC YES NO N/JI NOTE: All field blank results associated with a particular group of samples (may exceed one per case) must be used to qualify data. Trip blanks are used to qualify only those samples with which they were shipped and are not required for non-aqueous matrices. Blanks may not be qualified, because of contamination in another blank. Field Blanks & Trip Blanks must be qualified for system monitoring compound, instrument performance criteria, spectral or calibration QC problems. ACTION: Follow the directions in the table below to qualify TCL results due to contamination. Use the largest value from all the associated blanks. If any blanks are grossly contaminated, all associated data should be qualified as unusable "R" . For; Flag siusple result with a "U" when: Report CRQL &. qnalify "U" when: No q[uali£ication ia needed when: Methylene Chloride Acetone Toluene 2-Butanone Sample cone. ia > CRQL, but < lOx blank value. Sample cone. ia < CRQL and < lOx blank value. Sample cone, ia > CRQL and > lOx blank value. Other Sample cone, is Conta- > CRQL, but < 5x minants blank value. Sample cone, is < CRQL and < 5x blank value. Sample cone, is > CRQL and > 5x blank value. NOTE: Analytes qualified "U" for blank contamination are still considered as "hits" when qualifying for calibration criteria. ACTION: For TIC compounds, if the concentration in the sample is less than five times the concentration in the most contaminated associated blank, flag the sample data "R" . 6.3 Are there field/rinse/equipment blanks associated with every sample? ACTION: For low level samples, note in the Data Assessment that there is no associated field/rinse/equipment blank. For samples with -11- A 304814 US EPA Region II Mathod: CLP/SOW 0LM03.1 STANDARD OPERATING PROCEDURE Date: October 1995 SOP HW-6, Rev. 10 YES NO N/A high concentrations of suspected blank contaminants, use professional judgement to qualify these values and make a note in the Data Assessment. Exception: samples taken from a drinking water tap do not have associated field blanks. 7.0 GC/MS Inptrument Performance Check (Form V) Are the GC/MS Instrument Performance Check Forms (Form V) present for Bromofluorobenzene (BFB)? Are the enhanced bar graph spectrum and mass/charge (m/z) listing for the BFB provided for each twelve hour shift? Has an instrument performance check been analyzed for every analytical sequence on each instrument? 7.1 7.2 7.3 ACTION: List date, time, instrument ID, and sample analysis for which no associated GC/MS tuning data are available. A DATE TIME INSTRUMENT SAMPLE NUMBERS ACTION: If lab cannot provide the missing data, reject "R" all data generated outside an acceptable twelve hour calibration interval. 7.4 Have the ion abundances been normalized to m/z 95? ACTION: If mass assignment is in error, qualify all associated data as unusable "R". 7.5 Have the ion abundance criteria been met for each instrument used? ACTION: List all data which do not meet ion abundance criteria (attach a separate sheet), iA A _ -12- 304815 STANDARD OPERATING PROCEDURE US EPA R e g i o n I I M e t h o d : CLP/SOW 0LM03.1 D a t e : O c t o b e r 1995 SOP HW-6, R e v , IC YES NO N/J ACTION: If ion abundance criteria are not met, the Region II TPO must be notified. 7.6 Are there any transcription/calculation errors between mass lists and Form Vs? (Check at least two values, but if errors are found check more.) 7.7 Is the number of significant figures for the reported relative abundances consistent with the number given for each ion in the ion abundance criteria column? ACTION: If large errors exist, call lab for expianation/resubmittal, make necessary corrections and document any effects in the Data Assessments. 7.8 Are the spectra of the mass calibration compound acceptable? ACTION: Use professional judgement to determine whether associated data should be accepted, qualified, or rejected. 8.0 Target Coaapound List {TCh) Analytea 8.1 Are the Organic Analysis Data Sheets (Form I VOA) present with required header information on each page, for each of the following: a. Samples and/or fractions as appropriate? b. Matrix spikes and matrix spike duplicates? c. Blanks? 8.2 Are the VOA Reconstructed Ion Chromatograms, the mass spectra for the identified compounds, and the data system printouts (Quant Reports) included in the sample package for each of the following: a. Samples and/or fractions as appropriate? b. Matrix spikes and matrix spike duplicates (mass spectra not required)? c . Blanks? sA ^ _ i^ A s i sX l l l l 1 ^ • 1 3 - 304816 us EPA Region II Method: CLP/SOW 0LM03.1 STANDARD OPERATING PROCEDURE Date: October 1995 SOP HW-6, Rev. 10 YES NO NTA ACTION: If any data are missing, take action specified in 3.2 above. 8.3 Are the response factors shown in the Quant Report? 8.4 Is chromat;:ographic performance acceptable with respect to; a. Baseline stability? b. Resolution? c. Peak shape? d. Full-scale graph (attenuation)? e. Other: ? ACTION: Use professional judgement to determine the acceptability of the data. 8.5 Are the lab-generated standard mass spectra of the identified VOA compounds present for each sample? ACTION: If any mass spectra are missing, take action specified in 3.2 above. If the lab does not generate its own standard spectra, document in the Data Assessment in the Contract Non-compliance section and the Organic Regional Data Assessment Summary. 8.6 Is the RRT of each reported compound within 0.06 RRT units of the standard RRT in the continuing calibration? 8.7 Are all ions present in the standard mass spectrum at a relative intensity greater than 10% also present in the sample mass spectrum? 8.8 Do sample and standard relative ion intensities agree within ±20%? ACTION: Use professional judgement to determine acceptability of data. If it is determined that incorrect identifications were made, all such data should be rejected "R", flagged "N" (presumptive evidence of the presence of the compound) or changed to not detected "U" at the U — i l _ LX jvf iA _ • 1 4 - 304817 STANDARD OPERATING PROCEDURE US EPA Region II Method: CLP/SOW 0LM03.1 Date: October 199! SOP HW-6, Rev. 1( YIS NO N/; calculated detection limit. In order to be positively identified, the data must comply with the criteria listed in 8.6, 8.7, and 8.8. ACTION: When sample carry-over is a possibility, professional judgement should be used to determine if instrument cross-contamination has affected any positive compound identification. 9.0 Tentatively Identified Coapounds (TIC) 9.1 Are all Tentatively Identified Compound Forms (Form I Part B) present; and do listed TICs include scan number or retention time, estimated concentration and "JN" qualifier? 9.2 Are the mass spectra for the tentatively identified compounds and associated "best match" spectra included in the sample package for each of the following: a. Samples and/or fractions as appropriate? b. Blanks? c. Alkanea listed for each sample? ACTION: If any TIC data are missing, take action specified in 3.2 above. ACTION: Add "N" qualifier to all chemically named TICs, if missing. 9.3 Are any TCL compounds (from any fraction) listed as TIC compounds? (Example: 1,2- dimethylbenzene ia xylene, a VOA TCL analyte, and should not be reported aa a TIC.) ACTION: Flag with "R" any TCL compound listed as a TIC. 9.4 Are all ions present in the reference mass spectrum with a relative intensity greater than 10% also present in the sample mass spectrum? 9.5 Do TIC and "best match" standard relative ion intensities agree within ±20%? ACTION: Use professional judgement to determine the acceptability of TIC identifications. If it ia determined an incorrect identification was LI / f 1 [ 1 [ ] 1 ^ vJ xA UL J_L J_L X I y -15- 304818 STANDARD OPERATING PROCEDURE US EPA Region II Method: CLP/SOW 0LM03.1 Date: October 1995 SOP HW-6, Rev. 10 YES NO N/A made, change the identification to "unknown," or to some less specific identification as appropriate. (Example: "C3 substituted benzene.") Also, when a compound ia not found in any blank, but is detected in a sample and ia a suspected artifact of a common laboratory contaminant, the result should be qualified as unusable "R". .(E.g., Common Lab Contaminants: CO2 (M/E 44), siloxanes (M/E 73) hexane, aldol condensation products, solvent preservatives, and related by-products - see Functional Guidelines for more guidance.) 9.6 Are TICs with responses < 10% of the internal standard (as determined by inspection of the peak areas or height) reported? ACTION: If yes, cross out questionable TIC(s). 10.0 Compound Quantitation and Reportad Detection Limits 10.1 Are there any transcription/calculation errors in Form I results? (Check at least two positive values. Verify that the correct internal standards, quantitation ions, and RRF were used to calculate Form I results.) 10.2 Are the CRQLs adjusted to reflect sample dilutions and, for soils, sample moisture? ACTION: If errors are large, call the lab for explanation/resubmittals, make any necessary corrections, and note errors under Contract Problems/Non-Compliance section of the Data Assessment and the Organic Regional Data Assessment Summary. ACTION: When a sample is analyzed at more than one dilution, the lowest CRQLs are used (unless a QC exceedance dictates the use of the higher CRQL data from the diluted sample analysis) . Replace concentrations that exceed the calibration range in the original analysis by crossing out the "E" and its associated value on the original Form I and substituting the data from the analysis of the diluted sample. Specify which Form I is to be used, then draw a red "X" across the entire page of all Form Is -16- -U- -Vl y ^ _ ^ _ 304819 STANDARD OPERATING PROCEDURE US EPA Region II Date: October 199! Method: CLP/SOW 0LM03.1 SOP HW-6, Rev. IC that should not be used, including any in the summary package. 11.0 Standardfl Data (QC/MS) 11.1 Are the Reconstructed Ion Chromatograms, and data . system printouts (Quant. Reports) present for _Vr initial and continuing calibration? ACTION: If any calibration standard data are missing, take action specified in 3.2 above. 12.0 QC/MS Initial Calibration (Form VI) 12.1 Are the Initial Calibration Forms (Form VI) present and complete at concentrations of 10, 20, 50, 100, 200ng for separate calibrations of low water/med soils (unheated purge) and low soils (heated purge)? ACrriON: If any calibration standard forms are missing, take action specified in 3.2 above. 12.2 Were all low level soil standards, blanks and samples analyzed by heated purge? ACTION: If low level soil samples were not heated during purge, qualify positive hits "J" (estimated) and non-detects "R" . 12.3 Are the % relative standard deviation (%RSD) values for VOAs s 3 0% over the concentration range of the calibration? [_I ACTION: Circle all outliers in red. NOTE: Although 11 VOA compounds have a minimum RRF and no maximum %RSD, the technical criteria are the same for all analytea. ACTION: If %RSD is > 30.0%, qualify associated positive results for that analyte "J" and non-detects using professional judgement. When %RSD ia > 90%, flag all non-detects for that analyte "R" (unusable) and positive hits "J" (estimated). NOTE: Analytes previously qualified "U" for blank contamination are still considered as "hits" when qualifying for initial calibration criteria. id _ ^ A •17- 304820 US EPA Region II Method: CLP/SOW 0LM03.1 STANDARD OPERATING PROCEDURE Date: October 1995 SOP HW-6, Rev. IC YES NO N/il 12.4 Are any average RRFs < 0.05? Action: Circle all outliers in red. Action: If the average RRF is < 0.05, then qualify associated non-detects with an "R" and flag associated positive data as estimated "J". 12.5 Are there any transcription/calculation errors in the reporting of average relative response factors (RRF) or %RSD? (Checlc at least 2 values, but if errors are found, chec)< more.) NOTE: The SOW allows up to two of the required analytea to fail %RSD or RRF criteria, provided that the %RSD is s 40% and the RRF is i 0.010. (See Table 5, page D-5 9/VOA or analytes marked with a "." on Form VI for required analytes.) ACTION: If more than two analytes failed %RSD or RRF criteria, document in the Data Assessment under Contract Problems/Non-Compliance and the Organic Regional Data Assessment Summary. 13.0 GC/MS Continuing Calibration (Form VII) 13.1 Are the Continuing Calibration Forms (Form VII) present and complete for separate calibration of low water/med soil and low soil samples? 13.2 Has a continuing calibration standard been analyzed for every twelve hours of sample analysis per instrument? ACTION: If any forms are missing or no continuing calibration standard has been analyzed within twelve hours of every sample analysis, call lab for explanation or resubmittal. If continuing calibration data are not available, flag all associated sample data as unusable "R" . ACTION: List below all sample(s) that were not analyzed within twelve hours of the previous continuing calibration. il ^ _ A ^ -18^ 304821 STANDARD OPERATING PROCEDURE US EPA Region II Method: CLP/BOW 0LM03.1 Date: October 1995 SOP HW-6, Rev. 10 YSS NO M/« 13.3 Do any volatile compounds have a percent difference (%D) between the initial and continuing RRP which exceeds the ±25% criteria? ACTION: Circle all outliers in red. ACTION: Qualify both positive results and non-detects for the outlier compound(s) as estimated. When %D is > 90%, qualify all non-detects for that analyte "R" (unusable) and positive results "J" (estimated). 13.4 Are any continuing calibration RRFs < 0.05? ACTION: Circle all outliers in red. ACTION: If the RRF is < 0.05, qualify the associated non-detects as unusable "R" and the associated positive values "J". NOTE: The SOW allows up to two of the required analytes to fail %D and RRF criteria, provided that the %D ia s 40% and the RRF is i 0.010. (See Table 5 pg. D-5 9/VOA or analytes marked with a ' \ " on Form VI for required analytes.) ACTION: If more than two analytes failed %D and RRF, criteria document in the Data Assessment under contract Problems/Non-Compliance and on the Organic Regional Data Assessment Summary form. L - LL A - 13.5 Are there any transcription/calculation errors in the reporting of RRF or %D between initial and continuing RRFs? (Check at least two values, but if errors are found, check more.) ACrriON: Circle errors in red. _ l l ACTION: If errors are large, call lab for expianation/resubmittal, make any necessary corrections and document in the Data Assessment under the Contract Problems/Non-Compliance section and the Organic Regional Data Assessment Summary. •19- 304822 STANDARD OPERATING PROCEDURE US EPA Region II Method: CLP/SOW 0LM03.1 Date: October 1995 SOP HW-6, Rev. 10 YSS NO N/A 14.0 Intemal Standard (Form VIII) 14.1 Are the internal standard areas (Form VIII) of every sample and blank within the upper and lower limits (-50% to +100%) for each continuing / calibration? f^ If no, was the sample re-analyzed? ACTION: 1. Circle all outliers in red. 2. List all the outliers below. Sample # internal Std. Area U — Lower/Upper Limit X (Attach additional sheets if necessary.) (or attach copies of Form VIIIs) ACTION: If any sample was not re-analyzed, document in the Data Assessment under Contract Problems/Non-Compliance. ACTION: 1. If the internal standard area count is outside the upper or lower limit, flag with "J" all positive results quantitated with this internal standard. 2. Non-detects associated with IS area counts > 100% should not be qualified. 3. If the IS area in the sample is below the "lower limit," < 50%, qualify all analytes associated with that IS estimated, "J". If the area counts are extremely low, < 25% of the area in the 12 hour standard, or if performance exhibits a major abrupt drop- off, flag all associated non-detects as unusable, "R", and positive hits estimated, "J". 14.2 Are the retention times of the internal standards within 30 seconds of the associated calibration standard? -20- w o 00 to OJ A^^ STANDARD OPERATING PROCEDURE US EPA Region II Method: CLP/SOW 0LM03.1 Date: October 199! SOP HW-6, Rev. 1( YES NO N/J ACTION: Professional 'judgement should be used to qualify data if the retention times differ by more than 3 0 seconds. NOTE: Contractual requirements state that if any internal standard fails the acceptance criteria, the sample must be re-analyzed. If the affected sample was not re-analyzed, document in the Data Assessment under Contract Problems/Non- Compliance. NOTE: See Notes in section 3.4, page 7 for a description of sample data the laboratory must submit. 15.0 Field DuffllcateB 15.1 Were any field duplicates submitted for VOA analysis? ACTION: Compare the reported results for field duplicates and calculate the relative percent difference. A AtrriON: Any gross variation between duplicate results must be addressed in the reviewer narrative. However, if large differences exist, identification of field duplicates should be confirmed by contacting the sampler. 304824 -21^ STANDARD OPERATING PROCEDURE US EPA Region II Date: October 1995 Method: CLP/SOW OLM03.1 SOP HW-6, Rev. 10 YES NO N/A PART B : BNA ANALYSES l . O S a a p l a Cond^t-49nfl/P;rt;^^1flgp 1.1 Do the Traffic Reports/Chain-of-Custody Records or Lab Narrative indicate any problems with sample receipt, condition of samples, analytical problems or special notations affecting the ^ quality of the data? 1_J. V ACTION: If any sample analyzed as a soil, other than TCLP, contains 50% - 90% water, all data should be flagged as estimated "J". If a soil sample, other than TCLP, contains more than 90% water, all data should be qualified as unusable "R". ACTION: If samples were not iced or if the ice was melted upon arrival at the laboratory and the temperature of the cooler was elevated (> 10° C) , flag all positive results "J" and all non- detects "UJ" . 2.0 Holding Timeg 2.1 Have any BNA technical holding times, determined from date of collection to date of extraction, / been exceeded? f J V NOTE: T&ghnical Holding Time: Continuous extraction of water samples for BNA analysis must be started within seven days of the date of collection. Soil/sediment samples must be extracted within 7 days of collection. Extracts must be analyzed within 40 days of the date of extraction. Table of Holding Tine Violationa (See Chain-of-Custody Records) Sample Sample Date Date Lab Date Analyzed Matrix Sampled Received Extracted - - _ (jj o — . rfi _ _ ^ lo . cn •22- STANDARD OPERATING PROCEDURE US EPA Region II Method: CLP/SOW 0LM03 Date: October 1995 SOP HW-6, Rev. 10 YES NO N/A ACTION: If technical holding times were exceeded, flag all positive results as estimated "J" and sample quantitation limits as estimated "UJ", and document in the narrative that holding times were exceeded. If analyses were done more than 14 days beyond holding time, either on the first analysis or upon reanalysis, the reviewer must use professional judgement to determine the reliability of the data and the effects of additional storage on the sample results. At a minimum, all results should be qualified "J", but the reviewer may determine that non-detect data are unusable "R". if holding times are exceeded by more than 28 days, all non-detect data must be qualified "R", unstable. NOTE: Contractual Holding Times: Extraction of water samples must be started within 5 days VTSR. Soil/sediment samples must be extracted within 10 days of VTSR. This requirement does not apply to Performance Evaluation (PE) samples. Water and soil/sediment extracts must be analyzed within 40 days following extraction. ACTION: If contractual holding times are exceeded, document in the Data Assessment and on the Organic Regional Data Assessment Summary form. NOTE: The data reviewer must note in the Data Assessment whether or npt technical and contractual holding times were met. 3.0 Surrogate R^covarv (Form II) 3.1 3.2 Are BNA Surrogate Recovery Summaries (Form II) present for each of the following matrices: a. Low Water? [__] . ^ b. Low Soil? \ ] ^ c. Med Soil? j_j_ y / Are all the BNA samples listed on the appropriate Surrogate Recovery Summaries for each of the following matrices: a.'Low Water? ( \ ^ -23 304826 STANDARD OPERATING PROCEDURE US EPA Region II Date: October 1995 Method: CLP/SOW 0LM03.1 SOP HW-6, Rev. 10 YES NO NTA b. Low Soil? J_i ^ ^ c. Med Soil? f 1 x/A' ACTION: Call lab for explanation/resubmittals. If missing deliverables are unavailable, document effect in the Data Assessments. 3.3 Were outliers marked correctly with an asterisk? f 1 ACTION: Circle all outliers in red. A 3.4 Were two or more base-neutral QE acid surrogate recoveries out of specification for any sample or y method blank? [ } v^ If yes, were samples reanalyzed? J L X ^ Were method blanks reanalyzed? \ 1 V ^ ACTION: If all BNA surrogate recoveries are > 10%, but two within the base-neutral or acid fraction do not meet SOW specifications, for the affected fraction only (i.e. acid or base-neutral compounds): 1. Flag all positive results with "J" (estimated). 2. Flag all non-detects as estimated detection limits ("UJ") when recoveries are leas than the lower acceptance limit. 3. If recoveries are greater than the upper acceptance limit, do not qualify non-detects. If any base-neutral o^; acid surrogate has a recovery of < 10%: 1. Positive results for the fraction with < 10% surrogate recovery are qualified with "J". 2. Non-detects for that fraction should be qualified as unusable "R". Professional judgement should be used to qualify data that have method blank surrogate recoveries out of specification in both original and reanalyses. Check the internal standard areas. -24- 304827 us EPA Region II Method: CLP/SOW OLM03 STANDARD OPERATING PROCEDURE Date: October 1995 SOP HW-6, Rev. 10 YES NO N/A NOTE: Contractual requirements state that if any surrogate fails acceptance criteria, the sample must be re-analyzed. If sample was not re- analyzed, document in the Data Assessment under Contract Problems/Non-Compliance. NOTE: The laboratory must submit the following data: 1. If surrogate recoveries and internal standard responses meet the acceptance criteria in the re- analyzed sample, then the laboratory must submit only the re-analysis. 2. If surrogate recoveries and/or internal standard responses fail to meet the acceptance criteria upon re-analysis, then submit data from both analyses. 3.5 Are there any transcription/calculation errors between raw data and Form II? _ la ^ ACTION: If large errors exist, call the lab for expianation/resubmittal, make any necessary corrections and document effect in the Data Assessments. 4.0 Matrix Spikes (Form III) 4.1 Is the Matrix Spike/Matrix Spike Duplicate Recovery Form (Form III) present? 4.2 Were matrix spikes analyzed at the required frequency for each of the following matrices: a. Low Water? b. Low Soil? c. Med Soil? ACniON: If any matrix spike data are missing, take the action specified in 3.2 above. 4.3 How many BNA spike recoveries are outside QC limits? I-J. ^ I 1 t 1 ( 1 s / y V Water NA out of 22 Spils iNA out of 22 •25- 304828 STANDARD OPERATING PROCEDURE US EPA Region II Method: CLP/SOW 0LM03.1 Date: October 1995 SOP HW-6, Rev. 10 YES NO N/A 4.4 How many RPDs for matrix spike and matrix spike duplicate recoveries are outside QC limits? Water. NA out of 11 S9ils N ^ out of 11 ACTION: No action is taken baaed upon MS/MSD data ajlone. However, using informed professional judgement, the data reviewer may use the matrix spike and matrix spike duplicate results in conjunction with other QC criteria and determine the need for some qualification of the data. ACTION: Circle all outliers in red. 5.0 Blanka (Porm IV) 5.1 Is the Method Blank Summary (Form IV) present? 5.2 Frequency of Analysis: Has a reagent/method blank analysis been reported per 20 samples of similar matrix, or concentration level, and for each extraction batch? 5.3 Has a BNA method blank been analyzed for each GC/MS system used? (See SOW pg. D-54/SV0A, Section 12.1.2.) ACTION: If any method blank data are missing, call lab for expianation/resubmittal. If not available, use professional judgement to determine if the associated sample data should be qualified. 5.4 The validator should verify that the correct identification scheme for the EPA Blank samples were used. See page B-33, sec. 3.3.7.3 of the SOW for further information. J_J_ I_I 1_L y y Was the correct identification scheme used all BNA blanks? for y ACTION: Contact Che lab for resubmittals or make the required corrections on the forms. Document in the Data Assessment under Contract Problems/Non-Compliance if corrections were made by the validator. 5.5 Chromatography: review the blank raw data - •26- 304829 STANDARD OPERATING PROCEDURE US EPA Region II Date: October 1995 Method: CLP/SOW 0LM03.1 SOP HW-6, Rev, 10 YES NO N/A chromatograms (RICs), quant reports or data system printouts and spectra. Is the chromatographic performance (baseline stability) / acceptable for each instrument? LJ., . JL— ACTION: Use professional judgement to determine the effect on the data, 5.6 Are all detected hits for target compounds less than the CRQL for that analyte in all method / blanks? XJ. J_- Exception: Phthalate esters must be less than five times (SX) the CRQL. 6.0 Contamination NOTE: "Water blanks", "drill blanks" and "distilled water blanks" are validated like any other sample and are not used to qualify data. Do not confuse them with the other QC blanka discussed below. 6.1 Do any method/instrument/reagent blanks have / positive results (TCL and/or TIC)? J__L z J NOTE Water: When applied as directed in the table below (page 28), the contaminant concentration in method/ instrument/reagent blanks is multiplied by the sample dilution factor, where necessary. Soil: 30 grams of sodium sulfate (1 gram for medium level soils) are used to prepare the soil method blank as instructed on page D-54/SVOA, section 12.1.3. When applied as directed in the table of 6.2, the contaminant concentration in the method blank is multiplied by the sample dilution factor, where necesary. Contact the laboratory if the soil method blanks are not reported in soil units (/xg/kg) . 6.2 Do any field/rinse/blanks have positive BNA J results (TCL and/or TIC)? J_L A ACTION: Prepare a list of the samples associated with each of the contaminated blanks. (Attach a separate sheet.) NOTE: All field blank results associated to a particular group of samples (may exceed one per case) must be used to quality sample aata. Do not convert field bjgn}^ results to account for the difference in soil •^^" 304830 us EPA Region II Method: CLP/SOW 0LM03.1 STANDARD OPERATING PROCEDURE Date: October 1995 SOP HW-6, Rev. 10 YES NO N/A CRQLs. Blanks may not be qualified because of contamination in another blank. Field blanks must be qualified for surrogate, spectral, instrument performance or calibration QC problems. ACTION; Follow the directions in the table below to qualify TCL results due to contamination. Use the largest value from all the associated blanks. If gross contamination exists, all data in the associated samples should be qualified as unusable "R". For: Flag aample reault with a "U" when: Report CRQL t qualify "U" when: No qualification is needed when: Common Sample cone, is Pthalate- > CRQL, but < lOx Esters blank value. Sample cone, is < CRQL and < lOx blank value. Sample cone, is > CRQL and > lOx blank value. Other Sample cone, is Conta- > CRQL, but < 5x minants blank value. Sample cone, is < CRQL and < 5x blank value. Sample cone, is > CRQL and > 5x blank value. NOTE: Analytes gualified "U" for blank contamination are still considered as "hits" when qualifying for calibration criteria. ACTION: For TIC compounds, if the concentration in the sample is less than five times the concentration in the most contaminated associated blank, flag the sample data "R" (unusable). 6.3 Are there field/rinse/equipment blanks associated with every sample? ACTION: For low level samples, note in the Data Assessment that there is no associated field/rinse/equipment blank. For analytes with high concentration, use professional judgement on qualification of these values and make a note in the Data Assessment. Except inn - samples taken from a drin>:ing water tap do not have associated field blanks. LX. JL^ ^ -28- 304831 STANDARD OPERATING PROCEDURE US EPA Region II Date: October 1995 Method: CLP/SOW OLM03.1 SOP HW-6, Rev. 10 YES NO N/A 7.0 GC/MS InBtrymant Performance Check 7.1 Are the GC/MS Instrument Performance Check Forms • (Form V) present for Decafluorotriphenylphosphine X_L J L _ (DFTPP)? 7.2 Are the enhanced bar graph spectrum and • mass/charge (m/z) listing for the DFTPP provided J_L 3L_ for each twelve hour shift? 7.3 Has an instrument performance check solution been y analyzed for every twelve hours of sample .l_l. analysis per instrument? ACTION: List date, time, instrument ID, and sample number for which no associated GC/MS tuning data are valid. SAMPLE NUMBERS DATE TIME INSTRUMENT ID A ACTION: If lab cannot provide missing data, reject "R" all data generated outside an acceptable twelve hour calibration interval. ACTION: If mass assignment is in error, flag all associated sample data as unusable "R". 7.4 Have the ion abundances been normalized to m/z 198? 7.5 Have the ion abundance criteria been met for each instrument used? J L ACTION: List all data which do not meet ion abundance criteria (attach a separate sheet), ACTION: If ion abundance criteria are not met, the Region II TPO must be notified. 7.6 Are there any transcription/calculation errors between mass lists and Form Vs? (Check at least >- two values, but if errors are found check more.) [ 1 A— -29- 304832 us EPA Region II Method: CLP/SOW 0LM03.1 STANDARD OPERATING PROCEDURE Date: October 1995 SOP HW-6, Rev. 10 YES NO N/A • 7.7 Is the number of significant figures for the reported relative abundances consistent with the number given for each ion in the ion abundance criteria column? AcrriON: If large errors exist, call lab for expianation/resubmittal, make necessary corrections and document effect in the Data Assessments. 7.8 Are the spectra of the mass calibration compound acceptable? ACTION: Use professional judgement to determine whether associated data should be accepted, qualified, or rejected. 8.0 Target Compoujid List (TCL) Analytea 8.1 Are the Organic Analysis Data Sheets (Form I BNA) present wit.h required header information on each page, for each of the following: a. Samples and/or fractions as appropriate? b. Matrix spikes and matrix spike duplicates? c. Blanks? 8.2 Has GPC cleanup been performed on all soil/ sediment sample extracts? ACTION: If data ."suggests that GPC was not performed, use professional judgement. Make note in Contract Problems/Non-Compliance section of the Data Assessment and the Organic Regional Data Assessment Summary. 8.3 Are the BNA Reconstructed Ion Chromatograms, the mass spectra for the identified compounds, and the data system printouts (Quant Reports) included in the sample package for each of the following: a. Samples and/or fractions as appropriate? b. Matrix spikes and matrix spike duplicates (mass spectra not required)? c. Blanks? A y I-i LA. XL XL LX L± LX y_ >A_ A^ A A A A - 3 0 . 304833 STANDARD OPERATING PROCEDURE US EPA Region II Date: October 1995 Method: CLP/SOW OLM03.1 SOP HW-6, Rev. 10 YES NO N/A ACTION: If any data are missing, take action specified in 3.2 above. 8.4 Are the response factors shown in the Quant / Report? •" ^ 8.5 Is chromatographic performance acceptable with respect to: Baseline stability? t 1 Resolution? J—L Peak shape? ,1—3. Full-scale graph (attenuation)? LL Other: __? J-J. ACTION; Use professional judgement to determine the acceptability of the data. A_ AL Ai A 8.6 Are lab-generated standard mass spectra of ^/ identified BNA compounds present for each sample? \ 1 ACTION: If any mass spectra are missing, take action specified in 3.2 above. Note under Contract Non-compliance if lab does not generate their own standard spectra. If spectra are missing, reject all positive data. 8.7 Is the RRT of each reported compound within 0.06 RRT units of the standard RRT in the continuing / calibration? f 1 . . 8.8 Are all ions present in the standard mass spectrum at a relative intensity greater than 10% / also present in the sample mass spectrum? f 1 _ 8.9 Do sample and standard relative ion intensities / agree within ±20%? f 1 Z_ ACTION: Use professional judgement to determine acceptability of data. If it is determined that incorrect identifications were made, all such data should be rejected "R", flagged "N" (presumptive evidence of the presence of the compound) or changed to not detected "U" at the calculated detection limit. In order to be positively identified, the data must comply -31- 304834 STANDARD OPERATING PROCEDURE US EPA Region II Date: October 1995 Method: CLP/SOW 0LM03.1 SOP HW-6, Rev. 10 ' — —— ^^ ^ J J ^ with the criteria listed in 8.7, 8.8, and 8.9. ACTION: When sample carry-over is a possibility, professional judgement should be used to determine if instrument cross-contamination has affected any positive compound identification. 9.0 Tentatively Identified Compounds (TIC) 9.1 Are all Tentatively Identified Compound Forms (Form I, Part B) present; and do listed TICs include scan number or retention time, estimated / concentration and "JN" qualifier? LL 9.2 Are the mass spectra for the tentatively identified compounds and associated "best match" spectra included in the sample package for each of the following: a. Samples and/or fractions as appropriate? \ 1 .L b. Blanks? UL )JL c. Alkanes listed for each sample? i 1 ^ ACTION: If any TIC data are missing, take action specified in 3.2 above. ACTION: Add "N" qualifier to all chemically named TICs, if missing. 9.3 Are any TCL compounds (from any fraction) listed as TIC compounds? (Example: 1,2-diraethylbenzene is xylene • a VOA TCL - and should not be reported as a TIC.) [ 1 ACTION: Flag with "R" any TCL compound listed as a TIC. / 9.4 Are all ions present in the reference mass spectrum with a relative intensity greater than / 10% also present in the sample mass spectrum? f 1 X A 9.5 Do TIC and "best match" standard relative ion intensities agree within ±20%? f 1 ACTION: Use professional judgement to determine the acceptability of TIC identifications. If it is determined that an incorrect identification was made, change the identifidation to "unknown," or to some less specific identification -32- 304835 STANDARD OPERATING PROCEDURE US EPA Region II Method: CLP/SOW 0LM03.1 Date: October 1995 SOP HW-6, Rev. 10 YES NO N/A 9.6 (example: "C3 substituted benzene") as appropriate. Also, when a compound is not found in any blank, but is a suspected artifact of a common laboratory contaminant, the result should be qualified as unusable, "R". Are any TICs with responses < 10% of the intemal standard (aa determined by inspection of the peak areas or height) reported? xa _ -r i-1 ACTION: If yes, cross out questionable TIC(3). 10.0 Compound Ouantitation and Reported Detection Limits 10.1 Are there any transcription/calculation errors in Form I results? (Check at least two positive values. Verify that the correct internal standard, quantitation ion, and RRF were used to calculate Form I result.) 10.2 Are the CRQLs adjusted to reflect sample dilutions and, for soils, sample moisture? ACTION: If errors are large, call lab for expianation/resubmittal, make any necessary corrections and document effect in the Data Assessments. ACTION: When a sample is analyzed at more than one dilution, the lowest CRQLs are used (unless a QC exceedance dictates the use of the higher CRQL data from the diluted sample analysis). Replace concentrations that exceed the calibration range in the original analysis by crossing out the "E" and its associated value on the original Form I and substituting the data from the analysis of the diluted sample. Specify which Form I is to be used, then draw a red "X" across the entire page of all Form Is that should not be used, including any in the summary package. 11.0 Standards Data (GC/MS) 11.1 Are the Reconstructed Ion Chromatograms, and data system printouts (Quant. Reports) present for initial and continuing calibration? [ 1 ACTION: If any calibration standard data are missing, take action specified in 3.2 above. UL y v/ y •33- 304836 us EPA Region II Method: CLP/SOW 0LM03.1 STANDARD OPERATING PROCEDURE Date: October 1995 SOP HW-6, Rev. 10 YES NO N/A 12.0 GC/MS Initial Calibration (Form VI) 12.1 Are the Initial Calibration Forms (Form VI) present and complete for the BNA fraction? i_J. ACTION: If any calibration standard forms are missing, take action specified in 3.2 above. 12.2 Are the % relative standard deviation (%RSD) values for BNAs s 3 0% over the concentration range of the calibration? J_L ACTION: Circle all outliers in red. NOTE: Although 2 0 BNA compounds have a minimum RRF and no maximum %RSD, the technical criteria are the same for all analytes. NOTE: Eight BNA compounds do not require a 20ng standard. Check the SOW for a list of these compounds. ACTION: If the %RSD is > 30.0%, qualify positive results for that analyte "J" and non-detects using professional judgement. When %RSD is > 90%, flag all non-detect results for that analyte "R" (unusable) and all positive results "J" (estimated). NOTE: Analytes previously qualified "U" due to blank contamination are still considered as "hits" when qualifying for calibration criteria. 12.3 Are any average RRFs < 0.05? ACTION: Circle all outliers in red. ACTION; If the average RRF is < 0.05 then; 1. "R" a l l non-detects. 2. "J" a l l p o s i t i v e r e s u l t s . 12.4 Are there any transcription/calculation errors in the reporting of RRFs and/or %RSD3? (Check at least two values, but if errors are found check more.) ACTION: Circle errors in red. v / y LL ^ LL A J • 3 4 - 304837 us EPA Region II Method: CLP/SOW 0LM03.1 STANDARD OPERATING PROCEDURE Date: October 1995 SOP HW-6, Rev. 10 Yzi NO N/A ACTION: If errors are large, call lab for expianation/resubmittal, make any necessary corrections and document errors in the Data Assessments. NOTE: The SOW allows up to four of the required analytes to fail %RSD or RRF criteria provided that the %RSD is s 40% or RRF ia z 0-010. (See Table 5, page D-66/SVOA or analytes marked with a ' \ " on Form VI for a list of the required analytea.) ACTION: If more than four analytes fail %RSD or RRF criteria, document in the Data Assessment under Contract Problems/Non-Compliance and on the Organic Regional Data Assessment Summary form. 13.0 GC/MS Continuing Calibration (Form VII) 13.1 Are the Continuing Calibration Forms (Form VII) present and complete for the BNA fraction? 13.2 Has a continuing calibration standard been analyzed for every twelve hours of sample analysis per instrument? ACTION: List below all sample analyses that were not analyzed within twelve hours of a continuing calibration standard for each instrument used. IIL XL -VI y y ACTION: If any forms are missing or no continuing calibration standard has been analyzed within twelve hours of every sample analysis, call lab for explanation/ resubmittal. If continuing calibration data are not available, flag all aaaociated sample data as unusable "R". 13.3 Does any BNA compound have a percent difference (%D) between the initial and continuing calibration RRFs which exceeds the ±25.0% criteria? ACTION: Circle all outliers in red. 1_L y •35- 304838 STANDARD OPERATING PROCEDURE US EPA Region ii Date: October 1995 Method: CLP/SOW 0LM03.1 SOP HW-6, Rev. 10 YSS NO N/A ACTION: Qualify both positive results and non-detects for the outlier compound(s) as estimated "J". When %D is > 90%, reject all non-detects for that analyte, "R", and qualify positive results "J" (estimated). > 13.4 Are any continuing RRFs < 0.05? LJL ACTION: Circle all outliers in red. ACTION: If the RRF is < 0.05, qualify as unusable "R" asBociated non-detects and "J" associated positive values. NOTE: The SOW allows up to four of the required analytes to fail %D and RRF criteria, provided that the %D is s 40% and the RRF is a 0.010. (See Table 5 page D-66/SVOA or analytes marked with a "," on Form VI for a list of the required analytes.) ACTION: If more than four analytes failed %D and RRF criteria, document in the Data Assessment under Contract Problems/Non-Compliance and on the Organic Regional Data Summary Form. 13.5 Are there any transcription/calculation errors in the reporting of average relative response factors (RRF) or %difference (%D) between initial and continuing RRFs? (Check at least two values, but if errors are found, check more.) XJL ACTION: Circle errors in red. ACTION: If errors are large, call lab for expianation/resubmittal, make any necessary corrections and document effect in the Data Assessments. 14.0 Intemal standards (Form VIII) 14.1 Are the internal standard areas (Form VIII) of every sample and blank within the upper and lower limits (-50% to +100%) for each continuing / calibration? [ J I_ If no, was sample re-analyzed? f 1 X ACrriON: 1. Circle all outliers in red. -36- 304839 >A STANDARD OPERATING PROCEDURE us EPA Region II Date: October 1995 Method: CLP/SOW 0LM03.1 SOP HW-6, Rev. 10 _ _ — 2. List all the outliers below. ACrriON: If sample was not reanalyzed, document the Data Assessment in Contract Problems/Non-Compliance. Sample # Intemal Std. Area Lower/Upper Limit / I. (Attach additional sheets if necessary.) (or attach copies of Form VIIIs) ACTION: ^. If the internal standard area count is outside the "upper" or "lower" limit, flag with "J" all positive results and non-detects quantitated with this internal standard. 2. Non-detects associated with IS area > 100% should not be qualified. 3. If the IS area in the sample is below the "lower limit," < 50%, qualify all analytes associated with that IS estimated, "J". If area counts are extremely low, < 25% of the area in the 12 hour standard, or performance exhibits a major abrupt drop-off, flag all associated non- detects as unusable, "R", and positive hits estimated, "J". 14.2 Are the retention times of the internal standards within 3 0 seconds of the associated calibration standard? f 1 ACrrioN: Professional judgement should be used to qualify data if the retention times differ by more than 3 0 seconds. NOTE; Contractual requirements state that if any internal standard fails the acceptance criteria, the sample must be re-analyzed. If the affected sample was not re-analyzed, document in the Data Assessment under Contract Problema/Non- Compliance. -37- 304840 y STANDARD OPERATING PROCEDURE US EPA Region II Date: October 1995 Method: CLP/SOW 0LM03,1 SOP HW-6, Rev. 10 YSS NO N/A NOTE: See Notes in section 3.4, page 24 for a description of sample data the laboratory must submit. 15.0 Field Duplicates 15.1 Were any field duplicates submitted for BNA y^ analysis? i—1 -5— ACTION: Compare the reported results for field duplicates and calculate the relative percent difference. ACTION: Any gross variation between field duplicate results must be addressed in the reviewer narrative. However, if large differences exist, identification of field duplicates should be confirmed by contacting the sampler. • 3 8 - 304841