USVI Public Records

Document text

SL SAVANNAH LABORATORIES & ENVIRONMENTAL SERVICES, INC. COMPREHENSIVE QUALITY ASSURANCE PLAN Savannah Division 5102 LaRoche Avenue Savannah, Georgia 31404 (912) 354-7858 Tallahassee Division 2846 Industrial Plaza Drive Tallahassee, Florida 32301 (904) 878-3994 Mobile Division 900 Lakeside Drive Mobile. Alabama 36609 (205) 666-6633 South Florida Division 414 SW 12th Avenue Deerfield Beach, Florida 33442 (305) 421-7400 Tampa Bay Division 6712 Benjamin Road. Suite 100 Tampa. Florida 33634 (813) 885-7427 TUT 005 2367 *64573* 64573 COMPREHENSIVE QUALITY ASSURANCE PLAN TUT 005 2368 COMPREHENSIVE QUALITY ASSURANCE PLAN Prepared by and for: Savannah Laboraton'es and Environmental Services, Inc. Savannah Division 5102 LaRoche Avenue Savannah, GA 31404 912-354-7858 Tallahassee Division Deerfield Beach Division 2846 Industrial Plaza Drive 414 SW 12th Avenue Tallahassee, FL 32301 Deerfield Beach, FL 33442 904-878-3994 305-421-7400 Mobile Division Tampa Bay Division 900 Lakeside Drive 6712 Benjamin Road, Suite 100 Mobile, AL 36609 Tampa, FL 33634 205-666-6633 813-885-7427 September, 1992 . ,. .-^-ri,C? TUT 00b *--"- ' 2.0 TABLE OF CONTENTS SECTION I.0 Title and Signature Page 2.0 Table of Contents 3.0 Statement of Policy 4.0 Project Organization and Responsibility 5.0 Quality Assurance Objectives (Precision, Accuracy, and PQLs) 6.0 Sampling Procedures 7.0 Sample Custody 8.0 Analytical Procedures 9.0 Calibration Procedures and Frequency 10.0 Preventive Maintenance > II.0 Quality Control Checks and Routines to Assess Precision and Accuracy and Calculations of Method Detection Limits 12.0 Data Reduction, Review and Reporting 13.0 Corrective Action 14.0 Performance and System Audits 15.0 Quality Assurance Reports 16.0 Personnel Qualifications, Resumes Appendix A: Method Validations Section 2 Revision 0 Date: 9/92 NUMBER OF PAGES 1 4 1 10 104 21 19 7 17 7 10 29 4 3 2 54 43 REV. 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 DATE 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 TUT 005 2370 LIST OF FIGURES FIGURE DESCRIPTION 4.1 Corporate Organizational Structure 4.2 Organizational Structure of Savannah Division Laboratory 4.3 Organizational Structure of Tallahassee Division Laboratory 4.4 Organizational Structure of Mobile Division Laboratory 4.5 Organizational Structure of Deerfield Beach Division Laboratory 4.6 Organizational Structure of Tampa Bay Division Laboratory 6.1 Sample and Container Label 6.2 Monitoring Well Sampling Log Form 6.3 Custody Form 7.1 Custody Form 7.2 Sample and Container Label 7.3 Container Preparation Log 7.4 Custody Seal 7.5 Sample Custody Excursion 7.6 Sample Registry Form 7.7 Sample Container Request Form (obverse) 7.8 Sample Container Request Form (reverse) 7.9 Cyanide Distillation Log 7.10 Cyanide Analysis Log 7.11 Semivolatile Extract Custody Log 11.1 Quality Control Chart - Accuracy (% Recovery) 11.2 Quality Control Chart - Precision (X RPD) Section 2 Revision 0 PAGE 4.5 4.6 4.7 4.8 4.9 4.10 6.17 6.18 6.19 7.2 7.3 7.5 7.6 7.7 7.9 7.12 7.13 7.15 7.16 7.17 11.8 11.9 Date : REVISION 0 0 0 - 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 9/92 of 4 DATE 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 TUT 005 2371 FIGURE DESCRIPTION 12.1 Flow Diagram of Computerized Laboratory Information Management Systems (LIMS) 12.2 Result Only Report 12.3 SL Level I Report 12.4 SL Level II Report 12.5 SL Level III Report 13.1 Corrective Action Report (CAR) Form 14.1 Laboratory Internal Systems Audit Checklist Section 2 Revision 0 Date: 9/92 PAGE REVISION DATE 12.2 12.10 12.13 12.18 12.23 13.2 14.2 0 0 0 0 0 0 0 9/92 9/92 9/92 9/92 9/92 9/92 9/92 TUT 005 2372 Section 2 Revision 0 Date: 9/92 5.3 LIST OF TABLES DESCRIPTION OF TABLES 5.1 Analytical Methods and Quality Assurance Objectives for Water 5.2 Analytical Methods and Quality Assurance Objectives for Soils and Sediments 5.3 Field Methods and Quality Assurance Objectives 5.100 6.1 Required Containers, Sample Preservation Techniques and Maximum Holding Times for Water Samples 6.2 Required Containers, Sample Storage Tech- niques and Recommended Holding Times for Soil or Sediment Samples 6.3 Approved Water and Wastewater Procedures, Containers, Preservation and Holding Times for Parameters Not Found in 40 CFR 136 6.4 Field Reagent Storage and Transport 8.1 Reagent Storage 8.2 Waste Disposal Procedures 9.1 Laboratory Instruments 9.2 Field Instruments 9.3 Standard Source and Preparation 9.4 Standardization of Titrating Solutions 10.1 Laboratory Equipment Preventive Maintenance Schedule 10.2 Field Equipment Preventive Maintanance Schedule 10.3 Balance Calibration Checks 11.1 Methods Used to Generate Accuracy and Precision Targets 12.1 Summary of Equations Used in Calculations 13.1 Corrective Action PAGE REVISION DATE 9/92 5.66 5.100 6.8 6.13 6.14 6.20 8.4 8.6 9.2 9.5 9.6 9.9 10.2 10.6 10.7 11.10 12.4 13.3 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 9/92 K> (Si in 13.2 Corrective Action Report Criteria for Control Charts 13.4 9/92 Section 3 Revision 0 Date: 9/92 3.0 STATEMENT OF POLICY Savannah Laboratories is committed to providing quality data and will endeavor to use good quality control and quality assurance practices for all field sampling and laboratory analytical procedures in order to ensure the best possible precision, accuracy, and representativeness of results from testing of environmental samples. The objectives of the QA program are to: (1) Properly collect, preserve, and store all samples; (2) Maintain adequate custody records from sample collection through reporting and archiving of results; (3) Use properly trained analysts to analyze all samples by approved methods and within holding times; (4) Produce QC verifiable data which can be documented to show that the system was calibrated and within precision and accuracy control limits; (5) Accurately calculate, check, and enter all data into the Laboratory Information Management System; and (6) Document all the above activities in order that all data can be independently validated. Savannah Laboratories intends to follow all procedures referenced in this plan and to conform to EPA and state regulatory agency guidelines for each project reported. Any changes in EPA or other regulatory procedures will be incorporated during periodic revisions of this plan. Adherence to the procedures of this plan is assured by the assignment of an experienced project manager to each project. The project manager coordinates and is responsible for all phases of Savannah Laboratories' involvement in the project, including pre-project planning, sample bottle preparation, field sampling, computer entry of work, approving analytical and quality control data, final review of report, and discussion of results with client. The project managers are assisted by QA managers and staff at each laboratory. The QA Plan will be utilized by all five Savannah Laboratories facilities. Additionally, all labs use identical Standard Operating Procedures (SOP), all data are incorporated into a single Laboratory Information Management System (LIMS) network which generates common QA limits, etc., and is accessible to all employees. Each project is directed by a single project manager who supervises all employees involved on the project, and also reviews, approves, and signs all data reports. The following sections of this QA plan detail the organizational structures and procedures through which all laboratory results are generated. TUT 005 2374 Section 4 Revision: 0 Dace 9/92 4.0 ORGANIZATION AND RESPONSIBILITY Savannah Laboratories and Environmental Services, Inc. has laboratory facilities in, and conducts field operations from, Savannah, Georgia; Tallahassee, Florida; Mobile, Alabama; Deerfield Beach, Florida; and Tampa, Florida. All five facilities are structured under a common administrative, data management, and quality assurance (QA) system as outlined in Figures 4.1, 4.2, 4.3, 4.4, 4.5, and 4.6. Duties of the key personnel are as follows: A) Company President 1) Establish corporate policy; 2) Plan and oversee laboratory infrastructure construction/acquisition; 3) Negotiate contractual agreements; and 4) Other administrative and budgetary functions. B) Company Vice President 1) Provide guidance to lab directors; 2) Establish and maintain company-client relationships; and 3) Assist president in establishing and carrying out corporate policy. C) Controller 1) Supervise administration section; 2) Prepare financial reports; 3) Coordinate risk management program; and 4) Assist corporate officers with budgetary problems. D) Corporate Technical Staff 1) Provide technical support for all divisions; 2) Coordinate technical activities affecting all divisions; 3) Write SOPs and other technical documents; and 4) Inform all divisions about new methods. TUT GO5 2375 Section 4 Revision: 0 Date 9/92 E) Business Manager 1) Supervise accounting section; 2) Coordinate purchases and payables; and 3) Maintain equipment inventory and business records. F) Laboratory Director 1) Responsible for day-to-day operation of lab; 2) Provide project manager guidance; 3) Establish production priorities; and 4) Approve hiring decisions. G) Project Manager 1) Initial contact with client on individual job tasks; 2) Prepare all work plans, schedules and manpower allocations; 3) Initiate all procurement for the projects; 4) Day-to-day supervision of the project team including analytical department managers, field sampling crews and data management personnel; 5) Coordinate financial and contractual aspects of the projects; 6) Provide formatting and technical review of all reports; 7) Provide day-to-day communication with the client; 8) Exercise final review and approval on all reports and invoices for the project; and 9) Respond to post project inquiries. H) QA Manager 1) Coordinate with the project manager, and laboratory manager in order to insure that project QA is maintained; 2) Be available to discuss QA activities and results with client; 3) Prepare QA reports to management; 4) Perform periodic system audits; TUT 005 2376 Section 4 Revision: 0 Date 9/92 5) Review not-in-compliance reports and approve corrective actions; 6) Coordinate the preparation and approval of all QA plans, method SOPs and QA audit responses; and 7) Coordinate and be present during all external QA Audits. I) Laboratory Manager 1) Coordinate all production activities; 2) Work with project managers to ensure project objectives are met; 3) Provide guidance to department managers; and 4) Interview and hire technical personnel. J) Sample/Data Manager 1) Schedule bottle orders and supervise bottle prep staff; 2) Supervise custody staff; 3) Coordinate with project manager and field/sampling manager on scheduling field sampling efforts; 4) Identify and document custody discrepancies and communicate with client on custody problems; and 5) Supervise data management staff including computer login, data entry, report preparation, and data archiving personnel. K) Field/Sampling Manager 1) Coordinate and schedule sampling crews; 2) Prepare sampling reports; and 3) Ensure sampling protocols are followed. L) Department Manager 1) Organize work flow in department; 2) Assure adequate inventory of reagents and equipment; 3) Ensure effective maintenance and repair of instrumentation; 4) Investigate and evaluate new methodology and equipment; and 5) Train new employees. TUT OO5 2377 Section 4 Revision: 0 Date 9/92 A list of all technical employees and resumes for each of the professionals in the organization are provided in Section 16.0. In case of instrument failure, high sample volume, or rapid turnaround requirements, samples are interchanged among the five facilities. In these situations, samples or preserved extracts are transported under EPA recommended chain-of-custody, handling and storage procedures. This inter-exchange of workload practice is possible because of single administrative structure, the use of identical analytical and QA protocols, and the fact that all five facilities are tied into (via telephone modem) a central computerized Laboratory Information Management System (LIMS). TUT O05 2378 Section 4 Revision: 0 Date 9/92 CO cc UJ RPORATE OFFICI SIDENT James W. Andrews o S O CL _J oz CORPORATE TECH Computer Manager Larry Phillips cr LU O z ^ CO CO LLIZ COD m [ PRESIDENT Janelte D. Lonq LU O o O ^ 6 I PRESIDENT Thomas L. Stephens g to LJ O C . D ^ __ « 5 Z p E >= 1 § § < o o • 2 0 0 D C 0 I c. < to cz LJ0 _ 2 ^ ** O L. L_ O c LU _J O 1 Oo RETARY/TREASURER/ Jay W. Andrews O LU CO CO CC o O 5 -1 = 1- -> E E 0 Q ujt- w LLI o LJ c: -J — <ls w ? M CD 2~5 j -> J-3 <r $ j en ^ i ^ i Vic Safely Director Paul Meyers Organic Manager Derrick M. Simo Inorganic Manager ^ Ernest D. Wnlloi Air Manager Wayne Rohbins COc LJ0 Zi oo Oz LU <o O ^ 1 h- ^ ^ i c < o ^ 1 T Z < o z c Z 5 _l CO .5 0 "« DEERFIELD DEACI-I Paul K. Canovar TAMPA DAY Kallierine W. Sh LJ 0 c H- 1 0 i5 ^ z s CORPORATE ORGA Fign TUT OO5 2379 Section 4 Revision: 0 Date 9/92 t^ U c •7 Gj 3 c Ulo 1i < SU3OVNVW PROJECT c 'o 35 SMOJ|HIV 'M SOUJUT c Ul O 2 2 O AU01V O Q j 3 j 5 U30VNX O Z 2 q UJ — c > "c Sicvon J. l.inda A. \ > a0 c _o C 'c '£> in0 "o o o C C Uc 2 « 2 c 1 1 c e. O .= o w s. - Vs j.. o in g C ° S > ^ ^ ° 53 5 1 5 •= *2 c ?• » ™ o ." o | ^I5<2^s ? 1 i g 1 >. 02 -5 re § re 00 5 = w r > r5 i§ ?|i|li §i mill o ^ . >s-jl 2 slijl^ li Q </3 Q C -^ ^ 1 |ll| 2 ^. r ^ *• _5 re o U' i; . M 5 0 "in! < Z t— cl "5 C C < 0 c O Ul <f> 0 Ul 5 c: c o ^ 0 £ 5 2 < O •z. c 2 > CO ^ O 5 | lo s _l 2 a 2 ^ 5 < §1 11 c « 0 TUT O05 !3SO Section 4 Revision: 0 Date 9/92 1- LLJ 0 A MANAGER nmnd SAMPLE/DAT Ynmilla S < C ( 4 , 1 < c c vJG MANAGER ELD/SAMPLIf = 12 5 2 < c. I * = e _i r 3 re £ i II ANAGER O < >RATORY Z l >. c. ~c -5 1 1 3 E U /) -J - zN U CC Ul ^ 1 1 1 1 c J> 0 ^ C-oo <" ^ 1 1 2 0 i re LLJ T ^ » 1-1 v> .H re w O C 2 > ^ 5 O -= 0 « _ §• t- 00 — < E 'c>^ O a cc S i s si o j c- c: re c c OT ^: o -5, o & ~ 5 ^ | 5 mi _c 1 1 1 is o ^ S •§ o -> Q O w" LJ O5c: II 131 < O Q 111 LU CO <1 ii< o o TUT O05 2381 CLIENT LABORATORY QA MANAGER Michele Lersch PROJECT MANAGERS Jesse Smith J. Michael Nance Laura B. Snead SAMPLE/DATA MANAGERS Rhoda Smith Wynn Morgan FIELD/SAMPLING MANAGERS Chris Cook Tim Bentley Jim Overman LABORATORY MANAGER Van Priam GENERAL Bruce Barrett Cedric Crawley Leslie Evans Cindy Evertsen Sonya Reynolds Nan Scarborough METALS Panda Carter Stephanie Jones Tracy Owens Ed Oetken Joyce Zatarain CHROMATOGRAPHY Becky Bowen John Sims Mary Thrasher Virginia Vasquez Shao-Wei Li MASS SPECTROSCOPY Cora Pate Cindy Wilson CD ORGANIZATIONAL STRUCTURE OF THE MOBILE DIVISION LABORATORY Figure 4-4 SL SAVANNAH LABORATORIES & ENVIRONMENTAL SERVICES. INC. m o yo co PJ PI n> <D OT rt < n fl> n> H" rt in (-•• oo vo K- o \ O 3 o vo g hh ro •• £- LABORATORY QA MANAGER Kathy Irminger BIOLOGICAL/GENERAL Maria Marstill Tammy Katsikis CLIENT PROJECT MANAGERS Paul Canevaro Rhonda Moll SAMPLE/DATA MANAGER Marianne Walker FIELD/SAMPLING MANAGER Phill Taylor DEPARTMENT MANAGERS Kim Kostzer Alicia Stewart Carol-Ann Vassell METALS Linda Backus Catherine Katsikis CHROMATOGRAPHY Kim Puhl Lawrence Teich Jaelle Ben Add! Hassan Jaddaoui Nanette Kendall GC/MS Dave Kavanaugh ORGANIZATIONAL STRUCTURE OF THE DEERFIELD BEACH DIVISION LABORATORY Figure 4-5 SL SAVANNAH LABORATORIES & ENVIRONMENTAL SERVICES. INC. >rJ O pa </> <jq n < O (H fl> H- rt (n H- VO VO H* O \ O 3 O vo 3 HI isi •• *- CLIENT LABORATORY QA MANAGER Inas M. Sobky PROJECT MANAGERS Kalhy Sheffield Andra Rachmaninoff Dominic Frnlli SAMPLE/DATA MANAGER Andy Singleton FIELD/SAMPLING MANAGER Chris Harris DEPARTMENT MANAGERS Tracy Botto Marsha Martinovich Tayseer Zayan H C GENERAL Chris Harris METALS Carl Hoover Anlonius Lebrun Judi Sandel CHROMATOGRAPIIY Linda Dowd Natalie Park Dawn Wallner MASS SPECTROSCOPY Cheryl Howard Talicia C. Smith ORGANIZATIONAL STRUCTURE OF THE TAMPA BAY DIVISION LABORATORY Figure 4-6 SL SAVANNAH LABORATORIES & ENVIRONMENTAL SERVICES. INC. CO -b >r> O ?o in to (U <T> (B CN rt < o n> o> (-•• rt w I-. VO (-•• O O 3 Section 5 Revision: 0 Date: 9/92 5.0 QUALITY ASSURANCE OBJECTIVES (PRECISION, ACCURACY, AND PQLs) Savannah Laboratories has a comprehensive quality assurance program which is based on the program outlined in EPA's Interim Guidelines and Specifications for Preparing Quality Assurance Project Plans (QAMS-005/80), in the Handbook for Analytical Quality Control in Water and Wastewater Laboratories (EPA, 1979) and in the Association of Official Analytical Chemists' Quality Assurance Principles for Analytical Laboratories. The key to Savannah Laboratories QA/QC program is strict adherence to the program during all phases of the project including: presampling discussions; sample collection, preservation, transportation and storage; sample login and tracking; laboratory analyses; and validation and reporting of results. Project and QC data from all facilities are entered into a single Laboratory Information Management System (LIMS). The LIMS provides a computerized mechanism for storing field and login information, tracking sample holding times, scheduling and preparing laboratory work sheets, storing results and QC data, reviewing results and relating them to their corresponding QC data, and printing reports and invoices. The Project Manager, QA Manager, and data management and reporting personnel have direct access via a CRT terminal to all project and QA data from all five facilities. Tables 5.1 and 5.2 list the laboratory parameters determined by Savannah Laboratories, the methodology, the QA objectives for precision, accuracy and the normal practical quantification limits (PQLs) for relatively clean environmental samples. Accuracy control limits are for lab control standards (LCS) or blank spike recoveries and do not apply to matrix spike (advisory only). Table 5.3 gives the same information for field parameters. PRECISION The Savannah Laboratories objective for precision is to meet the precision data generated by the applicable method validation on similar matrices. Relative percent difference (RPD) is used to express precision between two replicate values. In routine analyses, the values for most parameters are usually below PQLs; therefore, precision data are derived from duplicate matrix spike or lab control standard results. The relative percent difference (RPD) is calculated as: RPD - VI - V2 X 100 (VI + V2)/2 VI, V2 - The two values obtained by analyzing the duplicate samples. ACCURACY The Savannah Laboratories objective for accuracy is to meet the accuracy data generated by the applicable method validation on similar matrices. Percent recovery (XR) is used to express accuracy from the analysis of blank spikes and other QC samples. TUT 005 2385 Section 5 Revision: 0 Date: 9/92 The percent recovery (XR) is calculated as below: *R - SPV - SAV X 100 SA SAV - The background value, value obtained by analyzing the sample SA - Concentration of the spike added to the sample SPV - Value obtained by analyzing the sample with the spike added COMPARABILITY The Savannah Laboratories objective for comparability is to strive toward the comparability of sample parameters on similar matrices as they relate to precision and accuracy determinations. Strict adherence to QA/QC procedures promotes the comparability of one set of reference data to another or comparability of data among all facilities. REPRESENTATIVENESS The Savannah Laboratories objective for representativeness of field samples is to ensure that a set of data accurately depicts the distinguishing characteristic of a sample source. Representativeness is enhanced by an attempt to mix samples prior to aliquot removal. Results are considered reliable and representative if the sample distribution is within statistically defined bounds of the population mean and variance. TUT Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL PRACTICAL QUANTITATION LIMITS (PQL) PARAMETER Aluninun Antimony Arsenic Bariun Beryllium Boron Cadmium Calcium Chromium Chromium, hexavalent Cobalt Copper Iron Lead L i th i urn Magnesium Manganese METHOD (Prep) 200. 7A 200.7/6010(3010) Saltwater CLP 200.7/6010(3010***) 204.2/704 1(3005) CLP 200. 7A 200.7/6010(3010) 206.2/7060(3020***) 206.3/7061 206. 3/7061 -Saltwater CLP 200. 7A 200.7/6010(3010) CLP 200.7/6010(3010) 210.2/7091(3020) CLP 200.7/6010(3010***) 200. 7A 200.7/6010(3010) 213.2/7131(3020) Saltwater CLP 200.7/6010(3010) CLP 200. 7A 200.7/6010(3010) 218.2/7191(3020) CLP 7196 200.7/6010(3010) CLP 200. 7A 200.7/6010(3010) 220.1/220.2(3020) Saltwater CLP 200. 7A 200.7/6010(3010) 236.2(3020) Saltwater CLP 200. 7A 200.7/6010(3010) 239.2/7421(3020) Saltwater CLP 3500-Li B 200.7/6010(3010) CLP 200. 7A 200.7/6010(3010) CLP METHODS, QA OBJECTIVES AND FOR WATER AND OTHER LIQUIDS REFERENCE 65 3/2 5 45 3/2 3/2 45 65 3/2 3/2 3/2 3/2/5 45 65 3/2 45 3/2 3/2 45 3/2 65 3/2 3/2 5 45 3/2 45 65 3/2 3/2 45 2 3/2 45 65 3/2 3 5 45 65 3/2 3 5 45 65 3/2 3/2 5 45 4 3/2 45 65 3/2 45 ACCURACY* (X Rec) 75-125 75-125 50-140 80-120 75-125 75-125 80-120 75-125 75-125 75-125 60-140 60-140 80-120 75-125 75-125 75-125 75-125 75-125 80-120 75-125 75-125 75-125 75-125 60-140 80-120 75-125 80-120 75-125 75-125 75-125 80-120 75-125 75-125 80-120 75-125 75-125 75-125 60-140 80-120 75-125 75-125 75-125 60-140 80-120 75-125 75-125 75-125 60-140 80-120 75-125 75-125 80-120 75-125 75-125 80-120 PRECISION* (X RPD) 0-20 0-20 0-40 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-40 0-40 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-40 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-40 0-20 0-20 0-20 0-20 0-40 0-20 0-20 0-20 0-20 0-40 0-20 0-20 0-20 0-20 0-20 0-20 0-20 PQL** (ug/L) 20 200 10 200 50 20 60 10 100 10 2.0 0.10 10 1.0 10 200 5.0 5.0 5.0 50 0.50 5.0 1.0 0.050 5.0 500 5000 1.0 10 10 10 10 10 50 2.5 25 10 0.50 25 5.0 50 10 2.0 100 5.0 50 5.0 0.50 3.0 100 500 5000 1.0 10 15 TUT GO5 2387 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Mercury Molybdenun Nickel Phosphorus Potassium Selenium Si lica Si Iver Sodium Strontium Thallium Tin Titanium Tributyl tin Vanadium Zinc Zinc phosphide Zirconium METHOD (Prep) 245.1/7470 Saltwater CLP 200.7/6010(3010) 200. 7A 200.7/6010(3010) 249.2 Saltwater CLP 200.7***/6010***(3010***) 200.7/6010(3010) 258.1/7610(3010) CLP 200.7/6010(3010) 270.2/7740(3020***) 270.3/7741 270.3/7741 - Saltwater CLP 200.7/6010(3010***) 200. 7A 200.7/6010(3010***) 272.1 272.2/7761 Saltwater CLP 200.7/6010(3010) 273.1 CLP 200.7***/6010***(3010***) 200.7/6010(3010) 279.2/7841(3020) CLP 200.7***V/6010***V (3010***V) 282.2 200 . 7***/60 1 0*** ( 30 1 0*** ) Atomic absorption 200.7/6010(3010) CLP 200. 7A 200.7/6010(3010) Saltwater CLP FDER Special Method 200.7***/6010***(3010***) REFERENCE 3/2 5 45 4/2 65 3/2 3 5 45 3/2 3/2 3/2 45 3/2 3/2 3/2 3/2/5 45 3/2 65 3/2 3 3/2 5 45 3/2 3 45 3/2 3/2 3/2 45 3/2 3 3/2 40 3/2 45 65 3/2 5 45 31 2 ACCURACY* (X Rec) 75-125 60-140 80-120 75-125 75-125 75-125 75-125 60-140 80-120 75-125 75-125 75-125 80-120 75-125 75-125 60-140 60-140 80-125 75-125 75-125 75-125 75-125 75-125 60-140 80-120 75-125 75-125 80-120 75-125 75-125 75-125 80-120 75-125 75-125 75-125 60-140 75-125 80-120 75-125 75-125 60-140 80-120 10-210 75-125 PRECISION* (X RPD) 0-20 0-40 0-20 0-20 0-20 0-20 0-20 0-40 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-40 0-40 0-20 0-30 0-20 0-20 0-20 0-20 0-40 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-40 0-20 0-20 0-20 0-20 0-40 0-20 0-80 0-20 POL** (ug/L) 0.20 0.10 0.20 10 4.0 40 10 1.0 40 50 1000 100 5000 100 10 2.0 0.10 5.0 500 1.0 10 10 1.0 0.050 10 500 500 5000 10 500 10 10 50 50 10 0.0040 10 50 2.0 20 1.0 20 2.0 5000 TUT 005 2388 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Acidity Alkalinity Ammonia (as N) Ammonia, un-ionized Bicarbonate BOO Bromate Bromide Carbon, total organic Carbonate CBCO Chloride Chlorine, residual Chlorophyll COD Col i form, fecal, MPN Col i form, fecal, MF Col i form, total, MPN Col i form, total, MF Color Corrosivity Cyanate Cyanide, amenable to ch I or i nation Cyanide, reactive Cyanide, total Cyanide, weak and dissociable Fluon'de METHOD (Prep) 305.1/402 310.1/403 350.1 350.3 FL-DER 403 405.1/507 300.0 9056/300.0 320.1 415.1/9060 403 507 325.2 325.3/9252 407A 9056/300.0 408A 330.4 330.5 1002G 508B 410.2 410.4 908C 909C 908A 909A 110.2/204A 203 412K 9012 335.1/9010 7.3.3.2 335.3/9012 335.2/9010 CLP 412H 340.2 REFERENCE 3/4 3/4 3 3 60 4 3/4 3 2/3 3 3/2 4 4 3 3/2 4 2/3 4 3 3 4 4 3 3 4 4 4 4 3/4 4 4 2 3/2 2 3/2 3/2 45 4 3 ACCURACY* (X Rec) 75-125 75-125 90-110 75-125 NA NA 60-140 75-125 75-125 75-125 60-140 NA NA 85-115 75-125 75-125 75-125 NA NA NA NA 60-140 60-140 60-140 NA NA NA NA NA NA 60-140 NA NA NA 85-115 75-125 85-115 NA 75-125 PRECISION* (X RPD) 0-30 0-30 0-30 0-30 NA NA 0-30 0-30 0-30 0-30 0-40 NA 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 NA NA NA NA 0-40 NA 0-40 0-50 0-40 0-50 0-30 0-30 0-30 0-40 0-30 PQL** (•g/L) 10 1.0 0.030 0.050 0.010 1.0 2.0 1.0 1.0 2.0 1.0 1.0 2.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 0.00010 20 20 20 2 MPN/ 100 mL 1 col/100 mL 2 MPN/ 100 mL 1 col/100 mL 5 PCU NA 0.10 0.010 0.010 0.010 0.010 0.010 0.010 0.010 0.20 TUT OO5 2389 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL HETHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Formaldehyde Halogens, total organic Hardness, total Hydrogen ion (pH) Nitrate (as N) Nitrate-Nitrite (as N) I gn i lability Nitrite (as N) Nitrogen, total Kjeldahl (TKN) Nitrogen, organic Nitrogen, total Odor Oil & Grease Orthophosphate (as P) Oxygen, dissolved Petroleum hydrocarbons Phenol ics, total recoverable Phosphorus, organic (as P) Phosphorus, total (as P) Plate count, heterotrophic Radioactivity, alpha Radioactivity, beta Residue, dissolved Residue, suspended Residue, total Residue, volatile METHOD (Prep) N10SH 450.1/9020 314A 150.1/9040 353.2 9056/300.0 352.1 353.3 353.2 1010 353.2 354.1 9056/300.0 353.3 351.2 351.3 EPA-CE EPA-CE 140.1/207 413.1/503A 413.2/5038 365.1 365.2 365.3 9056/300.0 360.1 418.1/503E 420.2/9066 420.1/9065 365.4 365.4 365.3 365.2 907 900.0/9310/703 900.0/9310/703 160.1/209B 160.2/209C 160.3/209A 160.4/2090 REFERENCE 35 3/2 4 3/2 3 2/3 3 3 3 2 3 3 2/3 3 3 3 46 46 3/4 3/4 3/4 3 3 3 2/3 3 3/4 3/2 3/2 3 3 3 3 4 54/2/4 54/2/4 3/4 3/4 3/4 3/4 ACCURACY* (X Rec) 70-125 60-140 NA 90-110 85-115 75-125 75-125 75-125 85-115 NA 85-115 75-125 75-125 75-125 65-135 75-125 NA NA NA 60-140 60-140 80-120 75-125 75-125 75-125 NA 60-140 75-125 75-125 NA 60-140 60-140 60-140 NA 48-162 NA 75-125 75-125 60-140 NA PRECISION* (X RPO) 0-30 0-40 NA 0-10 0-30 0-30 0-30 0-30 0-30 NA 0-30 0-30 0-30 0-30 0-40 0-30 NA NA NA 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 NA 0-40 0-40 0-40 NA 0-25 0-25 0-30 0-30 0-40 0-40 POL** (ng/L) 0.25 0.010 3.3 NA 0.050 0.10 0.10 0.050 0.050 NA 0.050 0.050 0.050 0.050 0.10 0.10 0.10 0.15 1 TON 5.0 1.0 0.050 0.050 0.050 0.10 0.10 1.0 0.010 0.010 0.10 0.10 0.050 0.10 1000 CFU/L 2.0 pCi/L 2.0 pCi/L 5.0 5.0 5.0 5.0 TUT OO5 239O Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Salinity Settleable matter Silica, dissolved Specific conductance Specific gravity Streptococcus, fecal, HPN Streptococcus, fecal, MF Sulfate Sulfide Sulfide, reactive Sulfite Surfactants (NBAS) Temperature Thiocyanate THM formation potential Turbidity METHOD <Prep) 210 160.5/209E 370.1 120.1/9050 213E 910A 910B 9036 375.3 375.4 9056/300.0 376.2/427 9030 -SL 7.3.4.2 428 377.1 425.1 170.1 412. L 5710 180.1/214A REFERENCE 4 3/4 3 3/2 3 4 4 2 3 3 2/3 3/4 2 2 4 3 3 3 4 4 3/4 ACCURACY* (X Rec) NA NA 75-125 90-110 NA NA NA 80-120 75-125 75-125 75-125 60-140 50-150 NA 75-125 75-125 70-130 NA 60-140 NA 60-140 PRECISION* (X RPO) NA 0-40 0-30 0-10 NA NA NA 0-30 0-30 0-30 0-30 0-40 0-50 0-50 0-30 0-30 0-30 0-10 0-40 NA 0-30 PQL** (mg/L) 100 0.20 ml 10 1.0 umho/cm NA 2 HPN/100 ml 1 col/100 ml 5.0 5.0 5.0 5.0 0.40 0.40 0.40 1.0 1.0 0.10 NA 0.10 0.010 0.10 NTU TUT OO5 2391 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Bromodi ch loromethane Bromoform Ch 1 orodi bromome thane Chloroform (MS) Bromodi chtorome thane Bromoform Ch 1 orod i bromomet hane Chloroform (MS) Surrogate - Bromoch loromethane METHOD (Prep) 501.1/501.2 501.1/501.2 501.1/501.2 501.1/501.2 501.3 501.3 501.3 501.3 501.1/501.2/501.3 REFERENCE 49/50 49/50 49/50 49/50 30 30 30 30 49/50/30 ACCURACY* (XRec) 54-128 50-140 60-125 65-137 50-125 50-127 50-125 50-125 46-118 PRECISION* tt RPO) 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 NA PQL** (ug/D 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 NA TUT 2392 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Broroo benzene Bromochloromethane Bromodichloromethane Bromoform Bromomethane Carbon tetrachloride Chlorobenzene (MS) Chloroethanc Chloroform Chloromethane 2-Chlorotoluene 4-Chlorotoluene Dibromochloromethane 1,2-Dibromoethane D i bromomethane 1 , 2-D i ch lorobenzene 1 ,3-Dichlorobenzene 1 , 4-D i ch lorobenzene Dlchlorodif luoromethane 1,1-Dichloroethane 1 ,2-Dichloroethane 1,1-Dichloroethene (MS) cis-1 ,2-Dichloroethene trans-1 ,2-Dichloroethene 1 , 2 - D i ch I oropropane 1,3-Dichloropropane 2,2-Dichloropropane 1 , 1 - D i ch I oropropene cis-1 ,3-Dich I oropropene trans-1 ,3-Dichloropropene Methylene chloride 1,1,1 ,2-Tetrachloroethane 1 , 1 ,2,2-Tetrachloroethane METHOD (Prep) 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 REFERENCE 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 ACCURACY* (I Rec) 57-129 60-125 55-125 50-140 60-140 55-125 25-134 39-147 35-131 54-125 58-125 50-140 55-140 54-132 50-140 56-134 58-125 51-129 43-163 60-125 59-131 55-133 55-125 60-125 53-125 55-125 50-150 61-125 51-129 54-125 49-125 59-125 58-125 PRECISION* (X RPD) 0-40 0-40 0-40 0-40 0-40 0-40 0-29 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-29 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 PQL** (ug/L) 0.50 0.50 0.50 5.0 5.0 0.50 0.50 1.0 0.50 1.0 0.50 0.50 0.50 1.0 0.50 0.50 0.50 0.50 1.0 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 TUT 005 2393 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Tet rach I oroethene 1,1,1-Trichloroethane 1 , 1 ,2-Trichloroethane Trichloroethene (MS) Trichlorof luoromethane 1,2,3-Trichloropropane Vinyl chloride Surrogate - Bromochloromethane METHOD (Prep) 502.1 502.1 502.1 502.1 502.1 502.1 502.1 502.1 REFERENCE 51 51 51 51 51 51 51 51 ACCURACY* (X Rec) 50-125 55-125 57-125 51-142 55-125 59-130 55-155 46-118 PRECISION* (X RPD) 0-40 0-40 0-40 0-24 0-40 0-40 0-40 NA PQL** (ug/L) 0.50 0.50 0.50 0.50 0.50 1.0 1.0 NA TUT OO5 2394 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Acetone Benzene (HS) Bromobenzene Bromochloromethane Bromodichloromethane Bromoform Bromcxnethane n-Butylbenzene sec-Butylbenzene tert-Butylbenzene Carbon tetrachloride Chlorobenzene (MS) Chloroethane Chloroform Chloromethane 2-Chlorotoluene 4-Chlorotoluene D i bromoch loromethane 1,2-Dibromo-3-chloropropane 1 ,2-Dibromoe thane D i bromomethane 1 , 2 - D i ch I orobenzene 1,3-Dichlorobenzene 1 ,4-Dichlorobenzene Dichlorodif luoromethane 1,1-Dichloroethane 1,2-Dichloroethane 1,1-Dichloroethene (MS) cis-1 ,2-Dichloroethene trans-1,2-Dichloroethene 1 ,2-Dichloropropane 1 , 3 - D i ch 1 oropropane 2 , 2-0 i ch I oropropane 1 , 1 -D i ch loropropene cis-1, 3-Dichloropropene trans-1 ,3-Dichloropropene Ethyl benzene Hexachlorobutadiene 1 sopropylbenzene 4-Isopropyltolucne HETHOD (Prep) 502.2*** 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 REFERENCE 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 ACCURACY* <X Rec) 50-130 73-144 57-129 60-125 55-125 50-140 60- HO 55-125 55-125 55-125 55-125 25-134 39-147 35-131 54-125 58-125 50-140 55-140 57-129 54-132 50-140 56-134 58-125 51-129 43-163 60-125 59-131 55-133 55-125 60-125 53-125 55-125 50-150 61-125 51-129 54-125 55-125 55-125 55-125 55-125 PRECISION* (X RPO) 0-40 0-22 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-29 0-50 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-50 0-40 0-40 0-29 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 PQL** (ug/L) 25 0.50 0.50 0.50 0.50 1.0 1.0 0.50 0.50 0.50 0.50 0.50 1.0 0.50 1.0 0.50 0.50 0.50 5.0 1.0 0.50 0.50 0.50 0.50 1.0 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 TUT GO5 2395 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Methyiene chloride Methyl ethyl ketone 4-Methyl-2-pentanone Naphthalene P ropy I benzene Styrene 1,1, 1 ,2-Tetrach loroethane 1 , 1 ,2, 2-Tetrach loroethane Tetrachloroethene Toluene (MS) 1,2,3-Trichlorobenzene 1,2,4-Trichlorobenzene 1 ,1 , 1-Trich loroethane 1, 1, 2- T rich loroethane Trichloroethene (MS) T r i ch 1 orof I uorome thane 1,2,3-Trichloropropane . 1,2,4-Trimethylbenzene 1,3,5-Trimethylbenzene Vinyl chloride o-Xylene m-Xylene p-Xylene Surrogate - 2-Bromo-1-chloropropane Surrogate - Fluorobenzene METHOD (Prep) 502.2 502.2*** 502.2*** 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 502.2 REFERENCE 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 ACCURACY* (X Rec) 49-125 60-130 65-125 55-125 55-125 55-125 59-125 58-125 50-125 68-138 55-125 55-125 55-125 57-125 51-142 55-125 59-130 55-125 55-125 55-155 55-125 55-125 55-125 81-113 69-108 PRECISION* (X RPD) 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-17 0-40 0-40 0-40 0-40 0-24 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 NA NA POL** (ug/L) 1.0 10 10 0.50 0.50 0.50 0.50 1.0 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 1.0 0.50 0.50 1.0 0.50 0.50 0.50 NA NA TUT CO5 2396 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Benzene (MS) p-Bromof luorobenzene Broroo benzene n- Butyl benzene sec- Butyl benzene 2,3-Benzofuran tert-Butylbenzene Chlorobenzene (MS) o-Chlorotoluene p-Chlorotoluene p-Cymene Cyc 1 opropy I benz ene p-D ich I orobenzene m- D i ch I orobenzene o-D i ch I orobenzene Ethylbenzene Hexachlorobutadiene Isopropylbenzene Naphthalene n-Propylbenzene Styrene Toluene (MS) Trichloroethene Trichlorotoluene Tetrachloroethene 1 ,3,5-Trimethylbenzene 1 , 2,4-Trimethylbenzene 1 ,2,4-Trichlorobenzene 1 ,2,3-Trichlorobenzene p-Xylene m-Xylene o-Xylene Surrogate - a,a,a-Trif luorotoluene METHOD (Prep) 503.1 503.1*** 503.1 503.1 503.1 503.1*** 503.1 503.1 503.1 503.1 503.1*** 503.1*** 503.1 503.1 503.1 503.1 503.1 503.1 503.1 503.1 503.1 503.1 503.1 503.1*** 503.1 503.1 503.1 503.1 503.1 503.1 503.1 503.1 503.1 REFERENCE 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 ACCURACY* (X Ret) 73-144 58-125 55-125 30-126 47-125 35-125 51-125 25-134 55-125 58-125 57-125 60-125 63-127 65-125 58-125 66-125 23-125 61-125 57-135 56-125 50-125 68-138 68-125 56-125 60-128 52-125 48-125 55-127 52-125 58-125 56-125 59-125 77-140 PRECISION* (X RPO) 0-22 0-40 0-40 0-40 0-40 0-40 0-40 0-29 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-17 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 NA PQL** (ug/L) 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 NA TUT 2397 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Chloropicrin 1,2-Dibromoethane (MS) (ED8) 1,2-Dibrocno-3-chloropropane (MS) 1 , 1 - D i ch I oropropane 1 ,3-Dichloropropene Methyl isothiocyanate METHOD (Prep) 504***V 504 8011 504 8011 504***V 504***V 504***V REFERENCE 51 51 2 51 2 51 51 51 ACCURACY* (X Rec) 60-140 60-140 60-140 60-140 60-140 60-140 60-140 60-140 PRECISION* (X RPO) 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 PQL** (ug/L) 0.010 0.020 0.020 0.020 0.020 2.0 1.0 20 TUT 005 2398 O< Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Alachlor Aldrin Atrazine alpha BHC beta BHC delta BHC gamma BHC (Lindane) (MS) alpha Chlordane gamma Chlordane technical Chlordane Chloroneb Chlorobenzi late Chlorothalonil Dacthal (DCPA) 4,4'-DDD 4,4'-DDE 4,4'-DDT (MS) Dieldrin (MS) Endosulfan I Endosulfan II Endosulfan sulfate Endrin (MS) Endrin aldehyde Etridiazole Heptachlor (MS) Heptachlor epoxide Hexach I orobenzene Hexach 1 orocyc I opentad i ene Methoxychlor cis-Nonachlor trans-Nonachlor cis-Permethrin trans-Permethrin METHOD (Prep) 505 505/508 505 508 508 508 505/508 505/508 505/508 505 508 508 508 508 508 508 508 505/508 508 508 508 505/508 508 508 505/508 505/508 505/508 505 505/508 505 505 508 508 REFERENCE 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 5 51 51 51 51 51 51 51 51 ACCURACY* (X Rec) 48-156 48-124 20-159 52-132 55-135 57-147 52-136 51-147 51-147 31-141 51-143 58-148 51-131 53-153 57-157 51-147 67-137 51-143 47-127 52-132 41-163 57-142 48-128 58-143 42-129 47-127 34-164 26-120 37-163 49-171 47-133 51-131 61-151 PRECISION* (X RPD) 0-30 0-30 0-40 0-30 0-30 0-30 0-18 0-30 0-30 0-40 0-30 0-30 0-30 0-30 0-30 0-30 0-28 0-46 0-30 0-30 0-40 0-23 0-30 0-30 0-22 0-30 0-40 0-40 0-40 0-30 0-30 0-30 0-30 PQL** (ug/D 1.0 0.010 1.0 0.010 0.020 0.010 0.010 0.010 0.010 0.10 0.50 0.20 0.20 0.20 0.020 0.020 0.050 0.020 0.020 0.050 0.10 0.020 0.10 0.10 0.010 0.020 0.050 0.20 0.50 0.050 0.020 1.0 1.0 TUT 005 2399 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR HATER AND OTHER LIQUIDS PARAMETER Propachlor Simazine Toxaphene Trif luralin PCB 1016 PCS 1221 PCB 1232 PCB 1242 PCB 1248 PCB 1254 PCB 1260 Surrogate - Dibutylchlorendate (OBC) Surrogate - 2,4,5,6-Tetrachloro-m-xylene (TCMX) Surrogate - Decachlorobiphenyl (DCS) METHOD <Prep) 508 505 505/508 508 505/508 505/508 505/508 505/508 505/508 505/508 505/508 505/508 505/508 505/508 REFERENCE 51 51 51 51 51 51 51 51 51 51 51 51 51 51 ACCURACY* (X Rec) 58-131 56-132 60-168 58-119 50-130 50-130 50-123 50-130 50-130 28-148 28-148 28-151 22-126 25-126 PRECISION* (X RPD) 0-30 0-40 0-40 0-30 0-40 0-40 0-40 0-40 0-40 0-40 0-40 NA NA NA POL** (ug/L) 1.0 1.0 1.0 0.050 0.50 0.50 0.50 0.50 0.50 0.50 0.50 NA NA NA TUT OO5 24GO Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Alachlor (MS) Ametryn Atraton Atrazine (MS) Bromacil Butachlor Butylate Carboxin Chlorpropham Cycloate Demeton Diazinon (MS) Dichlorvos Diphenamid Disulfoton EPTC Ethoprop Fenamiphos Fenarimol Fluridone Hexazinone (MS) Merphos Metalaxyl Metolachlor Metribuzin Mevinphos MGK 264 Molinate (MS) Napropamide Norf lurazon Parathion, ethyl (MS) Parathion, methyl Pebulate METHOD (Prep) 507 507 507 507 507 507 507 507 507 507 507*** 507 507 507 507 507 507 507 507 507 507 507 507*** 507 507 507 507 507 507 507 507*** 507*** 507 REFERENCE 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 ACCURACY* (X Rec) 45-140 51-131 47-135 40-125 55-127 56-136 38-145 62-142 49-137 46-159 50-140 40-140 57-137 53-133 10-178 46-154 55-120 58-122 59-139 51-123 50-130 56-136 40-160 53-133 61-141 51-139 50-150 37-127 61-141 54-134 18-171 50-135 58-130 PRECISION* (X RPO) 0-30 0-30 0-30 0-30 0-30 0-30 0-76 0-30 0-30 0-47 0-30 0-30 0-30 0-30 0-60 0-55 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-74 0-30 0-30 0-28 0-30 0-30 PQL** (ug/L) 1.0 1.0 5.0 1.0 2.0 1.0 2.0 1.0 1.0 2.0 2.5 1.0 1.0 2.0 2.0 2.0 2.5 1.0 1.0 5.0 1.0 2.5 1.0 1.0 1.0 10 20 2.0 1.0 1.0 1.0 1.0 2.0 TUT OO5 24O1 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Prometon Prometryn Pronamide Propazine Simaiine (MS) Simetryn Stirophos Tebuthiuron Terbacil Terbufos Tcrbutryn Triademefon Vernolate Surrogate - Tripheny (phosphate METHOD (Prep) 507 507 507 507 507 507 507 507 507 507 507 507 507 507 REFERENCE 51 51 51 51 51 51 51 51 51 51 51 51 51 51 ACCURACY* (Z Rec) 42-114 51-125 51-131 60-124 60-140 59-139 58-138 48-120 57-137 57-137 58-130 61-125 53-133 40-125 PRECISION* (X RPO) 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 NA POL** (ug/L) 1.0 1.0 2.0 1.0 1.0 1.0 10 5.0 10 1.0 1.0 1.0 2.0 NA TUT 24O2 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Acif luorfen Bentazon Chloramben 2,4-D (MS) Oalapon 2,4-DB D i camba 3,5-Dichlorobenzoic acid Dichlorprop D i noseb 5 - Hydroxydi camba 4-Nitrophenol Pentachlorophenol Picloram 2,4,5-T 2,4,5-TP (Silvex) (MS) METHOD (Prep) 515.1 515.1 515.1 515.1 515.1 515.1 515.1 515.1 515.1 515.1 515.1 515.1 515.1 515.1 515.1 515.1 REFERENCE 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 ACCURACY* (X Rec) 21-185 32-182 53-169 25-129 40-160 48-126 40-144 53-151 46-168 49-129 53-153 25-229 36-224 44-138 25-145 10-151 PRECISION* (X RPO) 0-40 0-40 0-40 0-60 0-50 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-62 0-81 PQL** (ug/L) 1.0 1.0 1.0 0.50 10 0.50 0.50 1.0 0.50 0.50 1.0 1.0 1.0 0.50 0.50 0.50 r(JT QO5 24 O3 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Benzene (MS) Bromo benzene Bromochloromethane Bromodi ch loromethane Bromofonn Bromomethane n-Butylbenzene sec -Butyl benzene tert- Butyl benzene Carbon tetrachloride Chlorobenzene (HS) Chloroethane Chloroform Ch loromethane 2-Chlorotoluene 4-Chlorotoluene D i bromoch 1 oromethane 1,2-Dibronw-3-chloropropane 1,2-Dibromoethane Dibromomethane 1 ,2-Dichlorobenzene 1 ,3-Oichlorobenzene 1 , 4 - D i ch I o robenzene D i ch lorodi f I uoromethane 1 ,1-Dichloroethane 1,2-Di Chloroethane 1,1-Dichloroethene (MS) cis-1 ,2-Dichloroethene trans-1 ,2-Dichloroethene 1,2-Oichloropropane 1,3-Dichloropropane 2,2-Dichloropropane 1 , 1 • D i ch I oropropene METHOD (Prep) 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 REFERENCE 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 ACCURACY* (X Rec) 73-144 62-122 50-150 49-151 60-130 50-150 50-150 50-150 50-150 55-121 68-136 50-150 63-133 50-150 50-150 50-150 47-137 46-154 51-135 58-130 60-130 50-150 63-151 60-132 65-135 57-127 60-136 50-150 58-128 61-131 60-130 50-150 50-150 PRECISION* (X RPO) 0-22 0-30 0-40 0-40 0-30 0-40 0-40 0-40 0-40 0-40 0-17 0-40 0-30 0-40 0-40 0-40 0-40 0-40 0-30 0-30 0-30 0-40 0-30 0-30 0-30 0-30 0-19 0-40 0-30 0-30 0-30 0-40 0-40 POL** (ug/L) 1.0 1.0 1.0 1.0 1.0 2.0 1.0 1.0 1.0 1.0 1.0 2.0 1.0 2.0 1.0 1.0 1.0 2.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 TUT ?404 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER cis-1,3-Dichloropropene trans-1,3-Dichloropropene Ethylbenzene Hexachlorobutadiene I sopropy I benzene 4 - 1 sopropy 1 1 o I uene Methylene chloride Naphthalene n- P ropy I benzene Styrene 1,1, 1 ,2-Tetrachloroethane 1,1,2,2-Tetrachloroethane Tetrachloroethene Toluene (MS) 1 ,2,3-Trichlorobenzene 1 ,2,4-Trichlorobenzene 1,1, 1 -Trich loroethane 1 , 1 ,2-Trich loroethane Trich loroethene (MS) Trichlorof luoromethane 1 ,2,3-Trichloropropane 1 ,2,4-Trimethylbenzene 1 ,3,5-Trimethylbenzene Vinyl chloride o-Xylene m-Xylene p-Xylene Surrogate - p-Bromof luorobenzene Surrogate - 1 ,2-Dichlorobenzene-d4 METHOD (Prep) 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 524.2 REFERENCE 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 ACCURACY* (X Rec> 50-150 50-150 50-150 50-150 50-150 50-150 40-160 50-150 50-150 50-150 50-150 62-150 60-126 68-138 50-150 50-150 65-135 50-150 66-136 69-139 50-150 50-150 50-150 34-131 62-132 50-150 61-141 79-125 77-135 PRECISION* (X RPO) 0-40 0-40 0-40 0-40 0-40 0-40 0-50 0-40 0-40 0-30 0-40 0-30 0-30 0-17 0-40 0-40 0-30 0-40 0-20 0-30 0-40 0-40 0-40 0-30 0-30 0-40 0-30 NA NA PQL** (ug/L) 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 NA NA Till OO'5 2405 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Acenaphthylene Alachlor Aldrin (MS) Anthracene Atrazine (MS) Benz(a)anthracene Benzo(b)f luoranthene Benzo(k)f luoranthene Benzo(a)pyrene Benzo(g,h, i )perylene Butyl benzyl phthalate alpha Chlordane gamma Chlordane Chrysene Dibenz(a,h)anthracene Di-n-butyl phthalate Diethylphthalate bis(2-ethylhexyl)adipate bis(2-ethylhexyl)phthalate Dimethylphthalate Endrin Fluorene Heptachlor Heptachlor epoxide Hexach I orobenzene Hexach 1 orocyc I opentadi ene Indeno(1,2,3-cd)pyrene Lindane (MS) Hethoxychlor trans-Nonachlor Pentachlorophenol (MS) Phenanthrene Pyrene (MS) METHOD (Prep) 525 525 525 525 525 525 525 525 525 525 525 525 525 525 525 525 525 525 525 525 525 525 525 525 525 525 525 525 525 525 525 525 525 REFERENCE 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 51 ACCURACY* (X Rec) 49-131 40-136 42-116 20-150 43-177 30-150 20-128 30-150 20-160 10-140 30-130 43-167 41-159 30-150 10-110 20-164 22-180 27-125 28-142 20-150 20-163 36-184 25-150 30-158 6-144 9-140 16-150 52-136 6-182 45-125 15-139 45-138 36-153 PRECISION* (X RPD) 0-40 0-40 0-25 0-40 0-50 0-50 0-40 0-40 0-40 0-50 0-40 0-40 0-40 0-40 0-50 0-50 0-50 0-50 0-50 0-40 0-40 0-50 0-40 0-40 0-40 0-50 0-50 0-18 0-50 0-40 0-39 0-40 0-21 PQL** (ug/D 0.50 1.0 1.0 0.50 2.0 0.50 0.50 0.50 0.50 0.50 1.0 1.0 1.0 0.50 0.50 10 2.0 1.0 2.0 1.0 5.0 0.50 1.0 1.0 0.50 0.50 0.50 1.0 1.0 1.0 3.0 0.50 0.50 TUT 2406 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Simazine Toxaphene METHOD (Prep) 525 525 REFERENCE 51 51 ACCURACY* (X Rec) 40-167 20-142 PRECISION* (X RPO) 0-50 0-50 POL** (ug/L) 2.0 50 PCBs: 2-Chlorobiphenyl 2,3-Dichlorobiphenyl 2,4,5-Trichlorobiphenyl 2,2',4,4'-Tetrachlorobiphenyl (MS) 2,2' ,3' ,4,6-Pentachlorobiphenyl 2,2',4,4',5,6'-Hexachlorobiphenyl 2,2',3,3',4,4',6-Hcptachlorobiphenyl 2,2',3,3',4,5',6,6'-Octachlorobiphenyl Surrogate - Perylene-d12 Surrogate - Pyrene-d10 525 525 525 525 525 525 525 525 525 525 51 51 51 51 51 51 51 51 51 51 38-142 34-136 10-150 10-150 10-150 10-150 10-150 10-150 40-150 40-150 0-40 0-40 0-50 0-50 0-50 0-50 0-50 0-50 NA NA 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 NA NA TUT 005 2407 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Aldicarb Aldicarb sulfone Aldicarb sutfoxide Carbaryl Carbofuran Ethylene thiourea 3- Hydroxycarbof uran Methiocarb Hethomyl Oxamyl Propoxur (Baygon) METHOD (Prep) 531.1 531.1 531.1 531.1 531.1 531.1*" 531.1 531.1 531.1 531.1 531.1 REFERENCE 33/51 33/51 33/51 33/51 33/51 51 33/51 51 33/51 33/51 33/51 ACCURACY* (X Rec) 50- HO 55-130 40-160 55-130 50-130 40-140 60-140 53-121 50-150 40-160 50-125 PRECISION* (X RPO) 0-20 0-20 0-40 0-30 0-20 0-50 0-20 0-40 0-20 0-30 0-40 PQL** (ug/L) 0.50 0.50 0.50 1.0 1.0 10 1.0 5.0 1.0 1.0 1.0 TUT 2408 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL HETHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Glyphosate Endothal Diquat Paraquat METHOD (Prep) 547 548 549/HRS 549/HRS REFERENCE 51 51 51/56 51/56 ACCURACY* (X Rec) 40-160 20-180 10-150 10-150 PRECISION* (X RPO) 0-50 0-50 0-50 0-50 POL** (ug/L) 50 25 1.0 1.0 TUT 24O9 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Benzyl chloride Bromo benzene Bromodich loromethane Bromoform Bromomethane Carbon tetrachloride Chlorobenzene (MS) Chloroethane Chloroform 1-Chlorohexane 2-Chloroethylvinyl ether Chloromethane Chlorotoluenes D i bromoch loromethane Dibromomethane 1,2-Dichlorobenzene 1,3-Dichlorobenzene 1 ,4-Dichlorobenzene 0 ich 1 orodif luoromethane 1.1-Dichloroethane 1,2-Di chloroethane 1,1-Dichloroethene (MS) cis/trans-1 ,2-D ich loroethene D ich loromethane (methylene chloride) 1 ,2-Dichloropropane cis/trans-1 ,3-Oichloroprooylene 1,1,2,2-Tetrachloroethane 1 ,1 ,1 ,2-Tetrachloroethane Tetrachloroethylene 1 ,1 ,1-Tri chloroethane 1 , 1 ,2-Tri chloroethane Tr ich loroethene (MS) T r i ch I orof I uoromethane METHOD (Prep) 8010(5030) 8010(5030) 601/8010(5030) 601/8010(5030) 601/8010(5030) 601/8010(5030) 601/8010(5030) 601/8010(5030) 601/8010(5030) 8010(5030) 601/8010(5030) 601/8010(5030) 8010(5030) 601/8010(5030) 8010(5030) 601/8010(5030) 601/8010(5030) 601/8010(5030) 601/8010(5030) 601/8010(5030) 601/8010(5030) 601/8010(5030) 601/8010(5030) 601/8010(5030) 601/8010(5030) 601/8010(5030) 601/8010(5030) 8010(5030) 601/8010(5030) 601/8010(5030) 601/8010(5030) 601/8010(5030) 601/8010(5030) REFERENCE 2 2 1/2 1/2 1/2 1/2 1/2 1/2 1/2 2 1/2 1/2 2 1/2 2 1/2 1/2 1/2 1/2 1/2 1/2 1/2 1/2 1/2 1/2 1/2 1/2 2 1/2 1/2 1/2 1/2 1/2 ACCURACY* (X Rec) 50-150 70-130 42-172 13-159 10-144 43-143 25-134 46-137 49-133 50-150 14-186 10-193 70-130 24-191 70-130 10-208 10-187 42-143 70-130 47-132 51-147 55-133 38-155 25-162 44-156 22-178 10-184 70-130 26-162 41-138 39-136 51-142 21-156 PRECISION* (X RPD) 0-30 0-30 0-30 0-30 0-30 0-30 0-29 0-30 0-30 0-30 0-80 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-29 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-24 0-30 POL** Cug/L) 1.0 10 1.0 5.0 1.0 1.0 1.0 1.0 1.0 1.0 10 1.0 10 1.0 5.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 TUT 241C Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER 1,2,3-Trichloropropane Vinyl chloride 1,2-Dibromoethane (EOB) Surrogate - Bromochloromethane METHOD (Prep) 8010(5030) 601/8010(5030) 8010***(5030)' 601/8010(5030) REFERENCE 2 1/2 2 1/2 ACCURACY* (X Rec) 50-150 28-163 75-125 46-118 PRECISION* (X RPO) 0-30 0-30 0-30 NA POL** (ug/L) 1.0 1.0 1.0 NA EDB determined on Hall detector with PQL of 1.0 ug/L at client's request. TUT 005 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Acetone 2-Butanone (HEK) Di ethyl ether Et Hanoi Ethyl methacrylate Isobutanol Isopropanol Methacrylonitrile Hethanol Methyl methacrylate 4-Methyl-2-pentanone (MIBK) Methyl t-butyl ether (MTBE) Propionitri le Gasoline Mineral spirits Methanol (MS) Ethanol n- Propane I Isopropanol (MS) n-Butanol Isobutanol Ethylene glycol (MS) Propylene glycol Diethylene glycol Triethylene glycol Tetraethylene glycol METHOD (Prep) 8015***(5030) 8015(5030) 8015(5030) 8015(5030) 8015***(5030) 8015***(5030) 8015***(5030) 8015***(5030) 8015***(5030) 8015***(5030) 8015(5030) 80 15*** (5030) 8015***(5030) 8015 (modified) 8015 (modified) 8015 (modified/DAI*) 8015 (modified/DAI*) 8015 (modified/DAI*) 8015 (modified/DAI*) 8015 (modified/DAI*) 8015 (modified/DAI*) 8015 (modified/DAI*) 8015 (modified/DAI*) 8015 (modified/DAI*) 8015 (modified/DAI*) 8015 (modified/DAI*) REFERENCE 2 2 2 2 2 2 2 2 2 2 2 2 2 12 12 2 2 2 2 2 2 2 2 2 2 2 ACCURACY* (X Rec) 40-130 60-130 10-130 20- HO 42-125 50-125 30-140 10-140 50-150 45-132 65-125 50-150 10-130 40-140 40-140 50-150 50-150 50-150 50-150 50-150 50-150 50-150 50-150 50-150 50-150 50-150 PRECISION* (X RPO) 0-30 0-40 0-50 0-45 0-40 0-40 0-40 0-60 0-40 0-42 0-40 0-30 0-50 0-40 0-40 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 POL** (ug/D 25 25 25 1000 10 1000 1000 100 1000 10 25 10 100 50 50 1000 1000 1000 1000 1000 1000 10000 10000 10000 10000 25000 * DAI = Direct Aqueous Injection TUT 2412 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Benzene (MS) Chlorobenzene (HS) 1 ,2-Dichlorobenzene 1 ,3-Dichlorobenzene 1,4-Dichlorobenzene Ethyl benzene Methyl t-butyl ether Toluene (HS) Xylenes Surrogate - a, a, a-Trif luorotoluene METHOD (Prep) 602/8020(5030) 602/8020(5030) 602/8020(5030) 602/8020(5030) 602/8020(5030) 602/8020(5030) 602/8020***(5030) 602/8020(5030) 602***/8020(5030) 602/8020(5030) REFERENCE 1/2 1/2 1/2 1/2 1/2 1/2 1/2 1/2 2 1/2 ACCURACY* (X Rec) 61-131 54-136 37-154 50-141 42-143 32-160 50-150 64-144 50-150 77-140 PRECISION* (X RPD) 0-25 0-24 0-30 0-30 0-30 0-30 0-30 0-29 0-30 NA PQL** (ug/L) 1.0 1.0 1.0 1.0 1.0 1.0 10 1.0 1.0 NA TUT COS 241!'*; Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Acrolein Acrylonitrile Acetonitrile METHOD (Prep) 603/8030(5030) 603/8030(5030) 8030*** (5030) REFERENCE 1/2 1/2 2 ACCURACY* (X Rec) 88-118 71-135 20-115 PRECISION* (X RPO) 0-30 0-30 0-30 POL** (ug/D 200 100 1000 TUT 005 2414 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER 2-Chlorophenol (MS) 4-Chloro-3-methylphenol (MS) 2,4-Dichlorophenol 2,4-Dimethylphenol 2,4-Dinitrophenol 2-Methyl-4,6-dinitrophenol 3-Methyl phenol (m-cresol) 2-Methyl phenol (o-cresol) 4-Methyl phenol (p-cresol) Cresols 2-Nitrophenol 4-Nitrophenol (MS) Pentachlorophenol (MS) Phenol (HS) Trichlorophenols 2,3,4,5-Tetrachlorophenol 2,3,4,6-Tetrachlorophenol Tetrachlorophenols 2,4,5-Trichlorophenol 2,4,6-Tn'chlorophenol Surrogate - 2 , 4 , 6- T r i bromopheno I METHOD (Prep) 604/8040(3520) 604/8040(3520) 604/8040(3520) 604/8040(3520) 604/8040(3520) 604/8040(3520) •"8040(3520) ***8040(3520) ***8040(3520) 8040(3520) 604/8040(3520) 604/8040(3520) 604/8040(3520) 604/8040(3520) 8040(3520) ***8040(3520) ***8040(3520) 8040(3520) ***8040(3520) 604/8040(3520) 604/8040(3520) REFERENCE 1/2 1/2 1/2 1/2 1/2 1/2 2 2 2 2 1/2 1/2 1/2 1/2 2 2 2 2 2 1/2 1/2 ACCURACY* (X Rec) 30-111 41-107 44-119 24-118 12-145 30-136 10-150 10-150 10-150 NA 43-117 10-140 10-135 10-122 NA 50-150 50-150 NA 53-119 53-119 32-160 PRECISION* (X RPO) 0-26 0-23 0-40 0-40 0-65 0-40 0-50 0-50 0-50 NA 0-40 0-40 0-41 0-60 NA 0-40 0-40 NA 0-40 0-40 NA PQL** (ug/L) 10 10 10 10 50 50 10 10 10 10 10 50 50 10 10 20 20 20 10 10 NA TUT 005 2415 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL HETHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Dichlorophen Hexachlorophene METHOD (Prep) 604.1 604.1 REFERENCE 18 18 ACCURACY* (X Rec) 22-125 73-125 PRECISION* (X RPO) 0-30 0-30 PQL** (ug/L) 10 10 TUT 005 2416 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Bis(2-ethylhexyl) phthalate (MS) Butyl benzyl phthalate (MS) Diethyl phthalate (MS) Dimethyl phthalate (MS) Di-n-butyl phthalate (MS) Di-n-octyl phthalate (MS) Surrogate - 2- F luorobi phenyl METHOD (Prep) 606/8060(3520) 606/8060(3520) 606/8060(3520} 606/8060(3520) 606/8060(3520) 606/8060(3520) 606/8060(3520) REFERENCE 1/2 1/2 1/2 1/2 1/2 1/2 1/2 ACCURACY* (X Rec) 10-162 10-137 10-142 10-158 18-137 12-145 27-123 PRECISION* (X RPD) 0-82 0-73 0-47 0-63 0-46 0-52 NA P<JL** (ug/D 10 10 10 10 10 10 NA TUT OO5 2417 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Aldrin (MS5 Benf luralin alpha BHC beta BHC delta BHC gamma BHC (Lindane) (HS5 Carbophenothion alpha Chlordane gamma Chlordane technical Chlordane Chlorobenzi late Chlorothaloni I 4, 4- -ODD 4,4'-DDE 4,4'-DDT (MS5 Dicofol «elthane5 Dieldrin (MS5 Endosulfan I Endosulfan 11 Endosulfan sulfate Endrin (MS5 Endrin aldehyde Endrin ketone METHOD (Prep) 608/8080(35205/617 CUP - 2/88; 3/90 608/8080(35205"* 608/8080(35205/617 CLP - 2/88; 3/90 608/8080(35205/617 CLP - 2/88; 3/90 608/8080(35205/617 CLP - 2/88; 3/90 608/8080(35205/617 CLP - 2/88; 3/90 608/8080***(35205 608/8080(35205/617 CLP - 2/88 CLP - 3/90 608/8080(35205/617 CLP - 2/88 CLP - 3/90 608/8080(35205/617 8081***V(35205 608/8080***(35205 608/8080(35205/617 CLP - 2/88; 3/90 608/8080(35205/617 CLP - 2/88; 3/90 608/8080(35205/617 CLP - 2/88; 3/90 8081***V(35205 608/8080(35205/617 CLP - 2/88; 3/90 608/8080(35205/617 CLP - 2/88; 3/90 608/8080(35205/617 CLP - 2/88; 3/90 608/8080(35205/617 CLP - 2/88; 3/90 608/8080(35205/617 CLP - 2/88; 3/90 608/8080(35205/617 CLP - 3/90 CLP - 2/88; 3/90 REFERENCE 1/2/26 6/62 1/2 1/2/26 6/62 1/2/26 6/62 1/2/26 6/62 1/2/26 6/62 1/2 1/2/26 6 62 1/2/26 6 62 1/2/26 2 1/2 1/2/26 6/62 1/2/26 6/62 1/2/26 6/62 1/2 1/2/26 6/62 1/2/26 6/62 1/2/26 6/62 1/2/26 6/62 1/2/26 6/62 1/2/26 62 6/62 ACCURACY* (X Rec) 42-116 40-120 40-140 37-134 17-147 19-140 52-136 56-123 50-110 45-140 45-140 45-119 50-150 55-125 31-141 30-145 67-137 38-127 55-115 51-143 52-126 45-153 10-202 26-144 57-142 56-121 10-150 NA PRECISION* (X RP05 0-25 0-22 0-40 0-40 0-40 0-40 0-18 0-15 0-40 0-40 0-40 0-40 0-40 0-30 0-50 0-50 0-28 0-27 0-40 0-46 0-18 0-40 0-65 0-50 0-23 0-21 0-50 NA PQL** (U9/L5 0.050 0.050 0.010 0.050 0.050 0.050 0.050 0.050 0.050 0.050 0.050 1.0 0.050 0.50 0.050 0.050 0.50 0.050 0.50 0.50 0.20 0.10 0.10 0.10 0.10 0.10 0.10 0.050 0.10 0.10 0.050 0.050 0.10 0.10 0.10 0.10 0.10 0.10 0.10 0.10 0.10 TUT OO5 2413 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Heptachlor (HS) Heptachlor epoxide Isodrin Kepone Methoxychtor Mi rex Toxaphene Trif luralin PCS 1016 PCB 1221 PCS 1232 PCB 1242 PCB 1248 PCB 1254 PCB 1260 Surrogate - Dibutylchlorendate (OBC) Surrogate - 2,4,5,6-Tetrachloro-m-xytene (TCMX) Surrogate - Decachlorobiphenyl (DCB) METHOD (Prep) 608/8080(3520)/617 CLP - 2/88; 3/90 608/8080(3520)/617 CLP - 2/88; 3/90 8081***V(3520> 8081***V(3520) 8080(3520)/617 CLP - 2/88; 3/90 8081***V(3530) 608/8080(3520)/617 CLP - 2/88 CLP - 3/90 608/8080***(3520) 608/8080<3520)/617 CLP - 2/88 CLP - 3/90 608/8080(3520 )/61 7 CLP - 2/88 CLP - 3/90 608/8080(3520)/617 CLP - 2/88 CLP - 3/90 608/8080(3520 )/61 7 CLP - 2/88 CLP - 3/90 608/8080(3520)/617 CLP - 2/88 CLP - 3/90 608/8080 ( 35 20 )/6 17 CLP - 2/88; 3/90 608/8080(3520)/617 CLP - 2/88; 3/90 608/8080{3520)/617 CLP - 2/88 608/8080 ( 3520 )/6 17 CLP - 3/90 608/8080(3520}/617 CLP - 3/90 REFERENCE 1/2/26 6/62 1/2/26 6/62 2 2 2/26 6/62 2 1/2/26 6 62 1/2 1/2/26 6 62 1/2/26 6 62 1/2/26 6 62 1/2/26 6 62 1/2/26 6 62 1/2/26 6/62 1/2/26 6/62 1/2/26 6 1/2/26 62 1/2/26 62 ACCURACY* <X Rec) 42-129 40-131 37-142 55-110 10-150 50-140 52-112 41-140 54-124 69-107 15-178 10-215 39-150 38-158 66-122 58-122 28-151 24-154 22-126 60-150 25-126 60-150 PRECISION* (X RPO) 0-22 0-20 0-40 0-40 0-50 0-40 0-37 0-50 0-40 0-21 0-20 0-20 0-20 0-20 0-23 0-20 NA NA NA NA NA NA POL** (ug/L) 0.050 0.050 0.050 0.050 0.050 0.10 0.50 0.50 0.50 5.0 1.0 5.0 0.010 1.0 0.50 1.0 2.0 0.50 2.0 1.0 0.50 1.0 1.0 0.50 1.0 1.0 0.50 1.0 1.0 1.0 1.0 1.0 NA NA NA NA NA NA TUT 005 2419 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL HETHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Chloroneb Chloropropylate Chlorobenzilate (MS) Etridiazole PCNB Propachtor Chlorothaloni I DCPA (Oacthal) Dichloran Methoxychlor Perrnethrin Surrogate - Dibutylchlorendate (DBC) Surrogate - 2,4,5,6-Tetrachloro-m-xylene (TCHX) METHOD (Prep) 608.1 608.1 608.1 608.1 608.1 608.1 608.2 608.2 608.2 608.2 608.2 608.1/608.2 608.1/608.2 REFERENCE 10 10 10 10 10 10 57 57 57 57 57 10/57 10/57 ACCURACY* (X Rec) 49-125 51-125 53-125 60-125 60-125 51-125 55-125 50-150 56-110 50-140 50-130 28-151 22-126 PRECISION* (X RPO) 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-40 0-40 0-40 0-40 NA NA POL** <ug/L) 0.4 0.5 0.5 0.01 0.6 0.5 0.20 0.50 5.0 0.50 1.0 NA NA TUT O05 7420 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER 2,4-Dinitrotoluene (MS) 2,6-Dinitrotoluene (MS) Isophorone (MS) Nitrobenzene (MS) Surrogate - 2-Fluorobiphenyl Surrogate - 2,4,5,6-Tetrachloro-m-xylene (TCMX) METHOD (Prep) 609/8090(3520) (FID) 609/8090(3520) (ECO) 609/8090(3520) (FID) 609/8090(3520) (ECD) 609/8090(3520) 609/8090(3520) 609/8090(3520) (FID) 609/8090(3520) (ECD) REFERENCE 1.2 1.2 1.2 1.2 1.2 1.2 ACCURACY* (X Rec) 10-125 10-125 10-126 10-126 10-117 10-118 27-123 22-126 PRECISION* (Z RPO) 0-40 0-40 0-40 0-40 0-40 0-40 NA NA POL** (ug/L) 10 0.3 10 0.3 10 10 NA NA TUT 005 2421 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Acenaphthene (MS) Acenaphthylene Benzo(a)pyrene (MS) Benzo(b+k)f luoranthene Benzo(g,h, i)perylene Carbazole Chrysene + Benzo( a) anthracene Ftuoranthene Fluorene CHS) Indeno(1,2,3-cd) pyrene + Dibenzo(a,h)anthracene 1 -Methyl naphthalene 2-Methyl naphthalene Naphthalene (MS) Phenanthrene + Anthracene Pyrene (MS) Diesel Surrogate - 2-Fluorobiphenyl Surrogate - Decaf luorobiphenyl METHOD (Prep) 610/8100(3520) 610/8100(3520) 610/8100(3520) 610/8100(3520) 610/8100(3520) 8100***(3520) 610/8100(3520) 610/8100(3520) 610/8100(3520) 610/8100(3520) 610/8100(3520) 610/8100(3520) 610/8100(3520) 610/8100(3520) 610/8100(3520) 8100 (modified) 610/8100(3520) 8100 (modified) (3520) REFERENCE 1/2 1/2 1/2 1/2 1/2 2 1/2 1/2 1/2 1/2 1/2 1/2 1/2 1/2 1/2 12 1/2 12 ACCURACY* (X Rec) 38-111 38-110 24-132 28-129 14-147 16-UO 29-129 12-155 39-115 15-151 20- HO 20- UO 34-103 38-119 36-124 40-140 27-123 20-150 PRECISION* (X RPO) 0-21 0-23 0-78 0-65 0-87 0-40 0-68 0-67 0-23 0-87 0-50 0-50 0-25 0-29 0-37 0-40 NA NA PQL** (ug/L) 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 300 NA NA TUT OO5 2422 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Acephate Azinphos methyl (MS) Bolstar (MS) Carbophenoth i on Chlorpyrifos Chlorpyrifos methyl Coumaphos Demeton-o Demeton-s Diazinon (MS) Dichlofenthion Dichlorvos Dimethoate Oioxathion Disulfoton (MS) EPN Ethion Ethoprop Famphur Fenamiphos Fensulfothion Fenthion Isofenphos Ma lath ion Merphos Methanridophos Metolachlor Mevinphos Monocrotophos Haled Parathion, ethyl (MS) Parathion, methyl (MS) Phorate (MS) METHOD (Prep) 6U***/8H1***(3520) 614/622/8141(3520) 622/8141(3520) 8141***(3520) 614/622/8141(3520) 622 622/8141(3520) 614/622/8141(3520) 614/622/8141(3520) 614/622/8141(3520) 614/8141***V(3520) 622/8141(3520) 8141(3520) 614/8141***V/3520) 614/622/8141(3520) 614.1/8141(3520) 614/614.1/8141(3520) 622/8141(3520) 8141***V(3520) 614*** 622/8141(3520) 622/8141(3520) 614*** 614/8141(3520) 622/8141(3520) 614*** 614/8141**«(3520) 622/8141(3520) 8141(3520) 622/8141(3520) 614/8141(3520) 614/622/8141(3520) 622/8141(3520) REFERENCE 52/2 14/2 14/2 2 52/14/2 14 14/2 52/14/2 52/14/2 52/14/2 52/2 14/2 2 52/2 52/14/2 58/2 52/58/2 52/14/2 2 52 14/2 14/2 52 52 14/2 52 52/2 52/14/2 52/2 14/2 52/2 52/14/2 14/2 ACCURACY* (X Rec) 25-140 16-129 58-156 20-150 82-115 20-130 51-147 36-120 36-120 36-124 62-104 49-120 38-120 25-140 10-178 48-124 40-138 58-113 10-129 40-160 43-145 10-128 40-160 60-140 50-130 40-160 53-133 34-125 25-140 54-102 18-171 40-104 36-125 PRECISION* (X RPD) 0-50 0-50 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-66 0-40 0-40 0-40 0-60 0-40 0-40 0-60 0-40 0-40 0-40 0-40 0-40 0-40 0-50 0-40 0-28 0-40 0-40 POL** (ug/L) 5.0 1.0 1.0 1.0 1.0 1.0 1.0 2.5 2.5 1.0 1.0 2.0 10 10 2.0 1.0 0.50 0.50 2.0 0.50 5.0 1.0 0.50 1.0 1.0 2.0 1.0 2.0 10 5.0 1.0 0.50 1.0 TUT 005 2423 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Ronnel Stirophos (Tetrachlorvinphos) Sulfotepp (MS) Terbufos Thionazin Tokuthion (Prothiofos) Trichloronate : Surrogate - Ronnet Surrogate - Tokuthion Surrogate - T r i pheny I phosphate NET HOD (Prep) 622/8141(3520) 622/8141(3520) 8141(3520) 614.1 8H1***V(3520) 622/8141(3520) 622/8141(3520) 8141/(3520) 622/8141 614/622/8141 REFERENCE 14/2 14/2 2 58 2 14/2 14/2 2 14/2 14/20/2 ACCURACY* « Rec) 45-135 48-125 10-241 40-160 25-160 44-125 49-161 45-135 44-125 40-125 PRECISION* (X RPD) 0-35 0-40 0-40 0-40 0-60 0-40 0-40 NA NA NA POL** (ug/D 1.0 1.0 0.50 0.50 1.0 1.0 1.0 NA NA NA TUT 005 2424 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER 2,4-D (MS) 2,4-DB 2,4,5-T (MS) 2,4,5-TP (Silvex) (MS) Oalapon Dicamba Dichlorprop Dinoseb MCPA MCPP Pentachlorophenol Picloram Surrogate - 2,4-Dichlorophenylacetic acid (OCAA) Surrogate - 2,4-Dichlorophenoxy butyric acid (2,4-DB) METHOD (Prep) 615/8150 615/8150 615/8150 615/8150 615/8150 615/8150 615/8150 615/8150 615/8150 615/8150 615/8150*** 615/8150***V 615/8150 615/8150 REFERENCE 53/2 53/2 53/2 53/2 53/2 53/2 53/2 53/2 53/2 53/2 53/2 53/2 53/2 53/2 ACCURACY* (X Rec) 25-129 40-140 25-145 10-151 10-160 10-150 10-150 10-150 10-150 10-150 10-150 10-150 10-135 40-140 PRECISION* (X RPO) 0-60 0-40 0-62 0-81 0-80 0-80 0-80 0-80 0-80 0-80 0-80 0-40 NA NA PQL** (ug/L) 0.50 0.50 0.50 0.50 10 5.0 0.50 0.50 10 10 0.10 0.050 NA NA !IJT OO5 24?:=; Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Benf luralin Captan (MS) Carbophenothion Chlorothalonil Dichloran Dicofol Isodrin (MS) M i rex PCNB Pendimethalin Permethrin Perthane Strobane Trif luralin Chlocopicrin Ethylene di bromide Surrogate - 2,4,5,6-Tetrachloro-m-xylene (TCMX) METHOD (Prep) 617*** 617 617 617*** 617 617 617 617 617 617*** 617*** 617 617 617 - 618 618 617/618 REFERENCE 26 26 26 26 26 26 26 26 26 26 26 26 26 26 27 27 26/27 ACCURACY* (X Rec) 40-140 55-125 50-110 55-125 56-110 55-115 55-110 54-104 54-100 52-128 50-130 55-115 48-127 54-124 62-134 48-90 22-126 PRECISION* (Z RPD) 0-40 0-40 0-40 0-30 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 NA POL** (ug/L) 0.010 0.10 1.0 0.20 5.0 0.10 0.050 0.50 0.01 2.0 1.0 5.0 2.0 0.01 1.0 0.50 NA TUT 2426 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Alachlor Ametryn Atraton Atrazine (MS) Bromaci I Hexazinone Metalaxyt Hetribuzin Norf lurazon Prometon Prometryn Propazine (MS) Secbumeton Simetryn Simazine Terbuthylazine Terbutryn Triadimefon Diphenylamine Surrogate - Triphenylphosphate METHOD (Prep) 619*** 619 619 619 619*** 619*** 619*** 619*** 619*** 619 619 619 619 619 619 619 619 619*** 620 619/620 REFERENCE 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 23 7/23 ACCURACY* (X Rec) 45-140 60-120 50-115 40-125 55-127 50-130 50-130 61-H1 54-134 55-100 55-120 33-100 30-130 50-200 25-174 60-130 53-113 61-125 56-125 40-125 PRECISION* (X RPO) 0-30 0-40 0-40 0-30 0-30 0-30 0-40 0-30 0-30 0-40 0-40 0-40 0-45 0-40 0-50 0-40 0-40 0-30 0-30 NA PQL** (ug/L) 2.0 2.0 5.0 2.0 2.0 2.0 1.0 2.0 2.0 2.0 2.0 2.0 5.0 2.0 2.0 2.0 2.0 2.0 2.0 NA TUT O05 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR HATER AND OTHER LIQUIDS PARAMETER Aspon Dichlofenthion Famphur Fenitrothion Fonophos Phosmet Thionazin Surrogate - Tripheny I phosphate METHOD (Prep) 622.1 622.1 622.1 622.1 622.1 622.1 622.1 622.1 REFERENCE 8 a 8 8 8 8 8 8 ACCURACY* (X Rec) 62-104 62-104 10-129 61-103 53-133 50-150 25-160 40-125 PRECISION* (X RPO) 0-40 0-40 0-40 0-40 0-40 0-40 0-40 NA PQL** (ug/D 1.0 1.0 2.5 2.0 1.0 1.0 1.0 NA TUT OOfi 2428 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL HETHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Acetone Acetonitrile Acrotein Acrylonitri le Benzene CMS) Benzyl Chloride Broroo benzene B romodi ch 1 oromethane Bromoform Bromomethane 2-Butanone (MEK) n- Butyl benzene sec-Butylbenzene tert-Butylbenzene Carbon disulfide Carbon tetrachloride Chlorobenzene (MS) 2-Chloro-1,3-butadiene (Chloroprene) Chloroethane 2-Chloroethyl vinyl ether Chloroform Ch I oromethane 3-Chloropropene (Allyl chloride) 2-Chlorotoluene METHOD (Prep) 8240(5030)/8260A(5030) CLP -2/88; 3/90 82406(5030) 8240(5030)/8260A(5030) 8240(5030)/8260A(5030) 624/8240(5030)/8260A(5030) CLP-2/88 CLP-3/90 82408(5030) 8260AC5030) 624/8240 ( 5030 )/CLP- 2/8S/ 8260AC5030) CLP-3/90 624/8240 ( 5030 ) /CLP - 2/S8/ 8260A(5030) CLP-3/90 624/8240(5030)/CLP-2/88; 3/90/ 8260AC5030) 8240(5030)/8260A(5030) CLP-2/88; 3/90 8260AC5030) 8260A(5030) 8260AC5030) 8240(5030)/CLP-2/88/ 8260AC5030) CLP-3/90 624/8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 624/8240(5030)/8260A(5030) CLP-2/88 CLP-3/90 82408(5030) 624/8240(5030)/CLP-2/88; 3/90/ 8260A(5030) 624/8240(5030)/8260A(5030) 624/8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 624/8240(5030)/CLP-2/88; 3/90/ 8260AC5030) 82408(5030) 624/8240***(5030)/8260A(5030) REFERENCE 2 6/62 2 2 2 1/2 6 62 2 ; 2 1/2/6 62 1/2/6 62 1/2/6/62 2 6/62 2 2 2 2/6 62 1/2/6 62 1/2 6 62 2 1/2/6/62 1/2 1/2/6 62 1/2/6/62 2 1/2 ACCURACY* (X Rec) 10-161 52-170 60-132 77-108 73-144 76-127 76-127 10-130 50-150 35-155 45-169 10-242 79-208 50-150 50-150 50-150 37-138 70-140 68-136 75-130 75-130 21-163 64-119 10-305 51-138 10-273 81-112 58-125 PRECISION* (I RPO) 0-40 0-40 0-40 0-40 0-22 0-11 0-11 0-70 0-40 0-40 0-40 0-65 0-40 0-40 0-40 0-40 0-40 0-40 0-17 0-13 0-13 0-50 0-65 0-65 0-40 0-65 0-40 0-40 PQL** (ug/L) 50 10 1000 100 100 5.0 5.0 10 100 10 5.0 10 5.0 10 10 50 10 5.0 5.0 5.0 5.0 10 5.0 10 5.0 5.0 10 5 10 50 5.0 10 10 5 5.0 TUT 005 2429 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR HATER AND OTHER LIQUIDS PARAMETER 4-Chlorotoluene D i bromoch I oromethane 1,2-Dibronio-3-chloropropane (DBCP) 1,2-Dibromoethane Dibromome thane 1 , 2- D i ch I orobenzene 1 ,3-Dichlorobenzene 1,4-Dichlorobenzene trans-1,4-Dichloro-2-butene Oich lorodi f luoromethane 1,1-Dichloroethane 1 ,2-Dichloroethane cis/trans-1,2-Dichloroethene 1,1-Dichloroethene (MS) 1 , 2 - D i ch I oropropane 1 , 3 - D i ch I oropropane 2, 2-D ich I oropropane 1 , 1 -D i ch loropropene cis-1 ,3-Dichloropropene trans-1, 3-D ich loropropene Ethanol Ethylbenzene Ethyl methacrylate Hexach lorobutadi ene 2-Hexanone METHCO (Prep) 8260A (5030) 624/8240/CLP - 2/88/8260A ( 5030 ) CLP-3/90 8240B(5030)/8260A(5030) 8240B(5030)/8260A(5030) 8240B(5030)/8260A(5030) 624/8240(5030)/8260A(5030) 624/8240 ( 5030 ) /8260A ( 5030 ) 624 /8240 ( 5030 ) /8260A < 5030 ) 82408(5030) 8240BC 5030 )/8260A< 5030) 624/8240(5030)/CLP-2/88/ 8260 A (5030) CLP-3/90 624/8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 624/8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 624/8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 624/8240( 5030 )/CLP - 2/88/ 8260AC5030) CLP-3/90 8260AC5030) 8260AC5030) 8260AC5030) 624/8240(5030)/CLP-2/88/ 8260AC5030) CLP-3/90 624/8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 8240(5030) 624/8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 8240(5030) 8260 A (5030) 8240(5030)/8260A(5030) CLP-2/88; 3/90 REFERENCE 2 1/2/6 62 2 2 2 1/2 1/2 1/2 2 2 1/2/6 62 1/2/6 62 1/2/6 62 1/2/6 62 1/2/6 62 2 2 2 1/2/6 62 1/2/6 62 2 1/2/6 62 2 2 2 6/62 ACCURACY* (X Rec) 50-150 53-149 37-127 70-112 78-110 69-112 32-180 39-158 11-129 72-146 59-155 49-155 54-156 60-136 10-210 50-150 50-150 50-150 10-227 17-183 40-160 37-162 37-139 50-150 10-164 PRECISION* (X RPO) 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-19 0-65 0-40 0-40 0-40 0-65 0-65 0-40 0-40 0-40 0-40 0-40 POL** (ug/D 5.0 5.0 10 10 5.0 5.0 5.0 5.0 5.0 10 5.0 5.0 10 5.0 10 5.0 10 5.0 10 5.0 10 5.0 5.0 5.0 5.0 10 5.0 10 1000 5.0 10 5.0 5.0 50 10 TUT :430 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER lodomethane Isobutyl alcohol I sopropy I benzene p- I sopropyl toluene Methacrylonitri le Methylene chloride Methylnethacrylate 4-Methyl-2-pentanone (MIBK) Methyl t-butyl ether (MTBE) Naphthalene Pentach loroethane Propionitri le (ethylcyanide) n-Propylbenzene Styrene 1,1,1, 2-Tetrach loroethane 1,1, 2, 2-Tetrach loroethane Tetrachloroethene Toluene (MS) 1 ,2,3-Trichlorobenzene 1,2,4-Trichlorobenzene 1 ,1 ,1-Trichloroethane 1 , 1 ,2-Trichloroethane Trichloroethene (MS) T r i ch 1 orof I uoromethane 1 ,2,3-Trichloropropane Trichlorotrif luoroethane 1 ,2,4-Trimethylbenzene METHOD (Prep) 8240B(5030)/8260A(5030) 82408(5030) 8260AC5030) 8260 A (5030) 82408(5030) 624/8240(5030)/CLP-2/88/ 8260 A (5030) CLP-3/90 82408(5030) 8240 ( 5030 )/8260A( 5030 ) CLP-2/88; 3/90 8240***(5030) 8260A(5030) 82408(5030) 82408(5030) 8260 A (5030) 8240(5030)/CLP-2/88/ 8260 A (5030) CLP-3/90 82408 ( 5030 )/8260A ( 5030 ) 624/8240(5030)/CLP-2/88/ 8260 A (5030) CLP-3/90 624/8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 624/8240( 5030 )/8260A( 5030 ) CLP-2/88 CLP-3/90 8260A(5030) 8260A(5030) 624/8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 624/8240(5030)/CLP-2/88/ 8260 A (5030) CLP-3/90 624/8240(5030)/8260A(5030) CLP-2/88 CLP-3/90 8240(5030>/8260A(5030) 8240(5030)/8260A(5030) 8240*** (5030) 8260A(5030) REFERENCE 2 2 2 2 2 1/2/6 62 2 2 6/62 2 2 2 2 2 2/6 62 2 1/2/6 62 1/2/6 62 1/2 6 62 2 2 1/2/6 62 1/2/6 62 1/2 6 62 2 2 2 2 ACCURACY* (X Rec) 37-137 51-179 50-150 50-150 76-111 10-221 50-130 68-111 50-150 50-150 10-276 63-112 50-150 60-109 34-138 46-157 64-148 68-138 76-125 76-125 50-150 50-150 52-162 52-150 66-136 71-120 71-120 17-181 44-103 82-130 50-150 PRECISION* <X RPO) 0-40 0-40 0-40 0-40 0-40 0-65 0-40 0-40 0-40 0-40 0-65 0-40 0-40 0-40 0-40 0-40 0-40 0-17 0-13 0-13 0-40 0-40 0-40 0-40 0-20 0-14 0-14 0-65 0-40 0-23 0-40 POL** (ug/L) 5.0 1000 5.0 5.0 100 5.0 5.0 50 10 10 5.0 25 100 5.0 5.0 10 5.0 5.0 10 5.0 10 5.0 5.0 10 5.0 5.0 5.0 10 5.0 10 5.0 5.0 10 5.0 5.0 5.0 5.0 TUT GO 5 21431 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER 1 ,3,5-Trimethylbenzene Vinyl acetate Vinyl chloride Xylenes Surrogate - Toluene-d8 Surrogate - p-Bromof luorobenzene Surrogate - D i bromof I uoromethane Surrogate - 1,2-Dichloroethane-d4 HETHOO (Prep) 8260AC5030) 8240(5030)/CLP-2/88/ 8260A(5030) 624/8240<5030)/CLP-2/88; 3/90/ 8260A(5030) 8240(5030)/CLP-2/88/ 8260AC5030) CLP-3/90 8240<5030)/8260AC5030) CLP-2/88; 3/90 624/8240(5030>/8260A(5030) CLP-2/88; 3/90 8260AC5030) 624/8240(5030) CLP-2/88; 3/90 REFERENCE 2 2/6 1/2/6/62 2/6 62 2 6/62 1/2 6/62 2 1/2 6/62 ACCURACY* <X Rec) 50-150 49-147 10-251 66-114 77-120 88-110 80-125 86-115 86-118 80-125 76-114 PRECISION* (X RPO) 0-40 0-40 0-65 0-40 NA NA NA NA NA NA NA PQL** (ug/L) 5.0 10 10 5.0 10 NA NA NA NA NA NA NA TUT O05 2432 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Acenaphthene (MS) Acenaphthylene Acetophenone 2-Acetylaminof luorene Aldrin 4-Aminobiphenyl Aniline Anthracene Arami te Benzidine Benzoic acid Benzo(a)anthracene Benzo( b) f I uoranthene Benzo(k)f luoranthene Benzo(g,h,i)perylene Benzo(a)pyrene Benzyl alcohol Benzyl chloride alpha-BHC beta-BHC delta-BHC gamma-BHC Bis(2-chloroethoxy) methane Bis(2-chloroethyl) ether Bis(2-chloroisopropyl) ether Bis(2-ethylhexyl) phthalate 4-Bromophenyl phenyl ether Butyl benzyl phthalate Carbazole technical Chlordane p-Chloroaniline 4-Chloro-3-methyl-phenol (MS) METHOD (Prep) 625/82708(3520) CLP-2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 8270(3520) 8270(3520) 625/8270(3520) 8270(3520) 8270(3520) 625/8270(3520)/CLP-2/88; 3/90 8270(3520) 625/8270(3520) 8270(3520)/CLP-2/88 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 8270(3520)/CLP-2/88 8270B***(3520) 625/8270(3520) 625/8270(3520) 625/8270(3520) 625/8270(3520) 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520 )/CLP- 2/88; 3/90 8270(3520)***/CLP-3/90 625/8270(3520) 8270(3520) CLP-2/88; 3/90 625/8270(3520) CLP-2/88; 3/90 REFERENCE 1/2 6/62 1/2/6/62 2 2 1/2 2 2 1/2/6/62 2 1/2 2/6 1/2/6/62 1/2/6/62 1/2/6/62 1/2/6/62 1/2/6/62 2/6 2 1/2 1/2 1/2 1/2 1/2/6/62 1/2/6/62 1/2/6/62 1/2/6/62 1/2/6/62 1/2/6/62 2/62 1/2 2 6/62 1/2 6/62 ACCURACY* (X Rec) 65-116 46-118 54-130 10-150 25-150 10-166 10-150 10-150 59-125 40-150 10-200 10-150 54-125 45-135 40-160 10-219 54-137 10-150 10-150 10-150 24-149 10-110 10-150 33-184 12-158 36-166 10-158 53-127 10-152 10-150 10-150 10-150 53-104 23-97 PRECISION* {» RPO) 0-20 0-31 0-24 0-50 0-50 0-40 0-50 0-50 0-19 0-50 0-100 0-50 0-20 0-21 0-33 0-50 0-21 0-50 0-50 0-50 0-40 0-40 0-50 0-50 0-50 0-50 0-40 0-40 0-40 0-50 0-50 0-50 0-17 0-42 POL** (ug/L) 10 10 10 10 10 10 10 50 10 10 80 50 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 50 20 10 10 10 TUT OO5 2433 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER 1-Chloronaphthalene 2-Chloronaphthalene 2-Chlorophenol (MS) 4-Chlorophenylphenyl ether Chrysene 3-Methyl phenol (m-Cresol) 2-Methyl phenol (o-Cresol) 4-Methyl phenol (p-Cresol) 4,4'-DDD 4,4'-DDE 4,4'-DDT Diallate Dibenz(a,h)anthracene Dibenzofuran Di-n-butyl phthalate 1 ,2-Dichlorobenzene 1,3-Dichlorobenzene 1,4-Dichlorobenzene (MS) 3,3'-Dichlorobenzidine 2,4-Dichlorophenol 2,6-Dichlorophenol Dieldrin Diethyl phthalate p-(Dimethylamino)azobenzene 7,12- D imethy I benz( a) anthracene 3,3'-Dimethylbenzidine a,a-DimethylDhenethylamine 2,4-Dimethylphenol Dimethylphthalate m-Dinitrobenzene 4,6-Dinitro-2-methylphenol METHOD (Prep) 8270(3520) 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520) CLP- 2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 8270(3520) 8270(3520)/CLP-2/88; 3/90 8270(3520)/CLP-2/88; 3/90 625/8270(3520) 625/8270(3520) 625/8270(3520) 8270(3520) 625/8270(3520)/CLP-2/88; 3/90 8270(3520)/CLP-2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520) CLP- 2/88; 3/90 625/8270(3520)/CLP-2/88 CLP 3/90 625/8270(3520)/CLP-2/88; 3/90 8270(3520) 625/8270(3520) 625/8270(3520)/CLP-2/88; 3/90 8270(3520) 8270(3520) 8270(3520) 8270(3520) 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 82708(3520) 625/8270(3520)/CLP-2/88 CLP 3/90 REFERENCE 2 1/2/6/62 V 6/62 1/2/6/62 1/2/6/62 2 2/6/62 2/6/62 1/2 1/2 1/2 2 1/2/6/62 2/6/62 1/2/6/62 1/2/6/62 1/2/6/62 1/2 6/62 1/2/6 62 1/2/6/62 2 1/2 1/2/6/62 2 2 2 2 1/2/6/62 1/2/6/62 2 1/2/6 62 ACCURACY* (X Rec) 10-150 60-118 54-99 27-123 25-158 45-131 10-150 10-150 10-150 10-145 10-136 10-203 10-150 47-135 10-150 10-118 32-129 10-172 46-110 36-97 10-262 39-135 10-150 29-136 10-114 10-150 10-150 10-200 10-200 44-112 10-112 10-150 10-181 PRECISION* (X RPO) 0-50 0-40 0-18 0-40 0-33 0-25 0-50 0-50 0-50 0-40 0-40 0-62 0-50 0-24 0-50 0-50 0-40 0-42 0-18 0-28 0-100 0-40 0-50 0-40 0-40 0-50 0-50 0-100 0-50 0-25 0-40 0-50 0-93 POL** (ug/L) 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 20 10 10 10 10 10 10 10 200 2000 10 10 10 50 25 TUT 2434 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER 2,4-Dinitrophenol 2,4-Dinitrotoluene (MS) 2,6-Dinitrotoluene Oinoseb (2-sec-Butyl-4,6- dinitrophenol) Oi-n-octyl phthalate 1,4-Dioxane Diphenylamine/ N-nitrosodiphcnylamine 1,2-Diphenyl hydrazine Endosulfan I Endosulfan 11 Endosulfan sulfate Endrin Endrin aldehyde Endrin ketone Ethyl carbamate Ethyl methane sulfonate Fluoranthene Fluorene Heptachlor Heptathlon epoxide Hexach 1 o robenz ene Hexachlorobutadiene Hexach I orocyclopentadi ene Hexach loroethane Hexach I oroph ene Hexach I oropropene IndenoO ,2,3-cd)pyrene Isophorone Isosafrole Hethapyrilene 3-Methylcholanthrene METHOD (Prep) 625/8270(3520)/CLP-2/88 CLP 3/90 625/8270(3520) CLP-2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 8270(3520) 625/8270(3520)/CLP-2/88; 3/90 8270***V(3520) 625/8270(3520)/CLP-2/88; 3/90 8270(3520) 625/8270(3520) 625/8270(3520) 625/8270(3520) 625/8270(3520) 625/8270(3520) 8270/(3520) 8270»*»V(3520) 8270(3520) 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520) 625/8270(3520) 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 8270(3520)/CLP-2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 8270(3520) 8270(3520) 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 8270(3520) 8270(3520) 8270(3520) REFERENCE 1/2/6 62 1/2 1/2/6/62 2 1/2/6/62 2 1/2/6/62 2 1/2 1/2 1/2 1/2 1/2 2 2 2 1/2/6/62 1/2/6/62 1/2 1/2 1/2/6/62 1/2/6/62 2/6/62 1/2/6/62 2 2 1/2/6/62 1/2/6/62 2 2 2 ACCURACY* (X Rec) 10-H3 39-133 24-96 50-158 10-150 10-146 10-150 10-150 10-150 10-150 10-150 10-107 10-150 10-209 10-150 52-100 10-150 58-124 59-121 10-192 26-155 10-152 24-116 10-150 40-113 10-200 10-150 33-147 21-196 10-150 10-150 10-150 PRECISION* (X RPO) 0-48 0-25 0-38 0-40 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-24 0-50 0-19 0-40 0-40 0-55 0-40 0-40 0-50 0-40 0-80 0-50 0-36 0-60 0-50 0-50 0-50 PQL** (ug/L) 50 25 10 10 10 10 10 10 10 10 20 20 20 20 50 50 10 10 10 10 20 20 10 10 10 10 5000 10 10 10 10 2000 10 TUT 005 2435 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Methylmethanesulfonate 2-Methylnaphthalene 1-Methylnaphthalene Naphthalene 1,4-Napthoquinone 1-Napthylamine 2-Napthylamine Nicotine 2-Nitroaniline 3-Nitroaniline 4-Nitroani line Nitrobenzene 2-Nitrophenol 4-Nitrophenol (MS) 4-Nitroquinoline-1 -oxide N-Nitrosodi-n-butylamine N-Nitrosodiethylamine N-Ni trosodi methyl ami ne N-Nitrosodi-n-propylamine (MS) N-Nitrosomethylethylamine N-Nitrosomorpholine N-Nitrosopiperidine N-Nitrosopyrrolidine 5-Nitro-o-toluidine PCS-1016 PCS-1221 PCS- 1232 PCS- 1242 PCS- 1248 PCS-1254 METHOD (Prep) 8270(3520) 8270(3520)/CLP-2/88; 3/90 82708(3520) 625/8270(3520)/CLP-2/88; 3/90 8270(3520) 8270(3520) 8270(3520) 8270(3520) 8270(3520)/CLP-2/88 CLP-3/90 8270(3520)/CLP-2/88 CLP-3/90 8270(3520)/CLP-2/88 CLP-3/90 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520) CLP-2/88 CLP-3/90 8270(3520) 8270(3520) 8270(3520) 625/8270(3520) 625/8270(3520) CLP-2/88; 3/90 8270(3520) 8270(3520) 8270(3520) 8270(3520) 8270(3520) 625/8270(3520) 625/8270(3520) 625/8270(3520) 625/8270(3520) 625/8270(3520) 625/8270(3520) REFERENCE 2 2/6/62 2 1/2/6/62 2 2 2 2 2/6 62 2/6 62 2/6 62 1/2/6/62 1/2/6/62 1/2 6 62 2 2 2 1/2 1/2 6/62 2 2 2 2 2 1/2 1/2 1/2 1/2 1/2 1/2 ACCURACY* (X Rec) 10-150 10-150 10-150 46- 1 1 1 10-150 10-150 10-150 10-150 10-150 10-150 10-150 35-180 29-182 10-112 10-80 10-80 10-150 10-150 10-150 10-150 39-142 41-116 10-150 10-150 10-150 10-150 10-150 10-150 10-150 10-150 10-150 10-150 10-150 PRECISION* (X RPD) 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-40 0-40 0-108 0-50 0-50 0-50 0-50 0-50 0-50 0-60 0-38 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 POL** (ug/L) 10 10 10 10 10 10 10 100 50 25 50 25 50 25 10 10 50 50 25 100 10 10 10 10 10 10 10 10 10 10 500 500 500 500 500 500 TUT GO5 2436 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER PCS -1260 Pentachlorobenzene Pentachloronitrobcnzene Pentachlorophenol (MS) Phenacetin Phenanthrene Phenol (MS) p-Phenylenediamine 2-Picoline Pronamide Pyrene (MS) Pyridine Safrole Strychnine 1 ,2,4,5-Tetrachlorobenzene Trichlorophenols 2,3,4,5-Tetrachlorophenol 2,3,4,6-Tetrachlorophenol o-Toluidine Toxaphene 1,2,4-Trichlorobenzene (MS) Tetrachlorophenols 2,4,5-Trichlorophenol 2,4,6-Trichlorophenol o,o,o-Triethyl- phosphorothioate 1,3,5-Trinitrobenzene Surrogate - Mitrobenzene-d5 per HOD (Prep) 625/8270(3520) 8270(3520) 8270(3520) 625/8270(3520) CLP 2/88 CLP 3/90 8270(3520) 625/8270(3520)/CLP-2/88; 3/90 625/8270(3520) CLP 2/88 CLP 3/90 8270(3520) 8270(3520) 8270(3520) 625/8270(3520) CLP-2/88; 3/90 8270(3520) 8270(3520) 8270(3520) 8270(3520) 8270(3520) 8270***(3520) 8270(3520) 8270(3520) 625/8270(3520) 625/8270(3520) CLP-2/88; 3/90 8270(3520) 8270(3520) CLP-2/88 CLP-3/90 625/8270(3520)/CLP-2/88; 3/90 8270(3520) 8270(3520) 625/8270(3520) CLP-2/88; 3/90 REFERENCE 1/2 2 2 1/2 6 62 2 1/2/6/62 1/2 6 62 2 2 2 1/2 6/62 2 2 2 2 2 2 2 2 1/2 1/2 6/62 2 2 6 62 1/2/6/62 2 2 1/2 6/62 ACCURACY* <X Rec) 10-150 10-150 10-150 15-139 9-103 9-103 10-150 54-119 10-96 12-89 12-110 10-200 10-150 10-150 36-153 26-127 10-150 10-150 10-150 10-150 NA 10-150 45-129 10-150 10-200 49-108 39-98 NA 45-113 37-144 10-150 10-150 61-115 35-114 PRECISION* (X RPO) 0-50 0-50 0-50 0-39 0-50 0-50 0-50 0-20 0-21 0-42 0-42 0-50 0-50 0-50 .. 0-21 0-31 0-50 0-50 0-50 0-50 NA 0-50 0-22 0-50 0-80 0-24 0-28 NA 0-21 0-40 0-50 0-50 NA NA ML** (ug/D 500 10 10 50 50 25 10 10 10 10 10 2000 200 10 10 10 200 10 100 10 10 50 50 10 2000 10 10 50 10 50 25 10 10 200 NA NA TUT 005 2437 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Surrogate - 2-Fluorobiphenyl Surrogate - p-Terphenyl-d14 Surrogate - Phenol -d5 Surrogate • 2-Fluorophenot Surrogate - 2,4,6-Tribromophenol Surrogate - 2-Chlorophenol-d4 Surrogate - 1 ,2-Dichlorobenzene-d4 NET HOD (Prep) 625/8270(3520) CLP -2/88; 3/90 8270(3520) CLP-2/88; 3/90 625/8270(3520) CLP-2/88 CLP 3/90 8270(3520) CLP-2/88 CLP 3/90 8270(3520) CLP-2/88; 3/90 CLP-3/90 CLP -3/90 REFERENCE 1/2 6/62 2 6/62 1/2 6 62 2 6 62 2 6/62 62 62 ACCURACY* (X ReO 59-119 43-116 46-136 33-141 10-106 10-94 10-110 10-104 21-100 21-110 41-143 10-123 33-110 16-110 PRECISION* (X RPO) NA NA NA NA NA NA NA NA NA NA NA NA NA NA PQL** (ug/L) NA NA NA NA NA NA NA NA NA NA NA NA NA NA TUT 005 2438 Section 5 Revision: 0 Date: 9/92" TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER 2,3,7,8-Tetrachlorodibenzo-p- dioxin (2,3,7,8-TCDD) (MS) METHOD (Prep) 613/8280 8270 (Screen) REFERENCE 1/2 2 ACCURACY* (X Rec) 63-137 PRECISION* (X RPO) 0-40 POL** (ug/L) 0.0050 10 Polychlorinated Oibenzo-p-dioxin and Dibenzofuran classes tetra-CDD (MS) tetra-CDF (MS) penta-CDO (MS) penta-CDF (MS) hexa-CDD (MS) hexa-CDF (MS) hepta-COD (MS) hepta-CDF (MS) octa-COD (MS) octa-CDF (MS) Internal Standard - "C,,- 2,3,7,8-TCDD Internal Standard - "C^-OCDD 8280 8280 8280 8280 8280 8280 8280 8280 8280 8280 8280 8280 2 2 2 2 2 2 2 2 2 2 2 2 63-137 60-142 37-163 52- U8 42-158 58-142 20-170 20-170 20-170 20-170 40-120 40-120 0-40 0-40 0-40 0-40 0-40 0-40 0-50 0-50 0-50 0-50 ...NA NA 0.0050 0.0050 0.0050 0.0050 0.0050 0.0050 0.010 0.010 0.010 0.010 NA NA TUT OO5 2439 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Benf luralin Ethalfluralin I sopropa I i n Prof luralin Trifluralin (MS) Surrogate - 2,4,5,6-Tetrachloro-m-xylene Cyanazine Benonyl METHOD (Prep) 627 627 627 627 627 627 629 631 REFERENCE 9 9 9 9 9 9 25 55 ACCURACY* (X Rec) 40- KO 40-140 48- HO 55-140 17-HO 22-126 20-180 50-126 PRECISION* (X RPD) 0-40 0-40 0-40 0-40 0-50 NA 0-50 0-30 POL** (ug/L) 0.010 2.0 0.10 0.20 0.010 NA 5.0 5.0 TUT 24 4 O Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Amobara Ferbam Mancozeb Haneb He tham Nabam Polyrara Zineb Ziram METHOD (Prep) 630 630 630 630 630 630 630 630 630 REFERENCE 63 63 63 63 63 63 63 63 63 ACCURACY* (X Rec) 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 PRECISION* OC RPO) 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-20 0-20 PQL** <ug/U * * * * * * * * 20 All compounds reported as Ziram TUT O05 2441 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Aminocarb Barban Bromaci I Carbaryl (MS) Carbofuran Chlorpropham Oiuron (MS) Fenuron Fluometuron Linuron Hethiocarb Hethomyl Monuron Neburon Oxarnyl Propham Propoxur Siduron Swep Surrogate - Propachlor METHOD (Prep) 632 632 632***V 632 632 632 632 632 632 632 632 632 632 632 632 632 632 632 632 632 REFERENCE 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 13 ACCURACY* (X Rec) 60-125 55-125 52-125 55-125 55-125 55-125 55-125 60-125 59-125 55-125 51-137 52-132 56-132 54-126 57-125 50-125 56-125 55-125 58-125 45-125 PRECISION* (X RPD) 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-40 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-35 NA PQL** <ug/L) 1.0 1.0 2.0 5.0 10 1.0 1.0 5.0 1.0 1.0 5.0 1.0 1.0 1.0 10 1.0 1.0 1.0 1.0 NA TUT 005 2442 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Bromacil DEET Hexazinone Hetribuzin Terbaci I Triadimefon Tricyctazole Surrogate - T r i pheny I phospha te MET HOC (Prep) 633 633 633 633 633 633 633 633 REFERENCE 41 41 41 41 41 41 41 41 ACCURACY* (X Rec) 52-125 55-125 52-125 50-125 50-130 46-125 53-125 40-125 PRECISION* (X RPD) 0-30 0-30 0-30 0-30 0-30 0-30 0-30 NA PQL** (ug/L) 2.0 5.0 0.50 1.0 5.0 1.0 5.0 NA TUT O05 2443 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Butylate (MS) Cycloate EPIC Holinate (MS) Pebulate Vernolate Surrogate - Tokuthion Surrogate - Tripheny I phosphate METHOD (Prep) 634 634 634 634 634 634 634 634 REFERENCE 15 15 15 15 15 15 15 15 ACCURACY* « Rec) 38-145 46-159 46-154 37-127 22-172 39-147 44-125 40-125 PRECISION* (Z RPO) 0-76 0-47 0-55 0-74 0-50 0-45 NA NA PQL** <ug/U 2.0 2.0 2.0 2.0 2.0 2.0 NA NA firr 2444 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL HETHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR HATER AND OTHER LIQUIDS PARAMETER Rotenone Bensutide Oryzalin Bendiocarb Bentazon 2,4,-D 2,4,-DB Dicamba Picloram ICTHCD (Prep) 635 636 638 639 643 644*" 644*** 644*** 644 REFERENCE 19 16 21 20 59 64 64 64 64 ACCURACY* « Rec) 59-125 22-140 50-130 10-165 50-150 25-129 48-126 40-144 44-138 PRECISION* (X RPO) 0-30 0-50 0-30 0-50 0-40 0-60 0-40 0-40 0-40 PQL** (ug/L) 2.0 2.0 1.0 2.0 5.0 2.0 1.0 0.50 0.50 TUT 005 2445 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Alachlor (MS) Butachlor Diphenamid Fluridone (.ethane Norf lurazon Surrogate - Triphenylphosphate METHOD (Prep) 645 645 645 645 645 645 645 REFERENCE 28 28 28 28 28 28 28 ACCURACY* (X Rec) 45-140 50-124 57-119 45-154 33-153 48-110 40-125 PRECISION* (X RPO) 0-30 0-40 0-40 0-40 0-50 0-40 NA POL** (ug/L) 1.0 1.0 1.0 1.0 1.0 1.0 NA TUT ^'446 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Acenaphthene (MS) Acenaphthylene Acridine Anthracene Benzo(a)anthracene Benzo(b)f luoranthene BenzodOf luoranthene Benzonitri le Benzo(g,h, i )perylene Benzo(a)pyrene 7,8-Benzoquinoline Carbazole Chrysene (MS) Dibenzo(a,h)anthracene 2, 4-Dimethylqu incline F luoranthene Fluorene (MS) Indenod ,2,3-cd)pyrene 1-Hethylnaphthalene 2 -Methyl naphthalene 8-Methylquinoline Naphthalene (MS) Phenanthrene Pyrene (MS) Quinaldine Quinoline Surrogate - 2-Fluorobiphenyl Surrogate - 4-Terphenyl-d4 METHOD (Prep) 8310 8310 8310*** 8310 8310 8310 8310 8310*** 8310 8310 8310*** 8310*** 8310 8310 8310*** 8310 8310 8310 8310 8310 8310*** 8310 8310 8310 8310*** 8310*** 8310 8310 REFERENCE 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 ACCURACY* (X Rec) 44-162 10-139 10-200 10-126 12-135 6-150 10-159 10-200 10-120 10-128 10-200 10-150 10-199 10-110 10-200 41-155 10-142 10-116 10-125 10-125 10-200 50-135 10-155 50-158 10-200 10-200 60-140 60-140 PRECISION* (X RPD) 0-52 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-54 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-43 0-40 0-40 HA NA PQL** (ug/L) 1.0 1.0 0.50 0.20 0.20 0.20 0.50 10 0.50 0.20 1.0 1.0 0.20 1.0 20 0.50 0.50 0.50 1.0 1.0 5.0 1.0 0.20 0.50 5.0 40 NA NA TUT 005 2447 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Acetaldehyde Formaldehyde Aldicarb (Temik) (MS) Aldicarb sulfone Aldicarb su If oxide Carbaryl (Sevin) Carbofuran (Furadan) (MS) Dioxacarb 3-Hydroxycarbofuran Methiocarb (Mesurol) Me thorny I (Lannate) Oxamyl (MS) Promecarb Propoxur (Baygon) METHOD (Prep) 8315 8315 8318 8318 8318*** 8318 8318 8318 8318 8318 8318 8318*** 8318 8318 REFERENCE 2 2 2 2 2 2 2 2 2 2 2 2 2 2 ACCURACY* « Rec) 30-110 50-155 34-124 54-116 30-140 55-125 52-125 56-124 47-123 51-137 57-125 50-150 48-122 47-127 PRECISION* (X RPO) 0-40 0-30 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 POL** (ug/L) 200 20 10 5.0 5.0 5.0 10 5.0 5.0 5.0 5.0 5.0 5.0 5.0 TUT CO5 2448 Section 5 Revision: 0 Date: 9/92 TABLE 5.1. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER 1,3-Dinitrobenzene (MS) 2,4-Dinitrotoluene (MS) 2,6-0 imtrotoluene Diphenylamine Hexahydro-1,3,5-trinitro-1,3,5-triazine (RDK) Methyl-2,4,6-trimtro-phenylnitramine (Tetryl) Nitrobenzene Nitroglycerin n-Nitrosodiphenylamine 2-Hitrotoluene (MS) 3-Nitrotoluene 4-Nitrotoluene Octahydro-1,3,5,7-tetranitro-1,3,5,7- tetrazocine (HMX) 1 ,3,5-Trinitrobenzene 2,4,6-Trinitrotoluene Surrogate - 2-Fluorobiphenyl METHOD (Prep) 8330 8330 8330 8330***V 8330 8330 8330 8330***V 8330***V 8330 8330 8330 8330 8330 8330 8330 REFERENCE 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 ACCURACY* (X Rec) 54-166 60-140 60-140 65-140 54-166 41-165 52-152 71-121 55-121 50-144 55-165 54-166 54-162 50-150 50-17 40-140 PRECISION* (X RPO) 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-22 0-30 0-30 0-30 0-30 0-30 " 0-30 0-30 NA POL** (ug/D 0.20 0.20 0.50 10 1.0 5.0 5.0 10 10 20 10 20 20 0.50 0.20 NA TUT O05 2449 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Aluminum Antimony (MS) Arsenic (MS) Barium (MS) Beryllium (MS) Boron Cadmium (MS) Calcium Chromium (MS) Cobalt (MS) Copper (MS) Iron Lead (MS) Lithium Magnesium Manganese (MS) Mercury (MS) Molybdenum Nickel (MS) Potassium METHOD (Prep) 6010(3050) CLP 6010(3050) CLP 7041(3050) 6010(3050) 7060(3050) 7061 CLP 6010(3050) CLP 6010(3050) CLP 7091(3050) 6010(3050***) 6010(3050) CLP 7131(3050) 6010(3050) CLP 6010(3050) CLP 7191(3050) 6010(3050) CLP 6010(3050) CLP 6010(3050) CLP 6010(3050) 7421(3050) CLP 3500-Li 8(3050***) 6010(3050) CLP 6010(3050) CLP 7471 CLP 6010(3050) 6010(3050) CLP 6010(3050) CLP 7610(3050) REFERENCE 2 45 2 45 2 2 2 2 45 2 45 2 45 2 2 2 45 2 2 45 2 45 2 2 45 2 45 2 45 2 2 45 4/2 2 45 2 45 2 45 2 2 45 2 45 2 ACCURACY* (X Rec) 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 PRECISION* (X RPO) 0-30 0-20 0-30 0-20 0-30 0-30 0-30 0-30 0-20 0-30 0-20 0-30 0-20 0-30 0-30 0-30 0-20 0-30 0-30 0-20 0-30 0-20 0-30 0-30 0-20 0-30 0-20 0-30 0-20 0-30 0-30 0-20 0-30 0-30 0-20 0-30 0-20 0-30 0-20 0-30 0-30 0-20 0-30 0-20 0-30 POL** (ng/kg) 20 40 5.0 12 5.0 10 1.0 1.0 20 1.0 40 0.50 1.0 0.10 5.0 0.50 1.0 0.10 50 1000 1.0 2.0 1.0 1.0 10 2.5 5.0 5.0 20 5.0 0.50 0.60 10 50 1000 1.0 3.0 0.030 0.030 1.0 4.0 8.0 100 1000 10 TUT O05 245O Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Seleniun (MS) Silica Silver (MS) Sodium Strontium Thallium (MS) Tin Titanium Tributyl tin Vanadium (MS) Zinc (MS) Zinc phosphide Zirconium METHOD (Prep) 6010(3050) 7740(3050) 7741 CLP 6010(3050***) 6010(3050) CLP 7761(3050) 6010(3050) CLP 6010***(3050***) 6010(3050) 7841(3050) CLP 6010***V(3050***V) 6010***(3050***) Atomic absorption 6010(3050) CLP 6010(3050) CLP FDER Special Method 6010***{3050**«) REFERENCE 2 2 2 45 2 2 45 2 2 45 2 2 2 45 2 2 40 45 2 45 31 2 ACCURACY* (X Rec) 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 70-130 NA 70-130 PRECISION* (X RPO) 0-30 0-30 0-30 0-20 0-30 0-30 0-20 0-30 0-30 0-20 0-30 0-30 0-30 0-20 0-30 0-30 0-40 "0-30 ,0-20 ' 0-30 0-20 NA 0-30 POL** (ng/kg) 50 1.0 1.0 1.0 50 1.0 2.0 0.10 50 1000 1.0 50 1.0 2.0 5.0 1.0 0.10 i.o — 10 2.0 4.0 NA 500 TU 005 2451 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Ammonia (as N) (extractable) BOO BTU Carbon, total organic Cation exchange capacity Chloride (extractable) Chloride, total COO Col i form, fecal Col i form, total Cyanide, amenable to chlorination Cyanide, reactive Cyanide, total EP Toxicity Formaldehyde Fluoride (extractable) Halogens, total Halogens, total organic (EOX) Hydrogen ion (pH) Igni lability Nitrate (as N) (extractable) Nitrate-Nitrite (as N) Nitrite (as N) (extractable) Nitrogen, organic Nitrogen, total Nitrogen, total Kjeldahl METHOD (Prep) EPA-CE-3-140 350.3(EPA-CE) EPA-CE D240-76 EPA-CE [Walkley- Black] 9060 9081 /EPA-CE 9251(5050) 9252 407A 9251(5050) 9056(5050) EPA-CE 908C(AOAC) 908A(AOAC) 9012 9010 7.3.3.2 9012(9010A) 9010 CLP 1310 NIOSH 340.2 9056(5050) EPA-600/4-84-008 9045 1010 EPA-CE EPA-CE EPA-CE EPA-CE EPA-CE EPA-CE REFERENCE 46 3/46 46 38 46 C43J 2 2/46 2 2 4 2 2 46 4(36) 4(36) 2 2 2 2 2 45 2 35 3 2 44 2 2 46 46 46 46 46 46 ACCURACY* (X Rec) 75-125 75-125 60-140 70-130 60-140 60-140 70-130 75-125 75-125 75-125 70-130 70-130 60-140 NA NA NA NA NA 75-125 75-125 85-115 NA 80-120 75-125 70-130 60-140 NA NA 75-125 75-125 75-125 NA NA 65-135 PRECISION* (X RPO) 0-30 0-30 0-40 0-30 0-40 0-40 0-40 0-30 0-30 0-30 0-40 0-40 0-40 NA NA 0-50 0-40 0-50 0-30 0-30 0-25 NA 0-20 0-25 0-40 0-50 0-10 NA 0-30 0-30 0-30 NA NA 0-30 POL** (•g/kg) 0.50 0.50 200 200 BTU/lb 50 50 0.0033 meq/100 g 20 20 20 100 100 100 3 MPN/g 3 MPN/g 1.0 1.0 1.0 1.0 1.0 0.30 NA 13 4.0 200 10 NA NA 5.0 5.0 5.0 25 30 25 TUT O05 245 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Oi I and Grease Orthophosphate Paint filter liquids Petroleun hydrocarbons Phenolics, total recoverable Phosphorus, total Radioactivity, alpha Radioactivity, beta Residue, fixed (X ash) Solids, total Solids, volatile Specific gravity Streptococcus, fecal Sulfate (extractable) Sulfide Sulfide, reactive Sulfur Surfactants (M8AS) (extractable) Toxic compound leaching procedure Water (Karl Fisher) METHOD (Prep) 9070(9071) 365.1 9095 9073 9066(EPA-CE) 9065-(EPA-CE) EPA-CE-3-2/3 EPA-CE-3-2/2 900.0/9310 900.0/9310 EPA-CE EPA-CE EPA-CE EPA-CE 91 OA 9036 9038 375.3 9030- SL 7.3.4.2 0129-64/9056(5050) 425.1 1311 D1744 REFERENCE 2 3 2 2 2 (46) 2 (46) 46 46 2 2 46 46 46 46 4/36 2 2 3 2 2 38/2 3 48 38 ACCURACY* (X Rec) 60-140 75-125 NA 60-140 60-140 60-140 60-140 60-140 NA NA NA NA 75-125 NA NA 75-125 75-125 75-125 50-150 NA 70-130 60-140 NA NA PRECISION* (X RPD) 0-50 0-30 0-40 0-50 0-40 0-40 0-40 0-40 0-30 0-30 0-40 0-30 0-30 0-10 NA' 0-25 0-25 0-25 0-50 0-50 0-30 0-40 NA 0-30 PQL** (ng/kg) 10 1.0 NA 10 0.40 0.40 25 5.0 NA NA 0.10X 0.10X 0.10X NA 3 HPN/g~ 100 100 10 10 10 170 20 NA 50 TUT CO5 2453 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Benzyl chloride Bronra benzene Brotnodi ch loromethane Bromoform Bromomethane Carbon tetrachloride Chlorobenzene (MS) Chloroethane Chloroform 1-Chlorohexane 2-Chloroethylvinyl ether Ch loromethane Chlorotoluenes D i bromoch 1 oromethane 0 i bromomethane 1 , 2 - D i ch I orobenzene 1,3-Dichlorobenzene 1,4-Dichlorobenzene Dich lorodi f luoromethane 1,1-Dichloroethane 1 ,2-Oichloroethane 1,1-Oichloroethylene (MS) cis/trans 1 ,2-Dichtoroethene Dich I oromethane (Methylene chloride) 1 , 2-Oichloropropane cis/trans-1 ,3-Dichloropropylene 1 , 1 ,2,2-Tetrachloroethane 1,1,1 ,2-Tetrachloroethane Tetrachloroethene 1,1,1-Tri Chloroethane 1,1 ,2- Tri Chloroethane Trichloroethene (MS) Tri chlorof luoromethane METHOD (Prep) 8010(5030) 8010(5030} 8010(5030) 8010(5030) 8010(5030) 8010(5030) 8010(5030) 8010(5030) 8010(5030} 8010(5030) 8010(5030) 8010(5030) 8010(5030} 8010(5030) 8010(5030) 8010(5030) 8010(5030) 8010(5030) 8010(5030) 8010(5030) 8010(5030) 8010(5030) 8010(5030) 8010(5030) 8010(5030) 8010(5030) 8010(5030) 8010(5030) 8010(5030) 8010(5030) 8010(5030) 8010(5030) 8010(5030) REFERENCE 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 ACCURACY* (X Rec) 50-150 70-130 42-172 13-159 10-144 43-143 31-122 46-137 49-133 50-150 14-186 10-193 70-130 24-191 70-130 10-208 10-187 42-143 70-130 47-132 51-147 51-132 38-155 25-162 44-156 22-178 10-184 70-130 26-162 41-138 39-136 56-133 21-156 PRECISION* (X RPO) 0-30 0-30 0-30 0-30 0-30 0-30 0-27 0-30 0-30 0-30 0-80 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-28 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-26 0-30 PQL** (ug/kg) 5.0 50 5.0 25 5.0 5.0 5.0 5.0 5.0 5.0 50 5.0 50 5.0 25 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 TUT OO5 2454 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER 1,2,3-Trichloropropane Vinyl chloride 1,2-Oibromoethane (EDB)1 Surrogate - Bromoch loromethane METHOD (Prep) 8010(5030) 8010(5030) 80 10*** (5030) 8010(5030) REFERENCE 2 2 2 2 ACCURACY* (X Rec) 50-150 28-163 75-125 43-127 PRECISION* (X RPD) 0-30 0-30 0-30 NA POL** (ug/kg) 5.0 5.0 5.0 NA EDB determined on Hall detector with PQL of 5.0 ug/kg at client's request. TUT 005 2455 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Acetone 2-Butanone (HEK) Oi ethyl ether Ethane I Ethyl methacrylate Isobotanol Isopropanol Methacrylonitri le Met Hanoi Methyl methacrylate 4-Methyl-2-pentanone (MIBK) Hethyl t-butyl ether (HTBE) Propionitrile Gasoline Hethanol (MS) Ethanol n-Propanol Isopropanol (MS) n-Butanol Isobutanol Ethylene glycol (MS) Diethylene glycol Propylene glycol Triethylene glycol Tetraethylene glycol METHOD (Prep) 80 15*** (5030) 8015(5030) 8015(5030) 8015(5030) 8015***(5030) 8015***(5030) 8015***(5030) 8015***(5030) 8015***(5030) 80 15*** (5030) 8015(5030) 8015***(5030) 8015***(5030) 8015 (modified) 8015 (modified/DEI*) 8015 (modified/DEI*) 8015 (modified/DEI*) 8015 (modified/DEI*) 8015 (modified/DEI*) 8015 (modified/DEI*) 8015 (modified/DEI*) 8015 (modified/DEI*) 8015 (modified/DEI*) 8015 (modified/DEI*) 8015 (modified/OE!*) REFERENCE 2 2 2 2 2 2 2 2 2 2 2 2 2 12 2 2 2 2 2 2 2 2 2 2 2 ACCURACY* (X Rec) 40-130 60-130 10-130 20-140 42-125 50-120 30-140 10-140 50-150 45-132 65-125 50-150 10-130 40-140 50-150 50-150 50-150 50-150 50-150 50-150 50-150 50-150 50-150 50-150 50-150 PRECISION* (X RPO) 0-30 0-40 0-50 0-45 0-40 0-40 0-40 0-60 0-40 0-42 0-40 0-30 0-50 0-40 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 PQL** (ug/kg) 130 130 130 5000 50 5000 5000 500 5000 50 130 50 500 250 1000 1000 1000 1000 1000 1000 10000 10000 10000 10000 25000 DEI = Direct Extract Injection TUT Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Benzene (MS) Chlorobenzene (MS) 1 , 2 - D i ch I orobenzene 1 , 3 - D i eh I orobenzene 1 , A -Di chlorobenzene Ethylbenzene Methyl tert-butyl ether (MTBE) Toluene (MS) Xylenes m-Xylene o+p Xylene Surrogate - a,a,a-Trif luorotoluene METHOD <Prep> 8020(5030) 8020(5030) 8020(5030) 8020(5030) 8020(5030) 8020(5030) 8020*** (5030) 8020(5030) 8020(5030) 8020(5030) 8020(5030) 8020(5030) REFERENCE 2 2 2 2 2 2 2 2 2 2 2 2 ACCURACY* (X Rec) 63-133 69-129 37-154 50-141 42-143 32-160 50-150 70-138 50-150 50-150 50-150 67-137 PRECISION* (X RPD) 0-27 0-25 0-30 0-30 0-30 0-30 0-30 0-26 0-30 0-30 0-30 NA POL** (ug/kg) 5.0 5.0 5.0 5.0 5.0 5.0 50 5.0 5.0 5.0 5.0 NA TUT OO5 2457 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Acrolein Acrylonitri le Acetonitrile METHOD (Prep) 8030(5030) 8030(5030) 8030«**(5030) REFERENCE 2 2 2 ACCURACY* (X Rec) 88-118 71-135 20-115 PRECISION* (X RPD) 0-30 0-30 0-30 PQL** (ug/kg) 1000 500 5000 TUT 2458 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER 2-Chlorophenol (MS) 4-Chloro-3-methylphenol (MS) 2,4-Dichlorophenol 2,4-Dimethylphenol 2,4-Dinitrophenol 2-Methyl-4,6-dinitrophenol 3-Methyt phenol (m-cresol) 2-Hethyl phenol (o-cresol) 4-Methyl phenol (p-cresol) Cresols 2-Nitrophenol 4-Nitrophenol (HS) Pentachlorophenol (MS) Phenol (MS) Trichlorophenols 2,3,4,6-Tetrachlorophenol 2,3,4,5-Tetrachlorophenol Tetrachlorophenols 2,4,6-Trichlorophenol 2,4,5-Trichlorophenol Surrogate - 2,4,6-Tribromophenol METHOD <Pr«p> 8040(3550) 8040(3550) 8040(3550) 8040(3550) 8040(3550) 8040(3550) ***8040(3550) ***8040(3550) ***8040(3550) 8040(3550) 8040(3550) 8040(3550) 8040(3550) 8040(3550) 8040(3550) ***8040(3550) **»8040(3550) 8040(3550) 8040(3550) ***8040(3550) 8040(3550) REFERENCE 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 ACCURACY* « Rec) 27-150 20-151 44-119 24-118 12-145 30-136 10-150 10-150 10-150 10-150 43-117 10-130 10-162 13-149 NA 50-150 50-150 NA 53-119 53-119 10-186 PRECISION* (X RPD) 0-26 0-39 0-40 0-40 0-65 0-40 0-50 0-50 0-50 0-50 0-40 0-34 0-80 0-30 NA 0-40 0-40 NA 0-40 0-40 NA POL** (ug/kg) 330 330 330 330 1700 1700 330 330 330 330 330 1700 1700 330 330 660 660 660 330 330 NA TU: 2459 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Butyl benzyl phthalate (MS) Bis(2-ethylhexyl) phthalate (MS) Di-n-butyl phthalate (MS) Diethyl phthalate (HS) Dimethyl phthalate (HS) Di-n-octyl phthalate (HS) Surrogate - 2-Fluorobiphenyl METHOD (Prep) 8060(3550} 8060(3550) 8060(3550) 8060(3550) 8060(3550) 8060(3550) 8060(3550) REFERENCE 2 2 2 2 2 2 2 ACCURACY* (X Rec) 10-137 10-151 14-123 10-145 10-147 10-K7 17-164 PRECISION* (X RPO> 0-66 0-54 0-41 0-34 0-31 0-86 NA PQL** (ug/kg) 330 330 330 330 330 330 NA TUT OO5 246O Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Aldrin (MS) Benf luralin alpha-BHC beta-BHC gamma -BHC (Lindane) (MS) delta-BHC Carbophenoth i on Chlordane alpha Chlordane gamma Chlordane Chlorobenzi late Chloroneb Chloropropylate Chlorothalonil 4,4'-DOD 4,4'-DDE 4,4'-DDT (MS) Dicofol (Kel thane) Dieldrin (MS) Endosulfan I Endosulfan 1 1 Endosulfan sulfate Endrin (MS) Endrin aldehyde Endrin ketone Etridiazole Heptachlor (MS) NETHOD (Prep) 8080(3550) CLP-2/88 CLP-3/90 8080***(3550) 8080(3550)/CLP-3/90 CLP-2/88 8080(3550)/CLP-3/90 CLP-2/88 8080(3550) CLP-2/88 CLP-3/90 8080(3550)/CLP-3/90 CLP-2/88 8080***(3550) 8080(3550) 8080(3550)/CLP-3/90 CLP-2/88 8080(3550)/CLP-3/90 CLP-2/88 8081***V(3550) 8080***V(3550) 8080***V(3550) 8080***(3550) 8080(3550)/CLP-3/90 CLP-2/88 8080(3550)/CLP-3/90 CLP-2/88 8080(3550) CLP-2/88 CLP-3/90 8081***V(3550) 8080(3550) CLP-2/88 CLP-3/90 8080(3550)/CLP-3/90 CLP-2/88 8080(3550)/CLP-3/90 CLP-2/88 8080(3550)/CLP-3/90 CLP-2/88 8080(3550) CLP-2/88 CLP-3/90 8080(3550)/CLP-3/90 CLP-2/88 CLP-3/90 8080***V(3550) 8080(3550) CLP-2/88 CLP-3/90 REFERENCE 2 6 62 2 2/62 6 2/62 6 2 6 62 2/62 6 2 2 2/62 6 2/62 6 2 2 2 2 2/62 6 2/62 6 2 6 62 2 2 6 62 2/62 6 2/62 6 2/62 6 2 6 62 2/62 6 62 2 2 6 62 ACCURACY* (XRec) 40-137 34-132 34-132 40-140 37-134 17-147 41-134 46-127 46-127 19-140 20-150 45-119 45-140 45-140 50-150 49-125 51-125 35-130 31-141 30-145 48-150 23-134 23-134 40-125 42-139 31-134 31-134 45-153 10-202 26-144 44-151 42-139 42-139 10-150 NA NA 50-125 40-136 35-130 35-130 PRECISION* (X RPO) 0-39 0-43 0-43 0-40 0-40 0-40 0-36 0-50 0-50 0-40 0-50 0-40 0-40 0-40 0-40 0-30 0-30 0-40 0-50 0-50 0-34 0-50 0-50 0-40 0-41 0-38 0-38 0-40 0-65 0-50 0-31 0-45 0-45 0-50 NA NA 0-30 0-34 0-31 0-31 PQL** (ug/kg) 1.7 8.0 1.7 0.33 1.7 8.0 1.7 8.0 1.7 8.0 1.7 1.7 8.0 33 17 1.7 80 1.7 80 17 13 16 6.7 3.3 16 3.3 16 3.3 16 3.3 20 3.3 16 3.3 1.7 8.0 3.3 16 3.3 16 3.3 16 3.3 3.3 16 3.3 0.33 1.7 8.0 1.7 TUT OO!5 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Heptachlor epoxide Isodrin Kepone Methoxychlor Hi rex Pendimethalin Permethrin (total) Propachlor Toxaphene Trif luralin PCS-1016 PCB-1221 PC8-1232 PC8-1242 PCS- 1248 PCB-1254 PCS -1260 Surrogate • Dibutylchlorendate (DBC) Surrogate - 2,4,5,6-Tetrachloro-m- xylen* (TCMX) Surrogate - Decachlorobiphenyl (DCB) METHOD (Prep) 8080(3550)/CLP-3/90 CLP-2/88 8081***V<3550) 8081***V(3550) 8080(3550)/CLP-3/90 CLP-2/88 8081***V(3550) 8080*** (3550) 8080***(3550) 8080***V(3550) 8080(3550)/CLP-3/90 CLP-2/88 8080***(3550) 8080(3550)/CLP-3/90 CLP-2/88 EPA-600/4-81-045 8080(3550)/CLP-3/90 CLP-2/88 EPA-600/4-81-045 8080(3550)/CLP-3/90 CLP-2/88 EPA-600/4-81-045 8080(3550)/CLP-3/90 CLP-2/88 EPA-600/4-81-045 8080(3550)/CLP-3/90 CLP-2/88 EPA-600/4-81-045 8080(3550)/CLP-3/90 CLP-2/88 EPA-600/4-81-045 8080(3550)/CLP-3/90 CLP-2/88 EPA-600/4-81-045 8080(3550) CLP-2/88 8080(3550) CLP-3/90 8080(3550) CLP-3/90 REFERENCE 2/62 6 2 2 2/62 6 2 2 2 2 2/62 6 2 2/62 6 61 2/62 6 61 2/62 6 61 2/62 6 61 2/62 6 61 2/62 6 61 2/62 6 61 2 6 2 62 2 62 ACCURACY* <X Rec) 37-142 10-150 10-150 50-140 20-100 35-125 40-140 51-125 41-126 40-140 69-107 50-130 15-178 50-130 10-215 50-130 39-150 50-130 38-158 50-130 66-122 50-130 58-122 50-130 45-131 24-150 19-132 60-150 47-126 60-150 PRECISION* <X RPO) 0-40 0-50 0-50 0-40 0-50 0-50 0-50 0-30 0-50 0-40 0-21 0-50 0-20 0-50 0-20 0-50 0-20 0-50 0-20 0-50 0-23 0-50 0-20 0-50 NA NA NA NA NA NA PQL** (ug/kg) 1.7 8.0 3.3 17 17 80 33 67 33 16 170 160 0.33 33 80 5000 67 80 5000 33 80 5000 33 80 5000 33 80 5000 33 160 5000 33 160 5000 NA NA NA NA NA NA TUT 005 2462 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER 2,4-Dinitrotoluene (MS) 2,6-Dinitrotoluene (MS) Isophorone (MS) Nitrobenzene (MS) Surrogate - 2-Fluorobiphenyl Surrogate - 2,4,5,6-Tetrachloro-m-xylene (TCMX) METHOD (Prep) 8090(3550)(FID) (ECO) 8090(3550)(FID) (ECO) 8090(3550) 8090(3550) 8090(3550)(FID) 8090(3550)(ECD) REFERENCE 2 2 2 2 2 2 ACCURACY* (X Rec) 10-125 10-125 10-126 10-126 10-117 10-118 17-164 19-132 PRECISION* (X RPD) 0-40 0-40 0-40 0-40 0-40 0-40 NA NA PQL** (ug/kg) 330 10 330 10 330 330 NA NA TUT GO 5 24 6 ^ Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Acenaphthene Acenaphthylene Benzo(a)pyrene Benzo(b+k)f luoranthene Benzo(g,h, i )perylene Carbazole Chrysene+Benzo(a)anthracene Fluoranthene Fluorene Indeno(1,2,3-cd)Pyrene + 0 i benzo( a , h ) anth racene 1 -Methy Inaphtha I ene 2-Methylnaphthalene Napthalene Phenanthrene + Anthracene Pyrene Diesel Mineral spirits Surrogate - 2-Fluorobiphenyl Surrogate - Decaf I uorobi pheny I METHOD (Prep) 8100(3550) 8100(3550) 8100(3550) 8100(3550) 8100(3550) 8100***(3550) 8100(3550) 8100(3550) 8100(3550) 8100(3550) 8100(3550) 8100(3550) 8100(3550) 8100(3550) 8100(3550) 8100 (modified) 8100 (modified) 8100(3550) 8100 (modified) (3550) REFERENCE 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 12 12 2 12 ACCURACY* (X Rec) 37-115 36-114 21-125 26-128 25-126 16-132 30-127 28-132 36-117 20-131 20-140 20-140 29-111 38-118 35-123 40-140 40-140 17-164 20-150 PRECISION* (X RPO) 0-32 0-32 0-45 0-41 0-42 0-31 0-42 0-33 0-33 0-47 0-50 0-50 0-45 0-32 0-32 0-40 0-40 NA NA PQL** (ug/kg) 330 330 330 330 330 330 330 330 330 330 330 330 330 330 330 10000 10000 NA HA TUT 2464 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Acephate Alachlor Ametryn Atrazine Azinphos methyl (MS) Bolstar (MS) Bromaci I Butylate Carbophenothion Chlorpyrifos Coumaphos Cycloate Demeton-0 Demeton-S Diazinon (MS) Dichlofenthion Dichlorvos Dimethoate Oisulfoton (MS) Dioxathion EPN EPIC Ethion Ethoprop Famphur Fenamiphos Fensulfothion Fenthion Fonofos Hexazinone Isofenphos Ma lath ion Merphos Metalaxyl Methamidophos Methyl chlorpyrifos Metolachlor Metribuzin Mevinphos Molinate Monocrotophos Ma led METHOD (Prep) 8U1***(3550) 8141***(3550) 8H1***V(3550) 8H1***V(3550) 8141(3550) 8141(3550) 8141***(3550) 8141***(3550) 8141***V(3550) 8HK3550) 8141(3550) 8141***(3550) 8141(3550) 8141(3550) 8141(3550) 8141***V(3550) 8141(3550) 8141(3550) 8141(3550) 8141***V(3550) 8141(3550) 8141***(3550) 8141(3550) 8141(3550) 8141(3550) 8141***(3550) 8141(3550) 8141(3550) 8141***(3550) 8141***(3550) 8141***(3550) 8141(3550) 8141(3550) 8141***(3550) 8141***(3550) 8141*«*(3550) 8141***(3550) 8141«**(3550) 8141(3550) 8141***(3550) 8141***(3550) 8141(3550) REFERENCE 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 ACCURACY* <X Rec) 40-140 45-140 40-140 40-125 16-129 58-156 40-140 38-145 20-150 82-115 51-147 46-159 36-120 36-120 36-124 40-140 49-120 38-120 10-134 40-140 48-124 46-154 40-138 58-113 10-129 40-160 43-145 10-128 40-160 40-140 40-160 60-140 50-130 40-140 40-140 40-140 40-140 40-140 34-125 37-127 40-140 54-102 PRECISION* (X RPD) 0-50 0-30 0-50 0-30 0-50 0-40 0-50 0-76 0-40 0-40 0-40 0-47 0-40 0-40 0-30 0-50 0-40 0-40 0-93 0-50 0-30 0-55 0-40 0-40 0-60 0-40 0-40 0-60 0-40 0-50 0-40 0-40 0-40 0-50 0-50 0-50 0-50 0-50 0-40 0-74 0-50 0-40 POL** <ug/kg) 167 33 66 66 66 33 66 66 66 33 330 66 83 83 33 33 66 2000 130 330 33 66 17 17 330 17 330 33 33 33 17 33 33 33 66 33 33 33 66 66 330 330 TUT 005 2465 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Norf lurazon Parathion, ethyl (MS) Parathion, methyl (MS) Pebulate Phorate Prometon Prometryn Propazine Rome I Simazine Stirophos (Tetrachlorvinphos) Sulfotepp (MS) Terbufos Terbutryn Terbutylazine Thionazin Tokuthion (Prothiofos) Triadimefon Trichloronate Vernolate Surrogate - Ronnel Surrogate - Tokuthion Surrogate - Tripheny I phosphate NETHGO (Prep) 8H1*»*(3550) 8141(3550) 8141(3550) 8141***(3550) 8141(3550) 8141***V(3550) 8141***V(3550) 8141***V(3550) 8141(3550) 8141**«V(3550) 8141(3550) 8141(3550) 8141*«*(3550) 8141***V(3550) 8141***V(3550) 8141(3550) 8141(3550) 8141***(3550) 8141(3550) 8141***(3550) 8141(3550) 8141(3550) 8141(3550) REFERENCE 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 ACCURACY* (X Rec) 40-140 15-141 40-104 22-172 36-125 40-140 40-140 40-140 22-127 20-150 48-125 13-171 40-140 40-140 40-140 25-160 44-125 40-140 49-161 39-147 22-127 50-125 40-125 PRECISION* (X RPO) 0-50 0-79 0-40 0-50 0-40 0-50 0-50 0-50 0-35 0-50 0-40 0-65 0-50 0-50 0-50 0-60 0-40 0-50 0-40 0-45 NA NA NA PQL** (ug/kg) 33 33 17 33 33 66 66 66 33 66 33 17 17 330 66 66 33 33 330 66 NA NA NA TUT 005 2466 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER 2,4-D (MS) Dalapon 2,4-DB Dicamba Dichlorprop Dinoseb MCPA HCPP Picloram 2,4,5-T (MS) 2,4,5-TP (Silvex) (MS) Surrogate - 2,4-Dichlorophenoxy butanoic acid (2,4-DB) Surrogate - 2,4-Dichlorophenyl acetic acid (DCAA) METHOD (Prep) 8150 8150 8150 8150 8150 8150 8150 8150 8150*** 8150 8150 8150 8150 REFERENCE 2 2 2 2 2 2 2 2 2 2 2 2 2 ACCURACY* (X Rec) 10-130 10-170 20-160 20-160 30-170 30-170 30-170 30-170 10-150 24-115 10-150 20-160 10-148 PRECISION* (X RPD) 0-47 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-46 0-54 NA -NA POL** (ug/kg) 50 2000 50 20 100 100 2000 2000 3.3 50 50 MA NA TUT 005 2467 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Acetone Acetonitrile Acrolein Acrylonitri le Benzene (MS) Benzyl Chloride Bromobenzene Bromodichloromethane Bromoform Bromomethane (Methyl bromide) 2-Butanone (MEK) n-Butylbenzene sec -Butyl benzene tert- Butyl benzene Carbon disulfide Carbon tetrachloride Chlorobenzene (MS) 2-Chloro-1,3-butadiene (Chloroprene) Chloroethane 2-Chloroethyl vinyl ether Chloroform Chloromethane Chloropicrin 3-Chloropropene (Allyl chloride) 2-Chlorotoluene 4-Chlorotoluene 0 i bromoch I oromethane METHOD (Prep) 8240(5030)78260(5030) CLP- 2/88; 3/90 82408(5030) 8240(5030)/8260A(5030) 8240(5030)/8260A(5030) 8240(5030)/8260A(5030) CLP-2/88 CLP-3/90 82408(5030) 8260A(5030) 8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 B240(5030)/CLP-2/88; 3/90/ 8260 A (5030) 8240(5030)/8260(5030)/ 8260A(5030) CLP-2/88; 3/90 8260A(5030) 8260A(5030) 8260A(5030) 8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 8240(5030)/8260A(5030) CLP-2/88 CLP-3/90 82406(5030) 8240(5030)/CLP-2/88; 3/90/ 8260A(5030) 8240(5030)/8260A(5030) 8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 8240(5030)/CLP-2/88; 3/90/ 8260 A (5030) 8240***(5030) 82408(5030) 8240***(5030)/8260A(5030) 8260A(5030) 3240/CLP-2/88/8260A(5030) CLP-3/90 REFERENCE 2 6/62 2 2 2 2 6 62 2 2 2/6 62 2/6 62 2/6/62 2 6/62 2 2 2 2/6 62 2/6 62 2 6 62 2 2/6/62 2 2/6 62 2/6/62 2 2 2 2 2/6 62 ACCURACY* (X Rec) 29-92 78-151 22-164 61-145 48-150 66-142 66-142 50-150 50-150 35-155 45-169 10-242 10-111 50-150 50-150 50-150 35-244 70-140 54-138 60-133 60-133 28-256 44-136 10-305 51-138 10-273 50-130 88-127 48-125 50-150 53-149 PRECISION* (X RPD) 0-40 0-40 0-65 0-40 0-27 0-21 0-21 0-40 0-40 0-40 0-40 0-65 0-40 0-40 0-40 0-40 0-65 0-40 0-33 0-21 0-21 0-65 0-40 0-65 0-40 0-65 0-40 0-40 0-40 0-40 0-40 POL** (ug/kg) 50 200 200 100 5.0 5.0 10 100 10 5.0 10 5.0 10 10 50 10 5.0 5.0 5.0 5.0 10 5.0 10 5.0 5.0 10 10 10 50 5.0 10 10 5.0 5.0 5.0 5.0 5.0 10 TUT OO5 2468 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER 1 ,2-Dibromo-3-chloropropane (DBCP) 1,2-Dibromoethane (EDB) Dibromomethane 1 , 2-D i ch I orobenzene 1 , 3-D i ch I orobenzene 1 ,4-Dichlorobenzene trans-1 ,4-Dichloro-2-butene Dichlorodif luorontethane 1,1-Dichloroe thane 1,2-Dichloroethane cis/trans-1,2-Dichtoroethene 1,1-Dichloroethene (MS) 1 ,2-Dichloropropane 1 , 3 -D i ch I oropropane 2 , 2-D i ch I oropropane 1 ,1-Oichloropropene cis-1 ,3-Dichlocopropene trans-1 ,3-Dichloropropene Ethanol Ethylbenzene Ethyl methacrylate Hexachlorobutadiene 2-Hexanone lodomethane Isobutyl alcohol Isopropylbenzene p- I sopropyt toluene Methacrylonitrile Hethylene chloride ICTHOD (Prep) 8240B(5030)/8260A(5030) 8240B(5030)/8260A(5030) 8240B ( 5030 ) /8260A ( 5 030 ) 8240(5030)/8260A(5030) 8240(5030)/8260A(5030) 8240(5030)/8260A(5030) 82408(5030) 8240B(5030)/8260A(5030) 8240(5030)/CLP-2/88/ 8260A(5030) CLP - 3/0 8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 8240(5030)/8260A(5030) CLP-2/88 CLP-3/90 8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 8260A(5030) 8260A(5030) 8260A(5030) 8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 8240(5030) 8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 8240(5030) 8260A(5030) 8240(5030)/8260(5030) CLP-2/88; 3/90 8240B(5030)/8260A(5030) 82408(5030) 8260A(5030) 8260A(5030) 82408(5030) 8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 REFERENCE 2 2 2 2 2 2 2 2 2/6 62 2/6 62 2/6 62 2 6 62 2/6 62 2 2 2 2/6 62 2/6 62 2 2/6 62 2 2 2 6/62 2 2 2 2 2 2/6 62 ACCURACY* (X Rec) 26-165 86-153 50-150 81-113 63-130 69-126 79-178 50-150 59-155 49-155 54-156 36-161 59-172 59-172 10-210 50-150 50-150 50-150 10-227 17-183 40-160 37-162 47-87 50-150 22-86 77-105 63-173 50-150 50-150 69-145 10-221 PRECISION* (X RPD) 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-50 0-22 0-22 0-65 0-40 0-40 0-40 0-65 0-65 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-60 0-65 POL** (ug/kg) 10 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 10 5.0 10 5.0 10 5.0 5.0 10 5.0 10 5.0 5.0 5.0 5.0 10 5.0 10 1000 5.0 10 5.0 5.0 50 10 5.0 1000 5.0 5.0 100 5.0 10 TUT 005 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Methyl i soth i ocyanat e Methyl methacrylate 4-Methyl-2-pentanone (MIBK) Methyl t-butyl ether (MTBE) Naphthalene Pentach I oroe thane Propionitri le (ethylcyanide) n-propylbenzene Styrene 1 ,1 ,1,2-Tetrachloroethane 1,1,2,2-Tetrachloroethane Tet rach I oroethene Toluene (MS) 1,2,3-Trichlorobenzene 1 ,2,4-Trichlorobenzene 1,1,1-Trichloroethane 1 , 1 ,2-Trich loroethane Trichloroethene (MS) T r i ch I orof I uoromethane 1 ,2,3-Trichloropropane Trichlorotrif luoroethane 1 ,2,4-Trimethylbenzene 1,3,5-Trimethylbenzene Vinyl acetate Vinyl chloride Xylenes Surrogate - Toluene- 68 METHOD (Prep) 8240***(5030) 82408(5030) 8240(5030)/8260A(S030) CLP-2/88; 3/90 8240*** (5030) 8260A(5030) 82408(5030) 82408(5030) 8260 A (5030) 8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 8240B(5030)/8260A(5030) 8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 8240(5030)/CLP-2/88/ 8260 A (5030) CLP-3/90 8240(5030)/8260A(5030) CLP-2/88 CLP-3/90 8260A(5030) 8260A(5030) 8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 8240(5030)/8260A(5030) CLP-2/88 CLP-3/90 8240(5030)/8260A(5030) 8240(5030)/8260A(5030) 8240***(5030) 8260 A (5030) 8260A(5030) 8240(5030)/CLP-2/88/ 8260 A (5030) 8240(5030)/CLP-2/88; 3/90/ 8260A(5030) 8240(5030)/CLP-2/88/ 8260A(5030) CLP-3/90 8240(5030)/8260A(5030) CLP-2/88 CLP-3/90 REFERENCE 2 2 2 6/62 2 2 2 2 2 2/6 62 2 2/6 62 2/6 62 2 6 62 2 2 2/6 62 2/6 62 2 6 62 2 2 2 2 2 2/6 2/6/62 2/6 62 2 6 62 ACCURACY* (X Rec) 20-120 32-118 64-125 40-150 50-150 41-165 73-227 50-150 89-101 50-150 46-157 64-148 51-141 59-139 59-139 50-150 50-150 52-162 52-150 43-140 62-137 62-137 17-181 43-105 60-140 50-150 50-150 50-150 10-251 50-150 68-123 81-117 84-138 PRECISION* (X RPO) 0-60 0-45 0-49 0-40 0-40 0-50 0-65 0-40 0-40 0-40 0-40 0-40 0-27 0-21 0-21 0-40 0-40 0-40 0-40 0-27 0-24 0-24 0-65 0-40 0-40 0-40 0-40 0-40 0-65 0-40 NA NA NA POL** (ug/kg) 100 5.0 50 10 50 5.0 25 200 5.0 5.0 10 5.0 5.0 10 5.0 10 5.0 5.0 10 5.0 5.0 5.0 10 5.0 10 5.0 5.0 10.0 5.0 5.0 5.0 5.0 5.0 10 10 5.0 10 NA TUT 247O Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Surrogate - p- Bromof luorobenzene Surrogate - D i bromof 1 uoromethane Surrogate - 1,2-Dichloroethane-d4 METHOD (Prep) 8240(5030)/8260A(5030) CLP-2/88 CLP-3/90 8260AC5030) 8240(5030) CLP-2/88; 3/90 REFERENCE 2 6 62 2 2 6/62 ACCURACY* (X Rec) 64-126 74-121 59-113 80-120 46-143 70-121 PRECISION* (X RPD) NA NA NA NA NA NA POL** (ug/kg) NA NA NA TUT 005 2471 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Acenaphthene (MS) Acenaphthylene Acetophenone 2-Acetylaminof luorene Aldrin 4-Aminobiphenyl Aniline Anthracene Aramite Benzidine Benr o( a ) anth racene Benzoic acid Benzo( b)f 1 uoranthene Benzo(k)f luoranthene Benzo(g,h, i)perylene Benzo(a)pyrene Benzyl alcohol Benzyl chloride alpha-BHC beta-BHC delta-BHC gaima-BHC Bis(2-chloroethoxy) methane Bis(2-chloroethyl) ether Bis(2-chloroisopropyl) ether Bis(2-ethylhexyl) phthalate 4-Bromophenyl phenyl ether Butyl benzyl phthalate Carbazole Technical Chlordane p-Chloroanillne 4-Chloro-3-methylphenol (MS) (p-Chloro-m-cresol) METHOD (Prep) 8270(3550) CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550) 8270(3550) 8270(3550) 8270(3550) 8270(3550) 8270(3550)/CLP-2/88; 3/90 8270(3550) 8270(3550) 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88 8270B***(3550) 8270(3550) 8270(3550) 8270(3550) 8270(3550) 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270***(3550)/CLP-3/90 8270(3550) 8270(3550) CLP-2/88; 3/90 8270(3550) CLP-2/88; 3/90 REFERENCE 2 6/62 2/6/62 2 2 2 2 2 2/6/62 2 2 2/6/62 2/6 2/6/62 2/6/62 2/6/62 2/6/62 2/6 2 2 2 2 2 2/6/62 2/6/62 2/6/62 2/6/62 2/6/62 2/6/62 2/62 2 2 6/62 2 6/62 ACCURACY* (X Rec) 51-108 31-137 54-140 10-150 25-150 10-166 10-150 10-150 48-130 40-150 10-200 42-143 10-150 49-123 24-137 10-219 44-141 10-150 10-150 10-150 24-149 10-110 10-150 33-184 12-158 36-166 10-158 53-127 10-152 10-150 10-150 10-150 38-112 26-103 PRECISION* (X RPD) 0-26 0-19 0-24 0-50 0-50 0-40 0-50 0-50 0-30 0-50 0-100 0-25 0-50 0-25 0-38 0-50 0-29 0-50 0-50 0-50 0-40 0-40 0-50 0-50 0-50 0-50 0-40 0-40 0-40 0-50 0-50 0-50 0-23 0-33 POL** (ug/kg) 330 330 330 330 330 330 330 330 330 2700 330 1700 330 330 330 330 330 330 330 330 330 330 330 330 330 330 330 330 330 1700 660 330 330 330 TUT OO 5 ?472 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER 1-Chloronaphthalene 2-Chloronaphthalene 2-Chlorophenol (MS) 4-Chlorophenylphenyl ether Chrysene m-Cresol o-Cresol p-Cresol 4,4'-DDD 4,4'-DDE 4,4'-DDT Dial late Dibenz(a,h)anthracene Dibenzofuran Di-n-butylphthalate 1 ,2-Dichlorobenzene 1 , 3 - D i ch 1 orobenzene 1,4-Dichlorobenzene (MS) 3,3'-Dichlorobenzidine 2,4-Dichlorophenol 2,6-Dichlorophenol Dieldrin Diethylphthalate p- (Dimethylanrino)azobenzene 7,12- Dimethylbenz(a)anthracene 3,3'-Dimethylbenzidine a,a-Dimethylphenethylamine 2,4-Dimethylptienol Dimethylphthalate m-Oinitrobenzene 4,6-Dinitro-2-methylphenol METHOD (Prep) 8270(3550) 8270(3550)/CLP-2/88; 3/90 8270(3550) CLP- 2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550) 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550) 8270(3550) 8270(3550) 8270(3550) 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550) CLP-2/88; 3/90 8270(3550)/CLP-2/88 CLP 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550) 8270(3550) 8270(3550)/CLP-2/88; 3/90 8270(3550) 8270(3550) 8270(3550) 8270(3550) 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 82708(3550) 8270(3550)/CLP-2/88 CLP 3/90 REFERENCE 2 2/6/62 2 6/62 2/6/62 2/6/62 2 2/6/62 2/6/62 2 2 2 2 2/6/62 2/6/62 2/6/62 2/6/62 2/6/62 2 6/62 2/6 62 2/6/62 2 2 2/6/62 2 2 2 2 2/6/62 2/6/62 2 2/6 62 ACCURACY* (X Rec) 10-150 60-118 45-105 25-102 25-158 40-148 10-150 10-150 10-150 10-145 10-136 10-203 10-150 40-147 10-150 10-118 32-129 10-172 46-112 28-104 10-262 39-135 10-150 29-136 10-114 10-150 10-150 10-200 10-150 15-151 10-112 10-150 10-181 PRECISION* (X RPO) 0-50 0-40 0-31 0-50 0-33 0-27 0-50 0-50 0-50 0-40 0-40 0-62 0-50 0-28 0-50 0-50 0-40 0-42 0-28 0-27 0-100 0-40 0-50 0-40 0-40 0-50 0-50 0-100 0-50 0-22 0-40 0-50 0-93 POL** (ug/kg) 330 330 330 330 330 330 330 330 330 330 330 330 330 330 330 330 330 330 330 330 660 330 330 330 330 330 330 330 1700 1700 330 330 330 1700 800 TUT 005 2473 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER 2,4-Dinitrophenot 2,4-Dinitrotoluene (MS) 2,6-Dinitrototuene Oinoseb (2-sec-Butyl-4,6- dinitrophenol) Di-n-octylphthalate 1,4-Dioxane Dipheny I online/ N-nitrosodiphenylamine 1,2-Diphenyl hydrazine Endosulfan I Endosulfan II Endosulfan sulfate Endrin Endrin aldehyde Endrin ketone Ethyl methanesulfonate Fluoranthene Fluorene Heptachlor Heptachlor epoxide Hexachlorobenzene Hexach I orobutadi ene Hexach 1 orocyc I opentadi ene Hexach I oroe thane Hexach I orophene1 Hexach I oropropene lndeno(1,2,3-cd)pyrene Isophorone Isosafrole Methapyrilene METHOD (Prep) 8270(3550>/CLP-2/88 CLP 3/90 8270(3550) CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550) 8270(3550)/CLP-2/88; 3/90 8270***V(3550) 8270(3550)/CLP-2/88; 3/90 8270(3550) 8270(3550) 8270(3550) 8270(3550) 8270(3550) 8270(3550) 8270/(3550) 8270(3550) 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550) 8270(3550) 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550) 8270(3550) 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550) 8270(3550) REFERENCE 2/6 62 2 6/62 2/6/62 2 2/6/62 2 2/6/62 2 2 2 2 2 2 2 2 2/6/62 2/6/62 2 2 2/6/62 2/6/62 2/6/62 2/6/62 2 2 2/6/62 2/6/62 2 2 ACCURACY* (X Rec) 10-167 35-111 28-89 50-158 10-150 10-146 10-150 10-150 10-150 10-150 10-150 10-107 10-150 10-209 10-150 10-150 54-135 59-121 10-192 26-155 10-152 24-116 10-150 40-113 10-200 10-150 18-157 21-196 10-150 10-150 PRECISION* (X RPO) 0-87 0-29 0-47 0-40 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-21 0-40 0-40 0-55 0-40 0-40 0-50 0-40 0-80 0-50 0-83 0-60 0-50 0-50 POL** (ug/kg> 1700 800 330 330 330 330 330 330 330 330 660 660 660 660 1700 1700 330 330 330 660 660 330 330 330 330 170,000 330 330 330 330 3300 Exhibits non-reproducible chromatographic behavior. TUT 2474 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER 3-Methylcholanthrene Methyl methanesulfonate 1-Methylnaphthalene 2-Methy I naphthalene Naphthalene 1 ,4-Napthoquinone 1-Napthylamine 2-Napthylamine Nicotine 2-Nitroaniline 3-Nitroaniline 4-Nitroaniline Nitrobenzene 2-Nitrophenol 4-Nitrophenol (MS) 4-Nitroquinoline-1 -oxide N-Nitroso-di-n-butytamine N-Nitrosodi ethyl ami ne N-Nitrosodi methyl ami ne N-Nitroso-di -n-propylamine (MS) N-Nitrosomethylethylamine N - N i t rosomorpho 1 i ne N-Nitrosopiperidine N-Nitrosopyrrolidine 5-Nitro-o-toluidine PCB 1016 PCB 1221 PCB 1232 PCB 1242 PCB 1248 METHOD (Prep) 8270(3550) 8270(3550) 82708(3550) 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550) 8270(3550) 8270(3550) 8270(3550) 8270(3550)/CLP-2/88 CLP-3/90 8270(3550)/CLP-2/88 CLP-3/90 8270(3550)/CLP-2/88 CLP-3/90 8270(3550)/CLP-2/88; 3/90 8270(3550)/CLP-2/88; 3/90 8270(3550) CLP- 2/88 CLP-3/90 8270(3550) 8270(3550) 8270(3550) 8270(3550) 8270(3550) CLP-2/88; 3/90 8270(3550) 8270(3550) 8270(3550) 8270(3550) 8270(3550) 8270(3550) 8270(3550) 8270(3550) 8270(3550) 8270(3550) REFERENCE 2 2 2 2/6/62 2/6/62 2 2 2 2 2/6 62 2/6 62 2/6 62 2/6/62 2/6/62 2 6 62 2 2 2 2 2 6/62 2 2 2 2 2 2 2 2 2 2 ACCURACY* (X Rec) 10-150 10-150 10-150 10-150 53-125 10-150 10-150 10-150 10-150 10-150 10-150 10-150 35-180 29-182 10-130 11-114 11-114 10-150 10-150 10-150 10-150 27-140 41-126 10-150 10-150 10-150 10-150 10-150 10-150 10-150 10-150 10-150 10-150 PRECISION* (X RPO) 0-50 0-50 0-50 0-50 0-21 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-40 0-40 0-34 0-50 0-50 0-50 0-50 0-50 0-50 0-35 0-38 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 PQL** (ug/kg) 330 330 330 330 330 330 330 330 3300 1700 800 1700 800 1700 800 330 330 1700 1700 800 3300 330 330 330 330 330 330 330 330 330 330 17000 17000 17000 17000 17000 TUT CO5 2 4 7 3 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER PCS 1254 PCB 1260 Pentachlorobenzene Pentachloroni trobenzene Pentachlorophenol (MS) Phenacetin Phenanthrcne Phenol (MS) p-Pheny I enedi ami ne 2-Picoline Pronanride Pyrene (MS) Pyridine Safrole Strychnine Trichlorophenols 1,2,4,5-Tetrachlorobenzene 2,3,4,5-Tetrachlorophenol 2,3,4,6-Tetrachlorophenot o-Toluidine Toxaphene 1,2,4-Trichlorobenzene (MS) Tetrachlorophenols 2,4,5-Trichlorophenol 2,4,6-Trichlorophenol 0.0,0- Triethylphosphorothioate 1, 3, 5-Trini trobenzene Surrogate - Ni trobenzene- d5 METHOD (Prep) 8270(3550) 8270(3550) 8270(3550) 8270(3550) 8270(3550) CLP-2/88 CLP-3/90 8270(3550) 8270(3550)/CLP-2/88; 3/90 8270(3550) CLP-2/88; 3/90 8270(3550) 8270(3550) 8270(3550) 8270(3550) CLP-2/88; 3/90 8270(3550) 8270(3550) 8270(3550) 8270(3550) 8270(3550) 8270*** (3550) 8270(3550) 8270(3550) 8270(3550) 8270(3550) CLP-2/88; 3/90 8270(3550) 8270(3550)/CLP-2/88 CLP-3/90 8270(3550)/CLP-2/88; 3/90 8270(3550) 8270(3550) 8270(3550) CLP-2/88; 3/90 REFERENCE 2 2 2 2 2 6 62 2 2/6/62 2 6/62 2 2 2 2 6/62 2 2 2 2 2 2 2 2 2 2 6/62 2 2/6 62 2/6/62 2 2 2 6/62 ACCURACY* (X Rec) 10-150 10-150 10-150 10-150 10-107 17-109 17-109 10-150 56-129 37-112 26-90 10-150 10-150 10-150 33-139 35-142 10-150 10-150 10-150 NA 10-150 10-150 36-121 10-150 10-150 48-107 38-107 NA 39-123 37-144 10-150 10-150 22-124 23-120 PRECISION* (X RPO) 0-50 0-50 0-50 0-50 0-89 0-47 0-47 0-50 0-21 0-36 0-35 0-50 0-50 0-50 0-25 0-36 0-50 0-50 0-50 NA 0-50 0-50 0-31 0-50 0-50 0-28 0-23 NA 0-27 0-40 0-50 0-50 NA NA PQL** (ug/kg) 17000 17000 330 330 1700 1700 800 330 330 330 330 1700 330 330 330 330 330 330 3300 1700 330 1700 1700 330 67000 330 330 1700 1700 800 330 330 330 NA NA TUT 005 2476 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Surrogate - 2-Fluorobiphenyl Surrogate - p-Terphenyl-dH Surrogate - Phenol -d5 Surrogate - 2-Fluorophenol Surrogate - 2 , 4 , 6- T r i bromopheno I Surrogate - 2-Chlorophenol-dA Surrogate - 1,2-Dichlorobenzene-d4 METHOD (Prep) 8270(3550) CLP-2/88; 3/90 8270(3550) CLP-2/88; 3/90 8270(3550) CLP-2/88; 3/90 8270(3550) CLP-2/88; 3/90 8270(3550) CLP-2/88; 3/90 CLP-3/90 CLP-3/90 REFERENCE 2 6/62 2 6/62 2 6/62 2 6/62 2 6/62 62 62 ACCURACY* (X Rec) 35-116 30-115 29-137 18-137 32-123 24-113 27-120 25-121 17-123 19-122 20-130 20-130 PRECISION* <X RPO) NA NA NA NA NA NA NA NA NA NA NA ~ NA PQL** <ug/kg) NA NA NA NA NA NA NA NA NA NA NA NA TUT 005 2477 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER 2,3,7,8-Tetrachlorodibenzo-p- dioxin (2,3,7,8-TCOO) METHOD (Prep) 8280 8270 (Dual. Screen) REFERENCE 2 2 ACCURACY* « Rec) 69-145 PRECISION* (X RPO) 0-40 ML** (ug/kg) 0.50 330 Polychlorinated Dibenzo-p-dioxins and Dibenzofurans classes tetra-CDD tetra-CDF pent a -COD penta-CDF hexa-COO hexa-COF hepta-CDD hepta-CDF octa-COD octa-COF Internal Standard - "d.-Z.S./.a-TCOD Internal Standard - 'X-OCDD 8280 8280 8280 8280 8280 8280 8280 8280 8280 8280 8280 8280 2 2 2 2 2 2 2 2 2 2 2 2 69-145 59-142 41-203 55-146 45-174 50-154 20-170 20-170 20-170 20-170 40-120 40-120 0-40 0-40 0-40 0-40 0-53 0-46 0-50 0-50 0-50 0-50 NA NA 0.50 0.50 0.50 0.50 0.50 0.50 1.0 1.0 1.0 1.0 NA NA TUT 2478 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Aminocarb Barban Bromacil Carbaryl (MS) Carbofuran Chlorpropham Diuron (MS) Fenuron Fluometuron Linuron Hethiocarb Methomyl Monuron Neburon Oxamyl Propachlor Propham Propoxur Siduron Swep METHOD (Prep) 632(3550)*** 632(3550)***V 632(3550)*** 632(3550)***V 632(3550)***V 632(3550)***V 632(3550)***V 632(3550)***V 632 ( 3550 )***V 632(3550)***V 632(3550)***V 632(3550)***V 632(3550)***V 632(3550)***V 632(3550)***V 632(3550)*** 632(3550)***V 632(3550)***V 632(3550)***V 632(3550)*** REFERENCE 13/2 13/2 13/2 13/2 13/2 13/2 13/2 13/2 13/2 13/2 13/2 13/2 13/2 13/2 13/2 13/2 13/2 13/2 13/2 13/2 ACCURACY* (X Rec) 50-150 50-150 50-150 50-150 50-150 50-150 50-150 50-150 50-150 50-150 50-150 50-150 50-150 50-150 50-150 25-148 50-150 50-150 50-150 50-150 PRECISION* (X RPD) 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 NA 0-50 0-50 0-50 0-50 POL** (ug/kg) 20 20 40 50 50 20 5.0 10 10 5.0 50 200 5.0 5.0 50 NA 50 50 20 20 TUT 005 2479 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER 2,4-D 2,4-DB Dicamba Picloram NET HOD (Prep) 644(3550)*** 644(3550)*** 644(3550)*** 644(3550)*** REFERENCE 64/2 64/2 64/2 64/2 ACCURACY* (X Rec) 40-150 40-150 40-150 40-150 PRECISION* (X RPD) 0-50 0-50 0-50 0-50 POL** (ug/kg) 67 33 17 17 TUT 005 2480 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Acenaphthene (MS) Acenaphthylcne Acridine Anthracene Benzo(a)anthracene BenzoC b) f I uoranthene Benzo(lc)f luoranthene Benzonitri le Benzo(g,h,i)perylene Benzo(a)pyrene 7,8-Benzoquinoline Carbazole Chrysene (MS) D ibenzo( a, h) anthracene 2,4-Dimethylquinol ine F luoranthene Fluorene (MS) lndeno(1,2,3-cd)pyrene 1-Methylnaphthalene 2-Methylnaphthalene 8-Methylquinoline Naphthalene (MS) Phenanthrene Pyrene (MS) Quinaldine Ou incline Surrogate - 2-Fluorobiphenyl Surrogate - 4-Terphenyl-d4 METHOD (Prep) 8310 8310 8310*** 8310 8310 8310 8310 8310*** 8310 8310 8310*** 8310*** 8310 8310 8310*** 8310 8310 8310 8310 8310 8310*** 8310 8310 8310 8310*** 8310*** 8310 8310 REFERENCE 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 ACCURACY* (X Rec) 11-144 10-139 10-200 10-126 12-135 10-150 10-159 10-200 10-120 10-128 10-200 10-150 10-199 10-110 10-200 56-136 10-142 10-116 10-125 10-125 10-200 31-159 10-155 49-156 10-200 10-200 60-140 60-140 PRECISION* (X RPD) 0-35 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-40 0-28 0-40 0-40 0-40 0-40 0-40 0-34 0-40 0-28 0-40 0-40 NA NA PQL** (ug/kg) 20 20 10 4.0 4.0 4.0 10 200 10 4.0 20 20 4.0 20 400 10 10 10 20 20 100 20 4.0 10 100 800 NA NA TUT 005 2481 Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER Acetaldehyde Formaldehyde Aldicarb (Temik) (MS) Aldicarb su I forte Aldicarb sulfoxide Carbofuran (Furadan) (MS) Carbaryl (Sevin) Dioxacarb Ethylene thiourea 3- Hydroxycarbof uran Methiocarb (Mesurol) Methomyl (Lannate) Oxamyl (MS) Promecarb Propoxur (Baygon) METHOD (Prep) 8315 8315 8318 8318 8318*** 8318 8318 8318 8318*** 8318 8318 8318 8318*** 8318 6318 REFERENCE 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 ACCURACY* CXRec) 30-110 50-155 44-1 K 58-118 33-143 53-123 56-126 55-125 30-140 60-120 52-122 54-114 45-161 44-120 46-116 PRECISION* (X RPO) 0-40 0-40 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 0-50 PQL** (ug/kg) 2000 100 20 50 50 30 50 100 330 20 50 20 50 20 20 ruT Section 5 Revision: 0 Date: 9/92 TABLE 5.2. LABORATORY ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR SOLIDS AND SEMISOLIDS PARAMETER 1 ,3-Dinitrobenzene (MS) 2,4-Dinitrotoluene (MS) 2,6-Dinitrotoluene Diphenylamine Hexahydro- 1,3,5- trim" tro- 1,3,5- triazine (ROX) Methyl-2,4,6-trinitro-phenylnitranrine (Tetryl) Nitrobenzene Nitroglycerin n-Nitrosodiphenylamine 2-Nitrotoluene (MS) 3-Nitrotoluene 4-Nitrototuene Octahydro-1,3,5,7-tetranitro-1,3,5,7- tetrazocine (HMX) 1 ,3,5-Trinitrobenzene 2,4,6-Trinitrotoluene Surrogate - 2-Fluorobiphenyl' METHOD (Prep) 8330 8330 8330 8330"*V 8330 8330 8330 8330***V 8330***V 8330 8330 8330 8330 8330 8330 8330 REFERENCE 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 ACCURACY* (X Rec) 54-166 60- HO 60-140 65-HO 54-166 41-165 52-152 46-190 55-121 50-144 55-165 54-166 54-162 50-150 50-170 40-140 PRECISION* (X RPO) 0-30 0-30 0-30 0-30 0-30 0-30 0-30 0-50 0-30 0-30 0-30 0-30 ... 0-30 0-30 0-30 NA PQL** (ug/kg) 100 100 100 100 50 200 50 1000 100 200 100 200 500 100 200 NA TUT 2483 Section 5 Revision: 0 Date: 9/92 TABLE 5-3. FIELD ANALYTICAL METHODS, QA OBJECTIVES AND PRACTICAL QUANTITATION LIMITS (PQL) FOR WATER AND OTHER LIQUIDS PARAMETER Chlorine, residual Hydrogen ion (pH) Oxygen (dissolved) Salinity Specific conductance Temperature Turbidity Water level METHOD (Prep) 330.5 150.1/9040 360.1 210 120.1/9050 170.1 180.1/214A EPA REFERENCE 3 3/2 3 4 3/2 3 3/4 12 ACCURACY* (X Rec) NA 85-115 NA NA 90-110 HA 60-140 NA PRECISION* (X RPO) 0-40 0-15 0-30 NA 0-10 0-10 0-30 0-5 POL** (•a/D 1.0 NA 0.20 100 5.0 unho/cm NA 0.10 NTU 0.10 ft. TUT GO5 2484 Section 5 Revision: 0 Date: 9/92 REFERENCES AND NOTES FOR TABLES 5.1, 5.2, AND 5.3 * Accuracy data are presented as recoveries for spikes, surrogates, or lab control standards (LCS). For routine analysis of organics, percent recoveries are evaluated only on the CLP or lab selected matrix spike/LCS compounds. The routine organic matrix spiking/LCS compounds are designated by an (MS) following the parameter name. Not all of the matrix spike or surrogate compounds listed in these tables are used with a given set of samples. Precision data are presented as relative percent difference (ZRPD). Since reportable levels (above PQL) for most of the organic parameters may not be detected in all environmental samples, precision is usually evaluated on duplicate matrix spike or LCS data. Accuracy and precision control limits are primarily derived from in- house laboratory data. For inorganic parameters, accuracy and precision control limits that have been generated from historical data have been rounded to the nearest "5". In some cases, published limits may be used in lieu of in-house limits because insufficient in-house data are available to calculate limits. In cases where insufficient data are available to generate in-house limits, and no EPA-approved method limits exist, limits are estimated based on available data. In-house data will be generated for all parameters by the next annual revision of this plan. ** PQL - Practical Quantitation Limits - These are the normal reporting limits for routine environmental samples. In all cases, PQLs are higher than laboratory established Method Detection Limits (MDL). These PQLs are taken from SW-846 (Third Edition) or derived from in- house data on routine environmental samples. If samples are highly contaminated or contain interfering substances, PQLs may be elevated by a dilution factor. *** This compound is not included in EPA's list of compounds for this method. However, Savannah Laboratories has verified (validated) that this coupound can be analyzed by this method and will report data for this compound if specifically requested by the client. ***V Method validation data for this compound are included in Appendix A. 1. Code of Federal Regulations, Title 40, Part 136; U.S. Government Printing Office: Washington, DC, July 1, 1988. 2. Test Methods for Evaluating Solid Waste, Third Edition with Revisions and Updates, SW-846; U.S. EPA Office of Solid Waste and Emergency Response: Washington, DC, November, 1986. 3. Methods for Chemical Analysis of Water and Wastes; U.S. EPA Office of Research and Development: Cincinnati, OH, March 1983; EPA 600/4-79-020. 4. Standard Methods for the Examination of Water and Wastewater, Sixteenth and Seventeenth Editions; American Public Health Association: Washington, DC, 1985 and 1989. 5. Deepwater Ports Maintenance, Dredging, and Disposal Manual; Florida DER. TUT 005 2485 Section 5 Revision: 0 Date: 9/92 6. CLP - US EPA Contract Laboratory Program Statement of Work for Organics Analysis, Multi-Medium, Multi-Concentration, Revision 2/88. 7. Determination of Triazine Pesticides in Industrial and Municipal Wastewater: EPA Method 619; January, 1982. 8. Determination of Thiophosphate Pesticides in Industrial and Municipal Wastewater: EPA Method 622.1; January, 1982. 9. Determination of Dinitroaniline Pesticides in Industrial and Municipal Wastewater: EPA Method 627; January, 1982. 10. Determination of Organochlorine Pesticides in Industrial and Municipal Wastewater: EPA Method 608.1; February, 1982. 12. Analytical Procedures for Detection and Quantification of Total Petroleum Fuel Hydrocarbons and Fuel Constituents: Calif. Method for Modified 8015; Don M. Eisenberg, Adam W. Olivier, Peter W. Johnson, Daniel S. Tempelis; September, 1985. 13. Determination of Carbamate and Urea Pesticides in Industrial and Municipal Wastewater: EPA Method 632; January, 1982. 14. Determination of Organophosphorus Pesticides in Industrial and Municipal Wastewater: EPA Method 622; January, 1982. 15. Determination of Thiocarbamate Pesticides in Industrial and Municipal Wastewaters by Gas Chromatography: EPA Method 636; January, 1982. 16. Determination of Bensulide in Industrial and Municipal Wastewaters by Liquid Chromatography: EPA Method 636. 17. Determination of Mercaptobenzothiazole in Wastewaters by Liquid Chromatography: EPA Method 640. 18. Determination of Hexachlorophene and Dichlorophen in Industrial and Municipal Wastewaters: EPA Method 604.1. 19. Determination of J?otenone in Industrial and Municipal Wastewaters by Liquid Chromatography: EPA Method 635. 20. Determination of Bendiocarb in Industrial and Municipal Wastewaters by Liquid Chromatography: EPA Method 639. 21. Determination of Oryzalin in Industrial and Municipal Wastewaters: EPA Method 638. 22. Determination of MBTS and TCMTB in Industrial and Municipal Wastewater by Liquid Chromatography: EPA Method 637. 23. Determination of Diphenylamine in Industrial and Municipal Wastewater by Gas Chromatography: EPA Method 620. 24. C, H, and 0 Compounds: EPA Method 616. 1 UT GO5 2486 Section 5 Revision: 0 Date: 9/92 25. Determination of Cyanazine in Industrial and Municipal Wastewater: EPA Method 629; January, 1982. 26. Determination of Organohalide Pesticides and PCBs in Industrial and Municipal Wastewater: EPA Method 617; January, 1982. 27. Determination of Volatile Pesticides in Municipal and Industrial Wastewater by Gas Chromatography: EPA Method 618. 28. Analysis of Certain Amine Pesticides and Lethane in Wastewater by Gas Chromatography: EPA Method 645. 30. Measurement of Trihalomethanes in Drinking Water with Gas Chromatography/ Mass Spectrometry and Selected Ion Monitoring: EPA Method 501.3. 31. Method from FDER Central Lab 33. Measurement of N-Methyl Carbamoyloximes and N-Methyl Carbamates in Drinking Water by Direct Aqueous Injection HPLC with Post Column Derivatization: EPA Method 531. 35. NIOSH - National Institute for Occupational Safety and Health, Third Edition, 1987. 36. Official Methods of Analysis of the Association of Official Analytical Chemists, Method for Formaldehyde 20.063 (Chromotropic Acid), Thirteenth Edition, 1980. 38. Annual Book of ASTM Standards, Part 23; ASTM: Philadelphia, PA, 1980. 39. Annual Book of ASTM Standards, Volume 11.01/11.02; ASTM: Philadelphia, PA, 1989. 40. Balls, P.W.; Atomic Absorption Spectrometric/Hydride Generation Determination of Tributyl Tin and Dibutly Tin in Sea Water at the Nanogram per Liter Level; ANALYTICA CHEMICA ACTA 197; 309-313 (1987). 41. Determination of Organophosphorus Pesticides in Industrial and Municipal Wastewater: EPA Method 633. 42. Methods for the Determination of Organic Substances in Water and Fluvial Sediments, USGS Book 5, 1983. 43. Methods of Soil Analysis, American Society of Agronomy, Inc., Number 9, Part 2, page 570, (Walkley-Black Procedure). 44. EPA 600/4-84-008, Appendix D: Method For Extractable Organic Halides (EOX) In Solids, January, 1984. 45. CLP-US EPA Contract Laboratory Program Statement of Work for Inorganics Analysis, Multi-Media, Multi-concentration; Revisions 7/88 and 3/90. 46. EPA/CE-81-1 Technical Report, May 1981: Environmental Protection Agency/Corps of Engineers Technical Committee on Criteria for Dredged and Fill Material; Procedures for Handling and Chemical Analysis of Sediment and Water Samples. TUT 2487 Section 5 Revision: 0 Date: 9/92 Page 10/4 of 104 48. Code of Federal Regulations, Title 40, Part 268; U.S. Government Printing Office: Washington, DC, November 7, 1986. 49. Analysis of THMs in Finished Waters by the Purge and Trap Method: EPA Method 501.1. 50. Analysis of THMs in Drinking Water by Liquid/Liquid Extraction; EPA Method 501.2. 51. EPA 600/4-88-039: Methods for the Determination of Organic Compounds in Drinking Water, December, 1988. 52. Determination of Organophosphorus Pesticides in Municipal and Industrial Wastewater: EPA Method 614, February, 1982. 53. Determination of Chlorinated Herbicides in Municipal and Industrial Wastewater: EPA Method 615. 1982. 54. EPA 600/4-80-032: Prescribed Procedures for Measurement of Radioactivity in Drinking Water, August, 1980. 55. Determination of Benomyl and Carabendazim in Wastewater: EPA Method 631. 56. Simon, Verne A.; A Novel Method for the Determination of Paraquat and Diquat in Water by HPLC; Florida HRS. 57. Pesticides in Wastewater: EPA Method 608.2. 58. Determination of Organophosphorus Pesticides in Wastewater: EPA Method 614.1. 59. Analysis of Bentazon in Wastewater by Liquid Chromatography: EPA Method 643. 60. Calculation of Un-Ionized Ammonia in Fresh Water; Florida DER, October, 1983. 61. Bellar, T.A. , and Lichtenberg, J. J.; The Determination of Poly chlorinated Biphenyls in Transformer Fluid and Waste Oils; U.S. EPA Environmental Monitoring and Support Laboratory: Cincinnati, OH, September, 1982; EPA- 600/4-81-045. 62. CLP - US EPA Contract Laboratory Program Statement of Work for Organics Analysis, Multi-Media, Multi-Concentration, Revision OLM01.0 (3/90) thru OLM01.6 (6/91). 63. Determination of Dithiocarbamate Pesticides in Industrial and Municipal Wastewater: EPA Method 630. 64. Analysis of Picloram in Wastewater by Liquid Chromatography; EPA Method 644. 65. Inductively Coupled Plasma Atomic Emission Analysis of Drinking Water, Appendix to Method 200.7, Revision 1.3; USEPA, March, 1987. TUT O05 2438 Section 6 Revision 0 Date: 09/92 6.0 SAMPLING PROCEDURES When Savannah Laboratories has field sampling responsibilities, an experienced field sampling crew will be sent to the site for sample collection and delivery of samples to the laboratory. Each crew will be supervised by a highly qualified field sampling manager who is trained according to EPA and DER protocol for groundwater and other environmental sampling. On past projects, these managers have had their field sampling techniques critiqued by FDER personnel (Bureau of Groundwater Protection), Georgia EPD personnel, and EPA Region IV field coordinators. The DER Interim Field Activity SOPs have been adopted by Savannah Laboratories. The notarized statement of intent is found at the end of this section. 6.1 Sampling Capabilities Savannah Laboratories has the capability for sampling groundwater, surface water, wastewater, soils, sediments/sludges, drinking water, and tissues for the following analyte classes: Analyte Class Volatile Organic: (VOCs) Semivolatile Organics Pesticides/Herbicides/PCBs Metals (total and/or dissolved) Coliform (total/fecal) Cyanide/Sulfide TRPH, TPH<" Nutrients'" General: pH, specific conductance, temperature, turbidity, TSS, IDS, IOC, DO, COD, BOD Sample Source Drinking water, groundwater, surface water, wastewater, soils, sediment, and tissues Drinking water, groundwater, surface water, wastewater, soils, sediment, and tissues Drinking water, groundwater, surface water, wastewater, soils, sediment, and tissues Drinking water, groundwater, surface water, wastewater, soils, sediment, and tissues Drinking water, groundwater, surface water, wastewater, soils, sediment and tissues Drinking water, groundwater, surface water, wastewater, soils and sediment Drinking water, groundwater, surface water, wastewater, soils and sediment Drinking water, groundwater, surface water, wastewater, soils and sediment Drinking water, groundwater, surface water, wastewater, soils and sediment Footnotes : (1) TRPH » Total Recoverable Petroleum Hydrocarbons TPH - Total Petroleum Hydrocarbons (2) Nutrients " Nitrogen, Phosphorus Series; Chloride, Sulfate TUT 2489 Section 6 Revision 0 Date: 09/92 6.2 Sampling Equipment Sampling equipment conforms to construction and usage conditions detailed in the DER General Sampling Protocols SOP, Revised October 29, 1991. A specific equipment listing is provided at the beginning of each subsection of "Sampling Procedures" (Section 6.4). Following is a list of other routinely used equipment. Item Ice chests, styrofoam or insulated plastic Sampling vehicles Field thermometer Field pB meter Field conductivity meter Electronic water level indicator Stainless steel tape measure Nylon line Sheet plastic Aluminum foil Plastic or metal buckets Cleaning brushes Liquinox detergent Analyte-free water contained in contaminant-free glass or plastic bottles Isopropyl alcohol (nanograde) contained in contaminant- free glass or plastic bottles 10Z Nitric acid (metals grade) contained in contaminant-free glass bottles Glass or plastic jugs Sample preservation reagents contained in dispenser bottles or reagent bottles Field carrier (covered, divided tray or box) pH paper Disposable pipettes Standard buffer solutions Standard KC1 solution Disposable unpowdered latex gloves Use Sample container and sample transport Sample container and sample transport Field measurement of temperature Field measurement of pH Field measurement of conductivity Well volume calculation Hell volume calculation Well volume calculation Contamination control Contamination control Collection of purge water or cleaning wastes Equipment decontamination Equipment decontamination Equipment decontamination Equipment decontamination Equipment decontamination (except for stainless steel equipment) Transport of cleaning wastes Sample preservation Transport of preservation reagents Field-check of sample preservation Addition of preservation reagents Calibration of field pH meter Calibration check of field conductivity meter Contamination control 6.3 Decontamination and Cleaning Procedures Sample containers will be obtained or cleaned by option 2a or 2b in the DER SOP for Cleaning and Decontaminating Sampling Equipment, revised October 29, 1991. TUT OO5 2490 Section 6 Revision 0 Date: 09/92 Sampling equipment will be cleaned and decontaminated according to protocols outlined in the DER SOP for Cleaning and Decontaminating Sampling Equipment, revised October 29, 1991. 6.4 Sampling Protocols 6.4.1 General Considerations All sampling will be performed according to the general protocols outlined in the DER General Sampling Protocols SOP, Section I, revised October 29, 1991. 6.4.2 Wastewater Sampling Wastewater samples will be collected according to the DER SOPs Sampling Procedures for Wastewater and Surface Water, revised October 25, 1991 and General Sampling Protocols, Section III.F, revised October 29, 1991. Below is a list of equipment available for wastewater sampling and the parameters which may be sampled. Type Autosampler1 Ketmerer Bucket, beaker, unpreserved sample bottle, dipper* Construction Materials Silicon tubing, plastic collection vessel Teflon tubing, glass collection vessel SS or glass, acrylic stopper SS, glass or Teflon Plastic Use Composite samples Composite samples Grab 8 specific depth Discrete grab Discrete grab Permissible Parameters Metals , -non-metallic inorganics, nutrients, demands, radiological Organics, non-metallic inorganics, nutrients, demands, radiological All inorganics All All inorganics ' Three automatic samplers are available among the five divisions. Refrigeration capability is available. * Device is lowered into stream via decontaminated lines or rods. 6.4.3 Surface Water Sampling Surface water samples will be collected according to the DER SOPs Sampling Procedures for Wastewater and Surface Water, revised October 25, 1991 and General Sampling Protocols, Section III.A revised October 29, 1991 and the EPA Region IV Standard Operating Procedures and Quality Assurance Hanual, Section 4.8.3, revised February 1991. Below is a list of equipment available for surface water sampling and the parameters which may be sampled. TUT •249.1 Section 6 Revision 0 Date: 09/92 Typ« DO Dunker Kemraerer Beaker Bailtr Peristaltic pump with weighted tubing Material SS or glass SS or glass acrylic stopper SS or glass SS or Teflon SS or Teflon silicon tubing Use discrete grab, depth composite grab 8 specific depth discrete grab1 grab 8 specific depth1 grab at specific depth Permissible Parameters All Inorganics All All Inorganics Footnotes : 1 Beaker is inverted, submerged, then turned over to fill. 2 Depth limited by length of bailer. 6,4.4 Groundwater Sampling Groundwater samples will be collected according to the DER SOP Groundwater Sampling Procedures, revised October 28, 1991. Below is a listing of pump types and tubing materials used by Savannah Laboratories. Equipment may be interchanged among the five laboratory locations according to need. Pump Type Units Use Parameters Description Positive displacement Submersible Bladder it 2 Purging Purging , sampling All Inorganics 1 2 Suction lift Centrifugal Peristaltic 4 4 Purging Field filtration, purging All Metals 3 4 1. Submersible pump housing, internal surfaces, and upper fitting for tubing are stainless steel. A 4' to 8' length of Teflon tubing is attached to the stainless steel fitting. The remainder of the discharge tubing is garden hose. The suspension cable is 3' to 4' of stainless steel or Teflon-coated stainless steel, attached to a nylon rope. A check valve at the upper stainless steel/Teflon junction prevents backflow of purge water into the well. 2. The bladder pump housing is Lexan plastic and the tubing is polyethylene. This pump is used for purging only in the case of 2" diameter deep wells. After bladder pump purging, one well volume is purged with an appropriate bailer prior to sampling. 3. Centrifugal surface pumps utilize 4' joinable sections of PVC pipe with a 3' to 4' Teflon tail piece. Only the Teflon portion contacts TUT Of) 5 249; the formation water, into the well. Section 6 Revision 0 Date: 09/92 A foot valve prevents backflow of purge water 4. Peristaltic pumps are routinely used only for in-line field filtration of metals samples. Tubing may be medical grade silicone, Tygon, or polypropylene flexible tubing. On rare occasions, a small diameter shallow well may be purged using this pump. In this case, a Teflon tailpipe arrangement would be used, with only the Teflon contacting the formation water. To prevent backflow of purge water, the tubing is withdrawn from the well while the pump is running. Below is a listing of bailer materials available for groundwater sampling. Bailer Material PVC Stainless Steel Teflon Clear FVC or acrylic Permissible Parameters Metals; non-metallic inorganics: nutrients, demands; biological All parameters All parameters Free product thickness Non-permissible Parameters Organics, volatile or extractable None None 6.4.5 Potable Water Sampling Potable water samples will be collected according to the DER SOP Groundwater Sampling Procedures, revised October 28, 1991, and the EPA Region IV SOP and QAM, Section 4.10.2, revised February 1991. Equipment available for potable water sampling is listed under groundwater sampling (6.4.4). 6.4.6 Sampling for Soil and Sediment Soil samples will be collected according to the DER SOPs Soil Sampling Procedures, Revised October 28, 1991, and General Sampling Protocols, Section 1II.D, revised October 28, 1991. Sediments will be collected according to the DER SOP General Sampling Protocols, Section III.B , revised October 29, 1991 and the EPA Region IV SOP and QAM, Section 4.8.3.3, revised February 1991. TUT GO 5 24 9 ~v Section 6 Revision 0 Date: 09/92 Below is a list of soil and sediment sampling devices used by Savannah Laboratories. Type | Material Trowel, spoon Shovel Corer Band auger Fonar grab sampler Mixing tray SS Teflon-coated SS Aluminum SS SS PVC pipe SS SS Metal, foil-lined glass Plastic Use sampling sampling sampling sampling sampling sampling sediment sampling homogenizing , compositing homogenizing compositing Permissible Parameters All Demands, nutrients Metals, organics All Inorganics All All Extractable organics Inorganics 6.4.7 Sludge Sampling Domestic waste residual sludges will be collected according to the EPA POTW Sludge Sampling and Analysis Guidance Document, revised August 1989. Sludges from solid and hazardous waste sites will be collected according to the EPA Region IV SOP and QAM, Sections 4.12.3 and 4.12.5, revised February 1991. 6.4.8 Liquid Hazardous Waste Hazardous wastes, drums, and tanks of unknown origins and concentrations are typically not sampled by Savannah Laboratories because the sample operations are inherently dangerous to the personnel involved. Drums and tanks are occasionally sampled when the primary constituents are known and do not present a toxic, fire, or explosion hazard. If drum tank or pit sampling is undertaken, it is performed according to the EPA Region IV SOP and QAM, Sections 4.12.3 and 4.12.4, Revised February 1991. 6.4.9 Biological Specimens and Tissues Fish tissues are prepared for analysis according to DER QA Guidance Document #90-01, revised August 15, 1990, using properly decontaminated stainless steel implements. Other biological specimens are obtained and prepared in a manner which will preclude contamination from implements or other specimens. TUT 005 2494 Section 6 Revision 0 Date: 09/92 6.5 Special Sampling Considerations Details of sampling such as compositing, duplicate or split samples, filtration, and special procedures for volatiles, oil and grease, and microbiological samples will be observed as outlined in the DER SOP General Sampling Protocols, Section IV.A through .E, revised October 29, 1991. 6.6 Sample Preservation and Holding Times Sample preservation, holding times, required sample volumes, and container types are listed in Table 6.1 for water samples and Table 6.2 for soil and sediment samples. These tables are taken from 40 CFR Part 136, Table II for water, and DER QAS Guidance Document # 90-02 for soil. Table 6.3 lists the approved procedures, preservation, and holding times for water for parameters not listed on Table 6.1. 6.7 Sample Preservation Protocols Sample preservation will be accomplished by option V.A.I of the DER SOP General Sampling Protocols, revised October 29, 1991. The efficacy of the preservation will be checked at the laboratory immediately upon receipt, for all preserved samples except volatiles. Necessary adjustments will be made and recorded in a laboratory logbook. The pH of volatiles samples will be checked upon analysis, unless the client requests a sacrificial vial to be checked upon receipt. Special preservation protocols will be followed as outlined in the DER SOP General Sampling Protocols, Section V.B. 2 .a, b, and c, revised October 29, 1991. 6.8 Sample Dispatch and Recordkeeping Samples will be labeled, packed, and shipped according to the DER SOP General Sampling Protocols, Section V.C, revised October 29, 1991. Examples of a sample label, monitoring well sampling log, and chain-of- custody forms are present in Figures 6.1, 6.2, and 6.3. See Section 7 for sample custody procedures. 6.9 Field Reagent and Standard Storage All reagents, standards, and solvents used in field activities are stored and transported as listed in Table 6.4 and according to the DER SOP General Sampling Protocols, Section VI.A, revised October 29, 1991. TUT GO5 249b Section 6 Revision 0 Date: 09/92 TABLE 6.1 REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIKES FOR WATER SAMPLES PARAMETER SAMPLE CONTAINER1 SAMPLE PRESERVATION2-3 RECOMMENDED HOLDING TIMES* Bacterial Tests: Coliform, fecal and total Fecal streptococci 250-mL P 250-mL P Cool, 4'C, 0.0081 Na.S.O,' Cool, 4'C. 0.0081 Na.S.O,1 6 hours 6 hours Inorganic Tests: Acidity Alkalinity Amnonia Biochemical oxygen demand Bromide Biochemical oxygen demand, carbonaceous Chemical oxygen demand Chloride Chlorine, total residual Color Cyanide, total and amenable to chlorination Fluoride Hardness Hydrogen ion (pH) KJeldahl and organic nitrogen Chromium VI Mercury' Metals', except chromium VI and mercury Nitrate Nitrate-nitrite Nitrite Organic carbon 250-mL P 250-mL P 100-mL P 1-L P 100-mL P 1-L P 100-mL P 100-mL P 250-mL amber G 250-mL P 1-L P 100-mL P 250-mL P 100-mL P 250-mL P 250-mL P 130-mL G 250-mL P 100-mL P 100-mL P 100-mL P 125-mL amber G Cool, 4'C Cool, 4'C Cool, 4'C, B^SO. to pH < 2 Cool, 4'C None required Cool, 4'C Cool, 4'C, H,SO, to pH < 2 None required None required Cool, 4'C Cool, 4'C, NaOH to pH > 12, 0.6 g ascorbic acid None required HNO, to pH < 2, H.SO. to pH < 2 None required Cool, 4'C, B,SO. to pH < 2 Cool, 4'C HNO, to pH < 2 HNO, to pH < 2 Cool, 4'C Cool, 4'C, H,SO, to pH < 2 Cool, 4'C Cool. 4'C, HC1 or H.SO, to pH < 2 14 days 14 days 28 days 48 hours 28 days 48 hours 28 days 28 days Analyze immediately 48 hours 14 days4 28 days 6 months Analyze immediately 28 days 24 hours 28 days 6 months 48 hours 28 days 48 hours || 28 days TUT CO5 2496 Section 6 Revision 0 Date: 09/92 TABLE 6.1 REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES FOR WATER SAMPLES PARAMETER Orthophosphate Oxygen, dissolved (Probe) Winkler Phosphorus (elemental) Phosphorus , total Residue, total Residue, filterable (IDS) Residue, nonfilterable (TSS) Residue, settleable Residue, volatile (VSS) Silica Specific Conductance Sulfate Sulfide Sulfite Surfactants Temperature Turbidity SAMPLE CONTAINER1 100-mL P G bottle & top G bottle & top G 250-mL P 500-mL P 500-mL P 500-mL P 500-mL P 500-mL P 250-mL P 100-mL P 100-mL P 250-mL P 100-mL P 1-L P 100-mL P 250-mL P SAMPLE PRESERVATION2-3 Filter immediately, cool, 4'C None required Fix on site and store in dark Cool, 4'C Cool, 4'C, H,SO. to pH < 2 Cool. 4'C Cool, 4'C Cool, 4'C Cool, 4'C Cool, 4'C Cool, 4'C Cool, 4'C Cool, 4'C Cool, 4'C, add zinc acetate plus sodium hydroxide to pH > 9 None required Cool, 4'C None required Cool, 4'C RECOMMENDED HOLDING TIMES* 48 hours Analyze immediately 8 hours 48 hours 28 days 7 days 7 days 7 days 48 hours 7 days 28 days 28 days 28 days 7 days Analyze immediately 48 hours Analyze immediately 48 hours Organic Tests:* Purgeable halocarbons Purgeable aromatic hydrocarbons Acrolein and acrylonitrile Phenols" 4 X 40-mL G, Teflon- lined septum 4 X 40-mL G. Teflon-lined septum 1-L G, Teflon- lined septum 1-L G, Teflon- lined cap Cool. 4'C, 0.0081 Na,S,03' or 0.061 ascorbic acid* Cool, 4'C, 0.0081 NajSjO,', HC1 to pH < 2* or 0.06: ascorbic acid* Cool. 4'C. 0.0081 NajSjO,'. adjust pH to 4-5'° or 0.06Z ascorbic acid* Cool, 4'C, 0.0081 Na,S,0,' 14 days 14 days 14 days Extraction-7 days Analysis-40 days TUT 005 M97 Section 6 Revision 0 Date: 09/92 TABLE 6.1 REQUIRED CONTAINERS, PRESERVATION TECHNIQUES , AND HOLDING TIMES' FOR WATER SAMPLES PARAMETER Benzidines"-" Fhthalate esters" Nitrosamines"'14 Pesticides" PCBs" Nitroaromatics and isophorone" Folynuclear aromatic hydrocarbons" Hale-ethers" Chlorinated hydrocarbons" TCDD" Total organic halogens Total petroleum hydrocarbons Phenols, total recoverable Oil and graasa Radiological Tests: Alpha, beta and radium SAMPLE CONTAINER1 l-L G, Teflon- lined cap l-L G, Teflon- lined cap l-L G, Teflon- lined cap l-L G, Teflon- lined cap l-L G, Teflon- lined cap l-L G, Teflon- lined cap l-L G, Teflon- lined cap l-L G. Teflon- lined cap l-L G, Teflon- lined cap l-L G, Teflon- lined cap 500-mL amber G, Teflon-lined cap l-L G, Teflon- lined cap l-L G l-L G P,G SAMPLE PRESERVATION2-3 Cool, 4*C, 0.0081 Ha^O,' Cool, 4*C Cool, 4*C. store in dark, 0.008Z NatS,0,' Cool, 4'C, pH 5-9" Cool, 4*C Cool, 4*C, 0.008Z Na,S,0,1 Cool, 4*C. 0.008Z Ha.S.0* »l«r. ti Mr* -J 1 J Cool, 4'C, 0.008Z Na,S,0,§ Cool, 4*C Cool, 4*C, 0.008Z Ha,S,0,s Cool, 4*C H.SO. to pH < 2 Cool, 4'C HC1 to < 2 Cool, 4'C, H,SO, to pH < 2 Cool, 4'C, H,S04 to pH < 2 RECOMMENDED HOLDING TIMES* Extraction-7 days" Extraction-7 days Analysis-40 days Extraction-7 days Analysis-40 days Extraction-7 days Analysis-40 days Extraction-7 days Analysis-40 days Extraction-7 days Analysis-40 days Extraction-7 days Analysis-40 days Extraction-7 days Analysis-40 days Extraction-7 days Analysis-40 days Extraction-30 days Analysis-45 days of collection 28 days 28 days 28 days 28 days HNO, to pH < 2 6 Months 1. Polyethylene (P) or Glass (G). In cases where more than one inorganic parameter with the sample preservative is required, a single sample container of sufficient size for all analyses is usually preferred. Such grouping of parameters will be indicated when bottles are provided for client sampling. 2. Sample preservation should be performed immediately upon sample collection. For composite chemical samples, each aliquot should be preserved at the time of collection. When use of an automated sampler makes it impossible to preserve each aliquot, chemical samples may be preserved by maintaining at 4°C until TUT CO5 2498 Section 6 Revision 0 Date: 09/92 compositing and sample splitting are completed. 3. When any sample is to be shipped by common carrier or sent through the United States mail, it must comply with the Department of Transportation Hazardous Materials Regulations (49 CFR Part 172). The person offering such material for transportation is responsible for ensuring such compliance. For the preservation requirements, the Office of Hazardous Materials, Materials Transportation Bureau, Department of Transportation has determined that the Hazardous Materials Regulations do not apply to the following: Hydrochloric Acid (HC1) in water solutions at concentrations of 0.04Z by weight or less (pH about 1.96 or greater); Nitric acid (HN03) in water solutions at concentrations of 0.15Z by weight or less (pH about 1.62 or greater); Sulfuric acid (H2S04) in water solutions at concentrations of 0.35X by weight or less (pH about 1.15 or greater); and Sodium hydroxide (NaOH) in water solutions at concentrations of 0.0802 by weight or less (pH about 12.30 or less). 4. Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that samples may be held before analysis and still be considered valid. 5. Sodium thiosulfate or ascorbic acid may be used only if residual chlorine is present. The dechlorination agent and hydrochloric acid must not be combined in pre-preserved vials. 6. Maximum holding time is 24 hours when sulfide is present. Optionally, all samples may be tested with lead acetate paper before pH adjustments in order to determine if sulfide is present. If sulfide is present, it can be removed by the addition of cadmium nitrate powder until a negative spot test is obtained. The sample is filtered and then NaOH is added to pH 12. 7. Samples should be filtered immediately on-site before adding preservative for dissolved metals. 8. Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific compounds. 9. Sample receiving no pH adjustments must be analyzed within seven days of sampling. 10. The pH adjustment is not required if acrolein will not be measured. Samples for acrolein receiving no pH adjustment must be analyzed within three days of sampling. 11. When the extractable analytes of concern fall within a single chemical category, the specified preservative and maximum holding times should be observed for optimum safeguard of sample integrity. When the analytes of concern fall within two or more chemical categories, the sample may be preserved by cooling to 4°C, reducing residual chlorine with 0.008X sodium thiosulfate, storing in the dark, and adjusting the pH to 6-9; samples preserved in this manner may be held for seven days before extraction and for forty days after extraction. Exceptions to this optional preservation and holding time procedure are noted in Footnote 5 (re: the requirement for thiosulfate reduction of residual chlorine), and Footnotes 12 and 13 (re: the analysis of benzidine). TUT OO5 2499 Section 6 Revision 0 Date: 09/92 12. If 1,2-dipheny Ihydraz ine is likely to be present, adjust the pH of the sample to 4.0 ± 0.2 to prevent rearrangement to benzidine. 13. Extracts may be stored up to seven days before analysis if storage is conducted under an inert (oxidant-free) atmosphere. 14. For the analysis of diphenylnitrosamine, add 0.008* Na2S203 and adjust pH to 7-10 within 24 hours of sampling. 15. The pH adjustment may be performed upon receipt at the laboratory and may be omitted if the samples are extracted within 72 hours of collection. For the analysis of aldrin, add 0.008X Na2S203. TUT O05 2500 Section 6 Revision 0 Date: 09/92 TABLE 6.2 REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES FOR SOIL OR SEDIMENT SAMPLES PARAMETER Cyanide Sulfide Oil & grease. Total petroleum hydrocarbons Nutrients/TOC Metals (except Mercury) Semivolatile organics, pesticides, etc. Volatile organics Mercury SAMPLE CONTAINER 500-mL P 500-mL P 500-mL G 500-mL P 500-mL P 500-mL G with Teflon- lined lid 125-mL amber G with Teflon-lined lid 500-mL P SAMPLE PRESERVATION Cool to 4*C Cool to 4'C Cool to 4'C Cool to 4'C None required Dark, cool to **C Dark, cool to 4'C Cool to 4'C RECOMMENDED HOLDING TIMES 14 days 7 days 28 days 28 days 6 months Extraction-14 days Analysis-within 40 days of extraction 14 days 28 days TUT OO6 OO01 **TABLE 6.3 APPROVED WATER AND WASTEWATER PROCEDURES, CONTAINERS, PRESERVATION AND HOLDING TIMES FOR PARAMETERS NOT FOUND IN 40 CFR 136 Parameter Bromine Bromates Chlorophylls Corrosivity Odor Salinity Taste Transparency Un- ionized Ammonia Organic Pesticides13 Method DPD Colorimetric5 Ion Chromatography Spec tropho tome trie Calculated (CaC03 Stability, Langelier Index) Human Panel Electrometric9 Hydrometric Argentometric Human Panel Irradiometric10 Calculated11 GC and HPLC Reference1 SM 408E EPA-SOP (300. O)6 SM 1002G SM 203 ASTM 0513-82 SM 207 SM 210A SM 211 A.B ASTM 1292-86 17-3.021 FAC DER-SOP12 EPA (600- Series)13 Container2 P, G P, G P, G7 P, G G only G, wax seal G only .... P, G u Preservation3 None required Cool, 4° C 14 d in dark Cool, 4° C8 Cool, 4° C Analyze immediately or use wax seal Cool, 4° C .... Cool, 4" C Na^Oj11 H Maximum Holding Times* Analyze immediately 30 days 30 days7 7 days8 6 hours 30 days9 24 hours Analyze in-situ 8 hours unpreserved 28 days preserved11 i* ffl O 70 V) 0) pi n> (D (N rt <J O CO (*(-•• rt • • W H" £ H- O ^ 0 3 O 3 _ ** Source: 17-160.700, F.A.C. TUT 006 OOO2 1. SM XXX - procedures from "Standard Methods for the Examination of Water and Wastewater", APHA-AWWA-WPCF, 16th Edition, 1985. 2. P - plastic, G - Glass 3. When specified, sample preservation should be performed immediately upon sample collection. 4. The times listed are the maximum times that samples may be held before analysis and still be considered valid. 5. The approved procedure is for residual chlorine. However, in the absence of chlorine, the DPD colorimetric procedure can be adapted to measure bromine content of the sample. In such case, the validity of this assumption must be verified by using another procedure for chlorine which is not affected by the presence of bromine (i.e., negligible interference). 6. "Determination of Inorganic Disinfection By-Products by Ion Chromatography, Method 300.0" by John D. Pfaff and Carol a. Brockoff, U.S. EPA, Cincinnati, Ohio 45268 (copy available from the DER QA Section). 7. Collect sample in opaque bottles and process under reduced light. Samples on filter taken from water having pH 7 or higher may be placed in airtight plastic bags and stored frozen for up to three weeks. Samples from acidic water must be processed promptly to prevent chlorophyll degradation. 8. Temperature and pH must be measured on site at the time of sample collection. Seven days is the maximum time for laboratory analysis of total alkalinity, calcium ion and total solids. ^ 9. The eletrometric and hydrometric analytical methods are suited for field use. The argentometric method is p? p? n> (? suited for laboratory use. Samples collected for laboratory analysis, when properly sealed with paraffin waxed °m o> »-•• rt ,~. stopper, may be held indefinitely. The maximum holding time of 30 days is recommended as a practical regulatory '-' " M- o O limit. o o 3 1 v " vo <y> ">\ o ro vo ,-, t-1 NJ c —! 10. Transparency in surface waters is defined as a compensation point for photosynthetic activity, i.e., the depth at which one percent of the light intensity entering at the water surface remains unabsorbed. The DER rule 17-3 FAC requires that the light intensities at the surface and subsurface be measured simultaneously by irradiance meters such as the Kahlsico Underwater Irradiometer, Model No. 268 WA 310, or an equivalent device having a comparable spectral response. 11. The results of the measurements of pH, temperature, salinity (if applicable) and the ammonium ion concentration in the sample are used to calculate the concentration of ammonia in the unionized state. Temperature, pH and salinity must be measured on site at the time of sample collection. Laboratory analysis of the ammonium ion concentration should be conducted within eight hours of sample collection. If prompt analysis of ammonia is impossible, preserve samples with H2SC>4 to pH between 1.5 and 2. Acid-preserved samples, stored at 4° C, may be held up to 28 days for ammonia determination. Sodium thiosulfate should only be used if fresh samples contain residual chlorine. 12. DER Central Analytical Laboratory, Tallahassee, FL, Revision No. 1, October 3, 1983. The 1983 draft is available from the DER QA Section. 13. Other pesticides listed in approved EPA methods (608.1, 608.2, 614, 614.1, 615, 617, 618, 619, 622, 622.1, 627, 629, 631, 632, 632.1, 633, 643, 644 and 645) which are not included in Table 10 of 40 CFR Part 136 (July 1989). 14. Container, preservation and holding time as specified in each individual method shall be followed. ^3 C^ ?O t/5 P) pi (0 (0 CTQ ft <! O (D (D H» rt M- ?. S" <* 03 O 23 os "•x. o to \o Section 6 Revision 0 Dace: 09/92 FIGURE 6.1 ^2 I SAVANNAH LABORATOR ^J L_ I EHVmONMENTAL SERVICES. INC. Savannah, GA (912) 354-7858 DMritM Btach. a (305)421-7400 Mobile. Al. (205) 666-6633 Client Sample ID . Location . Analysis _ Preservative __ Date____L. -By. TallahassM. a (904) 871-3994 Tampa, a (813) US-7427 TUT 006 0005 FIGURE 6.2 MONITORING WELL SAMPLING LOG CLIENT/FACILITY: WELL ID; ____ WELL LOCKED: ' WATER LEVEL: . YES __ NO BAILER PRESENT: (0.01ft) WELL DEPTH: BOTTLES LABELED: YES. NO SAMPLING COMPLETED: BAILER RETURNED & WELL LOCKED: __ CUSTODY FORM COMPLETED: __ YES. SAMPLES ICED: __ YES __ NO __ (Date/Time) . YES ___ NO __ NO COOLERS SEALED: CARRIER: YES NO COLLECTOR: NOTES: Signature SEAL NO: DATE/TIME: DATE/TIME: Section 6 Revision 0 Date: 09/92 .YES NO (ft) WATER EVACUATION: FLOATERS: pH: sn- TEMP: YFS (units) (umhos/cm) (oC) niters) YIELD: NO (ft) SINKFRS- CALIBRATED: / CALIBRATED: / CALIBRATED: / (L/H) YFS NO (Date/Time) (Date/Time) (Date/Time) * Fisher Electronic WL Meter ** Coming Checkmate 90 TUT OO6 OOO6 SAVANNAH LABORATORIES & ENVIRONMENTAL SERVICES. INC. ANALYSIS REQUEST AND CHAIN OF CUSTODY RECORD n 5102L«floch»Averue. S«v«-r«h.GA 31404 Phon* (91 2) 354-7838 F«K (912) 352-0165 Q 2848 IndJriiU Pb» DtK», Talatassee. FL 32301 Phone (804) 878-3994 Fs» (904) 8789504 O 4l4SWl2lhAvcrUB,OMrfWdBeacKFL 33442 Phona (305) 421 -7400 F« (305) 421-2584 O 900 Lakeskto Dfkn Mobta. AL 36693 Phon* (205) 668-6633 Fn (205) 666-6696 d 6712 BHarrin Road. Suke 100. Tamp*.F|_ 33634 Phone (813) 885-7427 Fw (813) 885-7049 curt TW SAMPLE IOENTIFICATON NUMBER OF CONTAINERS SUBMITTED WIMOUOICO IT: |SMH>runQ wc<vto n. (SMNiu Mti TME MCCVCO IT: WLMOUISKD B«: («MH>IU<Q REMARKS ftCLNOLISICO tt tSMMlTUfle) LADORATORY USE ONLY MCf «O ICO UMMIOW K: CU6IOOT MACT "• 1 D CUSIOC* UAl HO. G1 to ^d O po w W rr <J o n> (0 H- rt !_, •• tn H- ^ o' § O O 3 to vo (-1 hO Section 6 Revision 0 Date: 09/92 TABLE 6.4 FIELD. REAGENT STORAGE AND -TRANSPORT CHEMICAL Nitric Acid Hydrochloric acid Sulfuric acid Sodium hydroxide Zinc acetate solution EDTA Solution Isopropanol pH and conductivity standards METHOD OF STORAGE Stored in original container or dedicated repipet dispenser in vented acid storage cabinet; segregated from other acids. See above See above Dry flake or pellet form stored in original container in reagent cabinet, solutions stored in separate cabinet. Stored in dedicated repipet dispenser in reagent storage cabinet. Stored in dedicated repipet dispenser in reagent storage cabinet. Stored in original container in vented solvent storage cabinet in volatile analysis/custody area. Stored in reagent storage cabinet in air conditioned laboratory. METHOD OF TRANSPORT Transferred to dedicated reagent bottle or repipet dispenser; transported in divided box containing only acids (each acid in separate compartment). See above See above Dry forms transported in original or dedicated transfer container. Solutions transferred to dedicated plastic container and transported segregated from acids. Transported in compartmentalized box in capped repipet dispenser. Transported in compartmentalized box in capped repipet dispenser. Transported in bottle jacket in original container. Transported in dedicated plastic containers. TUT OO6 iOO8 Section 6 Revision 0 Date: 09/92 6.10 Field Waste Disposal Field-generated wastes will be handled according to the DER SOP General Sampling Protocols, Section VLB. Wastes transported back to the laboratory for disposal will be handled in accordance with section 8.4 of this document. 6.11 Analyte-Free Water Analyte-free water used in cleaning and field QC samples is defined as water from any source which exhibits no interferences or analytes of interest above the applicable reporting limits. Analyte-free water may be obtained from the following sources, but is not limited to these sources. Laboratory deionized: most inorganics Laboratory deionized with Milli-Q-type polishing: all analytes Laboratory deionized with 0.2 micron polishing filler: microbiology Private well water: any analysis for which acceptability is demonstrated Purchased deionized: any analysis for which acceptability is' demons trated Purchased organic-free: VOCs, extractable organics, and any analysis for which acceptability is demonstrated Analyte-free water will be used as the final rinse in field or lab cleaning procedures, and for trip blanks, field blanks, equipment blanks, and laboratory blanks. Documentation of analyte-free water sources is maintained via results of trip blanks, equipment blanks, laboratory blanks, control blanks, and container blanks. TUT 006 OOO9 Section 6 Revision 0 Date: 09/92 Page 21A of 21 FLORIDA DEPARTMENT OF ENVIRONMENTAL REGULATION — Quality Assurance Section STANDARD OPERATING PROCEDURES TO BE USED AND INCORPORATED BY REFERENCE IN THE COMPREHENSIVE QA PLAN Name of Organization: ' _____ Savannah Laboratories & Environmental Services, Inc._________________ Address: 5102 LaRoche Avenue Savannah, GA- 31404 Comprehensive OA Plan Number: 890142G Check the specific protocols that your organization, will be.using while collecting environmental samples. Note: check only documents and protocols as listed in the "DER Quality Assurance Interim Standard Operating Procedures" dated October 29, 1991 for wh-ich your organization has current equipment capabilities. SAMPLING PROTOCOLS X GeneraJ Sampling X Soil X Wastewatef • X Sediment X Surface Water x Domestic waste Sludges Potable Water x Sludges - Solid and Hazardous Waste X Groundwater x Liquid Hazardous Wastes X Fish Tissue CALIBRATIONS X pH x Dissolved Oxygen X Specific Conductance _ OVAs X Temperature x Residual Chlorine X Automatic WW Samplers " UECONTAMINATION AND CLEANING PROTOCOLS X Container Cleaning protocols X Sampling Equipment (includes teflon, stainless steel and other construction materials) X Lanyards and Well Sounders or Tapes used to Measure Groundwater Level X Wastewater automatic samplers X Teflon Tubing X Non-teflon tubing X Heavily contaminated equipment X Field Meters, Flow-Meters and Other Field Instruments __ Augers', soil boring and drilling rigs (not used for collecting samples) X Pumps used only for purging X Pumps used for purging and .sampling X Field filtration equipment»y.-. X • Analyte-free water containers PRESERVATION, HOLDING TIMES AND CONTAINERS TYPES X Aqueous samples - 40 CFR Part 136, Table II. X Aqueous samples - 17-160.700, F.A.C., Table 4 X Solid samples - 17-160.700, F.A.C., Table 5 QUALITY CONTROL REQUIREMENTS AND PROTOCOLS __ Minimum Field quality control requirements __ QA Targets for Field Protocols TUT O06 Section 6 Revision 0 STATEMENT OF INTENT TO COMPLY WITH THE STANDARD OPERATING PROCEDURES MANUALS Before me, the undersioned authority, personally appeared Janette D. Long _____ [ _____ (name) Vice-President ______ (title) Savannah Laboratories _________ (organization), and Alan C. Bailey" ____ (name) Quality Assurance Manager (title) Savannah Laboratories (organization), who were sworn ano said that they have obtained copies of ell documents pertinent to the protocols that they have identified on the opposite side of this statement and that these documents shall be incorporated by reference into the Comprehensive Quality Assurance Plan attached hereto or identified herein. They further state that the organization of which they are officials or officers as identified herein has the equipment and capability to perform the protocols specified by these documents and will require that said protocols shall be followed when performing the specified activity. They state that they understand that final approval of the Comprehensive Quality Assurance Plan attached hereto or identified herein is contingent upon satisfying the Department's review requirements in all other sections of the Plan. They further state that the information, statements, facts and repressntcticns given end made above are true and correct to the best of their knowledge and belief, and that they are aware that any misrepresentations or falsifications constitute grounds for rejection of approval of the Comprehensive QA Plan attached hereto or identified herein, and further constitute violations of Section 117.03(2), F.S., which provides that "(alny person making a false oath before a notary public shall be guilty of perjury and shall be subject to penalties, forfeitures, and disabilities that are prescribed by law in case of perjury under Chapter 873.' 9-10-92 C /44I&1 DATE . (print name Janette D. Long (Title: Vice-President _________ ) (Organization Savannah Laboratories ____ ) 9-10-92 DATE (print name Alan C. Bailey .Quality Assurance Officer (Organization Savannah Laboratories ____ ) Witness my hand and official seal at Savannah Laboratories _________ _________________ this Tenth _____ •_ day of September ____ , 19 92 ...... . _...,. a. My commission expires: _____ My common Expires July 10. 1994 (SIGNATURE OF NOTARY PUBLIC) Sheila Bryant Hoffman (NAME OF NOTARY PUBLIC TYPED, PRINTED OR STAMPED) TUT OO6 CO 11 Section 7 Revision 0 Date: 9/92 7.0 SAMPLE CUSTODY 7.1 Sample Custody Objectives The primary objective of sample custody is to provide accurate, verified, and traceable records of sample possession and handling from sample container shipment through laboratory receipt and sample disposition. Evidence of documentation of sample collection, shipment, laboratory receipt and custody is accomplished utilizing a chain-of-custody record (Figure 7.1). A sample is considered in custody if it is: in actual possession of the sampler or transferee in view after being in physical possession of the sampler or transferee sealed so that sample integrity will be maintained while in possession of the sampler or transferee in a secured area, restricted to authorized personnel. 7.1.1 Custody Record Maintenance Field and laboratory records are maintained in a secure area. All field and laboratory data are recorded in bound notebooks and entries are made in waterproof ink. Field and laboratory data entry errors are deleted with a one-line strike through the error. The correction is initialed and dated by the sampling or analytical staff member making the change. Field and laboratory information is documented on prepared forms. All forms for recording field and laboratory data include spaces for date and initials which must be completed by the data recorder. Field and laboratory documentation not recorded on prepared forms is also dated and initialed. 7.2 Sample and Legal Custody Procedures All samples requiring sample or special legal custody procedures are received by the laboratory custodian under a chain-of-custody procedure. Legal custody is a special type of sample custody in which all events associated with a specific sample are documented in writing. 7.3 Laboratory and Field Custody Procedures The following procedures apply to the custody activity observed by Savannah Laboratories during sample or legal custody procedures. 7.3.1 Selection and Preparation of Sample Containers Supplied to a Client or Sampling Team Sample containers provided by SL are constructed from EPA designated materials, contain EPA prescribed preservatives and are affixed with an SL identification label (Figure 7.2). In order to monitor container temperature, a 100-mL plastic container labeled "Sample Container JUT O06 OO12 SAVANNAH LADOnATOni£S « fwwnowAifwMt srnwces. we. ANALYSIS REQUEST AND CHAIN OF CUSTODY RECORD O >i»M«n«h«Ar«i..t, !>.»». s. CAjnei ri«>i:i«ii| ill-mi rn|tii|9li«iil O '•" Wkntu n»i ukt. lAiiiiiM.i. it JIMI n~.: |Mi| in mi ri< (w<| 1/1 iwi rtai»:|MlHl|.llM III |»l| III 1MI i sI S 1 § rn|ii>|ui-to<i M SAUn.CS TO IAVAMMAM OIOKATOMlCS e KcruftMto TO TOO MIX AMALTTCAI otfoni. 1 o- ^ r.o. nuuQin rliOJCCI nuunf II Cillllf IIAilC r"°'": ,,„,- MAIMIX ITI'C 1 TAOC Of ncouiiitn ANALYSES """'"' /*/£/// cutiif *6on(ii- Cilr. JIAII. J»'C<Mi£ iAurtin,*! MAU(|S| c SAMPLING OAIC HUE "'""""" t,J §< SAMPLE IOENIIFICAIIOM / / I / fKimouisiiCO •ri|(«MA 11111(1 n(C(rv(o tTMtiOiiAiunri niif -,„- - —— i? IT — — EK — —— —— — r IIKJUlSl — — "i lo\ w 77 / | | SIAMOAnO TAT / | j (XPEDIICOTAr • / m/uiiEiior coniAi/iens SUUUIIIEU / »SUOJECF lonusiiftts "HiliAUll T: (iiHii i'} Allnli-i IIAli 5JtrE l iij I- T~ FOn SAVANNAH LAIIORATOnY USC ONLY nccdvio /on LA»or\Aionf iv: ISICHAIUMC) UAlt IlMj custobf vitACf CIISI1XI* SCALIIO. I.I. lOO HO. liniutuinsi TiRTivfiT! cm iitiriAlu IC| UAII |iu( T:|ii<!llAlullCi 6AIC IMJC lAUUIIAIOIIV MIMAMUS C3£o O >T3 O JO M P) pi n> at OT It < O (9 (B K- ft ..(/I!-.. fO p. O O 3 O vo 3 H) \ -O VO O I-1 NJ VO Section 7 Revision 0 Date: 9/92 FIGURE 7.2 r f- » | SAVANNAH LABORATORIES "- M I—— * EMVM9QNMENT>U. SWVTCM. INC. Savannah, GA DttrtltW Btaeti. FL Mobilt. AL (9121 3S4-78M (305) 421-7400 (20S1 686-5433 Client _ ... - Irration Analysis . ,, Preservative , . , . Tallaltaun. FL ^ (904) 171-3994 By. Tamoa. FL (813) 8BS-7427 TUT OO6 OO1A Section 7 Revision 0 Date: 9/92 Temperature-Lab Use Only" is prefilled with tap water and supplied with each sample shipment to monitor sample temperature upon receipt. Projects which require sample containers to be screened for contaminating properties prior to shipment and certified "contaminant-free" can be provided upon the client's request and expense. Containers will be provided with a unique batch assignment number to permit traceability. A sample container preparation logbook (Figure 7.3) is maintained by custody personnel in the event this level of service is requested. All standard custody procedures are maintained for precleaned sample containers. 7.3.2 Chain of Custody Documentation, Traceability, and Sample Integrity Formal chain-of-custody procedures are initiated by a custody dispatch technician who is responsible for organization and relinquishment of sample containers to the client or field personnel. All field information must be properly recorded on the chain-of-custody form. Proper completion of the form is the responsibility of the field sampling manager and is required prior to relinquishment of the samples. If the site address is different from the client address, the site address is recorded in the "Project Name" space on the chain-of-custody form, or on the right hand side of the form if additional space is required. The sample identities assigned in the field are recorded in the "Sample Identification" column. Common carriers may identify themselves by signing the "Relinquished By" space on the chain-of-custody form. For samples transported from the field to the laboratory by common carrier, chain of custody is maintained. Completed custody forms must accompany each sealed cooler, and are placed in a plastic bag and taped to the inside lid of the cooler. Coolers are sealed in the field with the SL Custody Seal (Figure 7.4) or custody tape by the field sampling team to ensure that tampering will be immediately evident. A unique identification number is recorded on the seal and accompanying chain-of- custody form with waterproof ink. A copy of each airbill package tracking form associated with a shipment of samples is maintained in the appropriate client files. The sample receipt custodian is responsible for the inspection of shipping containers upon laboratory receipt for overall integrity and to ensure that the contents have not been altered or tampered with during transit. If tampering is apparent, the sample receipt custodian immediately contacts the assigned project manager. The sample manager is also notified of the incident and is responsible for client notification. A sample custody excursion form (Figure 7.5) is filed by the sample manager, and any corrective action required by the client is documented on the accompanying project chain-of-custody form which is dated and signed by the sample or project manager. TUT OO6 OO.1.5 FIGURE 7.3 Section 7 Revision 0 Dace: 9/92 o 55 O H Els KC W« A* H 55H g 2 O O —I t/1 - s • 0 * 4 Jjl U U O § U! *; £• U U U• br P4 rf ! U 1 S eu cu e- • • H• U ft. U U*0 0e 5 Ve *4 J cI E 4 SI u 1 q H "S1 1 3 1 H M U V r TUT OO6 O016 Section 7 Revision 0 Date: 9/92 FIGURE 7.4 SAVANNAH LABORATORIES .'im ieH'/lCSS. WC. OFFICIAL SAMPLE SEAL TUT OO6 OO17 SL SAMPLE CUSTODY EXCURSION SL Project/SCO t Sample Description Data Sampled Date Received Arrival Tump. Inappropriate Container Container llroakage Container Leakage Container L.l.ol Discrepancy Conmenti Initials CLIENT NOTIFICATION SL Contact Notification Data Via Fhone/Fu Client Contact Resolution en fO W re re on n < n (t> (B H- rt •• (n H- ^-J H- O O 3 O \0 3 H>\ ~J vo O EXCURSION:09./ 7:1 TUT O06 OOI8 Section 7 Revision 0 Date: 9/92 If shipping containers arrive intact, they are immediately opened by the sample receipt custodian in the receiving area, and the chain-of-custody form and temperature container removed for inspection. Container temperature upon receipt is documented in a bound sample registry (Figure 7.6), or if requested by the client, documented on the chain-of-custody form. 7.3.3 Field Custody When sample collection is performed by SL, Savannah Laboratories' field sampling manager is responsible for ensuring that chain-of-custody procedures for all sampling events are properly documented. The custody forms and login procedures follow the protocol outlined in Section 7.3. Prior to field sampling, it is preferable to place waterproof sample labels on each sample container and complete each sample label with as much information as possible in waterproof ink. Field sampling technicians are responsible for ensuring that labels are completely filled out upon sampling. Each sample is identified in the field by a unique alphanumeric designation on the label. All information included on each container label must be included on all field-generated records including: permanent field notebook, individual well log, groundwater elevation form, and chain-of-custody form. This field documentation demonstrates traceability of the containers and samples and links all ancillary records to specific sampling events. Each sample is packed to ensure against leakage or breakage and to maintain individual sample integrity. All glass containers are secured individually with bubble wrap. Each set of sample containers with the same sample identity is placed together in plastic bags and sealed. When more than one set of sample containers (different sample identities) are placed in the sample cooler, each set must be sealed in a separate plastic bag. All VOA sample vials are wrapped twice in bubble wrap and each set is sealed in a separate plastic bag. Sufficient ice is placed in sealed plastic bags to maintain the sample at 4° C until sample receipt by the laboratory. Additional information regarding sampling can be found in Section 6.0. Ten percent of samples collected by the SL field sampling team will consist of quality control samples for pH, specific conductivity, temperature, or other client specified parameters per site to satisfy DQO project requirements. When applicable to the site, the following information is documented by the field technicians in the bound field notebook. This field documenta- tion is reviewed, approved and initialed by the field sampling manager prior to client submission. TUT OO6 00.19 ocoo 9<:>o ini 1 SL LOG NO. CUSTODIAN INITIALS . TIME RECEIVED DATE RECEIVED DELIVERED BY CLIENT ID IrYmptestc L iVm amber gtess w/TFE SSO rrt. nVm plastic 539 rrC nVtn tmbar glass 250 rrt nVm plastic 2SO rrL tTVm na^flnc 1 25 ml m/m amber glass w/TFE lOOrrt rrYmpt»cc <0 ni. vW w/TFE tw/m glass Lw/m plastic 530 tri. orfm glass SX rrf. w/m plastic 253 rrt. w/m plastic 1 25 rrL nVm arrO*! glass w/TFE 1 00 rrL w/m glass 250 mt m/m glass ADDITIONAL SAMPLE INFORMATION CONTAINER TEMP. NOTIFY CLIENT LOGIN COMPUTER DATE REPORTED CO [— CO><: HD rn ID EGISTRY 5 m § w 2 O O m O i m O 3 5 61 5° 6 26/6 : 0 UOTSTAS'JJ i Section 7 Revision 0 Date: 9/92 Site location Date/time of sampling Sample identification (including specific location) Sample sequence number Site conditions Weather conditions Purging equipment used Description of QC samples collected Names of personnel/visitors Sampling equipment used Field analysis data Field decontamination techniques Well casing composition and diameter Drilling/boring method Drilling well type/name Water table and well depth Purge volume calculations Volume of water purged Date/time of purging Analytical data to monitor stabilization of well Use of fuel powered units Plumbing/tap material construction Purging flow rate Purging time Flow rate at sample collection Depth samples taken Beginning/ending time for composite sampling Depth soil samples taken Soil sampling technique used Type/description of drums Phases sampled in drums More complete information is provided regarding sampling procedures and documentation in Section 6. 7.3.4 Sample Documentation, Identification, and Login A seven-character project code is assigned by division and sequentially in order of sample receipt, recorded on the chain-of-custody form and each sample container submitted with the project and recorded in the bound Sample Registry. Proper and complete sample documentation must be provided on the chain-of-custody form in order to log samples into the sample registry. The sample registry includes all information necessary to maintain chain of custody including laboratory ID, client (field) ID, and initials of the sample receipt custodian. Ancillary information such as sample collection date and requested analyses is transferred directly from the chain-of-custody form into the LIMS, and appears on the client acknowledgement for each project. Once the chain of custody is verified, the project identified by this unique number is logged into the computerized LIMS (Figure 5.1) to disburse the desired work order request to the laboratory. The sample receipt custodian checks each sample against the chain-of-custody form for TUT OO6 OO21 Section 7 Revision 0 Date: 9/92 discrepancies between information on the sample label and information provided on the chain-of-custody form. The sample receipt custodian also inspects all samples for leakage or obvious seal tampering (if provided). All samples are unpacked in a well-ventilated sample receipt area. Personal respirators are provided to each sample receipt staff, member for use with any hazardous samples. Samples received in plastic containers which appear to be accumulating or evolving gas are treated cautiously because they may contain toxic fumes or be of an explosive nature. A space labeled "custody intact" provided on the chain-of-custody form is used to describe the sample condition upon receipt. A "Y" indicates no custody problem was identified and a "N" indicates samples or container integrity was compromised and client notification and corrective action is required. Discrepancies noted from the custody staff are transmitted to the project and sample manager and are resolved with the client prior to laboratory work assignment. The project manager or the sample manager attempt to resolve custody discrepancies expeditiously to avoid holding time compromises. After a decision concerning a sample has been made, the project manager or sample manager makes an initialed note on the original custody form which states person notified, time, date, and resolution, if applicable. 7.3.5 Sample Preservation After addition of the project sequential identification number, the samples are dispersed to the appropriate laboratory section sample storage areas. Color-code dots and unique sample bottle types correspond to specific analysis and are stored at designated sample storage areas throughout the laboratory sections. Bound sample storage temperature logs are maintained for all sample storage refrigerators to assure proper temperature maintenance throughout the analytical process. The color code scheme for the various preservatives used in SL's sample containers is in the Sample Container Request Form which is submitted by a client requesting sample containers. This two-sided form is shown in Figures 7.7 and 7.8. All sample containers used by the SL field sampling team contain premeasured portions of preservatives. Additional preservatives are obtained prior to each sampling event from parent stocks maintained by the shipping department. Documentation is kept for all additional preservatives used in the field. The effectiveness of pH adjustment by addition of acid or base to the samples is checked after sampling by pouring a small amount of the preserved samples into a small specimen cup and testing with narrow range pH paper. Because of the risk of compromising sample integrity, VOA samples cannot be checked in the field. TUT 006 0022 FIGURE 7.7 SAMPLE CONTAINER REQUEST FORM Section 7 Revision 0 Date: 9/92 The number, color-code preservative and container description for the analyses as requested are listed below. A summary of sampling instructions for general analysis categories is referenced on the reverse side. AQUEOUS _0 To c. 1 -_l LLJ j_ 3 VI V) 01 _J .0 To 500 mL m/m plz 500 mL n/m glass .0 To c. .£ _i s eg o oo 250 mL m/m na 1 25 mL m/m ambor glass w/TFE _0 To R C. c1 "EI 40 ml. vial w/TFE NONAQUEOUS «*ia c "? _i u M ts E "5_i iiOOmLw/rn glass 500 rnL w/m plastic 250 rnL rn/m plastic u. * V) VJ _reo o « C "E_j in CM 1 00 mL w/m glass COLOR PRESERVATIVE CODE Lab Pk Prep, by: Lab Pk checked bv: Quantity of Lab Pks. Shipped: SLProiect Mar.: Sample Coordinator: Comment- Temperature Container ... NO. OF CONTAINERS SHIPPPED NO. OF CONTAINERS/SAMPLE NO. OF TRIP BLANKS NO. OF FIELD BLANKS NO. OF EQUIPMENT BLANKS GENERAL PARAMETERS Lab Pack Shipping Address. Phone No: ___ Date of Shipment: Account No: ___ Method of Shipment: Project: ______ PRESERVATION COLOR CODE KEY RED <" CAUTION! STRONG OXIDIZER! CONTAINS NITRIC ACID. Avoid skin and eye contact. If contact is made. FLUSH IMMEDIATELY with water. GREEN (G) CAUTION! CONTAINS SULFURIC ACID. Avoid skin and eye contact. If contact is made. FLUSH IMMEDIATELY with water. BLUE (B) CAUT1ONI STRONG CAUSTICI CONTAINS SODIUM HYDROXIDE. Avoid skin and eye contact. If contact is made. FLUSH IMMEDIATELY with water. PURPLE (P) No preservative added. ORANGE (0) No preservative added. TAN 0) Contains Zinc Acetate. Avoid skin and eye contact If contact is made. FLUSH IMMEDIATELY with water. YELLOW (Y) Contains Sodium Thiosulfate. Sterilized container. LT. BLUE (LB) CAUTION I CONTAINS HYDROCHLORIC ACID. Avoid skin and eye contact. If contact is made FLUSH IMMEDIATELY with water. DO NOT inhale vapors that may be caused from a chemical reaction between the preservative and sample. Collect sample in a well-ventilated area or use appropriate breathing apparatus. NEVER RINSE sample containers. If skin contact with preservatives occurs, always wash hands IMMEDIATELY. SAMPCONT DRW:09.0192:3 TUT 006 0023 FIGURE 7.8 GENERAL SAMPLING INSTRUCTIONS Section 7 Revision 0 Date: 9/92 DO NOT PRE-IUNSE CONTAINERS. These containers have been specially prepared for specific analyses (See Presetvalive Color Code Key). Fill container to within 1" of capacity unless otherwise indicated, cap tightly, label and ice. Some requests require multiple containers to perform all analyses. (See Sample Request Form on reverse side.) LITER PLASTIC Purple n/m: Blue n/m: Red n/m: Purple w/m: (Nonaqueous) LITER GLASS Purple n/m: Orange n/m Green n/m: Purple w/m: (Nonaqueous) 500 PLASTIC Purple m/m: Red m/m: Purple w/m: (Nonaqueous) 500 ML GLASS W/TFE Lt. Blue w/m: Green w/m: Physical Properties. Miscellaneous General (BOD) Cyanide Radiological (Rad 226. Rad 228. alpha and beta) Metals and Miscellaneous Inorganics. General. Physical Properties Ettractable Organics (DNAs. Pcsticides/PCBs. MBAS. Herbicides) Dioxin/Dibenzofurans Total Recoverable Phenolic* All Organics (excluding Volatiles), Inorganics. Physical Properties. General Physical Properties. Miscellaneous General Metals with Mercury- Inorganics. Physical Properties Petroleum Hydrocarbons Oil and Grease Green n/m (amber): TOX. Fill to capacity. Purple w/m: (Nonaqueous) 250 ML PLASTIC Purple m/m: Red m/m: Green m/m: Tan m/m: 250 ML NALGENE Yellow m/m: 125 ML AMBER GLASS VWTFE Green m/m: Purple m/m: (Nonaqueous) 100 ML PLASTIC Purple m/m: Green m/m: 100 ML GLASS Purple w/m: (nonaqueous): 40 ML GLASS VIAL W/TFE Lt. Blue n/m: Purple n/m: Yellow n/m: All Organics (excluding Volatiles), Inorganics. Physical Properties. General Physical Properties. Inorganics (nutrients). Hexavalem Chromium Metals without Mercury Nitrogen series. Phosphorus Sulfide Bacteriological (Coliform. Standard Plate Count) Sterile container - do not touch cap or container interior. Remove faucet strainer and flush line prior to sample collection. TOC. Fill to capacity. Volatiles. Fill to capacity - no headspace. Physical Properties. Inorganics (single parameter) Nutrients. COD (single parameter) Organics, Inorganics. Physical Properties. General (single parameter) Volatiles (Aromatics and/or Halogenatcd constituents). Fill vials until slightly overflowing with minimum aeration. Place septa W/TFE liner facing sample and seal with NO headspace. EDB. Volatile Halocarboiu. Fill as referenced above. Trihalomethanes (THM). Fill as referenced above. Container Closure Key (n/m = narrow mouth, m/m = medium mouth, w/m = widemouth) CONTAINER SHIPPING INSTRUCTIONS After sample collection, please check all custody forms and sample containers for discrepancies. Sign the custody form and seal in the enclosed plastic bag. To avoid container leakage during transit, additional plastic bags have been included in the shipment to contain ice for sample preservation. Please place these ice bags between the samples and secure the lab pack for shipment. Return lab packs to Savannah Laboratories & Environmental Services, Inc., 5102 LaRoche Avenue. Savannah. GA 3W04. If you have any questions concerning containers shipped o acceptable Held substitution, please contact your project manager or sample coordinator for assistance at (912) 354-7858 or FAX (912) 352-0165. Thank you for your patronage. TLIT 006 OO24 Section 7 Revision 0 Date: 9/92 All samples received by Savannah Laboratories are checked for proper pH adjustment by the appropriate preparation or analytical department as soon after receipt as possible. The pH of each sample is checked, documented, and adjusted, if necessary. To avoid compromising sample integrity, volatile samples are checked for proper pH adjustment only at the time of analysis. The pH of volatile samples is not adjusted. 7.3.6 Sample Security, Accessibility, Distribution, and Tracking Only authorized personnel are permitted within the laboratory areas where sample access is possible. Sample storage areas are designed to segregate volatile and nonvolatile samples. Standards and extracts are also departmentally controlled and stored in segregated facilities. The set of analyses required for a group of samples is project-dependent. After sample login and verification, samples are relinquished from the receiving area to the appropriate sample preparation area. Those samples not requiring preparation are relinquished immediately to the sample analysis storage area. Using LIMS-generated sample preparation worksheets for guidance, samples are extracted, digested, or distilled as appropriate. An example sample preparation log (Cyanide Distillation Log) is shown in Figure 7.9. The extracts, digestates, or distillates are then transferred and relinquished to the appropriate analysis section, where analysis is performed. An example analysis log (Cyanide Analysis) is shown in Figure 7.10. For projects where in-laboratory custody records are required by the client, the SL project manager should inform the custodian and sample manager to coordinate custody activities prior to sample receipt. For those samples, department-specific in-laboratory sample tracking forms are executed by department staff. An example of a form of this type (Semivolatile Extract Custody Log) is shown in Figure 7.11. Samples and sample preparations are stored in a secure (locked) sample storage area. When samples or sample preparations are removed from or returned to designated storage areas, the form is signed and dated by the analyst. Sample holding times are tracked via the LIMS. Sample collection dates are routinely entered into the LIMS with all sample logins. This information allows holding times specific to each departmental analysis to be tracked by department managers, supervisors, chemists, and analysts through the use of daily status sheets, reference sheets, and preparation worksheets. Date analyzed is recorded via instrument outputs or analysis forms when applicable as an integral part of the raw data. Upon the analysis of each parameter, the date of analysis is entered into the LIMS and can be compared to the date sampled to validate that holding times have not been compromised. TUT OO6 O025 Section 7 Revision 0 Date: 9/92 FIGURE 7.9 CYANIDE DISTILLATION LOG Method CLP Spike Date Check 0 Level Date Stock CN Prepped Analyst Standard Batch # SL Log # Blank ERA Final Volume Sample Description Wet Weight Cyanide.Dis:06.25.92:l TUT O026 Section 7 Revision 0 Date: 9/92 FIGURE 7.10 CYANIDE ANALYSIS LOG Method CLP STANDARD CURVE mg/L A 0.50 0.30 0.10 0.070 0.040 0.010 * SL Log # Sample Description Sample Dilution Date Analyst Batch # Correlation Coefficient QC Check True Value Spike Level Volume or Het Height Sample A Result mg/L Dry Height Result BSAg Cyanide.CLP:06.25.92:1 TUT 006 OO27 FIGURE 7.11 Section 7 Revision 0 Date: 9/92 C3 O Q O to00 o PI Xw H ^ H g H2 H CO t/> •0 H o • a a|| B 1 oe ct § '11 Is 2 i>h s fas -i« • Q C Q *J B l^ • j « « « n *a »^ C w 8 ^^ 2 O £ H *Q a h « e* e « < OS Q »^ M n _. «j M ^1 O «»5 *• TUT 006 002 Section 7 Revision 0 Date: 9/92 7.3.7 Sample Disposition After analysis completion, custody of unused sample portions, extracts, or digests is relinquished to the central secured storage area. Unless a client requests the project manager to save unused samples, digests, or extracts, disposal from the central storage occurs as soon as holding times have expired or three weeks after results submission. Requests for extended sample, digest or extract storage must be provided by the client to the SL project manager in writing (or contract form) prior to sample receipt and extended storage will usually result in additional fees to be negotiated by the SL project manager prior to sample receipt. SL is not responsible for evaporation or other deterioration of samples, extracts, or digests during extended storage periods. Prior to report submission, the project manager reviews all analytical results, and if the results reveal that a sample is hazardous per 40 CFR Part 261 characteristics or contains 50 ppm or greater PCBs; or if client- supplied information (chain-of-custody forms, etc.) states that the sample is hazardous; or if client's instructions or a contract requires all samples be treated as hazardous waste, the project manager will arrange for samples to be returned to the client or disposed of per client's instructions at the client's expense. Tracking and disposal of hazardous samples is accomplished and documented via the LIMS system. 7.3.8 Interdivisional Custody The laboratory director at each location monitors the sample load and turnaround time through LIMS-generated reports. If it appears that analysis demand will exceed capacity, or if instrument failure occurs, samples may be transferred (provided client contracts or arrangements, project QA plans or certification limitations do not prohibit sample transfer) to another SL division to ensure that holding times and turnaround commitments are met. If samples are transferred to another division laboratory, full custody is maintained. Special determination codes specific to each laboratory location are entered into the LIMS to enable the project manager and laboratory director to track sample progress and maintain chain of custody. Copies of the original chain-of-custody form (executed for interdivisional sample submittal), computerized LIMS work order acknowledgements, and extract or digest preparation logs pertinent to the project order accompany the samples or preparations. This material includes dates of sample preparation and requested analyses. Upon sample receipt at the other division laboratory, standard custody procedures are followed. 7.4 Electronic Data Records By careful assignment of user passwords and file access/lock codes, Savannah Laboratories maintains a high level of data security for the LIMS. Thus, only authorized SL personnel can access client files to view TUT O06 OO'29 Section 7 Revision 0 Date: 9/92 data. In addition, data entry and editing is restricted to highly trained data management personnel. If requested, data can be electronically transferred to the client via modem. To insure data integrity, the specific client's data are first downloaded to an off-line PC and then electronically transferred to the client. Access to the PC via modem is controlled by assignment of a confidential password to the client. Signed hard copies of reports and not electronic or diskette deliverables are the official report and are always submitted to clients who request electronic data transfer, which allows verification of downloaded information. SL is not responsible for electronic transfer or diskette errors and maintains that it is the client's responsibility to check all electronic or diskette data against the hard copy. A download information file is maintained by the LIMS manager. Internal documentation is maintained by the LIMS manager for all LIMS programs. This documentation includes descriptions of any program additions, deletions, or modifications, the date of revision, and the initials of the responsible programmer. To verify proper program functioning of the hardware and software, a simulation account is maintained. When hardware/software modifications are made, this account uses actual data to model an account in order to verify the modifications are functioning as anticipated. Antivirus software serves the LIMS as a protective measure. At present, laboratory instrumentation is not interfaced directly to the LIMS and thus, no instrument-LIMS data transfer step requires verification. All instrument data is verified by chemists or analysts as described in Section 12.5.2. Entry of data into the LIMS from chemists' worksheets is performed three times weekly by data entry technicians. Immediately following data entry, approval sheets are printed with the entered data as it appears in the LIMS. Assistant project managers compare all data on the approval sheets, versus the chemists' worksheets for data transcription errors. 7.5 Verification of Hard Copy Records Forms that are routinely printed for verification and signatures include data worksheets, data approval forms, and final reports. Hard copies of final reports, field data, chain of custody forms, and any ancillary documentation pertinent to the project will be stored in a secured storage area and placed in files alphabetically by client and chronologically within each client folder. TUT Section 8 Revision 0 Date: 9/92 8.0 ANALYTICAL PROCEDURES The ultimate responsibility for analytical method selection lies with the client or regulatory agencies. Whenever possible, laboratory and field analysis of all samples are conducted by EPA-approved methodology. When EPA approved methods do not exist or project protocols require alternative methods, these methods must be approved by the client and the appropriate regulatory agency. Tables 5.1 and 5.2 list Savannah Laboratories' routine laboratory parameters with their respective method numbers. Table 5.3 lists field parameters with their respective method numbers. A detailed SOP has been prepared for each routine analytical method. Copies of SOPs are kept at the respective analytical benches, or by each department/section supervisors, and the QA manager or laboratory director. In cases where GC, LC, or GC/MS methods are used to determine compounds not included in the actual method list, these unlisted parameters are flagged in the tables with a triple asterisk (***) and method validation data are included in Appendix A. For those cases where no specific soil or sediment method exists, water methods are adapted. These adaptations are described in Section 8.2, and validation data are presented in Appendix A. Unless indicated in the appropriate SOP, all parameters listed in Tables 5.1 through 5.3 are analyzed by the methods referenced, without modifications. Interpretation of ambiguous method requirements is accomplished by consulting with regulatory agencies and EPA laboratory/QA personnel. 8.1 Glassware Cleaning Procedures Laboratory glassware washing procedures are adapted from SW-846, 40 CFR Part 136, Standard Methods, and EPA 600/4-79-019, and are as follows: Extractable Organics Prerinse each item with the solvent to be used in it. As soon as possible after use, rinse with lab-grade acetone. Wash with hot water and a nonphosphate detergent such as Alconox, scrubbing thoroughly with a brush. Rinse thoroughly with tap water at least three times. Rinse inside surface with Nochromix solution, catching rinsate for re-use. Rinse again with tap water, followed by pesticide-grade acetone. Rinsing with hexane is avoided to minimize the possibility of contamination of glassware used for total petroleum hydrocarbon determination. Air dry when possible, and do not bake Class A volumetric glassware. Store glassware inverted or cap openings with foil to exclude dust and other contaminants. Because of possible damage, caps, septa, and plastic items are not rinsed with Nochromix. Volatile Organics Wash with tap water and Alconox or Liquinox, then rinse thoroughly with organic free water. Oven dry at 110*- 120*C for at least two hours. Do TUT OO6 OO31 Section 8 Revision 0 Date: 9/92 not bake Class A volumetric glassware. Glassware is usually stored in the oven until use. Caps and septa are washed in the same manner, but caps are not oven-dried. Highly contaminated glassware is allowed to soak in Nochromix solution overnight, then washed as above. General Chemistry. Microbiology. Nutrients. Demands Wash with hot tap water and Liquinox, rinse thoroughly with tap and deionized water, and air dry. Store glassware inverted or cap openings with foil. Autoclave bacteriological laboratory glassware and collection bottles as described in analytical procedures. COD digestion tubes and caps are cleaned with brushing and tap water (no soap) and rinsed thoroughly with deionized water. Tubes for TKN and total phosphorus sample digestions are washed with hot water and Liquinox, and rinsed with tap water, Nochromix, and deionized water. Metals/Radionuclides Wash glass, plastic, and Teflon items in hot tap water and Alconox. Rinse with tap water, 1:1 nitric acid, tap water, and deionized water. Teflon beakers used for sample digestion are further decontaminated by adding 20 mL nitric acid and 12 mL hydrochloric acid, covering with a watch glass, and digesting on a hot plate for two hours. Following this treatment, they are rinsed with 10X nitric acid and deionized water and allowed to air dry. 8.2 Soil Sample Preparation Notes In the absence of an approved soil method, water methods are adapted for soil matrices. The following soil preparation procedures are applied to parameters in Table 5.2. 1. Fluoride (extractable): Method 340.2 Approximately 5 g of sample is weighed out exactly and placed in a screw- cap plastic bottle. One hundred mL of DI water is added to the sample, the bottle is capped, placed in a rotating extractor, and rotated for 2 hours. Upon removal, the sample is allowed to settle, the supernatant decanted, and the extract is analyzed as a liquid sample. 2. Alpha and Beta Radioactivity: Method 9310/900 Soil is ground to a fine powder with mortar and pestle, and 50 to 100 mg soil is weighed onto a tared planchet. Sample is distributed evenly over planchet surface, fixed with clear acrylic solution, dried, and counted. 3. Chloride (extractable): Method 9251/407A Approximately 5 g of sample is weighed out exactly and placed in a screw- cap plastic bottle. One hundred mL of DI water is added to the sample, the bottle is capped, placed in a rotating extractor, and rotated for 2 hours. Upon removal, the sample is allowed to settle and the supernatant is decanted. The extract is analyzed as a liquid sample. TUT OO6 OO32 Section 8 Revision 0 Date: 9/92 4. Sulfate (extractable): Method 9036/9038/375.3 Approximately 5 g of sample is weighed out exactly and placed in a 100-mL screw-cap plastic bottle. One hundred mL of DI water is added to the sample, the bottle is capped, placed in a rotating extractor, and rotated for 2 hours. Upon removal, the extract is filtered using a syringe filter with a 0.20-um pore size filter and analyzed as a liquid sample. 5. Orthophosphate (extractable): Method 365.1 Approximately 5 g of sample is weighed out exactly and placed in a screw- cap plastic bottle. One hundred mL of DI water is added to the sample, the bottle is capped and placed in a rotating extractor, and rotated for 2 hours. Upon removal, the sample is allowed to settle and the supernatant is decanted. The extract is analyzed as a liquid sample. 6. Surfactants: Method 425.1 Sample (10-20 g) is weighed out exactly into a 500-mL screw-cap bottle. A volume of water equivalent to 20 times the sample weight is added to the sample, the bottle is capped, placed in a rotating extractor, and rotated for 2 hours. Upon removal, the sample is allowed to settle and the supernatant is decanted. The extract is analyzed as a liquid sample. 8.3 Deviations from Referenced Analytical Methods In the determination of sulfide in liquid samples containing turbidity or color and in all soil or sediment samples, samples are distilled as per SW-846 method 9030. Upon distillation of the sample, the trapping solution is analyzed colorimetrically as a clear liquid sample as per EPA method 376.2. 8.4 Reagent Storage and Documentation Reagents are stored with consideration for safety and maximum shelf life. Storage conditions for various classes of reagents are given in Table 8.1, as well as discussed below. Documentation maintenance status for the reagent classes is also given in Table 8.1. All acids, except those poured up in small marked containers which are for immediate use, are stored in the original containers in acid storage cabinets. All bases, except those poured up in small containers for immediate use and those that are standardized for specific purposes, are stored in the original containers in designated areas or storage cabinets. All flammable solvents, except those poured up for immediate use are stored in original containers in approved vented flammable storage cabinets which are located in air conditioned areas. Dry reagents are stored in designated cabinets in cool, dry areas. Reactive chemicals, cyanides and sulfides are labeled and isolated from other chemicals. TUT OO6 oo: Section 8 Revision 0 Date: 9/92 TABLE 8.1 REAGENT STORAGE Chemical Acids Bases Nonflammable Organic Solvents Flammable Solvents Dry Reagents Reactive Chemicals Method of Storage Original containers in acid storage cabinets Original containers in designated storage cabinets Original containers in designated storage cabinets Original containers in vented flammable storage cabinets Original containers in designated cool, dry storage cabinets Original containers in isolated cool, dry storage cabinets Documentation Yes Yes Yes Yes Yes Yes TUT OO6 Section 8 Revision 0 Date: 9/92 All acids used for metal sample digestions and all solvents used for semivolatile sample extraction are tested prior to initial use. Specific acceptable chemical lots are reserved and stored by the vendor(s) and are requisitioned and received as needed by the laboratory. Lot numbers used for digestions or extractions are recorded in bound notebooks in the appropriate departments. Reagent blanks are analyzed with each sample batch for all methods, validating the purity of all reagents. All reagent containers are dated when received, and dated and initialed when opened (except high use items consumed in less than one week). Documentation is maintained to provide traceability of the reagents used with the analysis of any batch to specific reagent lot numbers. 8.5 Waste Disposal All waste disposal is carried out in accordance to Savannah Laboratories' Waste Disposal SOP. This document includes procedures for identification, storage, personnel training, tracking forms, report forms, safety, as well as details of the disposal. Hazardous waste disposal procedures are given in Table 8.2 and discussed below. Hazardous wastes must: be disposed of prior to accumulation of 1,000 kg (approximately 5 drums) of hazardous waste or 100 kg (0.5 drums) of acutely hazardous waste (261.33 (a) - (e) - P list). Be generated at a rate of less than 100 kg of total hazardous waste per facility per month (or 1 kg of acutely hazardous waste). be stored in non-leaking containers in good condition with close- fitting lids and kept closed when wastes are not being added or removed. be accurately labeled with waterproof labels. Labels must specify the words "Hazardous Waste", the composition and physical state of the waste, the hazardous properties of the waste (e.g., flammable, reactive, etc.), and the name and address of the generator. be clearly labeled with the date that the period of accumulation began on each container and the Hazardous Waste Tracking Log Form. be handled in containers and in a way that minimizes the possibility of spills and escape of wastes into the environment. be stored in an area which is regularly inspected for deteriorating or leaking containers. TUT OO6 OO35 Section 8 Revision 0 Date: 9/92 TABLE 8.2 WASTE DISPOSAL PROCEDURES Haste Type Halogenated Solvents Methylene Chloride Freon Mixed Solvents (Flamnable & nonhalogenated) All neat standards and mixes over 100 ppm Heavy Metals Solutions Acid Solutions Alkaline Solutions All samples containing Organics or Inorganics exceeding hazardous waste standards* Associated Analytical end Sanple Prep Methods Pesticides, Herbicides, BNA, GPC, etc. Oil & Grease, Petroleum. Hydrocarbons VCX: Standards, Herbicides. Pesticides All analyses Metals, COD, Chloride Metals, General Inorganics, Extractions General Inorganics, Extractions All analytical groups Storage Procedures Store in glass bottles, then in drums . ** Store in glass bottles, then in drums Store in glass bottles, then in drums Store in original bottles of glass/ plastic bottles, then lab pak Store in glass bottles, then in drums Store in glass bottles or add to neutralizing chambers Store in glass bottles Store in original bottles or jars in sample custody storage area Disposal Procedures Reclaimed by HH contractor Reclaimed by HH contractor Disposal by HW Contractor Disposal by HW contractor (Packed by also) Disposal by HH contractor Neutralize; sanitary sewer Neutralize, sanitary sewer Return to client, or disposal by HH contractor Hazardous Haste Characteristics (D001 - D017) (40 CFR Fart 261). HCN > 250 ing/kg, H,S > 500 mg/kg, TCLP Toxicity Characteristics (Federal Register. 55FR 11798), March 29, 1990, or contains greater than 50 ppm PCBs. Bottles are kept in each lab and are periodically moved by the Haste Coordinator to hazardous waste storage area. GO 3 6 Section 8 Revision 0 Date: 9/92 All waste must be segregated for temporary accumulation and storage as well as for disposal. Care must be taken to combine waste materials into categories or waste streams based upon their compatibility. The following four types of waste are stored in 55-gallon drums. 1. Halogenated solvents (methylene chloride and others) -- Store in closed cap metal drum) 2. Freon -- Store in closed cap metal drum 3. Nonhalogenated flammable solvents -- Store in closed cap metal drum 4. Heavy metals or other aqueous wastes (except cyanide) -- Store in poly drum All other wastes should be stored in the original container or 4-liter glass bottles and disposed of via lab pak. (Packed by disposal company in 55-gallon open top drums . ) TUT OO6 OO37 Section 9 Revision 0 Date: 09/92 9.0 CALIBRATION PROCEDURES AND FREQUENCY 9.1 Laboratory Equipment Savannah Laboratories is equipped with state-of-the-art instrumentation to provide quality analytical data to clients. A list of the instrumentation maintained by Savannah Laboratories for the determination of the parameters contained in Tables 5.1 and 5.2 is found in Table 9.1. A list of all field instrumentation maintained by the laboratory is contained in Table 9.2. 9.2 Standard Receipt and Traceability Standards are purchased from commercial sources in mixes designed for the specific methods or as neat compounds. Certificates of analysis are shipped with each ampule by the vendor. The standards are certified to meet or exceed the criteria established by the U.S. EPA. Upon receipt, dates are placed on all standard materials. Standard logbooks are maintained by all sections of the laboratory to document the traceability of working standards back to neat materials or prepared stock mixes. All standards are assigned a lot number that provides a unique identification as well as identifying the type of standard (i.e., working). This unique lot number is documented in a laboratory notebook along with date of preparation, initials of preparer, concentration, expiration date (if applicable), and solvent (if applicable). A standard preparation narrative is also provided in this notebook to detailing the preparation steps for each standard. 9.3 Standard Sources and Preparation Savannah Laboratories maintains an inventory of materials to produce stock standards or purchases stock standards from commercial vendors. Laboratory preparation of all lab-prepared stock, intermediate, and working standards is documented by the responsible analysts. Table 9.3 presents standard sources and preparation protocols for various sections of the laboratory. Field instruments requiring calibration standards (conductivity meters and pH meters) use the same sources as laboratory instrumentation. Table 9.4 lists titrants used by the laboratory and information regarding their standardization. 9.4 Laboratory Instrument Calibration The calibration procedures given below meet or exceed EPA method requirements. Any method calibration requirements which are more stringent than these procedures will be used. TUT OO6 OO38 TABLE 9.1 MAJOR LABORATORY INSTRUMENTS AT EACH SAVANNAH LABORATORIES LOCATION t 6 5 15 10 10 32 24 3 Instrument TCP Units Mercury Cold Vapor Units Atomic Absorption Furnace/Flam* GC/MS Semlvolatilas GC/MS Volatiles Gas Chromatography Semivolatiles Gas Chromatography Volatiles/F&T TOC Analyzers Deerfleld Beach 1-Jarrell Ash 61 1-Varian VGA/AA20 1-Varian 400Z 1-Perkin Elmer 2380 1-HP 5970 1-HP 5970 3-Varian 3400 with dual ECD 3-Varian 3400 with dual FID 1-Varian 3600 with PID/Hall 3-Varian 3300 with PID/Hall 1-Varian 3300 with PID/FID 1-Varian 3300 with FID/Hall 1-01 52* Tallahassae 1-Jarrell Ash 61 1-Varian VGA-76/AA20 2-Varian 400Z 1-Varian AA 20 2-HP 5970 2-HP 5970 1-Varian 3400 with NPD/ECD 1-Varian 3400 with dual NPD 2-Varian 3400 with dual FID 3-Varian 3400 with dual ECD 1-Shimadzu 9AM with dual ECD 1-HP 5880 with FID 1-Varian 3700 with Hall/FID 1-Varian 3300 with Hall/FID 1-Varian 3300 with PID/Hall 1-Varlan 3300 with PID/FID 1-Varian 3400 with PID/Hall 1-Varian 3600 with PID/Hall Savannah 1-Jarrell Ash 61 1-Jarrell Ash Envlro 36 1-Varlan VGA-76/AA20 2-Varian 400Z 2-Jarrell Ash 22/4000 1-Perkin Elmer 2380 5-HP 5970 3-HP 5970 2-HP 5971 1-Varlan 3400 with dual FID 1-Varian 3400 with quad FID 1-Varian 3400 with dual NPD 2-Varian 3400 with dual ECD 2-Varian 3700 with dual ECD 1-Varian 3700 with ECD 1-Varian 3700 with Hall/PID 1-Varian 3700 with Hall/FID 1-Varian 3600 with Hall/PID 1-Varlan 3400 with PID/FID 2-Varian 3300 with Hall/FID 1-Dohrmann DC80 Mobile 1-Jarrell Ash 61E 1-Perkin Elmer 5000 1-Varien 400Z 1-Perkin Elmer 5000 1-HP 5970 1-HP 5970 2-Varian 3400 with dual ECD 1-Varian 3300 with dual FID 1-Varian 3300 with dual NPD 1-Varian 3300 with Hall/FID 1-Varian 3300 with Hall/PID 1-01 524 Tampa Bay 1-Jarrell Ash 61E 1-Coleman 50B 1-Varlan 400Z 1-Varian AA 20 1-HP 5971A 1-HP 5971A 2-Varian 3400 with dual ECD 2-Varian 3300 with dual FID 1-Varian 3300 with FID/Hall 1-Tracor 540 with PID/Hall 1-Varlan 3600 with PID/Hall 1-Varian 3400 with FID/FID ^o c? ?o ^^ P> B) (B (t) OT rf < o (0 (D H- ft .. (fl H. Ni H. O ^s§: M \ O ^J VO N3 Section 9 Revision 0 Date: 09/92 H Ov H n zo H 520 S M 0 O pa i-1 1 1 M S3 3,, COH Z g H toZ Og2o pa * 2* fr & H •H 1 •Si\n * 5 <j au a PD 2• a 1 40 § *> a M * U ij g u 0 M •* 0 1 03 33 i U 2 C -H U w •»o M •* U 1 a x •"* o r* -H «M 11 U -4 O c to •» •H O M M » kl U 1 0 3 U B. to £ 1 1 « 141 u c M a<i 0 •H r^ 0 W C —4 Sa.ii-» M M 4J0 § 4J O •s. 0u o at a M « - on X « Co ~4 v4Z •H O • S3li 0 O g. 1 «H CO O CO W O£ M C C <0 0 -H €0 IE (2 § i i i o g. « 4J Z M 1 1 «I *1 n kl 4J g O •p. o OT kl - Oo 09 no 0ki H eou «4 U H 1n ki• N -JJ C 0 Nutria 1 Auto an n u •c o o 00 CO CT. •» c* •» 0 0 0 U O kl • 43 • 4J 0 4J 0 kt 0 a x s i i i ft i-t ^* •i CO 0 m nki0 *J0 Z ^ Jj C 1 - oo 10 u0 01 EH 1 0 0 CQI •H Oo 0 N *> — 1 M 10 n »J fl ^ Z Scalar - N 00 •H 0 g § 1 *-f kl •a 3 3 0 •J 0 i 0 u 0 4J Ou M M0 fc. g TJ « tH O 0 K| o .-1 * 0 •0o g kls co l-< - oa0 m t-t CO •H CO m ,_, CO>t 1 pa0 Ml *H §2I t-t n 0 M S 1 a 0 S •H n M0 0 - a 0 CO r-l U EI O O r-4 C4 JlU 0 S3 rf 5 0 tH JZua i «-« ao CO •H j. U 0 as 0 •0 2 ic• •eo ^ 20 0 E ~4 Turbid m «oi ki gi •§oi 0) *}kt N « g - fO h-t CO 1 *-< in en tH CO 1 ^ « HI CO 1 CO 1-1 nu0 1 X 4J -H _> ^) Conduc „ *H •9 •H kl Z 1 *H ^ * _! uo .H Cu t-H •og § •u -H 0 0 3 kl o e ki 0 0 -4 > Cm •oc0 c * O H 03 ki O 0 -4 X kl 14 > h, •Oc0 g 8 ki *J O • § i •a« 0 -H > U, TJ C0 C X kl Aj o • 3 kl O • > iZ •D C0 C 0 O k! kl 4J 3 14 O • -- X 0 -^ > b. M £ W Ui t-t E O. trt 00 " u• •J y •" 0 0 «C •! kl -4 0 kl -J O 0 0 Z en 1 1 O O <£ O «-« CM SS ki ki 0 0 •F-4 ———* r £ i i •H fH 0 sO kl .-H 0r t-4 (•) W 14 0 *J *J 0 Z •H 0 U Cc a CQ -H U I - TUT O06 OO4O TABLE 9.1 MAJOR LABORATORY INSTRUMENTS AT EACH SAVANNAH LABORATORIES LOCATION # 18 5 15 6 6 20 e 5 2 Instrument Top Loading Balance Autoclave Waterbath Biological Incubator BOO Incubator Drying Oven Block Digestor TCLP (nonvolatile) TCLP (ZHE) Deer field Beach 2-Sartorius 1-Napco 8000-DSE 2-Fisher Versabath 1-Baxter Tempcon 1-Hestinghouse 16.8 1-Fisher Isotemp 500 1-Hach SL Custom Tallahaasee 1-Mettler PE1600 1-Sartorius L2200-S 1-Sartorius PT1200 1-Napco 9000D 2-Fisher 1-Baxter 1-Blue M Stabil- Therm 1-Precision 815 1-Fisher Isotemp 500 3 -Blue M 2-Fisher Isotemp 6S5G 1-Tempcon 1-Thermolyne Dri- Bath SL Custom Savannah 1-Mettler PM 2000 2-Sartorius GMBH 2-Mettler 1600 PE 1-Fisher XLSOO 1-Sartorius 1202 1-Napco 9000D 1-C-M Equatherm 2-Fisher Versabath 1-Fisher 20L 1-Lab-Liner 3554-17 1-Precision Lo-Temp 4-Flsher Isotemp 500 1-Tempcon N8620-1 1-Blue M 2-Technicon BD-40 1-Thermolyne Dri-Bath 1-Lab-Line Multiblank 2093 SL Custom 1-ATCS ZHE Mobile 1-SP DTL4100 1-Sartorius B3100P 1-Sartorius FT600 1-Napco 9000D 1-Fisher Scientific 1-Baxter Durabath 1-Blue M Magi-Whirl 1-SPB7001-2 1-Fisher 630D 1-Precision Coliform 2-Precision Lo-Temp 3-Blue M 1-Precislon Scientific 1-Techni: Dri-Block DB-3H SL Custom 1-ATCS ZHE Tampa Bay 3-Mettler PM3000 1-Napco 9000D 1-Branson 3200 1-Baxter Durabath 1-Blue M 1-Fisher 307 3-VWR 1305* 1-Thermolyne SL Custom TJ O pa in p> (u n> o m rr < o fl> (B I-1' ft VO to TABLE 9.2 MAJOR FIELD INSTRUMENTS AT EACH SAVANNAH LABORATORIES LOCATION i * 4 3 3 2 2 2 Instrument pH/SC/DO/T' Meters pH/Tecnp Maters Conductivity Metiirs DO Maters Turbldlmeters Hater Level Meters Deerfleld Beach 1-Corning Checkmate 90 1 YSI 33 j Tallahaaaee 1-Cornlng Checkmate 90 1-Orlon 23A 1-YSI 33 1-YSI 51B 1-Hach 16800 1-Slope 31453 Savannah 1 -Coming Checkmate 90 1-Orion SA-230 1-YSI 33 1-YSI 51B 1-DRT 15C 1-Flsher Mobile 1-Orion 23A 1-YSI 33 1-YSI SOB Tampa Bay 1-Corning Checkmate 90 1-Orlon 23A >rJ O po to B> pi (t> (D On rt < O (l> (t> H- rt •• w h" ui P. O r-.j H CH TABLE 9.3 STANDARD SOURCE AND PREPARATION FOR LABORATORY INSTRUMENTATION Instrument Group ICP AA Autoanalyzer Ion Chromatograph UV-VIS Spectrophotometer IR Spectrophotometer Standard Source Baker/Spex Bakar/Spex Fisher Baker Fisher Baker MaUinckrodt Fisher Baker EM Fisher How Received Stock 1,000 or 10,000 ppm solutions Stock 1,000 ppm solutions Neat material Neat material Neat Material Neat liquids Source Storage Room tamp Room temp Room temp Room temp Room temp Room temp Preparation From Source Working std prepped directly from stock Intermediate stds prapped from stocks. Working stds prepped from intermediates. Stock stds prepped from solids. Intermediate stds from stocks. Working stds from intermediates. Stock stds prepped from solids. Intermediate stds from stocks. Working stds from Intermediates. Stock stds prepped from solids. Intermediate stds from stocks. Working stds from intermediates . Stock std prepped from neat liquid. Working stds from stock. Lab Stock Storage Room temp Room temp Room temp Refrigerator Used immediately Used immediately Refrigerator Used immediately Used immediately Refrigerator Used immediately Used immediately Refrigerator Refrigerator Prep Frequency Quarterly or as needed Biweekly Weekly Monthly Daily or as needed Daily or as needed Monthly Daily or as needed Dally or as needed Monthly Daily or as needed Daily or as needed Monthly Monthly o pt) in p> n> n> rt < o <r> H> rt vo vo \ O VO CO TABLE 9.3 STANDARD SOURCE AND PREPARATION FOR LABORATORY INSTRUMENTATION Instrument Group Turbidlnetar Conductivity Meter TOC pH Meter ISE TOX Bomb Calorimeter Standard Source Hach YSI or Fisher Mallinckrodt Fisher Baker Fisher Parr How Received Standard 4000 ppm fonnazin solution Standard solution or neat KC1 Neat KHP Calibration buffer solutions Neat material Neat material Neat tablets Source Storage Refrigerator Room temp Room temp Room temp Room temp Room temp Room temp Preparation From Source Working stds prapped from stock. Used as is or prepare from neat. Stock std from solid Working std from stock . Used as is. Stock std from source. Intermediate std from stock. Working std from intermediate. Std from source. Used as is. Lab Stock Storage Used immediately Room temperature Refrigerator Refrigerator —— - Refrigerator Refrigerator Used immediately Room temp —— Prep Frequency As needed to check Gelex stds As needed Monthly As needed —— Monthly Monthly or as needed As needed Monthly —— TUT 006 O044 »xt O 70 to (D p) (D (t> (N rt <J O (t (B p- rt •• W H- -•J (-.. o o °3 ° O 3 "> VD VO t-l ""-x O ro H '——,-i TABLE 9.3 STANDARD SOURCE AND PREPARATION FOR LABORATORY INSTRUMENTATION Instrument Group Gas Chromatographs and GC/MS (Volatiles) Gas Chromatographs and GC/MS (Seraivolatiles) High Performance Liquid Chromatographs Standard Source Supalco, Ultra. Accustandard, ChemSarvica, Baxter, Aldrich Restek, ChemSarvice, Crescent Chemical, Aldrich, Ultra ChemService, Crescent Chemical, Supelco Bow Received Neat Solutions (50-2000 ppm) Neat Solutions (50-10000 ppm) Neat Solutions > 1000 ppm Source Storage Freezer Refrigerator Refrigerator Preparation From Source Stock stds from neat sources. Intermediate stds from stocks. Working standards from intermediates and/or purchased solutions . Stock stds from neat sources. Intermediate stds from stocks. Working standards from intermediates. Stock stds from neat sources. Intermediate stds from stocks and/or purchased solutions. Working standards from intermediates. Lab Stock Storage Freezer Freezer Freezer Refrigerator or freezer Refrigerator or freezer Refrigerator or freezer Refrigerator Refrigerator Refrigerator Prep Frequency Annually or as noted by manufacturer expiration date. Semi annually — (2 months or sooner for gases, styrene, 2- chloroethylvinyl ether) Weekly Semi-annually or annually as required Semi-annually or annually as requied Semiannually or as needed Semi-annually Monthly Weekly TABLE 9.4 STANDARDIZATION OF TITRATING SOLUTIONS Analysis Acidity Alkalinity COD Chloride Sulfida TOC (Soil) Solution Requiring Standardization Sodium Hydroxide (0.02 N) Sulfuric acid Ferrous ammonium sulfate Silver nitrate Sulfide working standard Ferrous sulfate Standard Identity KHP Na,CO, K,Cr,0, NaCl I./Na.S.O, 1,/Na.S.O, Standard Source Malllnockrodt Mallinckrodt Mallinckrodt Baker VWR/Baker VWR/Baker Frequency of Standardization With each batch With each batch With each batch With each batch (or purchased certified) Weekly With each batch If" o- t) O ya in PI (>) (0 01 W rt <J o oi rt> H- rt •• w H- O 3 vo\ O vo N) Section 9 Revision 0 Date: 09/92 9.4.1 Metals ICP The inductively coupled plasma atomic emission spectrophotometer is standardized daily with single concentration standard solution containing metals of interest and a blank. After calibration, ICV standards are analyzed and must agree within ± 10% of true value. A blank is then run and must be below the PQL. A 2-5XIDL solution is then analyzed. This is followed by interference check standards A and AB which must be within ± 20% of true values. CCV standards are run after every 10 samples and sample data must be bracketed by calibration verification standards that are ± 10% of true values in order for data to be acceptable. Duplicate lab control standards are digested and analyzed with each batch of sample to determine accuracy and precision, and must be recovered 80-120% for liquid samples and 70-130% for soil samples. AA Furnace atomic absorption spectrophotometers are calibrated daily with a minimum of three standards and a blank. An initial calibration verification standard is analyzed immediately upon calibration, and must meet accuracy criteria of 90-110%. The initial calibration blank is analyzed, and must be less than the PQL. Lab control standards (digested standards) are analyzed in duplicate for every batch of 20 samples and must be recovered within 80-120% for liquids and 70-130% for soils for the batch to be acceptable. Calibration verification standards are analyzed after every 10 samples and must be recovered within 80-120% for bracketed data to be acceptable. 9.4.2 General Chemistry Autoanalyzer A calibration curve containing a minimum of five points is analyzed at least daily. The correlation coefficient from application of linear regression to these points must be > 0.995. Independent calibration verification standards and blanks are analyzed immediately following the calibration standards and thereafter, after every 10 samples. The initial calibration verification must be within accuracy control criteria given in Table 5.1 or 5.2 for any data to be acceptable. All data must be bracketed by calibration verification standards that meet all criteria given in Table 5.1 or 5.2 for that data to be acceptable. Ion Chromatograph For initial validation of the method and to determine linearity of the calibration curve, three to five standards are analyzed. Either linear regression or quadratic curve fitting is used, depending on analyte. The linear regression correlation coefficient must be > 0.990 for any analyte to be considered as giving a linear response. After initial validation, for linear analytes, the instrument is standardized daily with a single point standard. Calibration verification standards are analyzed immediately upon calibration and thereafter, after every 10 samples. The TUT 006 OO47 Section 9 Revision 0 Date: 09/92 calibration verification standards must be within control criteria given in Tables 5.1 or 5.2 to be acceptable. UV-VIS Spectrophotometer The spectrophotometer is calibrated at least daily with a minimum of five standards. Linear regression is used to find the calibration curve. The correlation coefficient must be > 0.995 in order for the curve to be acceptable. Calibration verification standards are analyzed immediately following the calibration standards and after every 10 samples. The calibration verification standards must meet control criteria given in Tables 5.1 or 5.2 in order for bracketed data to be acceptable. IR Spectrophotometer The infrared spectrophotometer is calibrated daily with a minimum of five standards. The curve is found by linear regression, and the correlation coefficient must be > 0.995. A calibration verification standard is analyzed immediately upon calibration, and after every 10 samples. Calibration verification standards must meet control criteria given in Tables 5.1 or 5.2 in order for bracketed data to be acceptable. Turbidimeter Gelex solid standards are calibrated against formazin standards initially and then quarterly. Then, the instrument is calibrated daily with one Gelex standard for each range of interest. A mid- range calibration verification is analyzed for every 10 samples and must meet control criteria specified in Table 5.1. Conductivity Meter The cell constant of each meter is determined at a minimum annually by the analysis of five KC1 standards. To verify the cell constant, a verification standard is analyzed at the beginning of each working day, using a KC1 standard in the expected range of the samples. For meters not having automatic temperature compensation, all samples are analyzed at 25* C ± 2' C. pH Meter The pH meter is calibrated daily with two standard buffers at pH 7.0 and either 4.0 or 10.0, and checked with a third buffer at 10.0 or 4.0 which must indicate ± 0.10 pH units of its given value. A calibration verification standard is analyzed immediately upon calibration and after every 10 samples. The calibration verification standard must meet criteria given in Table 5 . 1 in order for bracketed data to be acceptable. Manual or automatic temperature compensation is performed, depending on the meter. TOG A single point standard is used to calibrate the instrument daily. A calibration verification standard is analyzed immediately upon calibration Section 9 Revision 0 Date: 09/92 and after 10 samples. The calibration verification standards must meet control criteria given in Table 5.1 in order to accept bracketed data. ISE Ion selective electrodes are calibrated with a minimum of five standards. Linear regression applied to a plot of the log of the standard concentrations versus potential must result in a correlation coefficient > 0.995. Calibration verification standards are analyzed immediately upon calibration and after every 10 samples, and must meet control criteria given in Tables 5.1 or 5.2 in order for bracketed data to be acceptable. TOX Although the TOX instrument provides an "absolute" measurement, and is not subject to calibration, a check standard is analyzed daily immediately after the blank, and must meet control criteria given in Tables 5.1 or 5.2 in order for data to be acceptable. Bomb Calorimeter The energy equivalent of the bomb calorimeter is determined quarterly by bombing six standard benzoic acid tablets. A fuel oil standard is analyzed in duplicate for every batch of samples, and must meet control criteria given in Table 5.2 in order for data to be acceptable. DO Meter DO meters are calibrated prior to use either by Winkler titration or the air calibration technique, and annually by Winkler titration. Temperature All laboratory and field thermometers are calibrated annually by comparison with a NIST-certified thermometer. Field meters with automated temperature compensation are checked before use with a calibrated thermometer. 9.4.3 Gas Chromatographs Volatiles Initial calibration is performed upon instrument startup and whenever continuing calibration fails the acceptance criteria. A five-point standard curve is prepared using all target compounds. The low standard concentration is near the PQL, and the high standard defines the usable linear range of the detector. After the five standards are purged and analyzed, a calibration curve is generated using internal standard methodology. If the internal standard exhibits matrix interference in sample, external standard methodology may be used; however, an internal standard is preferred for purge-and-trap methods. Ideally, all volatile compounds should exhibit enough linearity to use a straight line fit forced through the origin. However, some compounds may exhibit true non- linearity but consistent performance using a quadratic fit. A quadratic TUT OO6 0049 Section 9 Revision 0 Date: 09/92 fit curve may be used. The analyst should visually inspect the curves before proceeding with sample analysis. An alternative to quantitation from a calibration curve is quantitation from an average response factor (RF). This is an acceptable technique for all SW-846 8000-series methods, all 40 CFR 136 600-series methods, and all 500-series drinking water methods. For the 8000-series methods, if the I RSD is < 20%, the average RF may be used. For the 500- and 600-series methods, if the X RSD is < 10X, the average RF may be used. Quantitation from the curve is preferred. Continuing calibration check (CCC) standards are analyzed at the intervals specified in the methods. The CCC standard concentration is normally the mid-point of the five-point calibration curve, and must be at the level specified in the method "Q-tables" for the 600- and 8000-series methods. The 500- and 600-series methods specify a mid-level CCC at the beginning of each working day. The 8000-series methods specify a mid-level standard at the beginning of each working day and after every ten samples thereafter if needed for further sample analyses. The acceptance criteria for the 600- and 8000-series methods for volatiles are listed in each method's "Q-table." The analyzed value of each standard component must fall within the range of values given in the table. For compounds not present on the Q-table, the analyzed value must fall within 15X of the true value, or the laboratory may generate internal acceptance ranges based on a minimum of thirty data points. The acceptance limits for the 500-series methods are ± 20X of the true value. If the CCC standard fails acceptance criteria, another CCC standard may be analyzed. If the second standard also fails, the initial calibration must be repeated. 2-Chloroethyl vinyl ether exhibits erratic chromatographic behavior. The Supelco, Inc. Purgeable A Mixture footnotes 2-chloroethyl vinyl ether with the following: "Due to instability of 2-chloroethyl vinyl ether, we cannot guarantee the concentration of this component." These problems with 2-chloroethyl vinyl ether impact the ability of SL to consistently analyze for this compound within the method requirements or PQL. If the requirements or PQL cannot be met for 2-chloroethyl vinyl ether, the appropriate flag should accompany the data for this compound in the report. Semivolatiles/Pesticides/Herbicides Initial calibration is performed upon instrument startup and whenever a CCC standard fails the acceptance criteria. A five-point standard curve is prepared using all target compounds. The low standard concentration is near but above the MDL and the high standard defines the usable linear range of the detector. 00 &0 TUT 00* - Section 9 Revision 0 Date: 09/92 After the five standards are injected, the computer software generates a calibration curve using either internal standard or external standard methodology. The analyst chooses the best fit type for each compound, either linear or quadratic. The analyst should inspect the curves before proceeding with sample analysis. An alternative to quantitation from a calibration curve is quantitation from an average response factor as long as the minimum 2RSD criterion is met. The 2RSD criteria are as follows: 1. < 102 for 600-series methods. 2. < 202 for 8000-series methods. 3. < 202 for 500-series methods, except Method 504 must be < 202. CCC standards are analyzed at the intervals specified in the methods. The 8000-series methods specify a CCC standard at the beginning of each working day and after every 10 samples thereafter if needed for further sample analyses. The 600-series methods specify a CCC standard at the beginning of each working day. The 8000- and 600-series methods CCC standard acceptance criteria are ± 15X difference from the true value. The 500-series methods specify a CCC standard at the beginning of each work day. An additional CCC standard, different in concentration from the initial standard, must be run at the end of the work day when using the external standard calibration technique for methods 507, 508, and 515.1. The acceptance criteria for these CCC standards is ± 20X difference from the true value. The 500-series methods allow a single point calibration as an alternative as long as the response produced by an unknown in the sample extract is ± 202 of the standard response. If the CCC standard fails acceptance criteria, another CCC standard may be analyzed. If the second standard also fails, the initial calibration must be repeated. The above calibration procedures meet or exceed EPA method requirements. The CLP protocol differs from the other EPA methodologies. Calibration curves with a minimum of three points are kept on record at the lab. The CLP statements of work for 2/88 and 3/90 (OLM01.6) are followed as written. 9.4.4 GC/Mass Spectrometer Hardware tuning is performed on each GC/MS prior to calibration as specified in the applicable EPA methods. Ion abundance acceptance criteria for semivolatile GC/MS tuning with DFTPP and volatile tuning with BFB are given below. Mass calibration is performed as an integral part of tuning. Tuning is performed at the beginning of each 12-hour clock for each GC/MS in accordance with EPA methods. TUT 006 0051 Section 9 Revision 0 Date: 09/92 SEMIVOLATILE ORGANIC GC/MS TUNING AND (DFTPP) m/e 51 68 70 127 197 198 199 275 365 441 442 443 Ion Abundance MASS CALIBRATION Criteria 30-60* of mass 198 < 22 of mass 69 < 2% of mass 69 40-602 of mass 198 < IX of mass 198 Base peak, 1002 relative abundance 5-92 of mass 198 10-302 of mass 198 > 12 of mass 198 Present but less than mass 443 > 402 of mass 198 17-232 of mass 442 VOLATILE ORGANIC GC/MS TUNING AND MASS CALIBRATION BROMOFLUOROBENZENE (BFB) m/e 50 75 95 96 173 174 175 176 177 Ion Abundance Criteria 15.0 - 40.02 of mass 95 30.0 - 60.02 of mass 95 Base peak, 1002 relative abundance 5.0 - 9.02 of mass 95 Less than 2.02 of mass 174 Greater than 50.02 of mass 95 5.0 - 9.02 of mass 174 Greater than 95.0 2, but less than 101.02 of mass 174 5.0 - 9.02 of mass 176 Initial calibration is performed at instrument startup and whenever a CCC standard fails acceptance criteria. A five-point standard curve is prepared containing all target compounds. Concentrations are those defined by CLP, which are also appropriate for other EPA methodology. Response factors are generated for each compound. The acceptance criteria used to assess the calibration are those specified in SW-846 for the 600- and 8000-series methods and in the various CLP SOWs for CLP analyses. These are as follows: rtr OO6 OO5>2 Section 9 Revision 0 Date: 09/92 Semivolatiles 625 and 8270 Semivolatile CLP 2/88 SOW 625. 8270. CLP 2/88 SOW CLP 3/90 SOW 525 Initial Calibration < 30Z RSD for CCCs < 30Z RSD for CCCs Z 0.050 SPCCs Continuing Calibration Check < 30Z difference for CCCs < 25Z difference for CCCs i 0.050 for SPCCs As specified in 6/91 Revision of Method (OLM01.6) £ 301 RSD or alternatively generate linear, 2nd order, or 3rd order calibration curve S 30Z difference or alternatively (using analyst discretion), all analytes fall on the curve from the initial calibration Volatiles 624 62*0 + CLP 2/88 SOW 624, 8240, CLP 2/88 SOW CLP 3/90 SOW 524.2 Initial Calibration < 30Z RSD for CCCs < 30Z RSD for CCCs 2 0.300 for SPCCs (except Bromoform i 0.250) Continuing Calibration Check 20 ug/L standard meets limits specified in Q Table S 25Z difference for CCCs Z 0.300 for SPCCs (except Bromoform Z 0.250) As specified in 6/91 Revision of Method (OLM01.6) < 20Z RSD or alternatively generate linear, 2nd or 3rd order curve ± 30Z difference or alternatively) using analyst discretion), all analytes must fall on the curve from the initial calibration CCC standards are analyzed at the intervals specified in the methods. These intervals are as follows: 1. 500-series -- every 8 hours 2. 600-series -- every working day 3. CLP & 8000-series -- every 12 hours. If the CCC standard fails acceptance criteria, another CCC standard may be analyzed. If the second standard also fails, the initial calibration must be repeated. Sample quantitation is based on the average RF or curve (when RTE data systems are not available) from the initial calibration for 500-, 600-, and 8000-series methods and the single point RF from the continuing calibration standard for CLP. Hexachlorophene exhibits very poor chromatographic behavior within the limits of the working calibration range. If this compound is not detected, ND (not detected) will be reported rather than a detection limit. 2-Chloroethyl vinyl ether exhibits erratic chromatographic behavior. The Supelco, Inc. Purgeable A Mixture footnotes 2-chloroethyl vinyl ether with the following: "Due to instability of 2-chloroethyl vinyl ether, we cannot guarantee the concentration of this component." These problems with 2-chloroethyl vinyl ether impact the ability of SL to consistently TUT OO6 OO5" Section 9 Revision 0 Date: 09/92 analyze for this compound within the method requirements or PQL. If the requirements or PQL cannot be met for 2-chloroethyl vinyl ether, the appropriate flag should accompany the data for this compound in the report. 9.4.5 High Performance Liquid Chromatographs Initial calibration is performed at instrument startup, following instrument maintenance or change in conditions, and whenever CCC fails acceptance criteria. A three-point curve is prepared for 500- and 600-series methods. Five points are used for 8000-series methods. The low standard is near the PQL and the high standard defines the usable linear range of the detector. After the three- or five-point standards are analyzed, response factors are generated by the data systems or manually. Due to limited data system capabilities, RSD criteria of 10Z for the 600-series methods and 20X for the 500- and 8000-series methods are applied. If the maximum RSD criteria are met, the average RF is used for quantitation. A CCC using a mid-level standard is performed at the beginning of each working day and after every ten samples. Acceptance criteria are less than or equal to 10% difference from the average RF for the 600-series methods, < 20X D for the 500-series methods, and < 15Z D for the 8000- series methods. If the CCC standard fails acceptance criteria, another CCC standard may be analyzed. If the second standard also fails, the initial calibration must be repeated. 9.5 Field Instrument Calibration Calibration of field instrumentation (conductivity meters, pH meters, DO meters, and turbidimeters) is performed in the field prior to use, in accordance with the DER Calibration and Use of Field Meter SOP, revised Oct. 18, 1991. All calibration data are documented in a bound field notebook. 9.6 Calibration Documentation All calibration records including raw data, response factors, standard concentrations, curves, reduced data, and instrument settings or conditions are stored and archived according to laboratory standard operating procedures. Current chromatograms, curves, and results transcribed onto forms are kept at the analysts' workstations and periodically archived into a data storage area. Initial and continuing calibrations are stored by date for ease of location. All standard ID numbers appear on graphs, plots, chromatograms, or curves for traceability purposes. TUT O0<b Section 10 Revision 0 Date: 9/92 10.0 PREVENTIVE MAINTENANCE 10.1 Maintenance Schedule All Savannah Laboratories facilities are equipped with up-to-date computerized instrumentation. In order to gain maximum performance and minimize downtime, regular inspection, maintenance, cleaning, and servicing of all laboratory and field equipment is performed according to the manufacturers' recommendations. A maintenance log is kept for each piece of laboratory and field instrumentation, detailing any malfunction and the steps taken to correct the problem. Routine repairs and maintenance are performed and documented by the analyst responsible for the particular instrument. Non-routine maintenance is signed and dated by the analyst or repair technician. Routine maintenance procedures for laboratory instrumentation are given in Table 10.1. The frequencies of routine maintenance procedures for Savannah Laboratories' field instrumentation are given in Table 10.2. Maintenance contracts are carried for most instrumentation, and close contact is maintained with service personnel to provide optimum instrument functioning. An extensive spare parts inventory is maintained for routine repairs at the facilities, consisting of GC detectors, AA lamps, fuses, printer heads, flow cells, tubing, certain circuit boards and other common instrumentation components. Since instrumentation is standardized throughout the laboratory network, spare parts and components can be exchanged among the labs. Equipment such as refrigerators, ovens, and incubators are not calibrated per se, but are periodically checked with calibrated thermometers. Refrigerators and incubators are checked twice daily and the temperatures documented in a notebook. Sample storage refrigerators must be 4 ± 2° C. All thermometers are calibrated annually against an NIST-certified thermometer. Electronic analytical balances are calibrated daily with internal mechanisms if available. Calibration checks are performed and documented on all balances at least weekly with Class S weights and must meet the criteria given in Table 10.3. 10.2 Contingency Plan In general, each facility has at least one backup unit for each critical unit. In the event of instrument failure, portions of the sample load may be diverted to duplicate instrumentation within each facility, the analytical technique switched to an alternate approved technique (such as manual colorimetric determination as opposed to automated colorimetric determination), or samples shipped to another properly certified or approved Savannah Laboratories location (where identical SOPs, QA procedures and instrument are utilized). When shipping samples to another facility, interdivisional chain-of-custody procedures are followed as given in Section 7. TUT OO6 OO55 Section 10 Revision 0 Date: 9/92 TABLE 10.1 LABORATORY EQUIPMENT PREVENTIVE MAINTENANCE SCHEDULE EQUIPMENT ITEM Service Interval D w M Q A SERVICE LEVEL ICAP Profile Nebulizer Filters Spray Chamber Quartz Torch D- Shaped Mirrors aflTH-HZEFTJE FURNACE AA SPECTRC Sapphire Window Flow Rate Graphite Tube Quartz Windows Contact Rings and Plates Filters X X X H*jIl>ltItK X X X X it£HA>i FUKHACE AA SPLLlKUFbOTtm.TKR Check sampler syringe for air Graphite Tubes Graphite Electrodes Quartz Windows X X X X X X X X Profile on a daily basis. Inspect and clean. Replace tubing daily. Check flow rate. Inspect and clean. Inspect and clean. Clean and realign. Inspect mirror surface and replace if necessary. Remove and clean with N-Propanol. Place 10 mL DI water in a 10-raL cylinder. Push Neb . Air button and run one minute . Flow should be 2.0 to 2.5 mL. Replace if necessary and condition before use. Clean window with lint-free cloth and distilled water. Replace contact rings if they are worn. Remove filter from instrument, clean with water and mild soap. X Flush syringe if necessary. Replace if necessary and condition before use. Replace contact rings if they are worn. Remove and clean with lint-free cloth and DI water and/or alcohol. COHTIHUUM FURNACE AA SFECTROPBOTCHETER Quartz Windows Graphite Tubes Contact Rings and Plates Filters D2 Arc Lamp TDRBIDIMETER CONDUCTANCE METER X X X X X X X Remove and clean with lint-free cloth and DI water. Replace if necessary and condition before use. Replace contact rings if they are worn. Remove filter from instrument, clean with water and mild soap. Check lamp. Adjust or replace as necessary. Focus optics. Inspect and replatinize cell as necessary. Section 10 Revision 0 Date: 9/92 TABLE 10.1 LABORATORY EQUIPMENT PREVENTIVE MAINTENANCE SCHEDULE EQUIPMENT ITEM pfl METER DRYING OVEN ANALYTICAL BALANCE TOP LOADER BALANCE Service Interval D X X ION CHROMATOGHAPH AS3 Column AS3 Guard Column Pump Pistons V X X M Q X X A X SERVICE LEVEL Inspect probe membrane, filling solution level . Verify correct temperature with calibrated thermometer . Check calibration with class S standard metric weights. Annual inspection. Check calibration with class S standard metric weights. Annual inspection. Inspect quarterly or as required. Inspect quarterly or as required. Inspect annually. ADTOANALYZEH Pump Platen Pump Tubes Flow Cell BLOCK DIGESTCR UV/VIS SFECTKOPBOTCHElEk IS SEECIJtoniuiuitTiK ION SELECTIVE ELECTRODE BOMB CALORIMETER DISSOLVED OXYGEN METER BOD INCUBATOR BACTERIOLOGICAL INCUBATOR AUTOCLAVE HATERBAIH TCLF EQUIPMENT X X X X X X X X X X X X X X Inspect weekly and replace as required. Inspect and replace as needed. Inspect and clean. Check calibration against thermometer. Semiannual check for wavelength verification. Inspect and clean exposed optics weekly, if necessary. Inspect and polish electrode. Inspect seals, replace if necessary. Check probe membrane for deterioration. Replace as necessary. Temperature checked twice daily. Temperature checked twice daily. Seals inspected and replaced as necessary. Temperature checked twice daily. Check rotation rate quarterly. GAS CHROMATOGHAPH - SEMTTOLATILES Autos ampler System Septa GC Columns (Packed) GC Capillary Columns X X X X Check daily for correct operation. Syringe and tubing solvent cleaned daily. Needles and tubing replaced as needed. Replace autosampler septa daily and injector as needed. Change glass wool plugs at front of column. Inspect daily. Change glass sleeve insert as needed and cut front of column if necessary. TUT 006 0057 Section 10 Revision 0 Date: 9/92 TABLE 10.1 LABORATORY EQUIPMENT PREVENTIVE MAINTENANCE SCHEDULE EQUIPMENT ITEM ECD FID Carrier Gases Oxygen Trap Service Interval D GAS CHHCMA10GHAPH - TOC Column Septum Gas Tank Oxygen/Moisture Trap Parti culate Trap Hall Detector FID PID X X X X X X w X M Q X A X X SERVICE LEVEL Semi annually cleaned and leak tested by service technician. In-house cleaning as needed. Tanks are changed when pressure reads 500 to ensure purity. Inspect and replace as necessary. X X Checked daily. Repack glass wool and replace column as needed. Checked daily. Replace as necessary. Levels checked daily. Replace when pressure < 500 psi. Inspect and replace as necessary. Checked and replaced if problem in GC flow rate. Checked daily for proper operation and response. Checked daily for proper operation and response. Checked daily for proper operation and response. GC/MS Column Septum Injection Port Liner Splitless Disc Autosampler Rough Pump Turbo Pump Mass Spectrometer Tape Head Tape Drive X X X X X X X X X X Front portion of column checked/maintained daily for contamination; replace every 1 month or as needed. Changed daily. Changed daily. Changed daily. Checked daily for proper function. Oil changed to ensure proper operation. Turbo molecular pump oiled as needed by instrument service representative. Cleaning of source every 1 month or as needed. Cleaned after each tape. Cleaned annually. PUHGE AHD TRAP Sorbent Trap Purge Flow Gas Tank X X X Checked daily. Replace and condition as necessary. Checked daily, adjust as needed. Check daily. FLIT OO6 O05S Section 10 Revision 0 Date: 9/92 TABLE 10.1 LABORATORY EQUIPMENT PREVENTIVE MAINTENANCE SCHEDULE EQUIPMENT ITEM Service Interval D w M TOC ARALYZER Pump Tubes Flow rate Detector Windows X X Q A SERVICE LEVEL X Inspect and replace if necessary. Check and adjust if necessary. Check and clean if necessary. TDK ANALYZER Pyrolysis Tube Electrodes Electrolyte X X X HFLC SYSTEMS Pumps Pumps Columns Detector fittings Detector optics Detector optics Autosampler Gases for sparging and autosampler operation X X X X X X X X Inspect and clean or replace if necessary. Inspect and clean if necessary. Replace as necessary. Filter all solvents, water, and extracts if pressure buildup occurs. Visual leak check. Prime pumps at startup. Inspect seals, replace as needed. Check for pressure buildup; store with ends capped in appropriate mobile phase. Visual leak check. Visual leak check. Inspect removable filters for dust, fingerprints. Clean as needed. Replace lamps as needed. Checked daily for proper operation. Clean, lubricate moving parts as needed. Change tanks when pressure reads 500 psi. TZNNELEC LB5100 Sample changer Detector Detector gas Flow meter X X X X Inspect moving parts, lubricate as needed. Checked daily for proper operation and response. Serviced by manufacturer only. Change tank when pressure reads 500 psi . Allow new tanks to dissipate radon for two weeks before use. Checked daily for proper operation. "UT OO6 CO59 Section 10 Revision 0 Date: 9/92 TABLE 10.2 FIELD EQUIPMENT PREVENTIVE MAINTENANCE SCHEDULE EQUIPMENT ITEM TURBIDIMETER BACH 16800/DRI- 13C COKDOCIAHCE METER YSI 33 FISHER AHD ORION pH METERS TSI MODEL SOB/SIB DISSOLVED OXYGEH METER CQRHIHG CHECKMATE 90 pH/SC/DO/T* METER FISHER/SLOPE HATER LEVEL METERS Service Interval D X X X X X W M Q X A SERVICE LEVEL Inspect and replace cell as needed. Inspect and replatinize cell as necessary. Inspect probe membrane, filling solution level. Check probe membrane for deterioration. Replace as necessary. Check probe, call, membrane. Check probe cord for integrity/cleanliness, meter for response. TUT OO6 OO60 Section 10 Revision 0 Date: 9/92 TABLE 10.3 BALANCE CALIBRATION CHECKS Analytical Balance Class S Weight 0.01 g 0.1 g 0.5 g 1 g 10 g 50 g Tolerance ± 0.0002 g ± 0.0002 g ± 0.0004 g ± 0.0004 g ± 0.0005 g ± 0.0010 g Top-Loading Balance Class S Weight 0.1 g 0.5 g 1 g 5 g 10 g 50 g Tolerance ± 0.02 g ± 0.02 g ± 0.04 g ± 0.04 g ± 0.05 g ± 0.10 g TUT GO 6 OO6J. Section 11 Revision 0 Date: 9/92 11.0 QUALITY CONTROL CHECKS AND ROUTINES TO ASSESS PRECISION AND ACCURACY AND CALCULATIONS OF METHOD DETECTION LIMITS The key to a successful QA/QC program is strict adherence to the program during all phases of the project, including: presampling discussions; sample collection, preservation, storage and analyses; and validation and reporting of results. Field and laboratory quality control checks are part of each sampling trip and laboratory analysis and meet or exceed all FL DER requirements. Without the proper quality control procedures, analyst and method performance cannot be measured. 11.1 Field QC Checks Savannah Laboratories recommends to their clients that proper control procedures meet or exceed FL DER field QC requirements. If particular field method QC requirements are more stringent than the general procedures given below, the method QC requirements are followed. Blanks which are collected in the field are an important link in the quality control data chain for a set of samples. The analytical data derived from these blanks are necessary to assess field sampling operations. These blanks are used to verify that sample containers, preserving reagents and equipment are contaminant-free. Blanks are also used as a check for potential on-site environmental contamination, to evaluate personnel expertise in sample collection and to reveal problems that may occur in sample storage and transport. The field quality control blanks should not be isolated from actual samples. They must be considered as samples and treated identically (preserved with the same reagents, stored and transported in the same containers as the samples, etc.). The types and frequency of blanks must be included in all Quality Assurance Plans. In cases where Data Quality Objectives dictate more stringent controls, additional field quality control blanks may be required. The following protocol outlines the minimum field blank requirements necessary to assure the validity and integrity of any sampling episode. If the client requires or submits field QC check samples, these will be analyzed for the same parameters as the accompanying samples (or per client's instructions) and invoiced as samples. Since field QC check samples are usually liquids, they are prepared and analyzed by liquid procedures and reported as liquids. Unless requested by clients or required by a project specific QA plan, lab QC deliverables are not provided for field QC check samples. 11.1.1 Trip Blanks PURPOSE: The trip blank is to be used when sampling for volatile organics and other sensitive parameters. The purpose is to determine if contamination has occurred as a result of improper sample container O06 Section 11 Revision 0 Date: 9/92 cleaning, contaminated blank source water, sample contamination during storage and transportation due to exposure to volatile organics (e.g., gasoline fumes) and other environmental conditions during the sampling event. PREPARATION: Trip blanks are prepared prior to the sampling event either by the laboratory providing sample containers, or by field team personnel who are responsible for the initial preparation of sample containers and field equipment. The water must be free of volatile organic contaminants. Any appropriate preservatives must be added at the time that the blanks are prepared. The sample containers are sealed, labeled appropriately, and transported to the field in the same sampling kits as the sample vials. These blanks are not to be opened in the field. They are to be transferred to the sample container designated for volatile sample storage and transport and accompany the samples to the laboratory. Subsequent blanks (field and equipment) for volatile organics should use the same source water as the trip blanks, unless the water used for field and equipment blanks can be proven equivalent. FREQUENCY: One trip blank for each volatile organic analysis (601, 602, 624, etc.) shall be provided per cooler used for storing and transporting volatile sample vials. If a laboratory requires submission of multiple vials for a method, the same number of vials must be submitted for the trip blank. 11.1.2 Field Blanks PURPOSE: Field blanks are used to evaluate the effects of on-site environmental contaminants, the purity of reagents used as preservatives or additives and the general sample container filling/collection techniques. Field blanks are recommended for all parameters. PREPARATION: Field blanks are prepared on-site by filling the sample container(s) with analyte-free water, adding preservatives, sealing the containers and completing the appropriate documentation. The field blanks must be handled in the same manner as the sample group for which it was intended (i.e., blanks must be stored and transported with the sample group). NOTE: The water for VOA field blanks should be equivalent to the trip blank water (see Trip Blank Preparation). FREQUENCY: One field blank per parameter group per day or at a frequency of 5X of the samples in the parameter group per day, whichever is greater. 11.1.3 Equipment Blanks PURPOSE: Equipment blanks are required if sampling equipment is precleaned or field-cleaned. These blanks are used to determine the effectiveness of field cleaning procedures as well as to reveal those sources of contamination that may be found in a trip blank. Equipment ;UT OO6 OO6": Section 11 Revision 0 Date: 9/92 blanks are recommended for all parameter groups and matrices to be collected and analyzed. PROCEDURE: The final rinse water (analyte-free) shall be rinsed on or through the sampling equipment, whether precleaned or field cleaned, collected, and placed in appropriate preserved containers. These blanks must be stored and transported with the samples. NOTE: The water used for volatile equipment blanks should be from the same or equivalent source as the trip blank water. FREQUENCY: When less than five samples of a similar matrix are taken, one equipment blank prepared on-site for precleaned or field-cleaned equipment must be collected and analyzed for each parameter. When five to ten samples of a similar matrix are taken, one equipment blank must be collected on field-cleaned equipment or one on-site blank must be collected in precleaned equipment if no equipment is cleaned in the field. For sampling events involving ten or more samples, a minimum of one blank must be taken on precleaned equipment or at the rate of 5% (whichever is greater) of the samples in each analyte group for all matrices. One blank must be taken on field-cleaned equipment or at the rate of 5% (whichever is greater) of the samples in each analyte group for all matrices. 11.1.4 Field Duplicates Field duplicates are taken, analyzed, reported and invoiced when requested by the client or specified by a project specific QA plan. Savannah Laboratories recommends that a minimum of one duplicate or 10% of samples be taken for all parameter groups and matrices to be collected and analyzed. 11.1.5 Field QC Summary The frequency of field blanks and duplicates is summarized below: No. Samples 10+ 5-9 < 5 Precleaned Equipment Blanks Minimum of one then 5X One* One* Field-cleaned Equipment Blanks Minimum of one , then 5% One* One* Trip Blank (VOCs) One per cooler Not required Not required Duplicates Minimum of one then 10Z One Not required * Note: For nine or fewer samples, one equipment blank is required from either precleaned or field-cleaned equipment. TUT GO 6 GG64 Section 11 Revision 0 Date: 9/92 If any equipment is cleaned in the field, the blank is to be taken from the field-cleaned equipment. 11.2 Laboratory QC Checks The laboratories employ control samples to assess the validity of the analytical results. Determination of the validity of sample results is based on the acceptance criteria being met by the control sample. The acceptance criteria for each type of control sample are defined in the appropriate SOP. These acceptance criteria are determined from historical data, and meet the EPA CLP acceptance criteria as a minimum. The control samples are analyzed in the same manner as the field samples. QC check samples are analyzed on an analytical batch frequency unless otherwise stated. An analytical batch is defined as a group of samples which are processed as a unit. If the number of samples in the group is greater than 20, each group of 20 samples or less is handled as a separate batch. Other QC check samples are analyzed for performance evaluations or as part of internal or external audits as given in Section 14. Blind QC check samples are analyzed at a minimum in duplicate and at least semiannually. Results of any unacceptable QC check sample results obtained during DER- reportable project analysis are submitted to DER QAS in the project report as discussed in Section 15. If particular laboratory method QC requirements are more stringent than the general procedures given below, the method QC requirements are followed. 11.2.1 Organics Method Blanks: A method blank will be run for each batch of samples. A blank is a clean sample (containing no reportable analyte). Lab Control Standards: Blank spikes or lab control standards will be run with each batch of samples processed. Surrogates: Appropriate surrogates (see Tables 5.1 and 5.2) will be added to all samples, standards and blanks. Matrix Spikes: Matrix spikes will be run with each batch at a frequency of 5% of samples. The CLP matrix spiking compounds will be used for all GC/MS semivolatile, volatile and chlorinated pesticides/PCB analyses (by GC) . Appropriate matrix spikes will be used for other chromatographic methods. Matrix Spike Duplicates/Sample Duplicates: Duplicate samples or matrix spikes will be run with each batch or at a frequency of 5X of samples. In cases where duplicate matrix spikes are used, precision data are obtained on only the matrix spiking compounds. I'UT OO6 O065 Section 11 Revision 0 Date: 9/92 11.2.2 Inorganic and General Chemistry Calibration Blanks: Calibration blanks are nondigested blanks which are run at a frequency of 10X of samples. Method Blanks: Method blanks should be run with each batch at a frequency of 5Z of samples of the same matrix. Lab Control Standards: Blank spikes or lab control standards will be run with each batch of samples processed. Matrix spikes: Matrix spikes will be run at a frequency of 5Z of samples. Duplicates: Duplicate samples or duplicate matrix spikes will be run at a frequency of 5Z of samples. In cases where batch QC is sufficient, the matrix spike/duplicate will be on a field replicate (if available) or a laboratory provided sample of the same matrix. In the case of nonliquid inorganics, the digestion blank or extraction blank will be spiked. Cost for analyses of batch QC matrix spikes/duplicates, laboratory blanks and blank spikes (lab control standards) are included in the individual costs for analysis. For CLP protocols or other cases where "sample specific" (non-batch) QC is required, matrix spike/duplicates will be conducted on replicate samples provided by the client. In this case, matrix spikes/duplicates analysis will be invoiced as samples. If the client does not provide sufficient sample replicates for matrix spikes/duplicates, laboratory generated samples will be provided. 11.2.3 Microbiology Quality control checks are routinely performed for all microbiological analyses. Strict requirements for the house deionized water must be met before it can be used in any testing. Each monitored parameter, its monitoring frequency, and its acceptance limits is as follows: residual chlorine, monthly, <0.1 mg/L; trace metals (total Cd, Cr, Cu, Ni, Pb, Zn) , annually, < 1.0 mg/L; conductivity, daily < 1.0 umho/cm; heterotrophic plate count, monthly, < 1000 CFU/mL; and suitability (inhibiting residue), annually or for each new lot of detergent, ratio between 0.8 and 3.0. Other laboratory QC practices are utilized to provide accurate microbiological results. These include the use of autoclave tape to insure proper sterilization of sample containers, media, etc. Incubators are maintained at 35 ± 0.5° C and water baths at 44.5 ± 0.2° C. Thermometers used for these monitoring purposes are calibrated annually against an NIST-certified thermometer. Other equipment, such as the dissecting microscope and colony counter are maintained in clean operating condition at all times. TUT 006 OO66 Section 11 Revision 0 Date: 9/92 Microbiological samples are analyzed in duplicate at a rate of 10X of positive samples. Positive controls are analyzed in association with ONPG-MUG analyses for total coliform monthly or upon receipt of a new lot of reagents. Blanks are routinely analyzed with microbiological samples. For membrane filter analyses, a sterile dilution water blank is run initially, after every 10 samples, and at the end of each analytical run. For MPN analysis, sterile dilution blank is added to a lauryl tryptose broth tube for a blank for each analytical run. 11.3 Routine Method Used to Assess Precision and Accuracy Control charts (Figures 11.1 and 11.2) for precision and accuracy are setup for each parameter immediately after the method is validated. Control charts are based on procedures in The Handbook for Analytical Quality Control in Water and Wastewater Laboratories (EPA, 1979) and contain both "Warning Limits" (+ 2 standard deviations) and "Control Limits" (+ 3 standard deviations). The initial limits used for a parameter are the values obtained from the method validation procedure (40 CFR Part 136). Control limits are updated annually for all parameters. A minimum of ten data points is used to update these limits. Formulas used for calculations of precision and accuracy are provided in Section 5.0. Accuracy and precision limits are established for a specified concentration range. Concentration is divided into three ranges: low, mid, and high. Low level is defined as concentrations from" the minimum detection limit to a level five times the MDL. Mid level is defined as the mean level between the minimum detection level and the upper and of the linear range. High level is defined as the concentration at the upper end of the linear range. Further information on these ranges is found in Section 9. The procedures used to determine the precision and accuracy targets in Section 5 are given in Table 11.1. 11.4 Method Detection Limits and Reporting Limits Method detection limits (MDLs) are determined annually in accordance with the procedures in SW-846 and Appendix B of 40 CFR Part 136. This procedure includes analyzing seven prepared spikes or standards in reagent water at levels 3-5 times the estimated detection limit. The standard deviation of the seven replicate measurements is calculated, and the MDL is computed by multiplying this standard deviation by 3.14 (the Student's t value appropriate for a 99Z confidence level with seven replicates). The method detection limit (MDL) calculated by the procedure described above is defined as the minimum concentration of a substance that can be measured in reagent water and reported with confidence that the analytical concentration is greater than zero. For other protocols (i.e. , Contract Laboratory), other procedures are used to estimate detection limits. TLIT 006 OO67 Section 11 Revision 0 Date: 9/92 Since MDLs are based on the analyses of standards in reagent water, they are not useful in reporting data for most environmental samples. Thus, practical quantitation limits (PQLs) are used for reporting a non-detected parameter. PQLs are defined as the lowest level that can be reliably achieved within specified limits of precision and accuracy during routine laboratory operating conditions. The new term from SW-846, Estimated Quantitation Limits (EQL) is used interchangeably with PQL. In all cases, PQLs are greater than MDLs. When PQLs are defined in SW-846 or the CLP protocols (CRDLs), these defined PQLs are generally used in data reporting provided they are achievable and within the range of 10 times the standard deviation used in determining the MDL and 10 times the MDL. TUT 006 0068 FIGURE 11.1 EXAMPLE OF CONTROL CHART FOR % RECOVERY Section 11 Revision 0 Date: 9/92 £| fcl D O O gi§ *>!! EC S la. Si O cc oc ... £££ O O S ij o j CO CM § %RECOVERY TUT 0069 Section 11 Revision 0 Date: 9/92 FIGURE 11.2 EXAMPLE OF CONTROL CHART FOR % RPD o OS o ^ 111 I in ^- %RPD TUT OOfc OO70 Section 11 Revision 0 Date: 9/92 TABLE 11.1 Methods used to Generate Accuracy and Precision Targets Method Quality Control Check Standards (QCCS) Quality Control Check Standards (QCCS) Duplicate Samples Matrix Spikes Matrix Spike Duplicates Purpose Accuracy Precision Precision Accuracy Precision Concentration Level Mid Level Mid Level Mid Level Mid Level Mid Level Method References All metal , general , and organic methods for which a QCCS is available . All metal, general, and organic methods for which a QCCS is available . All methods for which a QCCS is not available Methods for project- or agency-specific requirements . Methods for project- or agency-specific requirements . TUT OO6 OO71 Section 12 Revision 0 Date: 9/92 12.0 DATA REDUCTION, REVIEW, AND REPORTING 12.1 Introduction In order to provide the highest quality data possible, an extensive system for data reduction, review, and reporting has been implemented. 12.2 Sample Custody Upon receipt of the samples, the custody forms are checked against the sample identifications listed on the containers by the sample custodians, and a unique SL log number is assigned to each sample group. Any discrepancies are noted, including cooler temperatures, broken bottles and/or misidentified samples. The data manager or the project manager then notifies the client if discrepancies exist. After receipt, the samples are delivered to the appropriate laboratory sections where the samples are checked for proper preservation and this information is recorded in bound notebooks when applicable. When necessary, the samples are then stored in refrigerators that are monitored twice daily for-temperature. 12.3 Organization and Initiation of Sample Analyses The key to Savannah Laboratories' sample flow, analysis, data and QA review and archiving, and reporting system is the single LIMS network which controls the day to day production of the laboratories. This system, which is summarized in Figure 12.1, provides project managers, QA personnel, and all analysts immediate information on the status of any sample in all five facilities. This system schedules and prioritizes all work, provides a mechanism for sample tracking, review of reportables and QC data, generation of reports and invoices, and archiving of all reports and associated QC data. Upon receipt of custody forms, the project manager instructs data management personnel to log the sample analysis request and identification into the LIMS. The LIMS is based on an ADDS Mentor 7000 computer (NCR) which links the Tallahassee, Mobile, Deerfield Beach, Tampa, and Savannah facilities via telephone multiplex. This enables any project manager, section manager, QA manager, laboratory director, or chemist with authority to access projects to check the status of a project. If special handling or data packaging is required, the QA department receives copies of the custody forms and computer acknowledgement and then initiates a QA project file and determines the sample batching. A sample delivery group (SDG) sheet is established and distributed to all affected departments including the various laboratory chemists, project managers, and section managers. After the sample analysis request is logged into the LIMS and approved, the LIMS generates worksheets which are printed and distributed three times weekly. Figure 12.1 Section 12 Revision 0 Date: 9/92 FLOW CHART OF SL COMPUTERIZED LABORATORY INFORMATION MANAGEMENT SYSTEM (LIMS) SAMPLES SUBMITTED Client/Field Crew CUSTODY/UMS LOGIN Sample/Data Coordinator LOGIN APPROVED Project Manager ANALYSES AND INITIAL REVIEW Analyst "^ ——— PRINT WORKSHEETS DATA «, QC REVIEWED Chemist/QA PRINT APPROVAL SHEETS QC& DATA APPROVED Project/QA Manager REPORT & QC REVIEW Project/QA Manager FINAL REPORT AND INVOICE APPROVAL & SIGNATURE Project Manager TUT OO6 007:1 Section 12 Revision 0 Date: 9/92 12.4 Sample Analysis and Data Reduction Through the use of the worksheets and/or SDG sheets, the samples are prepared following the procedures given in each of EPA's approved methods. The preparation information is recorded in bound notebooks throughout the laboratory. 12.4.1 Data Reduction Most sample concentration results are read directly from instrumentation without further reduction or calculations. Dilution factors are applied upon the dilution of samples having concentrations above the calibration range. In many cases, these are input into the instrument computer and correct results are calculated automatically. In other cases, a manual calculation may be made. All soil/solid waste concentration results for all laboratory sections must be calculated on a dry weight basis prior to reporting by dividing the instrument result by the dry weight fraction. Other than the cases discussed above, data obtained by the following method/instrument are directly reportable: volatile GC, volatile GC/MS, semivolatile GC/MS, metals ICP, metals AA, general chemistry automated colorimetry, TOC, DO, turbidity, and pH. Methods data requiring reduction prior to reporting include semivolatile GC, titrimetric methods, BOD, COD, conductivity, manual UV/VIS/IR, residue, and TOX. Table 12.1 gives equations used in computer-controlled instrumentation for data reduction as well as equations used for the manual calculation of reportable concentration results. All laboratory pH meters are temperature compensated. Laboratory conductivity is always measured at 25"C. The laboratory raw data containing the instrument-generated reports, manually calculated results, and all supporting preparation, calibration, and analytical data are retained at the individual work stations until reports are issued unless additional handling or data packaging is required. All field pH and conductivity meters are temperature compensated. Cell constants for field conductivity meters are determined by laboratory personnel annually as given in Section 9.4.2. Field conductivity is calculated as given in Table 12.1. All other field data are read directly from instrumentation. Bound field notebooks are used for documentation of required data reduction. Calculations are recorded in waterproof ink. TUT O06 O074 Section 12 Revision 0 Date: 9/92 TABLE 12.1 SUMMARY OF EQUATIONS USED IN CALCULATIONS Equations BH/A Extractables by GC/MS [Internal Standard Method (625 and 8270)] YOG Response Factor - As X Cis (RF) Ais X Cs As • area of the characteristic ion of standard Ais ~ area of the characteristic ion of internal standard Cs - concentration of standard (ug/L) Cis - concentration of the internal standard (ug/L) Water - As x Cis Cone., ug/L Ais RF As - area of the characteristic ion (sample) Ais - area of the characteristic ion (internal standard) Cis - concentration of the standard (ug/L) RF - response factor Sediment - UR of internal standard z As x 1 Cone., ug/kg (kg of sample) (Z solids x .01) Ais RF As " area of the characteristic ion (sample) Ais " area of the characteristic ion (internal standard) RF " response factor Reporting Units Water ug/L (or mg/L) Solid* ug/kg (or mg/kg) by GC/MS [Internal Standard Method - See section on BN/A) VOCs by GC Response Factor - ua/L of compound to be measured (RF) peak height Hater - RF x peak height x dilution factor Cone . , ug/L Sediment ** RF x peak height x liter eouivalent of std. volume Cone., ug/L (kg of sample) (Z solids x .01) Pesticides/PCBa and Other GC Procedures Response Factor ™ UK of analvte (RF) (Standard) peak area Mater Cone . , ug/L - RF x peak area x extract volume in uL (liters of sample extracted) (injection volume in uL) Sediment Cone . , ug/kg - RF X peak area x extract volume in uL (kg of sample extracted) (I solids x .01) (injection volume in uL) ug/L (or mg/L) ug/L (or mg/L) ug/kg (or mg/kg) ug/kg (or mg/kg) TUT OO6 OO75 Section 12 Revision 0 Date: 9/92 TABLE 12.1 SUMMARY OF EQUATIONS USED IN CALCULATIONS Equations Metals Calibration curve construction y » mx + b y • absorbance m - slope - absorbance concentration x - concentration (mg/L) b - y intercept Calculation of water sample concentration Water Cone., ug/L ~ y - b x dilution factor m Sediment Cone . , mg/kg - mg/L 3t dilution factor X final volume (liters) of digest (kg of sample) (I solids x .01) UV/VIS and TR Procedures Calibration curve construction (see metals) Hater Cone., mg/L ™ y - b x dilution factor m Sediment ™ mg/L x liters of leachate (or digest) Cone. (kg of sample) (Z solids x .01) General Titrimetric Procedures Analyte. mg/L - N..._, X liter X etr. wt. X 1000 Vol. of sample titrated BOO BOD. mit/L " (Int. DO - Final DO) - Seed Correction Factor Vol. fraction of sample COO COD. m*/L - (Blk titer - sample titer) X N..« X 8000 Vol. of sample, mL Reporting Units Hater ug/L (or mg/L) mg/L mg/L mg/L mg/L Solid* ug/kg (or mg/kg) mg /kg TUT OO6 OO76 Section 12 Revision 0 Date: 9/92 TABLE 12.1 SUMMARY OF EQUATIONS USED IN CALCULATIONS i Equations Conductivity Cell constant - 1000 Observed conductivity of 1000 - j»S/cm std. Residue Residue. na/L - Total wt. - Wt. of dish or filter Vol. of sample, L TQX TOX. tfg/L - (Cl + C2 - 2C3) X 1000 mL Vol. of sample TOX. rag/kg - instrument reading X 5 I*L injected dry wt. fraction Reporting Units Hater fiS/cm mg/L mg/L Solid* mg/kg * Data for solid or semisolid sample are reported on a dry weight basis. TUT 006 0077 Section 12 Revision 0 Date: 9/92 12.4.2 Chromatographic and Data File Identification Chromatograms and data files are given a unique alphanumeric identification by the chemists initiating the analyses in each section where appropriate. These file identification numbers reflect either the date the sequence was initiated (GC sections), the order in which the samples were analyzed (GC/MS sections), and/or the sample identification and log numbers given by the client and listed on the LIMS. 12.5 Data Transfer and Review 12.5.1 Data Transfer to LIMS The analytical results are entered on the sectional worksheets after review. The worksheet data are entered into the LIMS by the data entry technicians. After the data are entered into the LIMS, project manager approval sheets are printed and the project managers and one of the data managers check each worksheet against the information entered into the LIMS for transfer errors and anomalies. 12.5.2 Data Review Laboratory analytical results are reviewed by the chemist responsible for the analysis and/or a peer chemist or a section supervisor. Prior to entering the reportable data into the LIMS, laboratory raw data have been reviewed, stamped, and signed to ensure that all of the method specifications have been met. This includes checking the extraction, digestion, distillation, and other preparation logs, as well as ensuring that all precision and accuracy requirements are addressed, and all steps of the analyses have been completed. If any problems arise during the analysis of the sample batch, it is the responsibility of the chemist and the section supervisor to bring this to the attention of the project manager, section manager, and QA manager through a written corrective action report. The field/sampling manager is responsible for data review of all field- generated data. This includes verifying that all field descriptive data is recorded as per Section 6, that all field calibration requirements have been met as per Section 9, that all field QC data have met criteria given in Table 5.3, and that field data are entered accurately on worksheets. For reports on which QA deliverables are required, data flags are used to inform the project manager and the client of any additional information that might aid in the interpretation of the data. The data flagging system incorporates the data qualifiers specified in the Contract Laboratory Program protocols, as well as additional flags used to help explain batch specific events. When data acquisition and reporting have been completed, the project manager reviews and prepares the final report. Because the project managers have extensive experience in evaluating analytical data, they TUT OO6 OO78 Section 12 Revision 0 Date: 9/92 have developed both objective and subjective techniques for data review. Each value reported is reviewed in the context of the respective environmental matrix and all available QC/QA data. Outliers or other abnormal values are carefully scrutinized, and samples are reanalyzed if the abnormalities cannot be explained. Where there are cases in which the results from spiked samples suggest interferences, attempts are made to remove the interferences, or alternate analytical procedures are used. If the interference problem cannot be resolved, the data are flagged and/or a narrative is included with the report. 12.5.3 Special Project or Data Package Review If special handling and/or data packages are requested by the client, the QA department also reviews the project report and the raw data. This includes checking to ensure that holding time requirements are met, reviewing internal chain of custody, recalculating results and detection limits, checking calibrations, reviewing all quality control data and/or control charts, and initiating any corrective action or reanalyses that might be appropriate. If requested, the data packages are paginated, copied, and bound by the QA staff. 12.6 Reporting The final report is printed and signed by the project manager after all review has been completed. Figures 12.2 - 12.5 are examples of RESULTS ONLY SL Level 0, SL Level 1, SL Level 2, and SL Level 3 (CLP equivalent) typical reports for liquids samples. For CLP parameters, the CLP forms from the CLP SOW are generated by instrument software and are submitted to the client. If requested by the client or a project specific QA Plan, hybrid/custom reports or CLP data packages with diskette deliverables can be provided. All LIMS reports can be downloaded onto diskettes or most client's computers. The data flags that may appear in a project report are defined on the signature page, and any additional comments are also footnoted on this page. If data packaging is requested, a paginated, copied, and bound data package is provided in addition to the project report. The format of the project report and/or data package can be adjusted to meet the needs of the client. 12.7 Data Storage The raw data are stored in metal filing cabinets at each work station until the cabinets are filled to capacity. The data are then transferred to a secured area and filed chronologically by laboratory section in banker's boxes for a period of 3-5 years. If the data are to be purged to the client or need to be separated from the general raw data files, the data can be boxed, labeled and stored in a separate secured area. TUT 006 0079 Section 12 Revision 0 Date: 9/92 Hard copies of all reports are maintained for 3-5 years in client file. All LIMS reports and associated QC data are kept for a minimum of three years on the LIMS hard discs or magnetic tape. All data on the LIMS are backed up daily on magnetic tape. All in-lab data generated by computer systems are stored to tape when the capability exists. The tapes are labeled and stored at the individual work stations. Keys to the data storage areas are retained by the QA staff and the section/department managers. TUT OO6 0080 Section 12 Revision 0 Date: 9/92 FIGURE 12.2 EXAMPLE OF RESULTS ONLY REPORT TUT 006 OO81 Section 12 Revision 0 Date: 9/92 LOG NO: SE-00010 Received: 21 FEE 91 Example Client 333 Main St. Savannah, GA 31404 Project: SL 0 (Results only) Report Sampled By: Client REPORT OF RESULTS LOG NO SAMPLE DESCRIPTION , LIQUID. SAMPLES 00010-1 Water Sample 1 (Collected 2-21-91) PARAMETER 00010-1 Purgeable Halocarbons (601/8010) Bromodichloromethane, ug/1 Bromoform, ug/1 Bromomethane, ug/1 Carbon Tetrachloride, ug/1 Chlorobenzene, ug/1 Chloroe thane, ug/1 2-Chloroethylvinyl Ether, ug/1 Chloroform, ug/1 Chloromethane, ug/1 Dibromochloromethane, ug/1 1.2-Dichlorobenzene, ug/1 1.3-Dichlorobenzene, ug/1 1.4-Dichlorobenzene, ug/1 Dichlorodifluoromethane, ug/1 1.1-Dichloroethane, ug/1 1.2-Dichloroethane, ug/1 1.1-Dichloroethene, ug/1 Trans-1,2-Dichloroethylene, ug/1 1.2-Dichloropropane, ug/1 Cis-1,3-Dichloropropene, ug/1 Trans-1,3-Dichloropropene, ug/1 Methylene Chloride, ug/1 1,1,2,2-Tetrachloroethane, ug/1 ''--IT O06 O082 SAVANNAH LABORATORIES l CNVWOMMCNML tamcts. MC Section 12 Revision 0 Date: 9/92 LOG NO: SE-00010 Received: 21 FEE 91 Example Client 333 Main St. Savannah, GA 31404 Project: SL 0 (Results only) Report Sampled By: Client REPORT OF RESULTS LOG NO SAMPLE DESCRIPTION , LIQUID SAMPLES 00010-1 Water Sample 1 (Collected 2-21-91) PARAMETER 00010-1 Tetrachloroethene, ug/1 <1.0 1.1.1-Trichloroethane, ug/1 <1.0 1.1.2-Trichloroethane, ug/1 <1.0 Trichloroethene, ug/1 <1.0 Trichlorofluoromethane, ug/1 <1.0 Vinyl Chloride, ug/1 <1.0 Purgeable Aromatics (602/8020) Benzene, ug/1 <1.0 Chlorobenzene, ug/1 <1.0 1.2-Dichlorobenzene, ug/1 <1.0 1.3-Dichlorobenzene, ug/1 <1.0 1.4-Dichlorobenzene, ug/1 <1.0 Ethylbenzene, ug/1 <1.0 Toluene, ug/1 <1.0 Xylenes, ug/1 <1.0 Lead , ug/1 <5.0 Methods: EPA 40 CFR Part 136 J. W. Andrews, Ph. D. TUT 006 0083 SAVANNAH LABORATORIES t tHvmomttHHL soniccs. we Section 12 Revision 0 Date: 9/92 FIGURE 12.3 EXAMPLE OF SL LEVEL I REPORT -TUT O06 0084 Section 12 Revision 0 Date: 9/92 LOG NO: SE-00011 Received: 21 FEE 91 Example Client 333 Main St. Savannah, GA 31404 Project: SL I Report Sampled By: Client REPORT OF RESULTS LOG NO SAMPLE DESCRIPTION , LIQUID SAMPLES 00011-1 Water Sample 1 (Collected 2-20-91) PARAMETER 00011-1 Purgeable Halocarbons (601/8010) Bromodichloromethane, ug/1 Bromoform, ug/1 Bromomethane, ug/1 Carbon Tetrachloride, ug/1 Chlorobenzene, ug/1 Chloroethane, ug/1 2-Chloroethylvinyl Ether, ug/1 Chloroform, ug/1 Chloromethane, ug/1 Dibromochloromethane, ug/1 1.2-Dichlorobenzene, ug/1 1.3-Dichlorobenzene, ug/1 1.4-Dichlorobenzene, ug/1 Dichlorodifluoromethane, ug/1 1.1-Dichloroethane, ug/1 1.2-Dichloroethane, ug/1 1.1-Dichloroethene, ug/1 Trans-1,2-Dichloroethylene, ug/1 1.2-Dichloropropane, ug/1 Cis-1,3-Dichloropropene, ug/1 Trans-1,3-Dichloropropene, ug/1 Methylene Chloride, ug/1 1,1,2,2-Tetrachloroethane, ug/1 TUT CO6 OO8!! SAVANNAH LABORATORIES I tWVWOWNFNMl JCTMCfl. WC. Section 12 Revision 0 Date: 9/92 LOG NO: SE-00011 Received: 21 FEE 91 Example Client 333 Main St. Savannah, GA 31404 Project: SL I Report Sampled By: Client REPORT OF RESULTS LOG NO SAMPLE DESCRIPTION , LIQUID SAMPLES 00011-1 Water Sample 1 (Collected 2-20-91) PARAMETER 00011-1 Tetrachloroethene, ug/1 <1.0 1.1.1-Trichloroethane, ug/1 <1.0 1.1.2-Trichloroethane, ug/1 <1.0 Trichloroethene, ug/1 <1.0 Trichlorofluoromethane, ug/1 <1.0 Vinyl Chloride, ug/1 <1.0 Purgeable Aromatics (602/8020) Benzene, ug/1 <1.0 Chlorobenzene, ug/1 <1.0 1.2-Dichlorobenzene, ug/1 <1.0 1.3-Dichlorobenzene, ug/1 <1.0 1.4-Dichlorobenzene, ug/1 <1.0 Ethylbenzene, ug/1 <1.0 Toluene, ug/1 <1.0 Xylenes, ug/1 <1.0 Lead , ug/1 <5.0 UT OO6 OO86 SAVANNAH LABORATORIES sstncci. we. Section 12 Revision 0 Date: 9/92 LOG NO: SE-00011 Received: 21 FEB 91 Example Client 333 Main St. Savannah, GA 31404 LOG NO REPORT OF RESULTS SAMPLE DESCRIPTION , QC REPORT FOR LIQUID SAMPLES Project: SL I Report Sampled By: Client 00011-2 Method Blank 00011-3 Laboratory Control Standard (LCS) % Recovery 00011-4 Precision (% RPD from LCS) PARAMETER 00011-2 00011-3 00011-4 Purgeable Halocarbons (601/8010) Bromodichloromethane, ug/1 Bromoform, ug/1 Bromomethane, ug/1 Carbon Tetrachloride, ug/1 Chlorobenzene, ug/1 Chloroethane, ug/1 2-Chloroethylvinyl Ether, ug/1 Chloroform, ug/1 Chlorome thane, ug/1 Dibromochloromethane, ug/1 1.2-Dichlorobenzene, ug/1 1.3-Dichlorobenzene, ug/1 1.4-Dichlorobenzene, ug/1 Dichlorodifluoromethane, ug/1 1.1-Dichloroethane, ug/1 1.2-Dichloroethane, ug/1 1.1-Dichloroethene, ug/1 Trans-1,2-Dichloroethylene, ug/1 1.2-Dichloropropane, ug/1 Cis-1,3-Dichloropropene, ug/1 Trans-1,3-Dichloropropene, ug/1 97 % 4.7 % 99 % 2.9 % TUT OO6 CO 8 7 SAVANNAH LABORATORIES . me. Section 12 Revision 0 Date: 9/92 LOG NO: SE-00011 Received: 21 FEE 91 Example Client 333 Main St. Savannah, GA 31404 LOG NO REPORT OF RESULTS SAMPLE DESCRIPTION , QC REPORT FOR LIQUID SAMPLES Project: SL I Report Sampled By: Client 00011-2 Method Blank 00011-3 Laboratory Control Standard (LCS) % Recovery 00011-4 Precision (% RPD from LCS) PARAMETER 00011-2 00011-3 00011-4 Methylene Chloride, ug/1 1,1,2,2-Tetrachloroethane, ug/1 Tetrachloroethene, ug/1 1.1.1-Trichloroethane, ug/1 1.1.2-Trichloroethane, ug/1 Trichloroethene, ug/1 Trichlorofluoromethane, ug/1 Vinyl Chloride, ug/1 Purgeable Aromatics (602/8020) Benzene, ug/1 Chlorobenzene, ug/1 1.2-Dichlorobenzene, ug/1 1.3-Dichlorobenzene, ug/1 1.4-Dichlorobenzene, ug/1 E thylbenz ene, ug/1 Toluene, ug/1 Xylenes, ug/1 Lead , ug/1 101 * 99 % 1.3 % 1.4 % <5.0 103 % 2.7 V 100 V 10 V Methods: EPA 40 CFR Part 136 J. W. Andrews, Ph. D. TUT OO6 OO88 SAVANNAH LABORATORIES t tNVMONMENML SBtnClf WC Section 12 Revision 0 Date: 9/92 FIGURE 12.4 EXAMPLE OF SL LEVEL II REPORT TUT 006 0089 Section 12 Revision 0 Date: 9/92 LOG NO: SE-00012 Received: 21 FEE 91 Example Client 333 Main St. Savannah, GA 31404 Project: SL II Report Sampled By: Client REPORT OF RESULTS LOG NO SAMPLE DESCRIPTION , LIQUID SAMPLES DATE SAMPLED 00012-1 Water Sample 1 (Collected 2-20-91) 02-20-91 PARAMETER 00012-1 Purgeable Halocarbons (601) Bromodichloromethane, ug/1 <:1.0 Bromoform, ug/1 <1.0 Bromomethane, ug/1 <1.0 Carbon Tetrachloride, ug/1 <1.0 Chlorobenzene, ug/1 <1.0 Chloroethane, ug/1 <1.0 2-Chloroethylvinyl Ether, ug/1 <1.0 Chloroform, ug/1 <1.0 Chloromethane, ug/1 <1.0 Dibromochloromethane, ug/1 <1.0 1.2-Dichlorobenzene, ug/1 <1.0 1.3-Dichlorobenzene, ug/1 <1.0 1.4-Dichlorobenzene, ug/1 <1.0 Dichlorodifluoromethane, ug/1 <1.0 1.1-Dichloroethane, ug/1 <1.0 1.2-Dichloroethane, ug/1 <1.0 1.1-Dichloroethene, ug/1 <1.0 Trans-1,2-Dichloroethylene, ug/1 <1.0 1.2-Dichloropropane, ug/1 <1.0 Cis-1,3-Dichloropropene, ug/1 <1.0 Trans-1,3-Dichloropropene, ug/1 <1.0 Methylene Chloride, ug/1 <1.0 1, l, 2,2-Tetrachloroethane, ug/1 <1.0 TUT OO6 OO9O SAVANNAH LABORATORIES I frntfOMHCHTti SOIWCfS IHC Section 12 Revision 0 Date: 9/92 LOG NO: SE-00012 Received: 21 FEE 91 Example Client 333 Main St. Savannah, GA 31404 Project: SL II Report Sampled By: Client REPORT OF RESULTS LOG NO SAMPLE DESCRIPTION , LIQUID SAMPLES 00012-1 Water Sample 1 (Collected 2-20-91) PARAMETER DATE SAMPLED 02-20-91 00012-1 Tetrachloroethene, ug/1 1.1.1-Trichloroethane, ug/1 1.1.2-Trichloroethane, ug/1 Trichloroethene, ug/1 Trichlorofluoromethane, ug/1 Vinyl Chloride, ug/1 Surrogate - Bromochloromethane, ug/1 Date Analyzed Purgeable Aromatics (602/8020) Benzene, ug/1 Toluene, ug/1 Ethylbenzene, ug/1 Total Xylenes, ug/1 Methyl-Tert-Butyl-Ether (MTBE), ug/1 Total Volatile Organic Aromatics, ug/1 Surrogate - a,a,a-Trifluorotoluene , ug/1 Date Analyzed Lead Lead , ug/1 Date Analyzed 94 % 02.22.91 97 V 02.22.91 <5.0 02.22.91 TUT OO6 CO 9.1 SAVANNAH LABORATORIES t nmnomKMMi minca. we. Section 12 Revision 0 Date: 9/92 LOG NO: SE-00012 Received: 21 FEE 91 Example Client 333 Main St. Savannah, GA 31404 LOG NO REPORT OF RESULTS SAMPLE DESCRIPTION , QC REPORT FOR LIQUID SAMPLES Project: SL II Report Sampled By: Client 00012-2 Method Blank 00012-3 Laboratory Control Standard (LCS) * Recovery 00012-4 Precision (V RPD from LCS) PARAMETER 00012-2 00012-3 00012-4 Purgeable Halocarbons (601) Bromodichloromethane, ug/1 Bromoform, ug/1 Bromome thane, ug/1 Carbon Tetrachloride, ug/1 Chlorobenzene, ug/1 Chloroethane, ug/1 2-Chloroethylvinyl Ether, ug/1 Chloroform, ug/1 Chloromethane, ug/1 Dibromochloromethane, ug/1 1.2-Dichlorobenzene, ug/1 1.3-Dichlorobenzene, ug/1 1.4-Dichlorobenzene, ug/1 D i chlorodi fluorome thane, ug/1 1.1-Dichloroethane, ug/1 1.2-Dichloroethane, ug/1 1.1-Dichloroethene, ug/1 Trans-1,2-Dichloroethylene, ug/1 1.2-Dichloropropane, ug/1 Cis-1,3-Dichloropropene, ug/1 Trans-1,3-Dichloropropene, ug/1 108 * 2.2 % 100 V 1.8 V TUT OO6 0092 SAVANNAH LABORATORIES t tumOMMfNTAL totncii. me. Section 12 Revision 0 Date: 9/92 FIGURE 12.5 EXAMPLE OF SL LEVEL III REPORT TUT OO6 O09:: Section 12 Revision 0 Date: 9/92 LOG NO: SE-00012 Received: 21 FEE 91 Example Client 333 Main St. Savannah, GA 31404 LOG NO REPORT OF RESULTS SAMPLE DESCRIPTION , QC REPORT FOR LIQUID SAMPLES Project: SL II Report Sampled By: Client 00012-2 Method Blank 00012-3 Laboratory Control Standard {LCS) * Recovery 00012-4 Precision (V RPD from LCS) PARAMETER 00012-2 00012-3 00012-4 Methylene Chloride, ug/1 1,1,2,2-Tetrachloroethane, ug/1 Tetrachloroethene, ug/1 1.1.1-Trichloroethane, ug/1 1.1.2-Trichloroethane, ug/1 Trichloroethene, ug/1 Trichlorofluoromethane, ug/1 Vinyl Chloride, ug/1 Surrogate - Bromochloromethane, ug/1 Date Analyzed Purgeable Aromatics (602/8020) Benzene, ug/1 Toluene, ug/1 Ethylbenzene, ug/1 Total Xylenes, ug/1 Methyl-Tert-Butyl-Ether (MTBE), ug/1 Total Volatile Organic Aromatics, ug/1 Surrogate - a,a,a-Trifluorotoluene , ug/1 Date Analyzed Lead Lead , ug/1 Date Analyzed 98 * 02.22.91 99 V 02.22.91 <5.0 02.22.91 93 V 97 % 99 % 102 V 1.3 * 4.5 * 4.5 V 6.7 V 104 * 90 % 5.9 % 10 * Methods: EPA 40 CFR Part 136 Case Narrative - No QC problems were encountered. J. W. Andrews, Ph. D. TUT OO6 OO94 SAVANNAH LABORATORIES t CWVMONMFMMl JCTWCO WC. Section 12 Revision 0 Date: 9/92 LOG NO: SE-00015 Received: 21 FEE 91 Example Client 333 Main St. Savannah, GA 31404 REPORT OF RESULTS LOG NO SAMPLE DESCRIPTION , LIQUID SAMPLES 00015-1 Water Sample 1 (Collected 2-20-91) PARAMETER Project: SL III Report (CLP Type) Sampled By: Client 00015-1 Purgeable Halocarbons (601) Bromodichloromethane, ug/1 Bromoform, ug/1 B romome thane , ug/1 Carbon Tetrachloride, ug/1 Chlorobenzene, ug/1 Chloroethane, ug/1 2-Chloroethylvinyl Ether, ug/1 Chloroform, ug/1 Chl orome thane, ug/1 Dibromochloromethane, ug/1 1,2-Dichlorobenzene, ug/1 1,3-Dichlorobenzene, ug/1 1,4 -Di chlorobenzene, ug/1 Dichlorodif luoromethane, ug/1 1, 1-Di chloroethane, ug/1 1,2-Dichloroethane, ug/1 1, 1-Dichloroethene, ug/1 Trans-1, 2- Dichloroethylene, ug/1 1, 2-Dichloropropane, ug/1 Cis-1, 3-Dichloropropene, ug/1 Trans-1, 3-Dichloropropene, ug/1 Methylene Chloride, ug/1 1, 1, 2, 2-Tetrachloroethane, ug/1 l.OU l.OU l.OU l.OU l.OU l.OU l.OU l.OU l.OU l.OU l.OU l.OU l.OU l.OU l.OU l.OU l.OU l.OU l.OU l.OU l.OU l.OU l.OU TUT O06 OO95 SAVANNAH LABORATORIES 1 fWMKMMewMl iOtfKCi WC Section 12 Revision 0 Date: 9/92 LOG NO: SE-00015 Received: 21 FEE 91 Example Client 333 Main St. Savannah, GA 31404 LOG NO REPORT OF RESULTS SAMPLE DESCRIPTION , LIQUID SAMPLES Project: SL III Report (CLP Type) Sampled By: Client 00015-1 Water Sample 1 (Collected 2-20-91) PARAMETER 00015-1 Tetrachloroethene, ug/1 1, 1, 1 -Tri chl oroe thane, ug/1 1, 1,2-Trichloroethane, ug/1 Trichloroethene, ug/1 Trichlorofluoromethane, ug/1 Vinyl Chloride, ug/1 Surrogate - Bromochlorome thane, ug/1 Date Analyzed Purgeable Aromatics (602/8020) Benzene, ug/1 Toluene, ug/1 Ethylbenzene , ug/1 Total Xylenes, ug/1 Methyl -Tert -Butyl -Ether. (MTBE) , ug/1 Total Volatile Organic Aromatics, ug/1 Surrogate - a, a, a-Trif luorotoluene , ug/1 Date Analyzed Lead Lead , ug/1 Date Analyzed l.OU l.OU l.OU l.OU l.OU l.OU 94 % 02.22.91 l.OU l.OU l.OU l.OU l.OU l.OU 97 % 02.22.91 5.0U 02.22.91 TUT OO6 OO96 SAVANNAH LABORATORIES we. Section 12 Revision 0 Date: 9/92 LOG NO: SE-00015 Received: 21 FEE 91 Example Client 333 Main St. Savannah, GA 31404 Project: SL III Report (CLP Type) Sampled By: Client LOG NO REPORT OF RESULTS SAMPLE DESCRIPTION , QC REPORT FOR LIQUID SAMPLES 00015-2 Method Blank 00015-3 Laboratory Control Standard (LCS) % Recovery 00015-4 Precision (* RPD from LCS) PARAMETER 00015-2 00015-3 00015-4 Purgeable Halocarbons (601) Bromodi chl orome thane, ug/1 Bromoform, ug/1 Br omome thane , ug/1 Carbon Tetrachloride, ug/1 Chlorobenzene, ug/1 Chloroethane, ug/1 2-Chloroethylvinyl Ether, ug/1 Chloroform, ug/1 Chl orome thane, ug/1 Dibromochloromethane, ug/1 1,2-Dichlorobenzene, ug/1 1,3-Dichlorobenzene, ug/1 1,4-Dichlorobenzene, ug/1 Dichlorodif luoromethane, ug/1 1, 1-Di chloroethane, ug/1 1, 2 -Di chloroethane, ug/1 1, 1-Dichloroethene, ug/1 Trans-1, 2-Dichloroethylene, ug/1 1, 2-Dichloropropane, ug/1 Cis-1, 3-Dichloropropene, ug/1 Trans-1, 3 -Dichloropropene, ug/1 1 . OU 1 . OU 1 . OU 1 . OU l.OU 108 * 1 . OU 1 . OU 1 . OU 1 . OU - - - 1 . OU - - - 1 . OU 1 . OU 1 . OU 1 . OU 1 . OU 1 . OU l.OU 100 V 1 . OU 1 . OU 1 . OU 1 . OU - - - - -- 2.2 V - - - - - - ... - - - - - - - - - - - - 1.8 % - - - - - - - - - TUT OO6 GO97 SAVANNAH LABORATORIES t CHYmomHMru. ttxncts. we Section 12 Revision 0 Date: 9/92 LOG NO: SE-00015 Received: 21 FEE 91 Example Client 333 Main St. Savannah, GA 31404 Project: SL III Report (CLP Type) Sampled By: Client LOG NO REPORT OF RESULTS SAMPLE DESCRIPTION , QC REPORT FOR LIQUID SAMPLES 00015-2 Method Blank 00015-3 Laboratory Control Standard (LCS) % Recovery 00015-4 Precision {* RPD from LCS) PARAMETER 00015-2 00015-3 00015-4 Methylene Chloride, ug/1 1,1,2,2-Tetrachloroethane, ug/1 Tetrachloroethene , ug/1 1, 1, 1-Tri chl or oe thane, ug/1 1, 1, 2-Trichloroethane, ug/1 Trichloroethene, ug/1 Trichlorof luoromethane, ug/1 Vinyl Chloride, ug/1 Surrogate - Bromochloromethane, ug/1 Date Analyzed Purgeable Aromatics (602/8020) Benzene, ug/1 Toluene, ug/1 Ethylbenzene , ug/1 Total Xylenes, ug/1 Methyl -Tert -Butyl -Ether (MTBE) , ug/1 Total Volatile Organic Aromatics, ug/1 Surrogate - a,a,a-Trif luorotoluene , ug/1 Date Analyzed Lead Lead , ug/1 Date Analyzed 1. 1. 1. 1. 1. 1. 1. 1. 98 02.22. 1. 1 . 1. 1. 1. 1. 99 02.22. 5. 02.22. OU OU OU OU OU OU OU OU % 91 OU OU OU OU OU OU * 91 OU 91 ... ... 93 V ... --- 97 V --- 99 V 102 * -- - ... ... ... 104 % 90 % - - - --- ... 1.3 * ... --- 4.5 % 4.5 % 6.7 * --- . . . . . . 5.9 % 10 % - - - TUT GO6 OO98 SAVANNAH LABORATORIES t CNYiKOMMturti. tarnca. we Section 12 Revision 0 Date: 9/92 LOG NO: SE-00015 Received: 21 FEE 91 Example Client 333 Main St. Savannah, GA 31404 Project: SL III Report (CLP Type) Sampled By: Client LOG NO REPORT OF RESULTS SAMPLE DESCRIPTION , QC REPORT FOR LIQUID SAMPLES 00015-5 Matrix Spike (% Rec) 00015-6 Matrix Spike Duplicate (% Rec) PARAMETER 00015-5 00015-6 Purgeable Halocarbons (601) Chlorobenzene, mg/1 1,1-Dichloroethene, mg/1 Trichloroethene, mg/1 Surrogate - Bromochloromethane, mg/1 Purgeable Aromatics (602/8020) Benzene, ug/1 Toluene, ug/1 Surrogate - a,a,a-Trifluorotoluene , ug/1 Lead Lead , ug/1 98 % 104 % 95 % 99 % 94 % 99 * 102 % 98 * 100 % 102 % 98 V 98 % 96 V 101 * 103 % 100 % Methods: EPA 40 CFR Part 136 See attached data package. J. W. Andrews, Ph. D. TUT OO6 OO99 SAVANNAH LABORATORIES . we. Section 12 Revision 0 Date: 9/92 CLP EQUIVALENT SUPPLEMENTAL DATA PACKAGE INCLUDES 1. Run sequence log 2. Five-point curves or data with chromatograms or instrument printouts 3. Daily check standard/continuing calibration form and standard chromatograms or instrument printouts 4. Sample spike, (LCS and matrix), method blank chromatograms, quant reports, and/or instrument printouts 5. Project narrative TUT CO6 O10O Section 13 Revision 0 Date: 9/92 13.0 CORRECTIVE ACTION Corrective action will be initiated when data are determined to be questionable or QC criteria are out of control. For routine operational problems, the analysts correct the problem and note the problem/corrective action on the run log or bench data sheet. A Corrective Action Report (CAR) is not necessary unless the problem is recurring. When formal corrective action is required, a Corrective Action Report (CAR) is prepared on the CAR form (Figure 13.1). CAR are required for: 1. Chronic problems which could affect data quality or production and are due to equipment or facility disrepair or inadequacy, improper training, employee attitude or ineptness, supply, reagent or standard quality, SOP inadequacy or error, or any other problems which could be corrected by management. CARs for this type of problem should be prepared by the analyst and channelled through the department manager/lab manager to the laboratory director. The box by "Request Lab Director's Attention" should be checked and final action should be taken by the lab director. 2. For uncorrectable nonconformance problems which are noted by an asterisk (*) in Table 13.1 which could affect the quality of report data, corrective action is initiated by the analyst or department manager. Before a CAR is prepared, the analyst/department manager will review raw data calculations, procedures, methods, operating conditions of the instrument and all data available. If this does not resolve the problem, analysis of the batch (samples plus QC samples) is repeated provided sufficient sample is available. If data are submitted in cases where QC is not in compliance, this is documented in a case narrative which is part of the data reports. The action must be approved by the project manager who submits the report. 3. When QA problems are discovered during data review, system audits, performance audits, audit sample results, client inquiries, external data review or validation, or audits, a CAR is prepared by the QA manager, and is filed for use in QA reports to management. 4. When QA data exceed the criteria in Table 13.2, the analyst or department manager initiates a CAR. All CARs are filed in the departmental corrective action notebook which has a pending and completed section. Follow-up is checked weekly by the department manager and monthly by the QA manager. If warning limits are exceeded, the department manager/supervisor points this out to the respective supervisors or chemists who attempt to define and correct the problem. Savannah Laboratories will abide by any corrective action deemed necessary by all pertinent agencies. TUT 006 O.1O.1 Section 13 Revision 0 Date: 9/92 FIGURE 13.1 CORRECTIVE ACTION REPORT (CAR) Date Prepared: __________________Sample ID:)_______________SL Project ID:_ Analysis: _____________________________ Date of Analysis:_______ Analyst: _________________ Department Manager: ____________ Project Manager: Description of Nonconformance/Condition:____________________________________ Corrective Action Implemented: QA Manager's Initials: _______________________ Date of Approval: D Request Lab Director's attention LD Initials: ______________ Date: D Request Project Manager's attention PM Initials: ______________ Date: Date Corrective Action Implemented: ________________ By: _________ Corrective Action Follow-up/Comments: ________________________________ Corrective Action Completed: Department Manager's initials: _________ Date: QA Manager's Initials: __________________ Date: _______________ Copies of this report should be filed in the laboratory Corrective Action Notebook. TUT OO6 01O2 Section 13 Revision 0 Date: 9/92 TABLE 13.1 CORRECTIVE ACTION QC Activity * GC/MS tuning or ICP/AA * Initial calibration standards * QC check/continuing calibration standard * Method blank * Surrogate recovery (GC/MS semivolatiles ) * Surrogate recovery (GC/MS volatiles) Surrogate recovery GC or LC Matrix spike recoveries * Lab control standard recoveries Acceptance Criteria Per SOPs or Chapter 9.0 Per SOPs or Chapter 9.0 Per SOPs, See Chapter 9.0 < PQL (for CLP procedures, use SOW guidelines) Tables S.I and 5.2. One acid and one base nay be out of criteria. 0 outside criteria in Tables S.I and 5.2 Tables S.I and 5.2 Tables S.I and 5.2 Tables 5.1 and 5.2 Recoonended Corrective Action Do not analyze samples unless criteria are met. Reanalyze standards. If still unacceptable, remake standards or instrument corrections. Reanalyze standard. If still unacceptable, remake standards, or recalibrate. Reanalyze blank. If problem, determine source of contamination. If necessary or possible, redigest/extract batch and reanalyze. Follow SW-846 method or CLP guidelines . Follow SW-846 method or CLP guidelines. Criteria advisory only; check for possible matrix interferences or other causes. Criteria advisory only; check for possible matrix interferences or other causes. Check calculations, reanalyze standards, and if necessary or possible, redigest or extract batch and reanalyze. * If criteria cannot be met, a corrective action report (CAR) must be prepared and approved by QA manager and project manager. TUT OO6 01O3 Section 13 Revision 0 Date: 9/92 TABLE 13.2 Corrective Action Report Criteria for Control Charts Criteria A point outside ± 3 standard deviations Obvious shift in the mean Any 8 consecutive points are on the same side of the mean Any 6 consecutive points are such that each point is larger (smaller) than its immediate predecessor Any obvious cyclic pattern is seen in the points Corrective Action Check calculations. Report the deviation and results of preliminary investigation to the division manager, and the QA manager, who will decide jointly what action to take. Complete the Corrective Action Report and submit it to the department manager and QA manager for approval . Check calculations, data entry, standards, instrument, calibrations, etc. Document results in a Corrective Action Report. Check accuracy of data entry and calculations . Document results in a Corrective Action Report. Have the report approved by the department, QA, and project managers. Check accuracy of data entry and calculations. Document results in a Corrective Action Report. Have the report approved by the department, QA, and project managers. Check accuracy of data entry and calculations. Document results in a Corrective Action Report. Have the report approved by the department, QA, and project managers. TUT 006 0104 Section 14 Revision 0 Date: 9/92 14.0 PERFORMANCE AND SYSTEM AUDITS Performance and system audits are performed in each laboratory throughout the year. 14.1 Internal System Audits 14.1.1 Annual Corporate Audits On an annual basis, an on-site systems audit is conducted on all aspects of the laboratory and field operations at each facility. This audit is coordinated by the president and is conducted by a multiperson audit team made up of individuals with expertise in the organic, inorganic, QA, project custody, data management, and field sampling areas, the corporate safety director, and a representative from the business office. This on- site audit may be supplemented by review of reports and QA data in the LIMS network and review of selected data packages. An audit report is issued by the team, to the president within two weeks of completion of the audit and a copy is provided by the QA manager to the lab director. The annual system audits consist of an examination of laboratory procedures and documentation to ensure that the entire laboratory is being operated according to established protocol. The auditors will ensure that the proper frequency of quality control standards, spikes,-duplicates, etc., are incorporated with each sample analytical run, and.all results are documented, up to date, and accessible for review. Control charts are checked to ensure their proper maintenance. Calculations are spot checked and data procedures are reviewed to ensure SOPs are being followed, and special attention is given to calibration procedures. The systems audit check also ascertains whether proper documentation exists to trace working analytical standards back to stock standards. Finally, analysts' techniques are evaluated against techniques as defined in the SOPs, the SL Training SOP, and recognized good laboratory practices. The QA manager and lab director respond to the audit and are responsible for following up on required corrective action. 14.1.2 Quarterly Internal Audits Quarterly audits are conducted by lab QA managers. Results of these audits are used in preparation of quarterly reports to management. Responses and follow-up corrective actions are addressed by department managers and monitored by the lab QA manager. 14.1.3 Internal Systems Audit Checklist Figure 14.1 is a page from a laboratory checklist used to conduct an internal systems audit at Savannah Laboratories. This particular example contains quality assurance questions directed to the custody section of the laboratory. TUT 006 O105 Section 14 Revision 0 Date: 9/92 FIGURE 14.1 LABORATORY -INTERNAL SYSTEMS AUDIT CHECKLIST I. CU (Custody) Section Contacts : A. Are comprehensive, up-to-date SOPs available for this section? Comments : B. Are custody logbooks properly maintained? Comments : C. Is sample preservation checked and documented on arriving samples? Comments : D. Is the temperature of each lab pack recorded and documented upon arrival? Comments : E. Are sample custody excursion forms used if required? Comments : F. Are chain- of -custody forms properly filed? Comments : Yes No if TUT OO6 O106 Section 14 Revision 0 Date: 9/92 14.2 External System Audits Each laboratory is certified by several state agencies and governmental or private certification programs. The laboratories submit to external on- site audits by these certifying agencies or organizations. Field system audits are performed periodically by various federal and state regulatory agencies. Field sampling and documentation procedures are examined to insure sampling is performed according to the protocols established in this document. 14.3 Performance Audits 14.3.1 Internal Performance Audits The laboratory QA manager periodically schedules blind audit samples into the work flow. Major methods are tested by at least two internal audit samples annually. Audit samples are treated as actual samples and are logged into the LIMS. Results are entered into the LIMS and summarized by the QA manager and presented to the department managers, lab manager, and lab director. Problem results are addressed in corrective action and/or quarterly QA reports to management. 14.3.2 External Performance Audit All facilities participate in the following performance evaluation audits quarterly: 1. U. S. EPA Water Supply Study (WS Series). 2. U. S. EPA Water Pollution Study (WP Series). Additionally, the laboratories participate in several regulatory agency, certifying group, or client requested performance audits. Results from these performance audits are included in quarterly QA reports to management. TUT 006 0107 Section 15 Revision 0 Date: 9/92 15.0 QUALITY ASSURANCE REPORTS A summary report of the performance of the QA monitoring system is prepared by the QA manager on a quarterly basis. The report is due at the end of the calendar quarter, and copies of this report are distributed to the lab managers, lab director, and president. The lab director's copy should circulate to project managers, the lab manager's copy to department managers, and the president's copy to other corporate officers. A file copy is kept by the QA manager. The QA summary report should contain, but is not limited to, the following: A one-page executive summary provides copies of uncompleted corrective actions which are more than one month old. Summaries of external system audits and any responses/corrective action to problems noted. Results of internal performance evaluation and corrective action. Results of external performance evaluation sample analyses and any responses/corrective action to deficiencies. Summaries of internal system audits and response/corrective action. Significant QA problems which may impact data quality or production (based on daily observations, external and internal data reviews and validations, and quarterly internal QA audits) and recommended solutions. Recommendations for changes in the standard laboratory operating procedures. Also, reports of external audits and responses should be prepared by the QA manager as soon as possible and given to the appropriate project manager, lab director, and president if a significant QA problem is encountered. In this case, these external audit results need not be included in the quarterly QA summary report. An annual QA assessment report is prepared by the QA manager and lab manager. This report is due October 31, addresses precision and accuracy limits, MDLs, PQLs, and major QA problems along with recommendations for improvement, and is submitted to the lab director and president for use in the updating of the QA plan. External QA reports are submitted to DER QAS as provided for in Table VI, Appendix D of DER-QA-001/90. Each project-specific report is submitted at the recommended frequency, and includes a title page, a table of contents, TUT OO6 O1O8 Section 15 Revision 0 Date: 9/92 specific information for either the performance or systems audits, significant QA/QC problems, and corrective action status as described in Appendix D. If no project audits are performed and no significant QA/QC problems occur for the duration of a project requiring a DER QA report, a letter stating these facts will be submitted in lieu of the QA report. TUT OO6 0.109 Section 16 Revision: 0 Date: 9/92 16.0 PERSONNEL QUALIFICATIONS Listing of Technical Employees: EMPLOYEE James W. Andrews Janette D. Long Jay W. Andrews Alan C. Bailey Steven J. White Linda A. Wolfe Beverly Hughes Larry E. Phillips Wayne Robbins Penny Carter Sheila B. Hoffman Virginia Baisden Derrick M. Simons Ernest B. Walton Karla J. Bier Karri L. Derr Mike Salum Myron J. Young Paul E. Meyers Kenneth R. Aegan Lisa D. Aegan Robert Bearden Jesse B. Blackwell, Jr. Bernetha Brayboy Nancy Brown Laura R. Bulluck Hsaio Lan Chang Glen A. Coder Katherine M. Cook Nannette H. Dasher Kelly T. Durden Dagmar Goley Sandra Grovenstein Robert K. Hamilton Phillip S. Harvey SAVANNAH DIVISION DEGREE TITLE Ph.D. President BS Vice President/Lab Director BS Controller/Secretary/Treasurer Ph.D. Quality Assurance Manager BS Project Manager BS Project Manager BS Project Manager BS Computer Manager BS Air Analysis Manager BS Computer Programmer BS Data Manager MS Field Sampling Manager BS Laboratory Manager BS Corporate Inorganic Manager BS SG Manager BS VG Manager BS Organic Extraction Manager BS VM Manager BS Chemist/Corporate Safety Director BS Chemist Technician Analys t BS Analyst BS Analyst BS Analyst BS Analyst MS Analyst BA Analyst BS Chemist BS SM Supervisor BS Analyst BS Inorganic CLP Coordinator BS SM Supervisor BS Chemist BS Chemist TUT 006 0110 Section 16 Revision: 0 Date: 9/92 SAVANNAH DIVISION (Continued) EMPLOYEE Reginald H. Hendrix Theresa Hornsby Daphne Hughes James Johnson Bernard Kirkland G. Anthony Lowman Carl E. Manning Deborah McDonald Sarah A. McMillan Kimberley D. McNeill Michael W. Mullenix Susan K. Norwood Everett W. Owens J. Robert Paddison, Jr. Ruth D. Rankin Lorene E. Reeves Michelle L. Long Cynthia E. Schlag Charles W. Schuman Elizabeth R. Sicay Julie L. Silvey Angela F. Stewart Melanie T. Walsh Ashton A. Waters Angela M. Weimerskirk Barry L. Williams Millicent A. Williams Laura Willman Jeff Wilmoth Angela Zealy DEGREE TITLE Technician BS Analyst BS Analyst Analyst BS Chemist BS Analyst BS Chemist Analyst BA Analyst BS Analyst Analyst BS Metals ICP/AA Supervisor BS Chemist MS VM Supervisor BS Digestion Supervisor BS Chemist BS Chemist BS Chemist BS Analyst BA Analyst BS Chemist BS Chemist BS Chemist BS Analyst BS General Lab Supervisor BA Analyst BS Analyst BS Chemist BS Analyst BS Chemist TIT, OO6 OJ.J.1 Section 16 Revision: 0 Date: 9/92 EMPLOYEE Thomas L. Stephens Janet B. Pruitt Wayne Word C. Henry Beauchamp Elizabeth L. Schneider Todd A. Baumgartner David A. Karns Bernard Ash Brian Corbin Robert D. Driver Susan Harrison D. Wayne Higgins Mavis LaBounty Andre Miley Richard Orr Tim Preston Paul Rygiel Deborah Sherwin Richard Stephens Martin Thomas Dana B. Till TALLAHASSEE DIVISION DEGREE TITLE BS MS BS BS BS BS BS BS BS BS BS BS BS BS BA BS BS BS BS BS Vice President/Project Manager Lab Director/Project Manager Project Manager Laboratory Manager Quality Assurance Manager Inorganic Section Manager GC/MS Manager Chemist Chemist Analyst Chemist Analys t Analyst Analys t Chemist Chemist Chemist Biological/General Supervisor Volatiles Section Manager Technician Chemist TUT 006 Oil- Section 16 Revision: 0 Date: 9/92 EMPLOYEE Jesse L. Smith James M. Nance, Jr. Michele H. Lersch Van Pham Cora Mae Pate Bruce H. Barrett Rebecca Bowen Panda W. Carter Chris Cook Cedric Crawley Sheryl S. Fuller Stephanie Jones Shao-Wei Li Katherine W. Morgan Edward Oetken Tracy Owens Michael Reardon Sonya Reynolds Letitia Saunders Nan Scarbrough John Shoemaker John Sims David Sweet Rhoda L. Smith Virginia Vasquez Cynthia Wilson Joyce Zatarain MOBILE DIVISION DEGREE TITLE BS Lab Director/Project Manager MS Project Manager BS Quality Assurance Manager Ph.D. Laboratory Manager BS Volatiles Supervisor BS Chemist Ph.D. Analyst/Chemical Hygiene Officer BS Metals Analyst BA Field Manager Technician/Extraction Group Leader BS Chemist BS Field Scientist Ph.D. Chemist BS Sample Coordinator BS Analyst BS Metals Supervisor Technician BS Analyst BA Analyst BS Analyst Technician BS Analyst Technician Data Coordinator BS Chemist BS Chemist Technician TUT OO6 Oil3 Section 16 Revision: 0 Date: 9/92 DEERFIELD BEACH DIVISION EMPLOYEE DEGREE Paul K. Canevaro BS Marianne J. Walker Rhonda Moll BS Kathy C. Irminger BA Phill Taylor, Jr. Kimberly L. Ambrisco-Kostzer BS Linda Backus BS David Graham BA Therona James BA Catherine Katsikis BS Nanette Kendall BA Kirn Puhl BS Eric Schinsing AA Alicia Stewart AA Lawrence Teich BS Mary Valest BS Carol-Ann Vassell BS Janice Wiltshire TITLE Lab Director/Project Manager Sample/Data Manager Project Managaer Quality Assurance Manager Field Coordinator SG Manager Chemist Analyst Chemist Chemist Chemist Chemist Technician Technician Chemist Chemist Chemist Data Coordinator TUT OO6 Oil4 Section 16 Revision: 0 Date: 9/92 EMPLOYEE Kathy Sheffield Andre Rachmaninoff Dominic Fralli Inas M. Sobky Tracy Botto Linda Dowd Chris E. Harris Carl John Hoover, Jr. Cheryl L. Howard Antonius Lebrun Marsha Martinovich Natalie Park Talicia C. Smith Tayseer Zayan TAMPA BAY DIVISION DEGREE TITLE BS Lab Director/Project Manager BA Project Manager MS Project Manager BS Quality Assurance Manager BS Inorganics Section Manager BS Analyst Field Coordinator BS Chemist BA Chemist BS Chemist BA Analyst BS Analyst BS Chemist BS Chemist Resumes of professional personnel are included in the following pages. TUT GO 6 Oil; Section 16 Revision: 0 Date: 9/92 JAMES W. ANDREWS President - Project Manager, Savannah Division Dr. Andrews holds a B.S. degree in chemistry and an M.S. and Ph.D. in nutritional physiology from the University of Georgia. Dr. Andrews' specialty is aquatic chemistry and biochemical and physiological effects of chemicals on animals. In 1962, Dr. Andrews began his professional career as an environmental chemist with the research division of Continental Forest Industries. During this employment, his duties involved developing techniques for reducing water and air pollution from pulp and paper mills and water quality evaluations of streams. From 1963 to 1968, he was a research assistant and lecturer at the University of Georgia. As part of this work, he was assigned to special projects at the Hormel Institute in Austin, Minnesota, and at INCAP in Guatemala City, Guatemala. In 1968, he became one of the initial scientists at the Skidaway Institute of Oceanography in Savannah, Georgia. During his tenure at Skidaway Institute, he was the principal investigator of many biological, physiological and fish cultural studies. Dr. Andrews is the author of more than 70 research papers in the aquatic field. In 1976, he was selected to be a member of a National Academy of Sciences subcommittee on aquatic nutrition. For several years, Dr. Andrews has worked as a volunteer with the Community Cardiovascular Council of Savannah and Dr. Curtis Hames of the Evans Cardiovascular Project. In this capacity, he has become involved in several multi-national research projects which were designed to relate environmental and dietary exposure to cardiovascular health. This work has lead to several scientific publications on the effect of environmental exposure to heavy metals on human health in the high cardiovascular disease area of the southeastern United States. Dr. Andrews has been a private consultant on environmental and water quality aspects of the coastal southeast since 1969. Since 1975, he has been the President of Savannah Laboratories and Environmental Services, Inc. His primary functions at Savannah Laboratories are the evaluation and interpretation of data and responding to the advisory needs of engineers, environmental specialists, legal experts, and production personnel, as well as supervising bioassay/bioaccumulation and environmental studies. TUT 006 01J.6 Section 16 Revision: 0 Date: 9/92 JANETTE D. LONG Vice President - Project Manager/Laboratory Director, Savannah Division Ms. Long has a B.S. degree in chemistry and 16 years experience in the analysis and data review of water, soil, biological and other environmental matrices. Prior to her association with Savannah Laboratories and Environmental Services, Inc., she was a research chemist with the University of Georgia Experiment Station evaluating biological tissues, enzymes and water samples. During her involvement with the Experiment Station, she co-authored several research papers in the aquatic field. For several years, she assisted the Community Cardiovascular Council of Savannah as a volunteer research chemist. During this time, she assisted in the research effort as well as co-authored several publications concerning the epidemiological aspects of heavy metal exposure on human health in the southeastern United States. Ms. Long has been active in the American Chemical Society activities in the environmental area. She has held several offices in the organization, including President of the Coastal Empire Region. Ms. Long began her association with Savannah Laboratories in 1975, and as a project manager, has worked closely with clients to review site-specific project plans, generic QA project plans, project regulatory concerns and to ensure that the analyses recommended will provide the desired data and QA/QC requirements requested by the client. She has been responsible for proposal preparation and project management for numerous RCRA, NPDES, environmental impact assessments and other related projects. TUT OO6 0117 Section 16 Revision: 0 Date: 9/92 STEVEN J. WHITE Project Manager, Savannah Division Mr. White has a B,S. degree in chemistry and seven years of experience with Savannah Laboratories and Environmental Services, Inc. As a project manager, he serves as a point of contact for clients needing technical support in the areas of sampling, analysis, and the evaluation of laboratory results. He has extensive experience in the analysis of environmental pollutants using gas chromatography, GC/MS, and atomic absorption techniques. He possesses comprehensive knowledge of EPA procedures for the determination of pesticides, herbicides, PCBs, PAHs, base/neutral and acid extractable organics in various sample matrices. Prior to his association with Savannah Laboratories in 1984, he pursued graduate studies at the Institute of Paper Chemistry and the University of Georgia. He has participated in EPA-sponsored workshops for pesticide residue analysis and has attended seminars on numerous topics in environmental analysis. Mr. White is an active member of the American Chemical Society. LINDA A. WOLFE Project Manager, Savannah Division Ms. Wolfe has a B.S. degree in chemistry and a B.S. degree in biology with four years laboratory experience in the determination of metals and one year in semivolatiles GC section in the analysis of samples for pesticides, PCBs, and herbicides. Prior to her association with Savannah Laboratories and Environmental Services, Inc., Ms. Wolfe was production specialist and wastewater lab specialist at SCM Corporation for two years. She joined Savannah Laboratories in 1985 as a laboratory metals analyst, and has done extensive work with inductively coupled plasma (ICP) spectroscopy and atomic absorption furnace and flame spectroscopy. Ms. Wolfe is trained in clean room techniques and trace level extractions. She is experienced with all inorganic methods contained in EPA 600/4-79-020, SW-846, and CLP documents. In her current role, Ms. Wolfe provides assistance for clients in areas of analysis and evaluation of laboratory results. TUT OO6 '-'1.3.8 Section 16 Revision: 0 Date: 9/92 BEVERLY HUGHES Project Manager, Savannah Division Ms. Hughes has a B.S. degree in biology/natural sciences and seven years experience in the analysis of environmental pollutants by gas chromatography. Prior to her association with Savannah Laboratories and Environmental Services, Inc. in 1987, she was an environmental specialist at the SCM Corporation. Since joining Savannah Laboratories, Ms. Hughes has worked extensively with semivolatile gas chromatography overseeing pesticides, PCBs, herbicides, and other semivolatile organic compounds. Her work has given her extensive experience with SW-846, 40 CFR, and CLP protocols. In her current role, Ms. Hughes provides assistance to clients in the areas of analysis and evaluation of laboratory results. ALAN BAILEY Laboratory QA Manager, Savannah Division Dr. Bailey holds a B.S. degree in chemistry and biology from the University of Georgia and a Ph.D. in analytical chemistry from Clemson University. Between his undergraduate and graduate studies, he worked as a chemist at Union Carbide Agricultural Products Company. Dr. Bailey's graduate research involved new approaches to the study of chemical exchange across the sediment water interface in both marine and freshwater systems. As a graduate student, he worked two summers in collaborative research in Environmental Research Division at Argonne National Laboratories. Also, while at Clemson, he taught laboratories in freshman chemistry, quantitative analysis, and instrumental analysis, devising and implementing several new experiments for the analytical teaching laboratories. Dr. Bailey is a member of the American Chemical Society and the International Association for Great Lakes Research. Dr. Bailey began his association with Savannah Laboratories in 1989. As manager of the General Laboratory section of the Savannah Division, Dr. Bailey is responsible for personnel management, production, and quality control for a wide variety of analyses. The General Laboratory section includes nutrients, cyanide, microbiological parameters, BOD, COD, TOC, TOX, and many other physical and chemical parameters. Currently, he is QA manager and, among other duties, is responsible for internal systems audits and performance evaluations, certifications, and updates/revisions to Savannah Laboratories' QA plan. Dr. Bailey is a member of the American Chemical Society and the International Association for Great Lakes Research. TUT OO6 O.I. 19 Section 16 Revision: 0 Date: 9/92 DERRICK M. SIMONS Lab Manager, Savannah Division Derrick M. Simons obtained a B.S. degree from the University of Florida in 1982, with majors in both chemistry and microbiology & cell science. While an undergraduate at the University of Florida, Mr. Simons worked as a research assistant in natural products chemistry. From 1982 to 1986, Mr. Simons served as a chemist in a commercial environmental testing laboratory, where his duties included the determination of Pesticides, PCBs, Herbicides, Volatile and Semivolatile Organic Compounds by GC and GC/MS methodologies. Mr. Simons was promoted in 1986 to GC and GC/MS group leader for both Volatile and Semivolatile Organic departments. In 1987, he was promoted to organics lab manager, supervising all GC, GC/MS, and organic extraction personnel where he obtained extensive knowledge of SW-846, 40 CFR, and CLP protocols. Mr. Simons joined Savannah Laboratories in 1990 as Corporate Organic Manager and Savannah Division Organic Manager. His duties included responsibility for GC, GC/MS, and the organic extraction sections. As well, he was responsible for organic analytical method development, overseeing the training of new personnel, and supervising the maintenance and troubleshooting of GC and GC/MS instrumentation. He was promoted to Lab Manager in the summer of 1992. Additional responsibilities of this position include overall administrative responsibility for all technical lab personnel. As Corporate Organic Manager, he is responsible for preparing SOPs, establishing analytical and QA procedures, evaluating instrumentation, and coordinating production among the organic departments. LARRY E. PHILLIPS Corporate Computer Manager, Savannah Division Mr. Phillips attended Armstrong State College where he received a B.S. degree in computer science. He has two years experience with Armstrong State College where he was responsible for maintaining system communications in addition to hardware maintenance and system backups. Mr. Phillips joined Savannah Laboratories and Environmental Services, Inc. in 1988. He is responsible for maintaining all software and hardware associated with Savannah Laboratories' Laboratory Information Management System (LIMS). In addition, Mr. Phillips is responsible for new software development and testing along with maintaining data communications between Savannah Laboratories Corporate Headquarters and Tallahassee, Mobile, Tampa Bay, and Deerfield Beach divisions. TUT OO6 O1.2O Section 16 Revision: 0 Date: 9/92 WAYNE ROB6INS Air Analysis Manager, Savannah Division Mr. Robbins has a B.S. degree in chemistry and has been trained in analytical and quality control techniques for a wide variety of procedures. He is thoroughly familiar with EPA approved procedures and has attended several EPA training schools on analytical techniques. He is currently in charge of implementing protocols for the analysis of ambient air samples and is responsible for coordinating production, preparing SOPs, and evaluating methodology for this section. Mr. Robbins has ten years experience in the analysis of environmental samples by EPA procedures. ERNEST WALTON Corporate Inorganic Manager/Inorganic Manager, Savannah Division Mr. Walton has a B.S. degree in chemistry from Mercer University and began his association with Savannah Laboratories in 1983. His major area of concentration is the analysis of metals in ground water, biological tissues, sediments and estuarine water. He has been trained in clean room sample preparation techniques and has participated in various training courses of metal analysis utilizing inductively coupled plasma spectroscopy and atomic absorption methodology. He also has experience with various automated, semiautomated, and manual nutrient analysis systems. Mr. Walton has been trained in quality control procedures for evaluating laboratory data and has attended the Waste Testing and Quality Assurance symposium in Washington, DC. He was responsible for the initial implementation of CLP protocol for the laboratory's inorganic section. Mr. Walton also pioneered the use of software by the laboratory for the production of CLP deliverables. As well as being thoroughly experienced with CLP protocol, Mr. Walton is knowledgeable in all the inorganic methods contained in EPA 600/4-79-020 and SW-846 documents. As Corporate Inorganic Manager, he is responsible for preparing SOPs, establishing analytical and QA procedures, evaluating instrumentation, and coordinating production among the inorganic departments. TUT GO 6 O121 Section 16 Revision: 0 Date: 9/92 SHEILA B. HOFFMAN Data Manager, Savannah Division Ms. Hoffman has a B.S. degree from Georgia Southern University and began her career with Savannah Laboratories and Environmental Services, Inc. in 1982 as a sample coordinator. She has been responsible for the development of the data management coordination of the laboratory as well as sample custodial responsibilities. Ms. Hoffman coordinates all project orders from the sample login to the computer project login. She interfaces with the clients and project managers to facilitate the data flow through the laboratory and coordinates client sample container requests. Ms. Hoffman has extensive experience with chain of custody for CLP projects and other client specific QA requirements. VIRGINIA BAISDEN Field Sampling Manager, Savannah Division Ms. Baisden has B.S. and M.S. degrees in biology and more than 12 years experience in field sampling and biological and chemical analyses of samples. Prior to her association with Savannah Laboratories and Environmental Services, Inc. in 1986, Ms. Baisden was employed by the Georgia Department of Natural Resources, Coastal Resources Division, where she was project leader of the Commercial Fisheries Program. While associated with the Coastal Resources Division, she authored several reports and publications of fisheries assessment studies. Ms. Baisden has worked with the Game and Fish Division where she identified zooplankton. She was a research assistant for the Environmental Protection Division on an estuarine water quality monitoring project. t Ms. Baisden's primary duties at Savannah Laboratories include responsibility for all biological and microbiological analyses and coordinating and supervising field sampling. TUT OO6 O122 Section 16 Revision: 0 Date: 9/92 MYRON J. YOUNG Volatiles GC/MS Manager, Savannah Division Mr. Young has a B.S. degree in chemistry and an A.S. degree in electronic engineering. Prior to his employment at Savannah Laboratories and Environmental Services, Inc. in 1987, he was employed as a chemist with Southeast Laboratories of Atlanta, Georgia. Mr. Young manages the GC/MS volatiles section at Savannah Laboratories and is responsible for coordinating all QA/QC requirements for that department. He is thoroughly familiar with techniques for performing analyses on many different compounds and the operation of the GC and GC/MS instrumentation used to perform such analyses. He is familiar with SW- 846, 40 CFR, and CLP protocols for data evaluation. KARLA BIER Semivolatiles GC Manager, Savannah Division Ms. Bier has a B.S. degree in chemical engineering and two years experience in the analysis of environmental pollutants by gas chromatography. Prior to her association with Savannah Laboratories, she was a polymer chemistry research assistant at the University of Missouri- Rolla. As manager of the semivolatile GC section of Savannah Laboratories, Ms. Bier has primary responsibility for overseeing the analysis of samples for pesticides, PCBs, herbicides, and other semivolatile organic compounds by GC. In addition, she is responsible for the implementation of new analytical procedures, training new personnel, and supervising maintenance and troubleshooting of semivolatile GC instrumentation. Her duties have given her extensive experience in SW-846, 40 CFR, and CLP protocols for data evaluation. KATHERINE M. COOK Semivolatiles GC/MS Chemist, Savannah Division Ms. Cook has a B.S. degree in chemistry from the University of Georgia and four years of experience in the analysis of organic substances using HPLC, FTIR, GC, and GC/MS methods. Her background includes research and development for a pharmaceutical company, technical and chemical support for law enforcement agencies, and oceanographic research. Ms. Cook began her career with Savannah Laboratories in 1990 as a GC/MS chemist. In this capacity, she is responsible for the operation and maintenance of two RTE/A GC/MS systems and determining the concentration of semivolatile organic compounds in extracts prepared from sample matrices using CLP, 8270, and 625 methodology. 'TUT GO 6 Section 16 Revision: 0 Date: 9/92 KENNETH R. AEGAN Chemist, Savannah Division Mr. Aegan has a B.S. degree in chemistry and an Associates degree in management and logistics from Georgia Southern University. He began his career with Savannah Laboratories in 1987. His work as both GC and GO/MS chemist has provided him with extensive knowledge of SW-846, 40 CFR, and CLP protocols. HSIAO-LAN CHANG Analyst, Savannah Division Ms. Chang received a B.S. in horticulture in 1964 from National Taiwan University and an M.S. in plant sciences in 1972 from the University of Georgia. From 1965 to 1968, Ms. Chang was a research assistant at Taiwan Agricultural Research Institute. From 1968 to 1969, she was laboratory technician for Naval Medical Research in Taipei. Ms. Chang served as a laboratory technician at the U.S. Department of Agriculture's Stored Products Insects Research and Development Laboratory from 1980 to 1982 and again from 1987 to 1989. Ms. Chang joined Savannah Laboratories in 1990 and is currently responsible for TOX determinations. NANNETTE H. DASHER Semivolatiles GC/MS Supervisor, Savannah Division Ms. Dasher has a B.S. degree in chemistry with six years of laboratory experience. She joined Savannah Laboratories and Environmental Services, Inc. in 1985, and gained experience in sample preparation and determination of metals by inductively couples plasma (ICP) spectroscopy and organic sample preparation and analysis by IR and GC. She has performed analyses by GC/MS for three years and is familiar with all SW-846 and CLP methodology. In her current role, Ms. Dasher supervises the analysis of samples for semivolatile organic compounds. She is responsible for the training of new personnel for this section, implementing new analytical procedures, and supervising maintenance and troubleshooting of semivolatile GC/MS ins trumentation. TUT 006 0124 Section 16 Revision: 0 Date: 9/92 KARRI DERR Volatiles GC/Manager, Savannah Division Ms. Derr has a B.S. degree in animal science from Iowa State University. She was a research assistant for two years at Iowa State University Veterinary College, Large Animal Resources division. She began her association with Savannah Laboratories in 1988, at which time she was responsible for performing determinations of metals utilizing inductively coupled plasma (ICP) emission spectroscopy and atomic absorption and flame spectroscopy. Ms. Derr's current responsibilities include personnel, production, and quality control management of a GC/MS volatile group. DAGMAR I. GOLEY Inorganic CLP Coordinator, Savannah Division Ms. Goley has an A.S. degree in chemical technology from Heinrich-Lanz- Schule II, in Mannheim, Germany. She began her association with Savannah Laboratories in 1987, and has gained experience in numerous inorganic preparation procedures. Her duties at Savannah Laboratories include supervising sample preparation for all metals sample determinations and assisting in the computer generation of CLP forms for inorganic data packages. She is trained in total digestion, dissolved sample preparation, and inorganic extraction/concentration procedures as well as proper sample handling. She has been trained in clean room techniques and is familiar with EPA 600/4-79-020 SW-846 and CLP protocols. SANDRA GROVENSTEIN GC/MS Semivolatiles Supervisor, Savannah Division Ms. Grovenstein received her B.S. degree in biology from Auburn University in 1978. She gained extensive experience in toxicology after graduation, working in several hospitals and laboratories. In 1986, she joined Laucks Testing Laboratories in Washington State where she was responsible for analysis and interpretation of GC/MS data relating to CLP 40 CFR and SW- 846 protocols. In 1990, Ms. Grovenstein joined Savannah Laboratories and is responsible for the supervision and analyses of samples and reporting of data for semivolatiles by GC/MS utilizing SW-846, 40 CFR and CLP protocol. TUT OO6 0125 Section 16 Revision: 0 Date: 9/92 SUSAN NORWOOD ICP/AA Production Supervisor, Savannah Division Ms. Norwood has a U.S. degree in chemistry from Armstrong State College and a B.A. degree in marketing from Georgia Southern College. She began work at Savannah Laboratories in 1988 in the inorganic section of the laboratory. After working briefly in the determination of nutrients and general parameters, Ms. Norwood transferred to the metals section where she has worked extensively with both ICP, flame and furnace AA instrumentation. As well, she has been involved with sample preparation procedures for metals determinations. Ms. Norwood is currently responsible for supervision of ICP analyses, associated data handling, and maintenance and troubleshooting for this instrument. She has extensive experience with EPA 600/4-79-020, SW-846, and CLP protocols. 6. ANTHONY LOWMAN Analyst, Savannah Division Mr. Lowman has a B.S. degree in geology from Georgia Southern University. He has worked in the hydrology departments with both the U.S. Army Corps of Engineers and the Georgia Geological Survey and with the Skidaway Institute of Oceanography in Savannah, Georgia conducting research in coastal sedimentology. Mr. Lowman joined Savannah Laboratories and Environmental Services, Inc. in 1989. He performs trace metal analyses of samples utilizing the ICP, Perkin Elmer HGA-400 Graphite Furnace and the SpectrAA-400 Zeeman Spectrophotometer as well as sample preparation by MIBK extraction and analysis, and back up for other trace metal work. He is familiar with EPA 600/4-79-020 and SW-846 and CLP protocols. TUT OO6 O126 Section 16 Revision: 0 Date: 9/92 PAUL E. MEYERS Chemist/Corporate Safety Director, Savannah Division Mr. Meyers obtained his B.S. in chemistry in 1953 from Marshall University. While still in school, he worked as a laboratory technician for Allied Chemical in South Point, Ohio. Within three years of his graduation from Marshall, he held the position of Senior Chemist with Allied. From 1956 to 1969, he was successively plant superintendent, plant manager, and manager of manufacturing for Kaiser Agricultural Chemicals and Southern Nitrogen Company in Savannah, Georgia. His responsibilities at these companies included startup and operation of a fertilizer manufacturing complex. As manager of manufacturing, he was responsible for the manufacturing process at several locations. From 1969 to 1970, he was Vice President of Valley Nitrogen Products in Fresno, California where he was responsible for startup and operation of what at that time was the largest fertilizer manufacturing complex west of the Mississippi River. From 1970 to 1988, Mr. Meyers served as Vice President of System Services and Industrial Corporation where his responsibilities included plant maintenance, engineering, and consulting with clients. In 1988, Mr. Meyers joined Savannah Laboratories. His initial responsibilities provided him with experience in sample preparation for metals determinations and ICP operation. He has worked with and supervised extraction, preconcentration, and other sample preparation techniques for dioxin samples. Mr. Meyers currently is responsible for nutrient analysis employing the TRAACS autoanalyzer system as well as acting Corporate Safety Director for Savannah Laboratories. RUTH D. RANKIN Digest Supervisor, Savannah Division Ms. Rankin has a B.S. degree in biology. She has five years laboratory experience with Southeast Labs in Atlanta, Georgia, where she performed various general chemistry determinations, sample digestions, and metals and mercury determinations by atomic absorption spectroscopy. Ms. Rankin began her career with Savannah Laboratories in 1987. Her duties include supervising the atomic absorption section of the laboratory. She is responsible for organizing the sample load, recording results on the worksheets, and performing analyses using the Perkin Elmer, Jarrell Ash, and Varian atomic absorption spectrophotometers. Her work has provided her with an extensive knowledge of EPA 600.4-79-020, SW-846, and CLP protocols. TUT OO& O127 Section 16 Revision: 0 Date: 9/92 J. ROBERT PADDISON, JR. Volatiles GC/MS Supervisor, Savannah Division Mr. Paddison has a B.S. degree in chemistry from the Georgia Institute of Technology and a M.S. degree in biochemistry from the University of Wisconsin - Madison. He began his association with Savannah Laboratories in 1990. Mr. Paddison started his career at the University of Wisconsin Clinical Cancer Center isolating and quantitating amino biphenyl-DNA adducts using HPLC, LC, and scintillation counting. Most recently, he has worked as an analyst to perform isomer specific quantitation of PCBs in sediment samples from Green Bay, Wisconsin, using GC and GC/MS techniques. This work was conducted in the Water Chemistry Program, U.S. - Madison, as part of the EPA-directed Green Bay Mass Balance Study. Mr. Paddison's current responsibilities at Savannah Laboratories are supervision of a GC/MS volatiles section utilizing 40 CFR, SW-846, and CLP protocols. MICHAEL J. SALUM Organic Extraction Manager, Savannah Division Mr. Salum has a B.S. degree in agronomy with a specialization in soil science from the University of Georgia. Mr. Salum spent over two years as an on-site contractor at the U.S. EPA Region IV Laboratory in Athens, Georgia, performing and supervising semivolatile organic extractions. He was also responsible for the preparation of blind QA samples for all PRP and CLP laboratories in Region IV. His background includes research in soil conversation and soil chemistry at the University of Georgia. Mr. Salum began his association with Savannah Laboratories in 1990 as a GC pesticide residue chemist. He is currently responsible for the operation of the organic extraction/GC screening laboratory. His duties include personnel, production, and quality control management of the extraction lab for all organic parameters. ANGELA F. STEWART Chemist, Savannah Division Ms. Stewart has a B.S. degree in chemistry from Armstrong State College. She joined Savannah Laboratories in 1989. She initially worked in the extraction and concentration of samples for semivolatile GC/MS analysis. Ms. Stewart is currently responsible for the determination of semivolatile organic compounds by GC/MS. Her work has provided her with extensive experience employing SW-846, 40 CFR, and CLP protocols. TUT OO6 O128 Section 16 Revision: 0 Date: 9/92 ANGELA M. WEIMERSKIRK General Laboratory Supervisor, Savannah Division Ms. Weimerskirk has a B.S. degree in chemistry. She began her career with Savannah Laboratories in 1986, at which time she was responsible for the determination of trace metals by ICP and the determination of mercury by cold vapor AAS. She has extensive experience in ion selective electrode determinations of fluoride, ammonia, and TKN, and several years experience with the determination of ions utilizing ion chromatography. Ms. Weimerskirk is responsible for the organization, coordination, and operation of the Traacs 800 autoanalyzer, the ion chromatograph, and ion selective electrode instrumentation section of the laboratory. She has been involved in method development of cyanide and phenolics by autodistillation/autoanalysis. In addition, her work has improved the efficiency and accuracy of sulfide determinations. She is familiar with EPA 600/4-79-020, SW-846, and CLP protocols. ANGELA ZEALY Chemist, Savannah Division Ms. Zealy has a B.S. degree from Armstrong State College with a major in biology and a minor in chemistry. She joined Savannah Laboratories in 1988. Ms. Zealy began her tenure with Savannah Laboratories performing microbiological determinations. Since that time, she has gained extensive experience in the extraction, clean-up, dilution, and preconcentration of samples for the determination of pesticides, herbicides, and PCBs. Her current position is GC chemist in the semivolatiles section of Savannah Laboratories. Ms. Zealy's responsibilities include GC/FID determination of phenolic compounds, phthalate esters, and PAH compounds. In addition, she is experienced in petroleum product identifications. Her work has given her experience with both SW-846 and 40 CFR methodologies. TL(T 006 0129 Section 16 Revision: 0 Date: 9/92 THOMAS L. STEPHENS Vice President/Project Manager, Tallahassee Division Mr. Stephens has a B.S. degree in chemistry and 20 years experience in analyses of pollutants in groundwater, sediments, tissues, agricultural products, wastewater, drinking water and hazardous wastes utilizing GC, GC/MS and HPLC analytical techniques. Prior to his association with Savannah Laboratories in 1985, he was supervisor of the organic section of the Florida Department of Environmental Regulation (DER) laboratory in Tallahassee and supervisor of the Florida Department of Agriculture Pesticide Residue Laboratory. In these capacities, he has gained an enormous amount of experience in laboratory management, quality assurance, method development, mass spectrometry interpretation and verification of results. He has attended several regulatory training schools and presented technical presentationsa at several pesticide residue conferences and regional meetings in the southeast. Mr. Stephens is thoroughly familiar with DER specific regulatory sampling procedures, analytical quality assurance and reporting requirements for hazardous and solid waste, air quality, groundwater, wastewater, and drinking water. His technical background enables him to provide accurate and cost effective assistance for the environmental and regulatory needs of Florida clients. He is a member of the Florida Society of Environmental Analysts, the Florida Association of Environmental Professionals, the Florida Environmental Auditors Association, and the Florida Air and Waste Management Association. TUT 006 0130 Section 16 Revision: 0 Date: 9/92 JANET PRUITT Laboratory Director/Project Manager, Tallahassee Division Ms. Pruitt has a B.S. degree in chemistry and a Master of Public Health degree. Her 25 years experience in the environmental field began with the South Carolina Department of Health and Environmental Control (SCDHEC) where she supervised the Environmental Chemistry Section. After nearly thirteen years with SCDHEC, she joined the United States Geological Survey (USGS) National Water Quality Laboratory in Atlanta, Georgia. At the USGS laboratory, she was responsible for the analyses of water, sediment, and fish tissues for various organic parameters utilizing gas chromatography, mass spectrometry and computer data systems. She also served as quality assurance officer for the organic chemistry section. In 1984, Ms. Pruitt transferred to the Tallahassee office of USGS where she was responsible for appraising water resources and providing basic hydrologic data on both surface and ground water in Florida. She was project chief of three investigative hydrologic studies, assisted with three water quality studies, and coauthored an indexing and classification system for earth-science data bases. She also served as technical advisor in the field of analytical organic chemistry for district, regional and headquarters personnel in the Water Resources Division. Ms. Pruitt joined Savannah Laboratories in 1987 as laboratory manager/QA manager. In her current position as laboratory director/project manager, she is responsible for the operation of the Tallahassee Division, and provides clients with assistance in field and analytical requirements. TUT OO6 O131 Section 16 Revision: 0 Date: 9/92 WAYNE WORD Project Manager, Tallahassee Division Mr. Word has a B.S. degree in chemistry and 16 years experience in the environmental field. He began his career with Technical Services, Inc. (TSI) in Jacksonville, Florida, where he was organics department manager responsible for general analysis and performing and instituting instrumental methods for new clients. After 10 years with TSI, Mr. Word joined OHM Corporation where he began as a project chemist and worked his way up to laboratory manager within four years. Mr. Word has experience in most major analytical techniques including: GC, GC/MS, HPLC, FTIR, UV/VIS, TOG, TOX, ICP, AA, and manual and automated potentiometric and spectrophotometric methods. He also has extensive experience with SW-846 and EPA approved methods. In addition, Mr. Word has received specialized training from Hewlett-Packard, Varian Associates, Jarrell-Ash, Perkin Elmer, and the American Chemical Society on instrumental and management techniques. Mr. Word joined Savannah Laboratories as project manager. In this position, he is able to provide technical assistance and support to clients for field and analytical services. HENRY BEAUCHAMP Laboratory Manager, Tallahassee Division Mr. Beauchamp holds a B.S. degree in chemistry from the University of Florida and has completed postgraduate course work in biochemistry. Prior to his association with Savannah Laboratories in 1989, he worked for the Florida Department of Agriculture and the University of Florida in biochemical laboratory analysis. Mr. Beauchamp has supervised all volatile organic compound determinations by GC and GC/MS, and has been actively involved in GC/MS analysis, spectral interpretation, data reporting, and instrument maintenance. In his current role at Savannah Laboratories, Mr. Beauchamp is responsible for the management of technical personnel, overseeing all method development and adherence to the Comprehensive QA Plan, coordinating all analyses with section managers, as well as handling all requests for laboratory supplies and instrument repairs. TUT OO6 Section 16 Revision: 0 Date: 9/92 ELIZABETH SCHNEIDER Quality Assurance Manager, Tallahassee Division Ms. Schneider has a B.S. degree in biology and over 17 years experience with gas chromatography and high performance liquid chromatography analyses. At Savannah Laboratories, Ms. Schneider is responsible for ensuring that method QA requirements are met, issuing and evaluating in- house check samples, and analyst training in safety, QA procedures, and analytical methodology. Ms. Schneider has a thorough knowledge of QA requirements, procedures, and evaluation as they apply to EPA-approved methodology. She is responsible for research into new methodologies and has developed several procedures now in use at Savannah Laboratories. She also supervises analyses of ordinance and explosives according to USATHAMA methods. Prior to her association with Savannah Laboratories in 1987, Ms. Schneider was lead technician in the quality assurance department for the Olin Corporation. There she supervised a staff of professionals in areas such as chemical, raw materials, water and waste treatment, ballistics and instrumental training. She is highly skilled in the operation and repair of gas chromatographs and high performance liquid chromatography systems. DANA TILL Chemist, Tallahassee Division Ms. Till holds a B.S. degree in chemistry from Pembroke (NC) State University. Prior to coming to Savannah Laboratories, she was employed by the City of Raeford and Berry College. During her employment with the City of Raeford, Ms. Till was responsible for the supervision of all daily laboratory activities, training of laboratory personnel, purchasing of equipment for the plant and laboratory, and performing wastewater analysis. She established a quality assurance program to test laboratory procedures, techniques, and methodology. She also was responsible for bringing the wastewater treatment laboratory into compliance with the State of North Carolina's standards, as well as publishing an operations manual for the laboratory. Her current responsibilities at Savannah Laboratories include the analysis of samples for polynuclear aromatic hydrocarbons and pesticides by GC. BERNARD ASH Chemist, Tallahassee Division Mr. Ash has a B.S. degree in chemistry from Florida A&M University and has completed Medical Laboratory Specialist Training in the U.S. Air Force. Prior to joining Savannah Laboratories, he was employed as a medical technologist in the Air Force as well as with Gadsden Memorial Hospital and Tallahassee Memorial Regional Medical Center. Mr. Ash's duties at Savannah Laboratories include performing analyses of metals in environmental matrices employing ICP and AA furnace techniques. Section 16 Revision: 0 Date: 9/92 TODD BADMGARTNER Inorganic Section Manager, Tallahassee Division Mr. Baumgartner holds a B.S. degree in chemistry and has completed one year of postgraduate course work. He began his career with Savannah Laboratories in 1985. His training since joining Savannah Laboratories has been broad, encompassing sampling as well as nutrient, volatile, organic compounds, and metal determinations. Mr. Baumgartner's current duties as manager of the inorganic section include overseeing all aspects of analysis from digestion to data reporting for metals, general (wet chemistry), and bacteriological parameters. He is responsible for ensuring adherence to QC procedures and method requirements, instrument troubleshooting and maintenance, and ordering of lab supplies. He is especially experienced in metal determination by ICP, furnace AA, and cold vapor AA. ROBERT D. DRIVER Analyst, Tallahassee Division Mr. Driver has a B.S. degree in business administration and two years experience as a laboratory analyst. He has experience over a wide variety of chemical analyses including general chemistry, bacteriology, extractions, metals, IR, and digestion. Currently, Mr. Driver's primary responsibility is HPLC analyses of pesticides and related compounds. D. WAYNE BIGGINS Analyst, Tallahassee Division Mr. Higgins has a B.S. degree in nutritional science with a minor in chemistry from Florida State University. Prior to coming to Savannah Laboratories, he was employed by Florida State University Chemistry Department. Mr. Higgin's duties include the analysis of samples for metals by ICP and furnace AA methodologies. He also checks data entered on worksheets for his section making sure QA/QC requirements are met and all data is entered correctly. TUT OO6 O134 Section 16 Revision: 0 Date: 9/92 DAVID KARNS Semivolatiles Organic Manager, Tallahassee Division Mr. Karns holds a B.S. degree in chemistry from the University of South Florida. His experience includes analysis of semivolatile organic compounds by GC/MS, spectral interpretation, and adherence to SW-846, 40 CFR, and CLP methodologies. Mr. Karns' has extensive knowledge of semivolatile method requirements, data reporting, and QC requirements. His duties as manager consist of installing new software updates on Hewlett-Packard GC/MS systems, advising and training on all systems, scheduling workloads, maintaining and troubleshooting instruments, and providing technical information to the laboratory director regarding new instrumentation and method requirements. Mr. Karns is experienced in review of CLP data packages. JOSEPH B. NORTH Analyst, Tallahassee Division Mr. North holds a B.S. degree in biology from Florida State University. Prior to his employment with Savannah Laboratories, he " worked for Environmental Planning and Analysis, Inc. as a laboratory technician. Mr. North's duties include the analysis of samples for biological parameters, including BOD, COD, bacteria, and other biological laboratory duties. TIMOTHY PRESTON Chemist, Tallahassee Division Mr. Preston holds a B.S. degree in chemistry with a minor in mathematics from Florida State University and also has an AA degree in liberal arts from Miami-Dade Community College. He is a member of Alpha Chi Sigma Chemistry fraternity. Mr. Preston is a GC/MS chemist and is responsible for analyzing environmental samples for volatile organic compounds using packed and capillary column GC/MS. He is also responsible for the review and interpretation of spectral data and review and analysis of CLP data packages. TUT 006 01 ••-• Section 16 Revision: 0 Date: 9/92 PAUL RYGIEL HPLC/IR Manager, Tallahassee Division Mr. Rygiel has a B.A. degree in biochemistry from Florida State University. Prior to joining Savannah Laboratories, he was employed as a chemist at the Florida Department of Business Regulation where he gained two years experience in gas and liquid chromatography. Mr Rygiel's current responsibilities include overseeing the analysis of soil and water samples by EPA methods 632, 531, 8320, and other methods for explosives, formaldehyde, and water soluble pesticides and herbicides by HPLC, and the IR analysis of soil and water samples for oil and grease and total petroleum hydrocarbons. DEBORAH SHERWIN Biological/General Lab Supervisor, Tallahassee Division Ms. Sherwin is a graduate of Florida State University where she obtained a B.S. degree in biological science. Her educational background includes completion of the Liberal Studies Honors program and memberships in Phi Eta Sigma National Honor Society and Golden Key National Honor Society. Ms. Sherwin joined Savannah Laboratories as an analyst in the Biological/General Lab section. Her current duties as supervisor include analysis and supervision in all areas of bacteriology and general chemistry. She is involved in analyses of coliforms, titrations, BODs, solids determinations, and determinations of physical parameters using EPA approved methodologies. RICHARD A. STEPHENS Volatiles Organics Manager, Tallahassee Division Mr. Stephens holds a B.S. degree and Postgraduate Certificate of Education from the University of Wales. His studies were in biology and zoology, and prior to his employment at Savannah Laboratories, he was a science educator. Mr. Stephens' duties at Savannah Laboratories include supervision of analyses by GC and GC/MS of volatile organic compounds, data interpretation and reporting, instrument maintenance and troubleshooting, review of CLP data packages, and ordering of gases and lab supplies for the volatiles section. TUT OO6 O136 Section 16 Revision: 0 Date: 9/92 MARTIN THOMAS Technician, Tallahassee Division Mr. Thomas came to Savannah Laboratories with more than 16 years experience. His duties at Savannah Laboratories have included supervision of the extraction laboratory as well as performance of extractions for all organic parameters. He has also been responsible for analysis of samples for petroleum hydrocarbons by IR techniques. At the present time, he analyzes all water samples for EDB following EPA methodology. TUT OO6 O137 Section 16 Revision: 0 Date: 9/92 JESSE L. SMITH Laboratory Director/Project Manager, Mobile Division Mr. Smith has a B.S. degree and has successfully completed the majority of graduate course work in a masters program in chemistry. Mr. Smith is the laboratory director of Savannah Laboratories, Mobile, Alabama Division and is responsible for overall management of this laboratory. He supervises project managers, QA and department managers, and ensures departments have adequate laboratory equipment and personnel to perform their jobs. He provides oversight in developing new laboratory methods and analytical techniques to meet client needs as regulatory programs change. Mr. Smith also functions as project manager and is the primary contact for his clients. He is responsible for assisting clients with pre-sampling discussions, suggesting analytical approaches, meeting regulatory agency requirements, and developing special analytical and treatability techniques. He is thoroughly familiar with EPA methods and QA/QC requirements for RCRA, NPDES, SDWA, and other EPA regulatory programs. Mr. Smith is an active member of the American Chemical Society and has attended ACS-sponsored courses in gas chromatography and atomic absorption spectroscopy. He has attended numerous continuing education courses covering new EPA regulatory programs. Mr. Smith joined Savannah Laboratories and Environmental Services, Inc. in 1987, as a project manager and was promoted to laboratory director of the Mobile, Alabama Division when it opened in 1988. Prior to joining Savannah Laboratories, he had fifteen years consulting laboratory experience as a bench chemist, supervisor, and laboratory manager for Southeast Laboratories, Inc. in Atlanta, Georgia. He has extensive experience in gas chromatography analysis of pesticide residue/PCBs and volatiles, metals by atomic absorption spectroscopy including graphite furnace analyses, and general chemistry laboratory experience. He has a broad base of experience in a variety of analytical chemistry and microbiological methods including: EPA, ASTM, NIOSH, AOAC, PDA, and USDA. TUT oo6 O13S Section 16 Revision: 0 Date: 9/92 J. MICHAEL NANCE Project Manager, Mobile Division Mr. Nance has a B.S. degree from the University of North Alabama and an M.S. degree in environmental science from the University of South Alabama. Mr. Nance's primary responsibility with Savannah Laboratories is project management of permitted wastewater and drinking water and RCRA projects as required by EPA and state regulatory programs. Mr. Nance provides oversight and supervises the field activities of the Mobile Division sampling team. He is highly skilled at coordinating and conducting field investigations. Mr. Nance has kept current with changes and refinements in existing regulatory programs through continuing education courses in Hazardous Waste/Land Disposal Bans, Reauthorized RCRA, Superfund (SARA), and NPDES storm water regulations. He has completed the forty-hour "Hazardous Assessment and Response Management" training program (20 CFR 1910.120). This certification is kept current through annual update courses. Mr. Nance has seventeen years experience in a wide variety of industrial laboratory and field investigations. Project experience includes: hazardous waste characterization, sediment and water quality studies, remedial investigations, and groundwater monitoring projects. TUT OO6 0139 Section 16 Revision: 0 Date: 9/92 MICHELE H. LERSCH Laboratory QA Manager, Mobile Division Ms. Lersch has a B.S. degree in medical technology with concentrations in chemistry and microbiology from the University of South Alabama. She has taken postgraduate courses in management and business law. Ms. Lersch is responsible for managing the quality assurance program for the Mobile Division laboratory. She initiates certifications with state and federal agencies, renews certifications, conducts internal audits, works with external auditors, edits QA plans and SOPs, and reviews project files. Her duties include initiating and maintaining training files for the technical staff and maintaining technical information resources and methods. Prior to her employment with Savannah Laboratories, Ms. Lersch was employed as metals analyst with Thompson Engineering Testing. She specialized in trace metals determinations using flame and graphite furnace AAS techniques. She also became experienced in inorganic analyses using wet chemical methods. When Ms. Lersch joined Savannah Laboratories in 1988, she was promoted to Inorganic Laboratory Manager. She gained extensive experience using inductively coupled plasma (ICP) techniques for metals determinations. She was responsible for instrument maintenance and trouble-shooting as well as day-to-day implementation of QC for the inorganic section. She became thoroughly familiar with EPA methods and reporting and QC requirements for environmental samples requiring metals and wet chemistry analyses. Ms. Lersch has ten years of laboratory experience, seven of which have been directly related to the chemical and biological analysis of water, wastewater, soils/sediments, and hazardous waste samples. She is familiar with SW-846 and 40 CFR methods, protocols, and QC requirements for both organic and inorganic analysis. OO6 OJL4O Section 16 Revision: 0 Date: 9/92 VAN PHAM Laboratory Manager, Mobile Division Dr. Pham has a Ph.D. in organic chemistry from Georgia Institute of Technology and a B.S. degree in chemistry from Saigon University. Dr. Pham joined Savannah Laboratories in 1990 as a GC/MS chemist. She was responsible for the analysis of base/neutral and acid semivolatile organics in environmental samples. In 1991, Dr. Pham was promoted to department manager and QC coordinator of the organic and extraction sections and to laboratory manager in 1992. She is responsible for the organic analytical method development, supervising, training new personnel, and maintaining and troubleshooting the GC/MS, GC, IR, ICP and AA/GF instruments. Dr. Pham is an active member of the American Chemical Society. She has attended several ACS-sponsored seminars on a variety of topics including GC and GC/MS techniques and methods. She took the quality assurance course offered by the EPA as part of its Seventh Annual Waste Testing and Quality Assurance Symposium held in Washington, D.C. Prior to joining Savannah Laboratories, Dr. Pham was employed with Eagle- Picher Environmental Service. She.performed a variety of organic and air pollutant analyses for volatile compounds, pesticides, herbicides, PCBs, PAHs, phenols, and dioxins. From 1987 to 1989, Dr. Pham was a postdoctoral associate with the University of Georgia, Department of Chemistry. She worked on enzymatic synthesis and reaction, and authored and co-authored a number of publications in the Journal of the American Chemical Society. Dr. Pham has extensive knowledge of EPA SW-846, 40 CFR, NIOSH, and ASTM methods and CLP protocols. She has several years of experience working with GC, GC/MS, FT-NMR, UV-VIS spectroscopy, and HPLC instruments. She is familiar with several instrument data systems including PE-Nelson, Maxima 280, and ChemStation. She is well-versed in the use of Lotus 1-2-3 and Quatropro as part of the organic lab information management systems. TUT OO6 O.141 Section 16 Revision: 0 Date: 9/92 CORA M. PATE Volatiles Manager, Mobile Division Ms. Pate has a B.S. degree in biology and a minor in chemistry from the University of South Alabama. Ms. Pate is responsible for supervising the volatiles laboratory. Her duties include training analysts, instrument maintenance and data review as well as the analysis of environmental samples for volatile organic compounds by GC/MS according to EPA methods 624 and 8240. Ms. Pate has previously analyzed volatile organic compounds by gas chromatography using Hall, Photo lonization (PID), and Flame lonization (FID) detectors according to EPA methods 501.1, 502.2, 601/602, and SW-846 8010/8020. She interprets chromatograms, calculates and reports results and checks QC on these instruments. Ms. Pate has attended seminars and courses on gas chromatography involving column maintenance and operation according to new methods and techniques. Ms. Pate previously worked as an office manager before obtaining her degree. Her duties included training and maintaining the office staff as well as being a personal assistant to the company president. She was responsible for implementing new computer programs and updating and efficiently utilizing existing programs and hardware. Ms. Pate has three years experience in an analytical and consulting laboratory atmosphere with two years of this in a supervisory position. She is familiar with SW-846 and 40 CFR methods, protocols, and QC requirements for the volatiles GC section. TUT OO6 O14; Section 16 Revision: 0 Date: 9/92 BRUCE H. BARRETT Chemist, Mobile Division Mr. Barrett has a B.S. degree in chemistry from Wittenberg University in Springfield, Ohio. He has done biochemical research of photophosphorylaton mechanisms in single celled algae at Kettering Memorial Laboratories in Yellow Springs, Ohio. Mr. Barrett joined Savannah Laboratories in 1990 as a chemist in the general laboratory. He is the senior level chemist for this department and performs cyanide, nutrient, titrimetric and demand analyses. Mr. Barrett possesses considerable problem solving skills for troubleshooting methods and dealing with difficult sample matrices. He is well versed in computer programming and practical computer applications. Mr. Barrett previously worked as a research lab technician with the Institute of Paper Chemistry studying reaction experiments on terpene hydrocarbons using gas-liquid chromatography and IR and NMR. He worked four years as senior chemist for Ventron Corporation troubleshooting products. He spent four years working for Lincoln Pulp and Paper as technical director and six years in the same capacity at Boise Cascade Corporation. As technical director, he was responsible for environmental and water plant operations as well as quality control of pulp and paper. Mr. Barrett has twenty-five years of analytical experience in industrial, environmental, and chemical analyses. He is thoroughly familiar with EPA, ASTM, TAPPI, and NIOSH methods for wet chemical testing of a variety of sample matrices including: waters, wastewaters, soils/sediments, and hazardous waste. TUT 006 0143 Section 16 Revision: 0 Date: 9/92 REBECCA BOWEN Analyst, Chemical Hygiene Officer, Mobile Division Dr. Bowen received a B.S. degree in biology in 1979 and a Ph.D. degree in basic medical sciences in 1989 from the University of South Alabama. As the Chemical Hygiene Officer, Dr. Bowen is responsible for training and educating employees about safety rules and regulations. She enforces the company safety policies and ensures that the laboratory chemical hygiene plan complies with OSHA guidelines. Additionally, Dr. Bowen is the primary analyst for determining pesticide residues, herbicides, and PCBs in extracted samples using GC-ECD techniques. Prior to employment with Savannah Laboratories, Dr. Bowen performed post- doctoral research at MacMaster University in Hamilton, Ontario. Her research involved investigating the pharmacological influences of prostaglandin and cyclic nucleotide metabolism on blood platelets in human tumor cells. She has several publications relating to her research in medical and other scientific journals. Dr. Bowen has one year of environmental laboratory experience. She is familiar with SW-846, 40 CFR Part 136, and SDWA protocols for the parameters for which she is responsible. PANDA CARTER Analyst, Mobile Division Ms. Carter has a B.S. degree in biology with a minor in chemistry from the University of South Alabama. Ms. Carter joined Savannah Laboratories in 1991. Her primary responsibilities include sample analyses by ICP, flame, GFAA, and cold vapor/hydride generation atomic absorption techniques. Ms. Carter has 12 years experience in atomic absorption spectroscopy and various wet chemistry techniques from past employment with Union Carbide Corporation and Protein Technologies International. She is thoroughly familiar with EPA-600 and SW-846 sample preparation and analytical methods for drinking waters, wastewaters, soils/sediments, hazardous waste samples, and TCLP extracts as well as the associated QC requirement. TUT <X>6 O144 Section 16 Revision: 0 Date: 9/92 CHRISTOPHER A. COOK Field Manager, Mobile Division Mr. Cook received a B.A. degree in biology from Clemson University in May, 1990. His primary responsibilities with Savannah Laboratories is scheduling field activities, coordinating field logistics for environmental programs and the field team leader for sampling events. Mr. Cook joined Savannah Laboratories in 1990, and has developed operating procedures which have satisfied the scrutiny of federal and state regulatory agencies performing on-site audits. Mr. Cook is skilled in providing field support for water quality programs, groundwater monitoring, solid/hazardous waste characterization, air monitoring for personnel exposure and other environmental programs. Mr. Cook has completed the forty hours "Hazardous Assessment and Response Management" training course to meet the requirements of 20 CFR 1910.120. CEDRIC CRAWLEY Technician/Extraction Lab Group Leader, Mobile Division Mr. Crawley has completed course work toward a degree in computer science. As extractions lab group leader, Mr. Crawley is responsible for scheduling the organic extractions of BNAs, herbicides, pesticides, PCBs, phenols, phthalates, and PAHs from drinking waters, wastewaters, solids/sediments, and TCLP extracts for analysis by GC and GC/MS. He performs analysis of oil and grease and petroleum hydrocarbons by gravimetric and infrared techniques, and total phenolics and MBAS using organic extraction/spectrophotometric techniques. Mr. Crawley's previous laboratory experience includes field sampling and analysis. He was responsible for sampling of NPDES projects and analysis of such parameters as D.O., conductivity, residual chlorine, turbidity, and pH. Mr. Crawley has three years of environmental laboratory experience, one of which has been in a group leader role. He is familiar with SW-846 and 40 CFR Part 136 methods, protocols, and associated QC requirements for semivolatile organic extractions. TU r OO6 O145 Section 16 Revision: 0 Date: 9/92 SHERYL S. FULLER Chemist, Mobile Division Ms. Fuller has a B.S. degree in chemistry from Stillman College. She has three years of analytical laboratory experience in the analysis of nutrients in waters, wastewaters, soils and sediment samples. She is also experienced in teh analysis of cyanides in a variety of sample matrices. Since joining Savannah Laboratories in 1989, Ms. Fuller has gained extensive experience using wet chemical and spectrophotometric methods and ion specific electrodes. She is currently specializing in the determination of demand analyses and phosphorous in waters, wastewaters, soils and sediments. Ms. Fuller is thoroughly familiar with EPA methodologies for wet chemistry testing and the associated QC requirements. STEPHANIE H. JONES Field Scientist, Mobile Division Ms. Jones has a B.S. degree in geology from the University of South Alabama. She joined Savannah Laboratories' field sampling department in 1991 as a trainee, bringing with her an extensive background in field sampling and analytical techniques. Ms. Jones has been involved in several major sampling projects for drinking water, groundwater, stormwater, soil/sediment and hazardous waste samples. She has worked with clients in establishing sampling programs and writing SOPs. Ms. Jones is thoroughly familiar with SW-846 sampling protocols, and is able to apply her extensive practical experience to any special sampling techniques as required. TllT 006 Section 16 Revision: 0 Date: 9/92 SHAU-WEI LI Chemist, Mobile Division Dr. Li received her Ph.D. in 1989 and M.S. in 1986 in organic chemistry from Shanghai Institute of Organic Chemistry, Shanghai, China. She received her B.S. degree in chemistry from the Zhe-Tsian University in 1983. Dr. Li joined Savannah Laboratories in 1991 as a pesticide residue chemist in the semivolatile gas chromatography (GC) laboratory. She is responsible for the analysis of pesticides/PCBs, PAHs, phenols and microextractable compounds in environmental samples, she is familiar with the operation of GCs equipped with electron capture, flame ionization, nitrogen-phosphorous detectors using capillary and packed columns, she is familiar with the Nelson and Hewlett Packard computerized data management system to collect and process analytical data. Dr. Li has attended seminars and courses on gas chromatography involving column maintenance and operation according to new methods and techniques. She regularly attends the Gulf Coast Chromatographers Discussion Group meetings. Prior to joining Savannah Laboratories, Dr. Li was a post-doctoral research associate for one year with the University of South Alabama Chemistry Department, she conducted research in the chemical synthesis of naturally occurring antibiotics. Dr. Li is thoroughly familiar with the GC methods regarding sample preparation and analytical methods for drinking water, wastewater, soils/sediments, hazardous waste samples and TCLP extract analyses, she has extensive knowledge of EPA SW-846, 40 CFR Part 136 protocols and associated QC requirements. TUT OO6 O147 Section 16 Revision: 0 Date: 9/92 KATHERINE WYNN MORGAN Sample Coordinator, Mobile Division Ms. Morgan has completed several courses toward a B.S. degree in chemistry. She is currently enrolled at the Faulkner State University and working toward completion of that degree. Ms. Morgan's duties at Savannah Laboratories include filling client requests for sample bottles, resolving discrepancies in requests for analysis at sample receipt, and disposing of samples when analysis and reporting are complete. She coordinates all project orders from sample login to computer login and interfaces with the clients and project managers to facilitate the sample flow through the laboratory. In addition, she is responsible for ordering and receiving supplies and materials for the laboratory. Prior to her employment with Savannah Laboratories in 1988, she worked in the petrochemical industry. As a laboratory technician, she performed chemical analysis of petrochemical products. She also developed skills such as data recording on a computer data system, interacting with clients, packaging and mailing restricted articles, and purchasing/receiving for the laboratory. Ms. Morgan has eight years of laboratory bench experience. She has extensive knowledge of field sampling procedures and packaging and transporting requirements of a variety of chemicals. Ms. Morgan is familiar with the laboratory information management system of Savannah Laboratories. She is available to assist clients with scheduling bottle order shipments and receipt of samples in the laboratory. EDWARD OETKEN Metals Digestion Coordinator, Mobile Division Mr. Oetken has a B.S. degree in biomedical sciences with a chemistry minor from the University of South Alabama. At Savannah Laboratories, Mr. Oetken supervises all digestion procedures and sample receipts in the metals section. In this role, he has acquired knowledge of laboratory techniques and become familiar with SW-846 and EPA 600 protocols. TUT 006 0148 Section 16 Revision: 0 Date: 9/92 TRACY S. OWENS Metals Supervisor, Mobile Division Ms. Owens has a B.S. degree in environmental sciences from Troy State University. She joined Savannah Laboratories in 1990, and has specialized in the determination of trace metals analysis using inductively coupled plasma (ICP), flame, cold vapor, hydride generation and graphite furnace atomic absorption spectroscopy techniques. Ms. Owens was promoted to metals lab supervisor in 1992. she is responsible for scheduling digestion and analysis for drinking water, waste water, soil/sediment, hazardous waste and TCLP projects. she ensures that proper preparation and analysis techniques are followed and method QC requirements are met. Ms. Owens oversees instrument maintenance and troubleshooting for the metals department. Ms. Owens has three years experience in the laboratory. She is familiar with EPA SW-846 and Title 40 Part 136 test method and associated QC requirements. SONYA REYNOLDS Inorganics Group Leader, Mobile Division Ms. Reynolds has a B.S. degree in biology and environmental science from Livingston University. She was a founding member of the L.U. Conservacy group and is active in promoting environmental awareness. Since joining Savannah Laboratories in 1991, she has gained extensive knowledge of EPA methodologies for demand, nutrient, and general wet chemical analyses. She is familiar with SW-846, Standard Methods, and EPA 600 series methods of analysis for waters, wastewater, soil/sediment, and hazardous waste samples as well as the associated QC requirements. Ms. Reynolds is responsible for analysis of TOG and COD, coliforms by both membrane filtration and multiple tube techniques, sulfides, and chlorides. She also oversees the analytical work of several other analysts and troubleshoots problems with data and QC. TUT i in A -6 0149 Section 16 Revision: 0 Date: 9/92 LETITIA SAUNDERS Analyst, Mobile Division Ms. Saunders has a B.A. degree in biology from Berea College. She has completed two years of study toward a degree in dentistry at the University of Kentucky. She joined Savannah Laboratories in 1991 as a nutrients analyst. In this position, she was responsible for the determination of TKN, NH3, N03, and N02 in waters, wastewaters, soils, and sediments. She is familiar with EPA-600 wet chemistry methodologies and associated QC requirements. Ms. Saunders has moved to the volatiles laboratory and is responsible for the analysis of environmental samples for volatile organic compounds by gas chromatography using Hall and Photo lonization (PID) detectors according to EPA mehtods 501.1, 502.2, 601/602. and SW-846 8010/8020. She interprets chromatograms, calculates and reports results, and checks QC for these instruments. Prior to joining Savannah Laboratories, Ms. Saunders was a research technologist at the University of South Alabama. She is experienced in the use of a variety of spectrophotometric equipment and is familiar with HPLC and column chromatography techniques. NAN SCARBROUGH Analyst, Mobile Division Ms. Scarbrough received a B.S. degree in wildlife biology from Livingston University. She also holds a Master of Education degree from Livingston University. Her primary responsibility at Savannah Laboratories is analyses of cyanide in waters, wastewaters, soils/sediments, and hazardous waste samples. Prior to joining Savannah Laboratories in 1991, Ms. Scarbrough worked as a lab technician for the Alabama Co-op Fish and Wildlife Research Unit performing habitat mapping and collection and identification of fish. She also has experience in bioassay analysis from her employment as an aquaculture specialist with TAI Environmental Sciences, Inc. Ms. Scarbrough has two years of laboratory experience. She is familiar with SW-846 and EPA-600 methods for cyanide analyses on a variety of sample matrices. TUT O06 015O Section 16 Revision: 0 Date: 9/92 JOHN SIMS Analyst, Mobile Division Mr. Sims has a B.S. degree in physics with a minor in computer science from Alabama State University. He joined Savannah Laboratories in 1991 as an analyst with the responsibility of extracting both volatile and non- volatile TCLP samples. Mr. Sims is currently responsible for the analysis of semivolatile extractable organics, primarily phenols, PAHs, and phthalate esters, by GC-FID methods. He is trained in both 40 CFR and SW-846 methods and QC requirements. Prior to joining Savannah Laboratories, Mr. Sims worked as a lab technician in the biomedical research department at Alabama State University. He also co-authored four publications regarding PIXIE analysis techniques for analyzing environmental samples. He has also worked as a computer programmer with Computer Graphic Management, writing programs on level 6 machines for report formats, payrolls, and invoices for a variety of businesses. RHODA SMITH Office Manger/Data Coordinator, Mobile Division Ms. Smith attended Georgia State University in Atlanta, Georgia, where she majored in business administration. She has held various positions in the financial field. She joined Savannah Laboratories in 1988 as office manager. Her duties include supervision of office personnel and coordination of data and billing. She is thoroughly familiar with Savannah Laboratories' Information Management System (LIMS) and is responsible for editing reports for complex projects. She reports directly to the Laboratory Director and works with project mangers, analysts, and clients to coordinate prompt data flow through the laboratory. TUT OO6 O151 Section 16 Revision: 0 Date: 9/92 VIRGINIA VASQUEZ Analyst, Mobile Division Ms. Vasquez has a B.S. degree in chemistry/biology from the University of Guadalajara, Mexico. She has four years of analytical laboratory experience. She is familiar with EPA SW-846 and CFR Title 40 Part 136 test methods, protocols, and associated QC requirements. She was previously employed as a laboratory supervisor in a wastewater control laboratory. She was responsible for assuring that proper methods, techniques and procedures were used. She also worked as an analyst in an instrumental, wet chemistry and biology laboratory. Ms. Vasquez's primary responsibility at Savannah Laboratories is the analysis of environmental samples for volatile organic compounds by gas chromatography using Hall and flame ionization detectors (FID) according to EPA Methods 601/602 and SW-846 8010/8020. She interprets chromatograms, calculates and reports results, and checks QC for these methods. CYNTHIA WILSON Chemist, Mobile Division Ms. Wilson has a B.S. degree in chemistry from East Carolina University in Greenville, North Carolina. She joined Savannah Laboratories in 1989. She is responsible for the semivolatile organic analysis of environmental samples by GC/MS. Her duties include standard preparations, instrument calibrations, data interpretation and reporting, and maintenance of quality control for the GC/MS instrument. Prior laboratory experience includes analytical testing to monitor plant operation for a municipal wastewater laboratory. She performed wet chemical analysis including BOD, DO, pH, specific conductivity, residual chlorine, chlorides, solids, and microbiological analysis for fecal and total coliforms. She previously worked at the Savannah, Georgia division of Savannah Laboratories as a GC volatiles chemist where she gained experience reporting volatile data and associated QC requirements. Ms. Wilson has three years of analytical environmental testing experience on a variety of sample matrices including wastewaters, soils/sediments, and TCLP extracts. She is experienced in the use of purge and trap systems, FID, PID, and HECD detectors, and PE-Nelson and ChemStation data systems. She is familiar with SW-846 and 40 CFR Part 136 test methods, protocols, and QC requirements for semivolatiles organic analysis. TUT OO6 OH Section 16 Revision: 0 Date: 9/92 PAUL CANEVARO Laboratory Director/Project Manager, Deerfield Beach Division Mr. Canevaro received his B.S. degree in chemistry from the University of Montevallo in 1982. He has a total of 12 years experience working in environmental laboratories. This experience includes the operation of GC, GC/MS, ICP, HPLC, and AA instruments using EPA protocols. Other related experience includes the coordination of inorganic and organic laboratories with a staff of 60 chemists and technicians, professional and technical guidance to laboratory supervisors, and development and maintenance of a quality control/quality assurance program. Mr. Canevaro joined Savannah Laboratories in June, 1989 as the Deerfield Beach, Florida facility laboratory director. He is responsible for the day-to-day operation of the laboratory, project design and implementation, and client relations. TUT 006 O153 Section 16 Revision: 0 Date: 9/92 RHONDA MOLL Project Manager, Deerfield Beach Division Ms. Moll received her B.S. degree in biology with a double minor in chemistry and physics from Troy State University. She began her career with Savannah Laboratories in 1987 at the Tallahassee Division where she determined volatile organic compounds using GC and GC/MS. Her past experience also includes the quality control testing and approval of raw materials used in the manufacture of pharmaceuticals and hospital supplies at Baxter Corporation in Miami, Florida. Ms. Moll joined the Deerfield Beach Division upon its opening in 1989, as the volatile organics manager. She was responsible for the initial set-up of the volatiles laboratory which included instrumentation, quality control, methodology and personnel, training. She coordinated all laboratory functions and reviewed all data generated from this department. Ms. Moll was promoted to quality control manager of this division where she oversees all laboratory quality control functions such as evaluations, inspections, data review, and implementing new procedures required by methodology or Savannah Laboratories' corporate quality assurance program. KATHY C. IRMINGER Quality Assurance Manager, Deerfield Beach Division Ms. Irminger received a B.A. degree in chemistry from Wake Forest University and began working at the Colorado School of Mines Research Center in Golden, Colorado. There she performed atomic absorption spectrophotometry in metallurgical and environmental applications and also developed inorganic bench methods. She also has worked for Camp, Dresser, and McKee and the Colorado State Department of Health performing inorganic EPA methods. At AC Laboratories in Florida, she developed expertise in gas chromatography for EPA Methods 601, 602, 502.2, 604, 610, 8010, and 8020. Ms. Irminger joined Savannah Laboratories' Deerfield Beach Division when it opened in 1989, as a volatiles chemist performing GC and GC/MS analyses. She is well versed in SW-846 and CFR 40 methodologies. TUT OO6 0154 Section 16 Revision: 0 Date: 9/92 LINDA BACKUS Chemist, Deerfield Beach Division Ms. Backus received a B.S. degree in microbiology and a B.A. degree in chemistry from Florida Atlantic University. She taught microbiology at the collegiate'level and performed extensive research on oral microbes. Upon graduation, she was employed with the University of Miami/Jackson Memorial Hospital initiating a tissue procurement facility for nationwide cancer research. Ms. Backus joined Savannah Laboratories in 1990 as a trace metal analyst. Her present duties include determinations and data reporting of metals utilizing ICP techniques. THERONA T. JAMES Analyst, Deerfield Beach Division Ms. James has a B.A. degree in chemistry with a minor in education from Columbia College in Columbia, South Carolina. Prior to her employment with Savannah Laboratories in 1991, she was employed by the South Carolina Department of Environmental Health and Control as a chemist. There her duties encompassed wet chemistry, metals, and asbestos analyses. Her previous experience also includes metals analysis, digestion, and QA/QC data responsibilities at AC Laboratories in Fort Lauderdale, Florida. Ms. James' current responsibilities at the Deerfield Beach facility include the analysis of volatile organic compounds by GC. CATHERINE KATSIKIS Analyst, Deerfield Beach Division Ms. Katsikis received a B.S. degree in chemistry from the Chemical Engineering College in Athens , Greece . Her previous experience as a chemical laboratory supervisor included working with PVC stabilizers, polymerics, co-polymers, and organic compounds. Ms. Katsikis joined Savannah Laboratories in 1990 as a trace metals analyst. Her duties include determinations and data reporting of metals utilizing ICP techniques. ERIC S CHINS ING Technician, Deerfield Beach Division Mr. Schinsing has been with Savannah Laboratories since 1990. He has an A.S. degree from the Community College of The Finger Lakes of New York and is currently pursuing a degree in oceanographic engineering. His responsibilities include assisting the analysts in the general chemistry laboratory. Section 16 Revision: 0 Date: 9/92 MARIANNE WALKER Sample/Data. Manager, Deerfield Beach Division Ms. Walker's experience with environmental analytical laboratories includes two years at Pioneer Laboratory, Inc. in Pensacola, Florida, where she served as reporting department manager as well as office manager. Ms. Walker joined Savannah Laboratories in 1989, where she assisted in coordinating the initial set-up of the Deerfield Beach laboratory operation. Her initial responsibilities included supervision of sample custody, sample bottle preparation, sample login, and data entry, as well as providing in-house project coordination. As Sample/Data Manager, Ms. Walker is currently responsible for coordinating analytical programs for many of Savannah Laboratories' clients, including major consulting firms, counties, and water management districts. JANICE WILTSHIRE Data Coordinator, Deerfield Beach Division Ms. Wiltshire obtained her diploma in computer science from Computer and Business Institute in Jamaica and has one year experience as a data entry clerk at AC Laboratories. She joined Savannah Laboratories in 1990, and her duties include all phases of data handling and assisting project mangers with client report preparation. PHILL TAYLOR, JR. Field Coordinator, Deerfield Beach Division Mr. Taylor joined Savannah Laboratories in 1990. His previous experience includes working as a water treatment plant operator for the cities of Deerfield Beach and Pompano Beach, Florida. Mr. Taylor's current responsibilities include all field sampling activities scheduled at the Deerfield Beach facility. KIMBERLY L. AMBISCO-KOSTZER Organics Manager, Deerfield Beach Division Ms. Ambisco-Kostzer has a B.S. degree in biology/pre-med with a minor in chemistry from Barry University of Miami Shores, Florida. She worked at the University of Miami School of Medicine as a research biochemist after graduation. Ms. Ambisco-Kostzer joined Savannah Laboratories in 1989. Her duties include the analysis of pesticides, herbicides, phthalates, EDB, PAH, phenols, hydrocarbons, and formaldehydes. TUT OO6 O156 Section 16 Revision: 0 Date: 9/92 LAWRENCE TEICH Chemist, Deerfield Beach Division Mr. Teich has a B.A. in chemistry with an emphasis in zoology from Florida Atlantic University. Prior to joining Savannah Laboratories in 1989, he taught laboratory course work in animal physiology at Florida Atlantic University in Boca Raton. Mr. Teich's responsibilities at Savannah Laboratories include mercury determinations by cold vapor atomic absorption. He also assists with trace metal analysis of As, Pb, Se, and Tl by graphite furnace atomic absorption and helps in the digestion of samples. MARY VALEST Chemist, Deerfield Beach Division Ms. Valest obtained a B.S. degree in chemistry from the Catholic University of Puerto Rico. She completed her Chemistry Practicum at Destileria Serralles, Inc., a rum manufacturing company, where she performed analysis of finished products by UV, GC, and colorimeter. In raw materials, she conducted water monitoring, testing and distillation of fermented sugars. Ms. Valest assisted on a temporary basis as quality control manager at Fruits Drinks, Inc. (Puerto Rico) where her responsibilities included the quality control process, documentation and daily production reports; coordination of chemical and microbiological testing of raw materials and finished products; supervision of laboratory technicians; and control of safety and sanitation systems. She then joined SmithKline Beecham Pharmaceuticals (Puerto Rico) where she worked as quality assurance analyst with bulk, finished products, and long term stability samples conducting testing procedures by HPLC, GC, UV, turbidimeter, osmometer and extractions. In the area of raw materials, she worked with IR, TLC, gravimetric analysis, all process sterile water monitoring and process rinse water testings. In 1990, she moved into the continental United States and worked on a temporary basis with Schering-Plough (Pembroke Pines, Florida) where she performed dissolution technology and HPLC and assisted in identification of chromatographic samples and calculation of resolution and tailing factors for a new quantitation method for fatty acids. Ms. Valest joined Savannah Laboratories in 1991, and she is currently working in the semivolatile GC department performing EDB and pesticide residue analysis. TUT GO6 0157 Section 16 Revision: 0 Date: 9/92 CAROL-ANN VASSELL Chemist, Deerfield Beach Division Ms. Vassell obtained a B.S. degree in chemistry from the City College of New York. Upon graduation, she worked as a research chemist at the Institute of Food and Agricultural Sciences. Ms. Vassell joined AC Laboratories where she performed trace metal determinations by AA as well as EDB and trihalomethane determinations by GC. She also conducted sample extractions for organic compounds as well as chloride, cyanide, and phenols determinations. Ms. Vassell joined Savannah Laboratories in 1990 as a chemist. Her responsibilities include the analysis of acids, base neutral and pesticide compounds by GC/MS techniques. TUT OO6 O158 Section 16 Revision: 0 Date: 9/92 KATHY SHEFFIELD Laboratory Director/Project Manager, Tampa Bay Division Ms. Sheffield has B.S. degrees in chemistry and biology plus seven years of analytical chemistry experience. Throughout her career, she has specialized in the field of organic chemistry and has developed considerable expertise in pesticide and volatile organic analysis. Ms. Sheffield was employed by the Florida Department of Agriculture in the Pesticide Use Monitoring Section of the Chemical Residue Laboratory. She was responsible for the analysis of water, soil, and food products for a variety of pesticides and herbicides using gas chromatography and high performance liquid chromatography (HPLC). She was instrumental in the development of new procedures using HPLC, and wrote several standard operating procedures. Ms. Sheffield was promoted to a supervisory level where she was responsible for all data generated by the analytical section. Ms. Sheffield began her employment with Savannah Laboratories and Environmental Services, Inc. as senior chemist. She performed analyses on environmental samples using instrumental techniques including GC/MS, GC, and HPLC. She was promoted to organic section manager, with additional duties in the administration of the quality assurance program. As laboratory director/project manager, Ms. Sheffield is responsible for coordinating analytical programs for many of Savannah Laboratories' clients, including major consulting firms, counties, governmental agencies, and industries. ANDRE RACHMANINOFF Project Manger, Tampa Bay Division Mr. Rachmaninoff has a B.A. degree in biology from Kalamazoo College and eight years of experience in environmental analytical work. Six years of this experience was in a supervisory or laboratory management capacity. Mr. Rachmaninoff is thoroughly familiar with analytical, microbiological, and radiochemistry techniques. He has extensive bench experience in both flame and furnace AA spectroscopy, ICP emission spectroscopy, IR and UV/VIS spectroscopy, Gamma spectrometry, alpha and beta particle emissions analysis, and numerous automated and manual wet chemistry analyses. Mr. Rachmaninoff is an active member of the Florida Society of Environmental Analysts, and served as President from 1990-1991. Mr. Rachmaninoff provides technical assistance and support to clients for field and analytical services as a project manager. TUT OO6 0159 Section 16 Revision: 0 Date: 9/92 DOMINIC P. FRALLI Project Manager, Tampa Bay Division Mr. Fralli holds an M.S. degree in environmental science from the University of Texas in Dallas. He has more than seven years experience as a gas chromatography chemist and supervisor. Mr. Fralli was an environmental scientist with the Hillsborough County Environmental Protection Commission where he was responsible for the operation of the organic section of the laboratory prior to joining Savannah Laboratories. He implemented EPA methods for analysis of water and soil samples and was in charge of the QA/QC generated for these methods. He supervised two chemists and provided information concerning organic chemicals to the public and to agency personnel. As QA Manager, he is responsible for ensuring that method QA requirements are met and also issues and evaluates in-house check samples. TRACY H. BOTTO Inorganics Manager, Tampa Bay Division Ms. Botto holds a B.S. degree in microbiology from the University of Maine and has five years experience in a variety of laboratory techniques. Her specialty is trace metals determinations by ICP, though she is familiar with flame, furnace, and cold-vapor techniques. Her responsibilities as inorganics manager include management of personnel, overseeing of all method development, and adherence to EPA methodology and QA/QC requirements of the Tampa Bay Division laboratory. INAS M. SOBKY Quality Assurance Manager, Tampa Bay Division Ms. Sobky has a B.S. degree in chemistry/zoology from Ain Shames University, Cairo, Egypt and seven years of experience in organic environmental analytical work. Four years was spent in an organic laboratory management capacity. Ms. Sobky is familiar with EPA 500, 600, and 8000 series gas chromatography (GC) methodologies. She has additional training from ACS in gas chromatography system maintenance and troubleshooting. She attended an analytical gas chromatography workshop with the Southeastern Chromatography Association and she is an active member of the Florida Society of Environmental Analysts. Ms. Sobky's responsibilities include management and implementation of technical EPA GC methods, training and supervision of organic chemists and technicians, and maintenance of GC instrumentation as a GC manager for Savannah Laboratories, Tampa Bay Division. TUT 006 0160 Section 16 Revision: 0 Date: 9/92 LINDA DOWD Analyst, Tampa. Bay Division Ms. Dowd has a B.S. degree in biology from York College and an A.S. degree in environmental health technology from Queensboro Community College. While working toward her degrees, she was employed as an environmental educator for the New York City Department of Parks. Her duties included flora and fauna identification and inventories, water sampling, and the creation and implementation of a variety of environmental education programs for the public. Her responsibilities as an analyst include the preparation of standards, calibration and loading of the GC, and assisting the chemist in charge with identification and calculation of volatile organic compounds for the volatiles section at Savannah Laboratories. CHRIS E. HARRIS Field Sampler/Lab Technician, Tampa Bay Division Mr. Harris has more than three years of experience as a field/laboratory technician in the environmental field. He has collected soil, groundwater, surface water, drinking water, and industrial waste samples using current EPA protocol. In the laboratory, he has performed a wide variety of titrimetric, gravimetric, and colorimetric analyses according to EPA protocol for both aqueous and nonaqueous sample matrices. Mr. Harris is responsible for the scheduling and planning of all field sampling projects for the Tampa Bay facility. When not collecting field samples, he is responsible for all analyses associated with the general and biological laboratories. CARL JOHN HOOVER, JR. Chemist, Tampa Bay Division Mr. Hoover holds a B.S, in zoology from the University of South Florida. He has more than six years experience in the environmental field. Mr. Hoover was a chemist with PBS&J Environmental Laboratories where he was responsible for trace metals analysis by GFAA, hexavalent chromium analysis, mercury analysis by cold vapor method and TCLP extractions prior to joining Savannah Laboratories. He was an environmental scientist and laboratory technician at Southwest Florida Water Management District where he assisted in environmental impact studies and performed wet chemistry analysis before his employment with PBS6J. At Savannah Laboratories, Mr. Hoover is responsible for trace metals analysis by GFAA and by ICP. TUT GO6 0161 Section 16 Revision: 0 Date: 9/92 ANTONIUS LEBRUN Chemist, Tampa Bay Division Mr. Lebrun has a B.S. degree in chemistry from University of Florida. He was a chemist with Cargill/Gardinier, Inc., in Riverview, Florida, where he worked in the environmental department prior to joining Savannah Laboratories. At Savannah Laboratories, Mr. Lebrun is responsible for analysis of samples for metals by ICP and GFAA. MARSHA MARTINOVICH Analyst, Tampa Bay Division Ms. Martinovich has a B.A. degree in sociology with a minor in chemistry from West Virginia University in Morgantown, West Virginia, and has more than three years experience in the environmental field. She was responsible for analysis of organic contaminants in water, wastewater, soil, and hazardous waste samples prior to joining Savannah Laboratories as a GC analyst. At Savannah Laboratories, Ms. Martinovich is responsible for volatile analysis by GC using methods 601, 602, 8010, and 8020. NATALIE L. PARK Analyst, Tampa Bay Division Ms. Park has a B.S. degree in biology from Florida State University. She has two years experience doing organic extractions at an environmental laboratory. She was responsible for extraction of soil and water samples for EPA Methods 604, 606, 608, 610, 614, 615, 625, and all SW-846 series methods. She is also familiar with Methods 418.1 and 413.2. Ms. Park's duties at Savannah Laboratories include metal digestions, TCLP extractions, and mercury analysis using cold vapor techniques. Section 16 Revision: 0 Date: 9/92 TALICIA C. SMITH Chemist, Tampa Bay Division Ms. Smith has a B.S. degree in chemistry from Florida A&M University, plus five years of analytical chemistry experience. Ms. Smith was employed by the Florida Department of Agriculture and Consumer Services, Chemical Residue Laboratory, prior to joining Savannah Laboratories. Her duties included method development, quality control and supervision of a technical staff. She also developed considerable expertise in gas chromatographic procedures. Ms. Smith is in charge of volatile GC/MS analysis following EPA Methods 624 and 8240. TAYSEER E. ZAYAN Chemist, Tampa Bay Division Ms. Zayan has a B.S. degree in chemistry from the University of Cairo in Cairo, Egypt, and more than six years experience as a chemist in the environmental field. She was a section manager with an environmental laboratory where she was responsible for analysis of water, wastewater, and soil samples prior to joining Savannah Laboratories. At Savannah Laboratories, Ms. Zayan is responsible for semivolatile analyses by GC using Methods 608/8080, 610/8100, and 504. TUT 006 O163 Appendix A GQAP #8901420 Savannah Laboratories Appendix A: Method Validations Summary of Contents Method 630 8U1 8141 632/3550 632/3550 632/3550 632/3550 632/3550 632/3550 632)0550 632/3550 632/3550 632/3550 632/3550 632/3550 632/3550 632/3550 632/3550 8081 8081 632/3550 632/3550 6010 6010 8081 8081 8081 8081 8081 8081 8081 8081 8H1 8H1 8U1 3141 8141 8U1 8U1 8U1 8U1 8H1 8U1 8141 8141 8141 8141 8141 8270B 8270B Matrix water soil soil soil soil soil soil soil soil soil soil soil soil soil soil soil soil soil soil groundwater soil soil water soil groundwater groundwater groundwater soil soil soil groundwater soil groundwater groundwater groundwater groundwater groundwater groundwater groundwater groundwater soil soil soil soil soil soil soil soil groundwater soil Analyte ziram ethion trithion carbofuran fenuron monuron baygon (propoxur) fluometuron' diuron propham methiocarb Snuron chlorpropham barban neburon oxamyi methomyl carbaryl dicofol (kelhane) dicofol (kelhane) mexacarbate siduron tin tin '• chlorobercilate isodrin mirex chlorobenzilate isodrin mirex kepone kepone thionazin sutfotepp phorate dimethoate disulfoton methyl parathion ethyl parathion fampnur thionazin sulfotepp phorate dimethoate disulfoton methyl parathion ethyl parathion famphur 1 ,4-dioxane 1 ,4-dioxane Page* 1 2 2 3 4 4 4 4 4 5 5 5 5 5 6 7 7 7 8 9 10 10 11 12 13 13 13 14 14 14 15 16 17 17 17 17 17 18 18 18 19 19 19 19 19 20 20 20 21 22 Date Submitted 06/01/91 07/16/91 07/16/91 07/16/91 08/05/91 08/05/91 08/05/91 08/05/91 08/05/91 08/05/91 08/05/91 08/05/91 08/05/91 08/05/91 08/05/91 08/05/91 08/05/91 08/05/91 08/05/91 08/05/91 08/09/91 08/09/91 08/09/91 08/09/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 08/12/91 TUT' OO6 O164 Appendix A GQ*P«890142G Savannah Laboratories Appendix A: Method Validations Summary of Contents Method 8080/608.1 8080/608.1 8080/608.1 8080/608.1 8080 8080 8080 8080 8150 8150 8U1 8U1 8U1 8U1 8U1/619 8U1/619 8141/819 8U1/619 8U1/819 8H1/619 8U1/619 8U1/619 8U1/619 8U1/619 8U1/619 8U1/819 8U1/619 8U1/619 8H1/619 8U1/619 8U1/619 632 504 504 504 504 504 504 8330 8330 8330 8330 8330 8330 8270 8270 7041/3005 7041/3050 631/3550 Matrix water water water water soil soil soil soil water soil water water soil soil soil water water water water water water water water soil soil soil soil soil soil soil soil water water water water water water water water water soil soil water soil water soH water soil soil Analyte chtaroneb propachbr chloropropytate etridiazole chbroneb propachbr chbropropytete etridiazole pick) ram picks ram dioxathion dichbfenthion dioxathion dichbfenthion terfautryn ametryn atrazine prometryn prometon propazine simazine terbuthyiazine terbutryn ametryn atrazine prometryn prometon propazine simazine terbuthyiazine terbutryn bromacl! EDB DBCP chbropicrin 1,1-dichbropropane methyl isothiocyanate c/l-1 ,3-dichbropropene diphenyfamine n-nrtrosodiphenytamine dipherryiamine n-nttrosodiphenytamine nitrogjycerin nitroglycerin ethyl carbamate ethyl carbamate antimony anhimony benobnyl Page* 23 23 23 23 24 24 24 24 25 25 26 26 27 27 27 28 28 28 28 28 29 29 29 30 30 30 30 30 31 31 31 32 33 33 33 33 33 34 35 35 36 36 37 38 39 40 41 42 43 Date Submitted 05/06/92 05/06792 05/06/92 05/06/92 05/06/92 05/06/92 05/06/92 05/06/92 05/06/92 05/06/92 05/06792 05/06/92 05/06/92 05/06/92 05/06/92 05/06/92 05/06/92 05/06/92 05/06/92 05/06/92 05/06/92 05/06/92 05/06/92 05/08/92 05/06/92 05/06/92 05/06/92 05/06/92 05/06792 05/06/92 05/06/92 05/06/92 05/06/92 05/06/92 05/06/92 05/06/92 05/06/92 05/06/92 12/17/92 12/17/92 08/23/92 06/23/92 07/14/92 07/14/92 07/14/92 07/14/92 07/14/92 07/14/92 07/14/92 METHOD VALIDATION Appendix A Page Number 1 Date: 05/31/91 Method: 630 Reference: EPA 1982, Pressly/Longbottom Matrix: water Instrument: Milton/Roy Spec. 21 Analytical technique: colorimetric Single lab validation by SL Division: Tallahassee Extractables Volume ext: 1000 mL -or- Wt. ext. (dry) : q Extraction Solvent: SnCl2/HCll Final Solvent: Cupric acid/ethanol; Final Volume: 25 mL ii Purgeables Amount purged: mL -or- g soil in mL K20 aine2 Analyte: Spike level (unit) Replicate 1 Replicate 2 Replicate 3 Renlicate 4 Replicate 5 Replicate 6 Renlicate 7 Average result (n-l)sd MDL* PQL** Is spike level<10x calculated MDL? SL GQAP PQL j ———————————————— Ziraia 25 ug/L 23 25 26 29 26 27 26 26 1.826 5.7 ug/L 18 ug/L yes NA *MDL = sd(n-l) x 3.14 **PQL = sd(n-l) x 10 Analyst: Robert Berry QA Manager: E.L. Schneider Remarks: IDecomposition reagent. 2Color reagent. All dithiocarbamates are reported as Zirara. Absorbance was determined at 435nm and 380nm. Results presented are from the 435nm determination. Correct absorbance is based on the analyte concentration. QA Objectives z Analyte: ind PQL's to be Accuracy (%Rec) added to Table f Precision (%RPD) 5: Completeness (%) PQL ( ) _____________ _________ TUT OO6 O.166 METHOD VALIDATION Appendix A Page Number 2 Date: 07/16/91 Method: 8141 Reference: SW846 Proposed Update I Matrix: soil Instrument: Varian 3400 Analytical technique: GC/NPD Single lab validation by SL Division: Tallahassee Extractables Volume ext: _____mL -or- Wt. ext.(dry): 10 g Extraction Solvent: MeC12 Final Solvent: Kexane Final Volume: 10 mL Purgeables Amount purged: ______mL -or- ___g soil in ______mL H20 Analyte: Spike level (unit) Replicate 1 Replicate 2 Replicate 3 Replicate 4 Replicate 5 Replicate 6 Replicate 7 Average result (n-l)sd MDL* PQL** Is spike level<6x calculated MDL? SL GQAP PQL ————————— t Ethion 100 ug/kg 84.1 78.6 76.9 77.7 89.2 74.7 79.8 80.1 4.938 15.5 49.4 yes 300 Trithion 100 ug/kg 100 80 133 113 120 103 93.3 106 17.59 55.2 176 yes 200 * *MDL = sd(n-l) X 3.14 **PQL = sd(n-l) x 10 Remarks: Analyst: D. Koren QA Manager: E.L Schneider QA Objectives c Analyte: ind PQL's to be Accuracy (%Rec) added to Table ! Precision ( %RPD) >: Completeness (%) PQL { ) TUT 006 O.167 XIIHOD VALIDATION Date: 7/13/92 Appendix A Page Kur-ber Reference: EPA/SW8ij> 631/3550 Instrument: Waters 600£/Waters detector Sincle lab validation by SL Division: Katrix: Soil Analytical technique: HPLC/UV Zxtrectables Volume ext: -or- Vt. ext.(cry): 30 g Extraction Solvent: MeCl? Final Solvent: ACK Final Volume: 1 771! Purceables Aaount purged: -or- ___g soil in ral _ni :-:2o Analyte: Spike level (unit) _ He^licate 1 rleolicate 2 Reolicate 3 Reolicate < Serlicate 5 Reolicate 6 Reolicate 7 Averace result (n-l)sd MDL* ?QL** Is soike level<6x calculated KDL? £L GQAP ?QL _ 3enom}"j._ 0.667(ue/ke: 0.228 0.25! •0.2" 0.201 0.275 0.20i 0.221 0.232 0.0266 0.084 0.27 NO ========== ========== jsia at as as ^ re szxx = =========== *KDL = sd(n-l) X 3.14 **?QL = sd(n-l) x 10 Analyst: Paul Rygiel QA Manager: E.L. Schneider Resarks: Benomyl can be extracted and analyzed concurrently »ich Method QA Objectives and PQL's to be added to Table 5: Analyte: Benomyl • Accuracy (%Rec) 18 - 60 Precision (%R?D) 0 - 3 5 Completeness (%) ?QL kc/kc d-j 1.0 TUT 006 0.168 METHOD VALIDATION Date: 08/01/91 Method: 632/3550 Reference: EPA/SW846 Matrix: soil Instrument: Waters HPLC Analytical technique: HPLC/UV Single lab validation by SL Division: Tallahassee Appendix A Page Number 4 Extractables Volume ext: mL -or- Wt. ext. (dry) : 30 g Extraction Solvent: MeC12 Final Solvent: Acetonitrile Final Volume: 1.0 mL Purgeables Amount purged: mL -or- g soil in mL H2O Analyte: Spike level (unit) _ Replicate 1 Replicate 2 Replicate 3 Replicate 4 Replicate 5 Replicate 6 Reolicate 7 Average result (n-l)sd MDL* PQL** Is spike level<6x calculated MDL? SL GQAP PQL ————————— i Fenuron 10 ug/kg 9.29 10.6 10.2 9.58 9.69 9.42 8.17 9.57 0.77 2.42 7.7 yes 100 Monuron 3 . 0 ug/kg 2.54 2.30 1.87 1.73 2.02 2.02 1.73 2.03 0.30 0.94 3.0 yes 20 Baygon 120 ug/kg 106 106 108 88.9 89.8 86.9 84.2 95.7 10.4 32.8 104 yes 20 Fluoiaeturon 8 . 0 ug/kg 7.28 7.47 7.32 6.20 5.82 6.48 6.14 6.67 0.67 2.10 6.7 yes 20 Diron 3 . 0 ug/kg 2.97 3.19 3.10 2.48 2.66 2.72 2.79 2.84 0.23 0.74 2.3 yes 20 *MDL = sd(n-l) **PQL = sd(n-l) Remarks: 3.14 10 Analyst: Paul Rygiel QA Manager: E.L. Schneide: QA Objectives and PQL's to be added to Table 5: Analyte: Fenuron Monuron Baygon Fluometuron Diron Accuracy (%Rec) Precision ( %RPD)Completeness (%) PQL (ug/kg) 10 5.0 100 10 5.0 TUT OO6 O169 METHOD VALIDATION Date: 07/15/91 Method: 632/3550 Reference: EPA/SW846 Matrix: soil Instrument: Waters/LC Analytical technique: HPLC/UV Single lab validation by SL Division: Tallahassee Appendix A Page Number 3 h ———————————————— ——— Extractab Volume ext: -or- Wt. ext. (dry) : 30 Extraction Solvent: Final Solvent: Final Volume: <- ——— ——— —— ——— —— les mL .7 g dw MeCl2 Acetonitrile 1.0 mL Purgeables Amount purged: -or- g soil in . mL mL K20 , Analyte: Spike level (unit) Replicate 1 Replicate 2 Replicate 3 Replicate 4 Replicate 5 Replicate 6 Replicate 7 Average result (n-l)sd MDL* PQL** Is spike level<6x calculated MDL? SL GQAP PQL Carbofuran 29.3 ug/kg 28.3 31.3 26.7 28.3 28.3 26.7 23.4 27.6 2.395 7.51 24 yes 200 *MDL = sd(n-l) X 3.14 **PQL = sd(n-l) X 10 Analyst: R. Driver QA Manager: E.L. Schneider Remarks: QA Objectives i Analyte : md PQL's to be Accuracy ( %Rec) added to Table f Precision (%RPD) >: Comoleteness (%) PQL ( ) ™ TUT CO6 O17O METHOD VALIDATION Date: 08/01/91 Method: 632/3550 Reference: EPA/SW846 Matrix: soil Instrument: Waters HPLC Analytical technique: HPLC/UV Single lab validation by SL Division: Tallahassee Appendix A Page Number 5 1 Jf. Extracta Volume ext: -or- Wt. ext. (dry) : Extraction Solvent Final Solvent: Final Volume: bles mL 30 g : MeC12 Acetonitrile 1.0 mL j_ Purgeables Amount purged: mL -or- g soil in mL E20 Analyte: Spike level (unit) Reolicate 1 Replicate 2 Replicate 3 Replicate 4 Reolicate 5 Replicate 6 Replicate 7 Average result (n-l)sd MDL* PQL** Is spike level<6x calculated MDL? SL GQAP PQL Prophara 60 ug/kg 51.2 47.8 48.0 41.1 40.3 41.0 41.9 44.5 4.40 13.8 44 yes 20 Methiocarb 40 ug/kg 41.3 42.4 42.3 33.1 32.9 36.4 35.4 37.7 4.23 13.3 42 yes 100 Linuron 4 . 0 ug/kg 3.66 3.64 3.68 3.13 3.04 3.28 3.18 3.37 0.28 0.87 2.8 yes 20 Chlorpropham 40 ug/kg 15.6 13.0 14.9 12.3 11.7 11.7 10.4 12.8 1.86 5.84 19 no(x6. 8) 20 Barban 50 ug/kg 15.0 15.0 16.7 11.7 11.7 13.3 13.3 13.8 1.85 5.81 19 no(x8.6) 20 *MDL = sd(n-l) x 3.14 **PQL = sd(n-l) x 10 Analyst: Paul Rygiel QA Manager: E.L. Schneider Remarks: Average %recovery for Chlorpropham is 32%. Average %recovery for Barban is 28%. QA Objectives and PQL's to be added to Table 5: Analyte: Propham Methiocarb Linuron Chlorpropham Barban Accuracy ( %Rec) Precision (%RPD) Completeness (%) PQL (ug/kg) 50 50 5.0 20 20 TUT OO6 O171 METHOD VALIDATION Date: 08/01/91 Method: 632/3550 Appendix A Page Number 6 Reference: EPA/SW846 Matrix: soil Instrument: Waters HPLC Analytical technique: KPLC/UV Single lab validation by SL Division: Tallahassee Extractables Volume ext: -or- Wt. ext.(dry): mL 30 g Extraction Solvent: MeCl2 Final Solvent: Acetonitrile Final Volume: 1.0 mL Purgeables Amount purged: -or- ___g soil in mL H20 (reiteration of previous data) -+———————————-t-—————————————-r ———————— Analyte: Spike level(unit) _ Replicate 1______ Replicate 2_______ Replicate 3_______ Replicate 4______ Replicate 5______ Replicate 6______ Replicate 7_______ Average result___ (n-1)sd________ MDL*___________ PQL* *___________ Is spike level<6x calculated MDL?__ SL GQAP PQL_____ Neburon 3 . 0 ug/kg 2.97 2.97 2.97 2.43 2.30 2.57 2.70 2.70 0.28 0.88 2.8 yes 20 Carbofuran 29.3 ug/kg 28.3 31.3 26.7 28.3 28.3 26.7 23.4 27.6 2.395 7.51 24 yes 200 *MDL = sd(n-l) x 3.14 **PQL = sd(n-l) x 10 Remarks: Analyst: Paul Rygiel QA Manager: E.L. Schneider QA Objectives z Analyte: - Neburon Carbofuran md PQL's to be Accuracy ( %Rec) added to Table ! Precision (%RPD) >: Completeness (%) PQL (ug/kg) 5.0 50 TUT O06 O172 METHOD VALIDATION Date: 08/01/91 Method: 632/3550 Reference: EPA/SW846 Matrix: soil Instrument: Waters KPLC Analytical technique: HPLC/UV Single lab validation by SL Division: Tallahassee Appendix A Page Number 7 -1 Extracta Volume ext: -or- Wt. ext. (dry) : Extraction Solvent Final Solvent: Final Volume: bles raL 30 g : MeCl2 Acetonitrile 1. 0 mL Purgeables Amount purged: mL -or- g soil in mL K20 1 1 * Analyte: Spike level (unit) Replicate 1 Replicate 2 Replicate 3 Replicate 4 Replicate 5 Replicate 6 Replicate 7 Average result (n-l)sd MDL* PQL** Is spike level<6x calculated MDL? SL GQAP PQL Oxamyl 50 ug/kg 39.9 39.9 39.9 43.9 39.9 51.8 41.8 42.4 4.415 13.9 44 yes 200 Methomyl 120 ug/kg 119.9 114.2 102.7 125.6 119.9 148.4 114.2 120.7 14.15 44.5 142 yes 20 Carbaryl 30 ug/kg 54.9 59.7 57.3 59.7 57.3 59.7 54.9 57.6 2.16 6.8 22 yes 100 *MDL = sd(n-l) X 3.14 **PQL = sd(n-l) x 10 Analyst: Paul Rygiel QA Manager: E.L. Schneider Remarks: Average %recovery for carbaryl was 192%. Baseline interfence is suspected; the study will be rerun as soon as possible for carbaryl, QA Objectives z Analyte: Oxarayl Methomyl Carbaryl md PQL's to be Accuracy ( %Rec) added to Table i Precision (%RPD) Completeness (%) PQL (ug/kg) 50 200 50 TUT 006 O173 METHOD VALIDATION ' Appendix A Page Number 8 Date: 08/03/91 Method: 8081 Reference: SW846 Proposed Update II Matrix: soil Instrument: Varian 3400 GC Analytical technique: GC/ECD Single lab validation by SL Division: Tallahassee Extractables Volume ext: -or- Wt. ext.(dry): mL 10 g Extraction Solvent: MeC12/Acetone Final Solvent: Hexane Final Volume: 10.0 mL Purgeables Amount purged: _____mL -or- ___g soil in _____mL K20 Analyte: Spike level (unit) Replicate 1 Replicate 2 Replicate 3 Replicate 4 Replicate 5 Replicate 6 Replicate 7 Average result (n-l)sd MDL* PQL** Is spike level<6x calculated MDL? SL GQAP PQL Dicofol 50 ug/kg 52.4 50.4 50.9 54.1 51.4 51.8 50.8 51.7 1.258 3.95 12.6 no(xl2.6) *MDL = sd(n-l) x 3.14 **PQL = sd(n-l) X 10 Analyst: Amy Kayes QA Manager: E.L. Schneider Remarks: DB-608 column reported. DB-5 results were similar. Spike level is greater than lOx calculated MDL. Study will be rerun at a lower level as soon as possible. QA Objectives z Analyte: Dicofol md PQL's to be Accuracy (%Rec) added to Table £ Precision (%RPD) i : Completeness (%) PQL (ug/kg) 20 ^.- TUT 006 0174 METHOD VALIDATION Appendix A Page Number 9 Date: 08/03/91 Method: 8081 Reference: SW846 Proposed Update II Matrix: groundwater Instrument: Varian 3400 GC Analytical technique: GC/ECD Single lab validation by SL Division: Tallahassee Volume ext: -or- Wt. ext.(dry): Extractables 1000 mL Extraction Solvent: MeCl2 Final Solvent: Kexane Final Volume: 10.0 mL Purgeables Amount purged: ______mL -or- ___g soil in _____mL H20 Analyte: Spike level (unit) Reolicate 1 Reolicate 2 Reolicate 3 Replicate 4 Reolicate 5 Replicate 6 Replicate 7 Average result (n-l)sd MDL* PQL** Is spike level<6x calculated MDL? SL GQAP PQL Dicofol 0.05 ug/L 0.0597 0.0649 0.0595 0.0555 0.0610 0.0592 0.0517 0.0588 0.00418 0.0131 0.042 yes *MDL = sd(n-l) x 3.14 Analvst: Amy Hayes **PQL = sd(n-l) x 10 QA Manager: E.L. Schneider Remarks: DB-608 column renorted. DB-5 results were similar. QA Objectives a Analyte: Dicofol tnd PQL's to be Accuracy ( %Rec) added to Table f Precis ion ( %RPD) 5: Completeness (%) PQL (ug/L) 0.10 TUT 006 0175 METHOD VALIDATION Appendix A Page Number 10 Date: 08/07/91 Method: 632 Reference: ZPA SW-846 Matrix: soil Instrument: Waters HPLC Analytical technique: KPLC Single lab validation by SL Division: Tallahassee Volume ext: -or- Wt. ext.(dry): Extractables __ mL 30 g Extraction Solvent: MeC12 Final Solvent: Acetonitrile Final Volume: 1 mL Purgeables Amount purged: ______mL -or- ___g soil in ______mL H20 Analyte: Spike level (unit) Replicate 1 Replicate 2 Replicate 3 Replicate 4 Replicate 5 Reolicate 6 Replicate 7 Average result (n-l)sd MDL* PQL** Is spike level<6x calculated MDL? SL GQAP PQL Mexacarbate 25 ug/kg 11.3 14.6 14.6 14.6 12.9 12.1 11.3 13.06 1.54 4.8 15.4 yes 20 Siduron 16.7 ug/kg 12.7 12.7 11.4 11.4 13.9 13.9 10.8 12.40 1.24 3.9 12.4 yes 20 *MDL = sd(n-l) x 3.14 **PQL = sd(n-l) x 10 Remarks: Analyst: Paul Rygeil QA Manager: E.L. Schneider QA Objectives z Analyte: md PQL's to be Accuracy ( %Rec) added to Table f Precision (%RPD) >: ComDleteness(%) PQL ( ) r TUT 006 O.1..76 METHOD VALIDATION Date: 08/07/91 Method: 6010(3010) Reference: USEPA SW-846 Matrix: water Instrument: Jarrell Ash ICAP61 Analytical technique: _____ Single lab validation by SL Division: Tallahassee Appendix A Page Number 11 Inorganics (digestion) Volume ext: 100 mL -or- Wt. ext. (dry): ____ c Extraction Solvent: n/a' Final Solvent: n/a Final Volume: 100 mL Purgeables Amount purged: _____mL -or- ___g soil in ______mL H20 Analyte: Spike level(unit) _ Replicate 1______ Replicate 2_______ Replicate 3_______ Replicate 4_______ Replicate 5_______ Replicate 6______ Replicate 7_______ Average result (n-l)sd_____" MDL*_________ PQL* *________ Is spike level<6x calculated MDL?__ SL GQAP PQL______ Tin 0.10 lag/L 0.1023 0.0978 0.0945 0.0912 0.0973 0.0939 0.0939 0.0966 0.00367 0.0115 0.0366 no (x8.7) 20 .... -- • *MDL = sd(n-l) x 3.14 **PQL = sd(n-l) x 10 Remarks: Analyst: Todd Baumgartner QA Manager: E.L. Schneider QA Objectives z Analyte: i ——————————— . md PQL's to be Accuracy (%Rec) added to Table f Precision (%RPD) >: Completeness (%) PQL ( ) TUT 006 01.77 METHOD VALIDATION Date: 08/07/91 Method: 6010(3010) Reference: USEPA SW-846 Matrix: soil Instrument: Jarrell Ash ICAP61 Analytical technique: ____ Single lab validation by SL Division: Tallahassee Appendix A Page Number 12 ^ Inorganics (digestion) Volume ext: roL -or- Wt. ext. (dry) : 1.40 g Extraction Solvent: n/a Final Solvent: n/a Final Volume: 100 nL Purgeables Amount purged: mL -or- g soil in mL K20 Analyte: Spike level (unit) Replicate 1 Replicate 2 Replicate 3 Replicate 4 Replicate 5 Replicate 6 Reolicate 7 Average result (n-l)sd MDL* PQL** Is spike level<6x calculated MDL? SL GQAP PQL Tin 7.46 mg/kg 4.73 3.25 5.30 5.02 4.84 5.64 4.61 4.77 0.757 2.37 7.57 yes 5.0 •-— ' *MDL = sd(n-l) x 3.14 **PQL = sd(n-l) x 10 Remarks: Analyst: Todd Baumgartner QA Manager: E.L. Schneider QA Objectives e Analyte: ind PQL's to be Accuracy ( %Rec ) added to Table f Precision ( %RPD)Completeness (%) PQL ( ) TUT GO 6 O.178 METHOD VALIDATION Appendix A Page Number 13 Date: 08/07/91 Method: 8081 Reference: EPA SW-846 Matrix: groundwater Instrument: Varian 3400 Dual ECD Analytical technique: GC/ECD Single lab validation by SL Division: Tallahassee Volume ext: -or- Wt. ext.(dry): Extractables 700 mL g Extraction Solvent: MEC12 Final Solvent: Hexane Final Volume: 10 mL Purgeables Amount purged: _____-mL -or- ___g soil in _____mL H20 Analyte: Spike level (unit) Replicate 1 Replicate 2 Reolicate 3 Replicate 4 Replicate 5 Renlicate 6 Replicate 7 Average result (n-l)sd MDL* PQL** Is spike l-evel<6x calculated MDL? SL GQAP PQL Isodrin 0.023 ug/L 0.0235 0.0248 0.0199 0.0222 0.0220 0.0170 0.0174 0.0210 0.00298 0.00936 0.0298 yes 0.020 SChlorb 0.57 ug/L 0.650 0.6640 0.572 0.634 0.778 0.630 0.580 0.641 0.0677 0.212 0.677 yes 0.50 Mirex 0.23 ug/L 0.201 0.206 0.183 0.204 0.207 0.163 0.150 0.188 0.023 0.0722 0.230 yes - --..-, .... - - *MDL = sd(n-l) x 3.14 **PQL = sd(n-l) x 10 $ Chlorb=Chlorbenzilate Remarks: Analyst: D. Koren QA Manager: E.L. Schneider QA Objectives and PQL's to be added to Table 5: Analyte: Isodrin Chlorbenzilate Mirex Accuracy (%Rec) Precision (%RPD) Completeness (%) PQL (ug/L) 0.050 1.0 0.50 TUT OO6 0179 METHOD VALIDATION Date: 08/07/91 Method: 8081 Reference: EPA SW-846 Appendix A Page Number 14 Matrix: soil Instrument: Varian 3400 Dual ECD Analytical technique: GC/ECD Single lab validation by SL Division: Tallahassee Extractables mL Volume ext: ___ -or- Wt. ext.(dry): 10.8 g Extraction Solvent: MEC12 Final Solvent: Kexane Final Volume: 10 mL Purgeables Amount purged: _____raL -or- ___g soil in _____mL K20 Analyte: Spike level(unit) _ Replicate 1_______ Replicate 2_______ Replicate 3______ Replicate 4______ Replicate 5______ Replicate 6______ Replicate 7______ Average result___ (n-1)sd_________ MDL*____________ PQL* *___________ Is spike level<6x calculated MDL?__ SL GQAP PQL______ Isodrin _yes 4.0" schlorb 37 ug/kg 14.6 15.7 14.6 19.0 12.4 12.5 15.6 14.9 2.24 7.03 22.4 yes 80 Mirex 15 ug/kg 6.59 6.44 6.45 6.51 4.08 5.24 6.05 5.91 0.923 2.93 9.32 yes ~~^i *MDL = sd(n-l) X 3.14 **PQL = sd(n-l) x 10 $Chlorb=Chlorbenzilate Remarks: Analyst: D. Koren QA Manager: E.L. Schneider QA Objectives c Analyte: Isodrin Chlorobenzilatt Mirex md PQL's to be Accuracy ( %Rec ) » added to Table £ Precision (%RPD) >: Completeness (%) PQL (ug/kg) 2.0 50 20 ^1 TUT 006 0180 METHOD VALIDATION Appendix A Page Number 15 Date: 08/07/91 Method: 8081 Reference: EPA SW-846 Matrix: groundwater Instrument: Varian 3400 Dual ECD Analytical technique: GC/ECD Single lab validation by SL Division: Tallahassee Volume ext: -or- Wt. ext.(dry): Extractables 1000 mL Extraction Solvent: MEC12 Final Solvent: Hexane Final Volume: 10 mL Purgeables Amount purged: _____mL -or- ___g soil in _____mL K20 Analyte: Spike level (unit) Replicate 1 Replicate 2 Reolicate 3 Replicate 4 Reolicate 5 Replicate 6 Replicate 7 Average result (n-l)sd MDL* PQL** Is spike level<6x calculated MDL? SL GQAP PQL Kepone 10 ua/L 9.56 10.9 10.7 8.60 7.95 10.2 9.26 9.60 1.10 3.45 11.0 yes 0.050 *MDL = sd(n-l) x 3.14 Analyst: Amy Hayes **PQL = sd(n-l) x 10 QA Manager: E.L. Schneider Remarks: Spike level was too high. Reanalysis at a lower level will result in a lower MDL and PQL. QA Objectives and PQL's to be added to Table 5: Analyte: Kepone Accuracy (%Rec) Precision (%RPD) Completeness (%) PQL (ug/L) 10 TUT 018.1 Appendix A Page Number 16 METHOD VALIDATION Date: 08/07/91 Method: 8081 Reference: EPA SW-846 Matrix: soil Instrument: Varian 3400 Dual ECD Analytical technique: GC/ECD Single lab validation by SL Division: Tallahassee Extractables Volume ext: ___ -or- Wt. ext.(dry): 10 mL Extraction Solvent: MEC12 Final Solvent: Hexane Final Volume: 10 mL Purgeables Amount purged: _____mL -or- ___g soil in _____mL K20 Analyte: Spike level(unit) _ Replicate !_______ Replicate 2______ Replicate 3______ Replicate 4______ Replicate 5 - • - • • Replicate 6_______ Replicate 7 •- Average result - (n-l)sd__________ MDL*____________ PQL* *____________ Is spike level<6x calculated MDL?___ SL GQAP PQL______ Kepone 2000 ug/kg 1850 1940 1920 1890 1920 1920 1810 1890 47.7 150 477 no 100 *MDL = sd(n-l) x 3.14 **PQL = sd(n-l) x 10 Analyst: Amy Hayes QA Manager: E.L. Schneider Remarks: Spike level was too high. Reanalysis at a lower level will result in a lower MDL and PQL. QA Objectives z Analyte: Kepone md PQL's to be Accuracy (%Rec) added to Table ! Precision ( %RPD)Completeness (%) PQL (ug/kg) 500 ~ TUT O06 0.1.82 METHOD VALIDATION Appendix A Page Number 17 Date: 08/09/91 Method: 8141 Reference: SW846 Proposed Update I Matrix: groundwater Instrument: Varian 3300 GC Analytical technique: GC/NPD Single lab validation by SL Division: Tallahassee Volume ext: -or- Wt. ext.(dry): Extractables 1000 mL __ g Extraction Solvent: MeCl2 Final Solvent: Hexane Final Volume: 10.0 mL Purgeables Amount purged: '_____mL -or- ___g soil in _____mL H20 Analyte: Spike level (unit) _ Replicate 1 Reolicate 2 Replicate 3 Replicate 4 Reolicate 5 Replicate 6 Replicate 7 Average result (n-l)sd MDL* PQL** Is spike level<6x calculated MDL? SL GQAP PQL Thionazin 0.50 ug/L 0.445 0.420 0.470 0.458 0.421 0.442 0.405 0.437 0.0230 0.072 0.23 no (x6.9) 1.0 Sulfotepp 0.50 ug/L 0.438 0.423 0.433 0.435 0.395 0.401 0.365 0.413 0.0270 0.085 0.27 yes 1.5 Phorate 0.50 ug/L 0.406 0.400 0.432 0.422 0.380 0.385 0.351 0.397 0.0273 0.086 0.27 ves 1.5 Dimethoate 5.0 ug/L 3.81 3.50 5.58 5.96 4.52 4.72 - 5.02 -• 4.73 - 0.887 2.79 8.87 yes 10 Disulfoton 0.50 ug/L 0.484 0.467 0.506 0.505 0.454 0.432 0.420 •••--. 0.453 0.0356 0.112 0.36 yes 2.0 *MDL = sd(n-l) x 3.14 Analyst: Talicia Smith **PQL = sd(n-l) x 10 QA Manager: E.L. Schneider Remarks: DB-17 column reported; DB-5 results similar.__________ QA Objectives and PQL's to be added to Table 5: Analyte: Thionazin Sulfotepp Phorate Dimethoate Disulfoton Accuracy (%Rec) Precision (%RPD) Completeness (%) PQL (ug/L) 0.50 0.50 0.50 10 0.50 TUT OO6 O.183 METHOD VALIDATION Appendix A Page Number 18 Date: 08/09/91 Method: 8141 Reference: SW846 Proposed Update I Matrix: groundwater Instrument: Varian 3300 GC Analytical technique: GC/NPD Single lab validation by SL Division: Tallahassee Extractables 1000 mL Volume ext: -or- Wt. ext.(dry): Extraction Solvent: MeC12 Final Solvent: • Kexane Final Volume: 10.0 mL Purgeables Amount purged: _____roL -or- ___g soil in _____mL H20 Analyte: Spike level(unit) _ Replicate 1______ Replicate 2_______ Replicate 3______ Replicate 4______ Replicate 5______ Replicate 6______ Replicate 7 Average result___ (n-1)sd_________ MDL*____________ PQL* *___________ Is spike level<6x calculated MDL?__ SL GQAP PQL_____ Methyl oarathion no(x9.3)_ ~0.30 Ethyl parathion 0.50 ug/L "0.438___ "0.410___ "0.443___ "0.435___ "0.389___ ~0.416___ "0.382___ "0.416___ "0.0241___ "0.076___ "0.24 no(x6.6)_ "l.O Faiaphur 2.0 ug/L_ "l.79 _yes 10 *MDL = sd(n-l) x 3.14 **PQL = sd(n-l) x 10 Analyst: Talicia Smith QA Manager: E.L. Schneide: Remarks: DB-17 column reported; DB-5 results similar. QA Objectives c Analyte: Methyl parath. Ethly parath. Famphur md PQL's to be Accuracy ( %Rec) added to Table 5 Precision (%RPD) Completeness ( % )PQL (ug/L) 0.30 0.50 2.0 ^ TUT OO6 0184 METHOD VALIDATION Date: 08/07/91 Method: 8141 Reference: EPA SW846 Appendix A Page Number 19 Matrix: soil Instrument: Varian 3300 Dual NPD Analytical technique: GC/NPD Single lab validation by SL Division: Tallahassee t- ———————————— Extractables Volume ext: ___ -or- Wt. ext. (dry) : 10 Extraction Solvent: Final Solvent: Final Volume: L ——————— _______ _ mL g MeCl2 Kexane 10.0 mL Purgeables Amount purged: mL -or- g soil in mL K20 —————— i ———————————— I ———————————— : ————— —————— , Analyte: Spike level (unit) Reolicate 1 Reolicate 2 Replicate 3 Replicate 4 Replicate 5 Reolicate 6 Renlicate 7 Average result (n-l)sd MDL* PQL** Is spike level<6x calculated MDL? SL GQAP PQL Thionazin 50 ug/kg 56.5 35.9 53.2 48.9 53.8 46.2 50.5 49.3 6.81 21.4 68.1 ves 200 Sulfotepp 50 ug/kg 54.9 49.6 51.0 51.7 51.2 49.3 48.7 50.9 2.07 6.51 20.7 no 300 Phorate 50 ug/kg 48.1 44.4 48.8 43.1 41.3 34.9 41.5 43.2 4.69 14.7 46.9 yes 300 Dimethoate 500 ug/kg 754 569 269 595 472 601 *** . 543 162 509 1621 yes 2000 Disulfoton 50 ug/kg 39.5 46.8 52.8 36.8 29.6 14.6 32.0 • • --• 36.0 12.4 39.0 124 yes 400 *MDL = sd(n-l) X 3.14 **PQL = sd(n-l) X 10 Analyst: Talicia Smith QA Manager: E.L. Schneider Remarks: DB-17 column reported; DB-5 results similar. ***-Replicate 7 for dimethoate had a result of 178 and was not used. Calculations based on (n-l)sd of 6 points. (factor=3.36) QA Objectives c Analyte: Thionazin Sulfotepp Phorate Dimethoate Disulfoton md PQL's to be Accuracy ( %Rec) added to Table f Precision ( %RPD) Completeness (%) PQL (ug/L) 100 20 50 2000 200 TUT OO6 0185 METHOD VALIDATION Date: 08/07/91 Method: 8141 Reference: EPA SW-846 Appendix A Page Number 20 Matrix: soil Instrument: Varian 3300 Dual NPD Analytical technique: GC/NPD Single lab validation by SL Division: Tallahassee Extractables Volume ext: -or- Wt. ext.(dry): 10 Extraction Solvent: MeC12 Final Solvent: Kexane Final Volume: 10.0 mL Purgeables Amount purged: _____mL -or- ___g soil in _____mL H20 Analyte: Spike level(unit) _ Replicate 1______ Replicate 2______ Replicate 3______ Replicate 4______ Replicate. 5______ Replicate 6______ Replicate 7 Average result___ (n-1)sd________ MDL*_____________ PQL* *___________ Is spike level<6x calculated MDL? SL GQAP PQL______ Methyl parathion _50 ug/kg_ 51.5___ "40.4____ "49.5____ "45.8____ "50.2____ "44.6____ "45.2____ "4 6 .7____ "3.87____ "12.2 "38.7 _yes_ 60 Ethyl parathion _yes 200" 81 _yes mphur 0 ug/kg 9 3 61 0 6 9 3 .8 3 >s )00 *MDL = sd(n-l) X 3.14 **PQL = sd(n-l) X 10 Analyst: Talicia Smith QA Manager: E.L. Schneidej Remarks: DB-17 column reported; DB-5 results similar._ QA Objectives 2 Analyte: Methyl parath. Ethly parath. Fanrohur md PQL's to be Accuracy ( %Rec) added to Table f Precision (%RPD) Completeness (%) PQL (ug/kg) 50 50 500 TUT 006 01.86 METHOD VALIDATION Appendix A Page Number 21 Date: 08/07/91 Method: 8270 Reference: USEPA SW-846 Matrix: groundwater Instrument: HP SVMS 2 Analytical technique: GC/MS Single lab validation by SL Division: Tallahassee Extractables Volume ext: -or- Wt. ext.(dry): 700 mL __ 9 Extraction Solvent: MeCl2 Final Solvent: MeC12 Final Volume: 1 mL Purgeables Amount purged: _____mL -or- ___g soil in _____mL H20 Analyte: Spike level(unit) _ Replicate 1______ Replicate 2 ___ Replicate 3______ Replicate 4______ Replicate 5______ Replicate 6______ Replicate 7______ Average result____ (n-1)sd__________ MDL*_____________ PQL* *____________ Is spike level<6x calculated MDL?___ SL GQAP PQL______/ 1, 4-Dioxane 20 ug/L 7.64 10.0 9.56 9.11 8.84 7.53 8.71 8.76 0.920 2.89 9.2 yes 10 ========== ========== ========= - • • •-«••' *MDL = sd(n-l) x 3.14 **PQL = sd(n-l) x 10 Remarks: Analyst: David Karnes QA Manager: E.L. Schneider QA Objectives and PQL's to be added to Table 5: Analyte: 1,4-Dioxane Accuracy ( %Rec )Precision ( %RPD) Completeness (%) PQL (ug/L) 10 TUT OO6 O187 METHOD VALIDATION Date: 08/07/91 Method: 8270 Reference: USEPA SW-846 Matrix: soil Instrument: HP SVMS 2 Analytical technique: GC/MS Single lab validation by SL Division: Tallahassee Appendix A Page Number 22 Extractables Volume ext: ___ -or- Wt. ext.(dry): 30 mL Extraction Solvent: MeC12 Final Solvent: MeC12 Final Volume: 1 inL Purgeables Amount purged: ______raL -or- ___g soil in ______nL K20 Analyte: Spike level(unit) _ Replicate 1______ Replicate 2_______ Replicate 3______ Replicate 4______ Replicate 5______ Replicate 6_______ Replicate 7_______ Average result____ (n-1)sd__________ MDL*_____________ PQL* *____________ Is spike level<6x calculated MDL?___ SL GQAP PQL_______ 1,4-Dioxane 467 ug/kg 287 213 289 254 288 245 257 261 28.3 88.9 283 yes 330 *MDL = sd(n-l) x 3.14 **PQL = sd(n-l) x 10 Remarks: Analyst: David Karnes QA Manager: E.L. Schneider QA Objectives z Analyte: 1,4-Dioxane ind PQL's to be Accuracy ( %Rec) added to Table I Precision (%RPD) > : Completeness (%) PQL (ug/kg) 330 ~ TUT O06 GIB8 Appendix A Page Number 23 METHOD VALIDATION Date: 05/06/92 Method: 3080/608.1 Reference: SW846 3rd Ed. Matrix: water Instrument: Varian 3400 Dual ECD Analytical technique: GC/ECD Sinale lab validation by SL Division: Tallahassee Volume ext: —or — Wt. ext.(dry): Extractables lOOOmL cont liq-liq ___ a Extraction Solvent: MeCl 2 Final Solvent: Hexane Final Volume: lOmL Purgeables •Amount purged: "______ml_ -or- ____a soil in ______mL H20 Analyte: Spike level (unit) Replicate 1 Replicate 2 Replicate 3 Repl icate 4 Repl icate 5 Repl icate 6 F:epl icate 7 Averaoe result Cn-nsd MDL* PEL** Is spike level<6x calculated MDL? SL GQAP PQL i ———————— _. — , Chloroneb 0.20 uq/L 0.23/0.24 0.25/0.25 _0.24/0.25_ 0.25/0.26 _0.23/0.24_ 0.24/0.24 _0.24/0.24_ 0. 240/0. 246 0.008/0. 008 0.026/0.025 0.082/0.079 noC7.8/8. 1) 0.4 Propachlor 0.21 uq/L 0.21/0.21 0.21/ —— 0.20/0.21 0.22/0.22 0.20/0.20 0.21/0.21 _0.21/0.21_ 0.209/0.210 0.007/0.006 0.022/0.021 0.069/0.06'' no (9. 2/9. 6) 10 #Ch lore-prop 0.25 uq/L _0.25/0.26_ 0.27/0.24 0.^7/0.26 0.23/0.28 0. 25/0. 26 0.25/0.26 0.25/0.21 0.263/0.253 0.011/0.022 0.035/0.070 0. 111/0.221 no-7. 16 /yes 2 . 0 i —— . ——— • ———— ttEtridiaz* 0.010 ug/L_ —— /0.011 —— /0.010 —— /0.011 —— /0.011 —— /0.011 —— /0.011 —— / 0.011 —— /O. 01 036 —— /O. 00038 —— /O. 00 119 —— /O. 00378 not —— /8. 4) 0.4 *MDL = sdt'n-l) x 3.14 Analyst: Dana B. Till **PQL = sd(n-l) x 10 GA Manager: E.L. Schneider Remarks:Results are presented from both GC columns: DB5/DB608. *Etridiazole exhibited matrix interference in water on the DB—5 column. ItChl ore-prop = Chl oropropyl ate ttEtridiar = Etridiazole !QA Objectives and PQL's to be added to Table 5: ! Analyte: ! Chloroneb ! Propachlor 1 Chl oropropyl at« ! Etr idiarol e l l Ac c ur ac y C XRec !> ? PrecisionCXRPD) Compl eteness O'.) PQL Cug/L) 0.40 0. 50 0 . 50 0.01 0 TUT 006 0.189 METHOD VALIDATION Appendix A Page Number 24 Date: 05/06/92 Method: 8080 Reference: SW846 3rd Ed. Matrix: soil Instrument: Varian 3400 Dual ECD Analytical technique: GC/ECD Single lab validation by SL Division: Tallahassee Extractables Volume ext: ___ mL —or — Wt. ext.(dry): 30g sonic. Extraction Solvent: MeC12 Final Solvent: Hexane Final Volume: 1OmL Purgeables Amount purged: ______mL —or — ____a soil in ______mL H20 Analyte: Spike 1 evel (uni t ) Renl icate 1 Reel icate 2 RBD! icate 3 Reol icate 4 Reel icate 5 Reel icate 6 Reol icate 7 Averaae result (n-l)sd MDL* FQL** Is spike level<6x calculated MDL? SL GQAP PQL Chloroneb 6.60 ua/ka 7.0/6.7 7.3/7.7 7.4/7.3 6.9/7.4 7. 1/7.6 6.7/7.4 6.7/7.4 7.01/7.34 0.27/0.32 0.86/1.01 2.73/3.21 no<7.7/6.6) Pr op ac hi or 6.6O ug/kq 7. 1/6.5 7.8/7.2 8.0/7. 1 S. 1/6.9 7.3/6.7 7.4/6.7 7.3/6.7 7. 57/6. S3 0.39/0.25 1.23/0.78 3. 90/2. 50 yes/no-8.42 ttChloroprop 8.25 ua/ka 9.9/12.0 11.0/13.0 11.0/13.0 10.0/12.0 9.9/10.0 10.0/10.0 9.7/10.0 10.21/11.43 0.55/1.40 1.71/4.39 5.46/13.97 ve= #Etr idia:* 1.65 ua/ka 1.0/1.3 1.3/1.5 1.4/1.6 1.4/1.6 1.3/1.7 1.4/1.6 1.4/1.6 1.31/1.56 0. 15/0. 13 0.45/0.40 1.46/1.27 yes • *MDL = sd(n-l) x 3.14 **PQL = sd(n-l) x 10 Remarks:Results are presented from both . 4tChlor opr op = Chlor opropylate Analyst: Dana B. Till QA Manager: E.L. Schneider QC columns: DB5/DB608. ttEtridiaz = Etridiazole !QA Objectives and PQL's to be added to Table 5: ! Anal yt e: , _ _ — — __ —— —— ! Chloroneb ! Propachlor ! Ch 1 or op r op y 1 at E ! Etr id iazol e ii AccuracyCXRec ) i PrecisionC/.RPD) Compl eteness<*/) PQL (ug/L) 13 16 16 0.33 TUT OO6 O19O METHOD VALIDATION Appendix A Page Number 25 Date: 05/06/92 Method: 8150 Reference: SWS46 3rd ed. Matrix: water/soil Instrument: Varian 3400 dual ECD Analytical technique: GC/ECD Single lab validation by Sl_ Division: Tallahassee Volume ext: —or — Wt. ext.(dry): Extractables SOOmL water 30a soil Extraction Solvent: ethyl ether Final Solvent: hexane Final Volume: S.OmL Puraeables Amount purged: -or- ____q soil in mt_ mL H20 water soil DB-5 DB-1301 DB-5 DB-1301 Anal yte: Spike level Cunit) _ Repl icate 1 Reel icate 2 Repl icate 3 Repl icate 4 Repl icate 5 Repl icate 6 Rep 1 i c at e 7 Averaae result Cn-1 i>sd MDL* PQL** Is spike level<6x calculated MDL? SL GQAP PQL Picl or am 0. lOua/L 0. 108 0 . OS6 0.090 0. 101 0.094 0.097 0.097 0.0976 0.0057 0.0178 0.0568 yes Pic lor am 0. lOuq/L 0. 110 0. 102 0.091 0. 104 0.098 0.098 0 . 098 0. 1001 0.0060 0.0187 0.0596 yes Pic lor am 1 . 67ug/kq 2.7 2.7 2.8 2.7 3.2 *7* 1 O.I 2.8 2.857 0.^-07 0 . 650 2.070 yes Pic 1 or am 1 . 67uq/ka 3.0 3.0 3. 1 3. 1 3.6 3. 1 3.0 3. 129 0.214 0 . 67 1 2. 138 yes *MDL = sd(n-i:> x 3. 14 **PQL = sd(n-l) x 10 Remar ks: Analyst: Susan Harrison QA Manaaer: E.L. Schneider QA Objectives c Anal yte: Picl or am and FQL's to be Ac c ur ac y < 7.Rec ) added to Table ! Precision(7.RPD) 5: Completeness C7.) PQL tug /kg) wf • O TUT OO6 0191 VAL1 DAT I ON ' App.ji-i.j i .-.. A Page Number 2£ Date: 05/06/92 Method: 8141 Reference: SW846 3rd ed. Final update Matrix: water Instrument: Varian 3400 Dual NPD Analytical technique: GC/Ni'D Single lab validation by SL Division: Tallahassee 4 — ——————————— —— ; ——— ——— ——— ——— —— —— ———— —— ——— — ——— • Extrac tables Pi Volume ext : lOOOmL cont liq-liq —or— Amount pi UJt. ext. (drv) : q Extraction Solvent: MeC12 Final Solvent: hexane Final Volume: lOmL jrgeabl es arqed: mL -or - q soil in mL H20 DB-5 DB-1701 DB-5 DB-1701 ! Anal yte: j =================== ! Spike level (unit ) IRepl icate 1 ! Reel ic ate 2 I Reel icate 3 IRepl icate 4 IRepl icate 5 IRepl icate 6 1 Reel icate 7 lAveraae result 1 Cn-l)sd :MDL* : PQL** !Is spike leveKGx Calculated MDL? ISL GQAP PQL Di ox at hi on 6.0ua/L 5.26 5. 15 6.21 5.90 6.17 5.08 6.63 5.771 0.610 1 . S 1 5 6.O97 ves 2.0 Dioxath ion 6.0uq/L 4.08 4.03 O • GO 3.49 3.92 3.58 5.52 4.079 0.675 2. 121 6.754 ves 2.0 SDichlof en l.Ouq/L 1. 14 1. 13 1. 10 1 . 09 1 . 09 1 . OS 1. 14 1.110 0.026 0.081 0 . 258 noC12.3) 1.0 TrDichl of en l.Oua/L 0 . 96S 0 . 899 0.833 0.867 0.87S 0.855 0 . 89""-' 0.893 0.036 0.114 0.364 noCS.8) 1.0 *MDL = sd(n-l) x 3. 14 **PDL = sdCn-1) x 10 Remarks: #Dichlofen = Dichlofenthion Analyst: Susan Harrison QA Manaqer: E.L. Schneider QA Objectives < Analyte: Dioxath ion Dichlofenthion t- — __ — ———— _ —— •ind PQL's to be AccuracyCy.Rec) added to Table J PrecisionCXRPD) •j: Comp 1 et eness < '/.") PGL <ug/L) 10 1 .0 TUT OO6 O192 METHOD VALIDATION Appendix A Page Number 27 Date: 05/O6/92 Method: 8141 Reference: SW346 3rd Ed. Final update Matrix: soil Instrument: Varian 3400 Dual NFD Analytical technique: GC/NPD Single lab validation by SL Division: Tallahassee Extractables Volume ext: • ___mL —or — Wt. ext.(dry): 30g Extraction Solvent: MeC12 Final Solvent: Hexane Final Volume: lOmL Purgeables Amount purged: ______mL —or — ____a soil in ______mL H20 ! Analyte: I Spike level (unit) IRepl icate 1 IRepl icate 2 I Replicate 3 IRepl icate 4 IRepl icate 5 IRepl icate 6 ! Reel icate 7 lAveraae result 1 (n-l)sd IMDL* 1 PQL** lls spike level<6x 1 calculated MDL? ,'SL GQAP PQL H ——————————————————————————— | *MDL = sd<n-i:> x **PQL = sdCn-1) x Dioxath ion 200 ua/kq 245/140 250/160 248/149 236/116 247/94.3 192/74.0 247/94.3 233/118.2 20.7/32.3 65.05/101.5 207/323 ves 66 ——————————— i 3. 14 10 4tDichlof en 33.3 uq/kq 37.7/28.6 39.3/33.2 38.2/30.9 39.7/31.3 38. 3/25.4 39.8/27.6 38.3/25.4 38.77/23.91 O.S'VS.Ol 2.57/9.47 8. 18/30. 15 no-13. 0/yes 33 ——————————— i Ter butryn 66.7 ua/kq 66.0/57.0 73.0/64.3 70.3/61.7 54.0/53.6 21.8/23.2 54.9/55.3 78.4/28.2 59.77/49.76 19.02/15. 17 59.72/47.65 190/152 ves 66 ——————————————— H Analyst : Su<;an Harr ison QA Manager: E.L. Schneider Remarks:Results are presented from both GC columns: DB5/DB1701. • ttDichlofen = Dichlofenthion !QA Objectives and PQL's to be added to Table 5: I Analyte: ! Dioxath ion ! D i c h 1 o f en t h i on ! Terbutryn ii i j —————————— _. —— Accuracy(7.Rec) Precision<7.RPD) Compl et eness CX) FQL Cug/kgj 330 *~t~\ «_>O *?TA •^<*j*.f TUT 019."=% METHOD VALIDATION Appendix A Page Number 28 Date: O5/06/32 Method: 8141/613 Reference: SW846 3rd Ed. Final Update I/EPA Matrix: wj Instrument: Varian 3400 Dual NPD Analytical technique: GC/NFD Binale lab validation by SL Division: Tallahassee Extractables Volume ext: lOOOmL -or - Wt. ext.(dry): __g Extraction Solvent: MeC12 Final Solvent: Hexane Final Volume: lOmL Furqeables Amount purged: ______ml_ —or — ____Q soil in _______ml_ H20 •*• ——— —————————————— —— — ! Analyte: ISpike level (unit) IReolicate 1 ! Repl icate 2 ! Repl icate 3 SRepl icate 4 !Repl icate 5 JRepl icate 6 ! Repl icate 7 ' ! Average result __ I (n-l)sd ;MDL* ; PQL** ! Is spike level<6x ! calculated MDL? !3L GQAP PQL *MDL = sd<n-i:> x **PDL = sdCn-1.1 x Ametryn __ 1.5 ug/L_ 2.05/1.44 1.56/1.67 1.63/1.42 1.50/1.60 2.20/1.55 1.34/1.52 1.56/1.63 _1.70/1 .56_ 0.312/0. 106 0.373/0.332 3. 12/1.06 yes 2.0 i ——————————— | 3. 14 10 i — .__ — —— ___. — | Atr az ine _ 1 . 5 ug/L_ 1.61/lIlS 1. 17/0.333 1. 16/1.02 1. 10/0.362 1.70/1. IS 1.00/0.865 1.07/0.331 _1.26/1.01_ 0.^79/0. 115 O.S76/0.362 2.73/1. 15 ves 2.0 i ——————————— i GA I— —— • ———————— i Prometryn _1.5 ug/L_ 2. 14/1.45 1.66/1.56 1.67/1.38 1.56/1.50 2.20/1.52 1.51/1.43 1.58/1.54 _1.76/1.43_ 0.285/0.060 0.835/0. 183 2.85/0.603 _yes/no-7. 3 *> ("t ~ . ^.' Analyst: Sus Manager : E. L >.— . _____ .___ —— i Prometon* _ 1 . 5 ug/L_ —— /I. 13 —— /0.913 —— /I. 14 —— /0.43S —— /I. 25 —— /0.442 —— / 0.338 _ —— /0.301_ —— 10.320 —— / 1 . 00 —— /3.20 —— /yes 2.0 ;an Harr ison .. Schneider h— —————————— ———— —— t Propaz ine _1.5 ug/L _ 2.52/1.73 1.85/1.57 1.87/1.53 1.76/1.51 2.28/1.7? 1.66/1.4 1.72/1.47~* _1.35/1.5S_ 0.3^-VO. 120 1.01/0.375 3.22/1. 135 yes "> ii ^. • U i Remarks: Results are presented from both GC columns: DB5/DB1701. *Prometon and Simasine co-elute on the DB-5 column. !QA Objectives and PDL's to be added to Table \ Analyte: ! Ametryn ! Atr az ine ! Prometryn ! Prometon ! Prop a- ine Ac c ur ac y C 7.P*ec )Pr ec i s i on C 7.RPD )Comp 1 et en ess C '/. ')FQL (ug/L) 2.0 2. . 0 2. 0 2. 0 2. 0 TUT OO6 O194 Append i >: A Paae Number 2'5 METHOD VALIDATION Date: 05/06/92 Method: 3141/619 Reference: SW846 3rd Ed. Final Update I/EPA Matrix Instrument: Varian 3400 Dual NPD Analytical technique: GC/NPD Single lab validation by SL Division: Tallahassee wat er Extractables Volume ext: —or - Wt. ext.(dry): lOOOmL Extraction Solvent: MeC12 Final Solvent: Hexane Final Volume: lOmL Purgeables Amount purged: ______ml_ —or — ____a soil in ______ml_ H20 1 ————————————— ———— — 1 ! Analyte: i — ——————————— iSpike level (unit) [Replicate 1 ! Replicate 2 IReol icate 3 IReol icate 4 ! Repl icate 5 ! Replicate £ ! Repl icate 7 lAveraae result ! (n-l)sd !MDL* :FQL** ! Is spike level<&x 1 calculated MDL? !SL GQAP PQL Simaz ine* 1.5 ua/L —— /I. £4 —— /I. 41 —— /I. 44 —— /I. 38 —— /I. 77 —— /I. 17 —— /I. 33 —— /I. 45 —— / 0.201 —— /O.£30 —— /2.01 —— /yes 2.0 STerbuthyl 1.5 ua/L 2.40/1.78 2.50/1.54 1.89/1.53 1.76/1. 43 2.44/1.80 2.34/1.35 1.73/1.45 2. 15/1. 5£ 0.343/0. 1£S 1.08/0.529 3.43/1.68 yes 2.0 Ter butryn 1.5 uq/L 2.50/2.89 2.96/3.42 3.08/3.57 2.79/3. 17 2.74/3. 14 2. £5/3. 05 2.94/3.37 2.81/3.23 0.20^/0. ''35 0. £35/0. 739 *> C\"> f~' ^^ — • i.'^./ •_. ^^^j no— £. 30/yes 2.0 *MDL = sdCn-1) x 3.14 **PQL = sdCn-1) x 10 Analyst: Susan Harrison QA Manaaer: E.L. Schneider Remarks: Results are presented from both GC columns: DB5/DB1701. . *Prometon and Simazine co—elute on the DB-5 column. ttTerbuthyl = Terbuthylazine 4—————————————————————————:_:———————————————————————————————————————————. !QA Objectives and PQL's to be added to Table 5: ! Analyte: ! Simaz ine ! Terbuthyl az ine ! Ter butryn i i i Ac c ur ac y < X.Rec )PrecisionC/RPD) Completeness (X.1 PQL Cug/L) 2 . 0 2. <> 2.0 TUT 006 0195 METHOD VALIDATION Appendix rt Page Number 3O Date: 05/06/92 Method: 8141/619 Reference: SWB46 3rd Ed. Final Update I/EPA Matrix: so Instrument: Varian 3400 Dual NPD Analytical technique: GC/NPD Sinole lab validation by SL Division: Tallahassee Extractables Volume ext: ____ml_ -or - Ult. ext. (dry) : 30g Extraction Solvent: MeC12 Final Solvent: Hexane Final Volume: lOmL Puraeables Amount purged: ______ml_ -or - ____a soil in ______ml_ H20 Anal yte: Spike level (unit) Repl icate 1 Repl icate 2 Reol icate 3 Repl icate 4 Repl icate 5 Repl icate 6 Repl icate 7 Averaae result <n-l)sd MDL* PQL** Is spike level<&x calculated MDL? SL GQAP PQL Ametryn __ 50 ug/kg_ 54.8 49.3 49.8 56.5 - 52.9 56.5 55.6 53.6 3.02 9.49 30 . 2 yes 66 Atraz ine __ 5O ug/kg_ 36.9 34.0 34.6 29.5 28.2 29.0 29.0 31.6 3.49 10.95 34.9 yes <-%*^ *Jn-> Prometryn __ 50 ug/kg_ 48.9 45.0 45. 1 50.6 47.5 50 . 6 49.6 4S . 2 '•• . 38 7. 43 23.8 no C 6.7) 66 Prometon __ 50_ug/kg_ 54.9 47.2 50.0 39. 1 *!>O • Cr ^Q ^% wO • w 37.7 43.0 7.77 24.4 77.7 yes 66 Pr opaz ine 50 ua/ka 53.4 4S.8 49.5 45.4 i^ p ^ *J . O 45. 1 45.2 47.3 O -^ ^ fcj • *T h_i 1 0 . 76 ^l .4 ^ >*J^ • ^ yes 66 ——I————————————I———————————(.. Analyst: Susan Harrison QA Manaqer: E.L. Schneider *MDL = sd(n-l) x 3.14 **PQL = sd(n-l) x 10 Remarks: DB-17 Meqabore column !QA Objectives and PQL's to be added to Table 5: ! Anal yte: ! Ametryn ! Atr ar ine ! Prometryn ! Prometon ! Pr opaz ine Ac c ur ac y C '/.Rec )PrecisionC/RPD) Compl eteness (7.) PQL <ug/kg) 66 £6 66 £6 66 TUT OO6 0196 Appendix ft Paae Number 31 METHOD VALIDATION Date: 05/O6/92 Method: 8141/619 Reference: SW846 3rd Ed. Final Update I/EPA Matrix: soil Instrument: Varian 3400 Dual NPD Analytical technique: GC/NPD Single lab validation by SL Division: Tallahassee 1 ——————————————————————————————————— - Extractables Vol ume ext : mL -or- Wt. ext. (dry) : 20g Extract ion Solvent : MeC12 Final Solvent : Hexane Final Vo 1 ume : 1 OmL Pur geabl es Amount pur aed : mL — or — a soil in mL H20 Analyte: Spike level (unit) Repl icate 1 Replicate 2 Reel icate 3 Reel icate 4 Reol icate 5 Reol icate & Reol icate 7 Averaae result <n-i:>sd MDL* PQL** Is spike leveKSx calculated MDL? SL GQAP PQL Simaz ine 50 Lia/ka 56.8 52.4 53.7 42.5 39.8 41.2 41.7 46.9 7. 13 22.4 71.3 ves ^^ u»sO ttTerbuthyl 50 uq/ka C'C' < O^J. 1 50.9 51.8 44.5 43.0 43.9 44.6 47.7 4.83 15.2 43.3 ves 66 Ter butryn 133 ua/ka 104.8 92. 1 90.6 111.4 99.3 106.0 109.9 102. 1 8.26 25 . 9 82. 6 ves 66 *MDL = sd<n-l) y. 3.14 **PGL = sd<n-l> x 10 Remarks: ttTerbuthyl = Terbuthylazine DB-17 Meqabore column. Analyst: Susan Harrison QA Manaqer: E.L. Schneider !QA Objectives and PQL's to be added to Table ! Analyte: ! Simaz ine ! Terbuthyl az ine ! Ter butryn ! ; +• —————————————————————— Ac c ur ac y ( XRec )PrecisionC/.RFD) Compl etenessOO PQL (ug/kg) 66 66 330 ——— .__ —— . — —— i T I. IT- 006 O197 -iGTHOD VALIDATION Appendix A Page Number 22 Date: 04/28/92 Method: 632 Reference: EPA Matrix: water Instrument: Waters 600E/WISP Analytical technique: HPLC/UV Sinale lab validation by SL Division: Tallahassee 1 ——————————————— Extrac Volume ext: — or — Wt. ext. (dry) : Extraction Sol Final Solvent: Final Volume: tables lOOOmL a vent: MeC12 ACN ImL _. — .-i ——————— ———— i — . —— . —— . ——— — — ——— — —— — . —— —— _ — — __ — —— ^ Pur geabl es Amount ouroed: mL -or - a so i 1 i n mL H20 -. —— . ———— 1 ——————————————— ———— 4- — . ————————————————— 1 —— ——— ———————————— Analyte: Spike level (unit) Real icate 1 Reol icate 2 Reel icate 3 Real icate 4 Replicate 5 Repl icate 6 Real icate 7 Average result (n-l)sd' MDL* PQL** Is spike level<6x calculated MDL? SL GQAP PQL Bromac il — — — _ __ _ _ ^ _ «. ~. 1.0 ua/L 1.01 1.01 0.96 1. 10 0.92 1.01 1.06 1.01 0.059 0. 19 0.6 yes 2.0 • *MDL **PQL Remar ki sd(n-l) x 3. 14 sdCn-1) x 10 CIS column. Analyst: Paul Rygiel QA Manaaer: E.L. Schneider QA Objectives < Analyte: Br omac i 1 ind PQL's to be Ac c ur ac y < "/.Rec ) added to Table ! Precision(7.RPD) C-omp letenessCX) PQL (ug/L) 2.0 TUT OO6 O.198 Appendix A Paae Number 33 METHOD VALIDATION Date: 05/O4/92 Method: 504 Rev. 2.0 Reference: EPA/60O/4-SS/039 Matrix: water Instrument: Shimadzu GC '5AM Dual ECD Analytical technique: GC/ECD Single lab validation by SL Division: Tallahassee Extractables Volume ext: —or — Wt. ext.(dry): 38mL _ g Extraction Solvent: Hexane Final Solvent: Hexane Final Volume: 3.0ml_ Purgeables Amount purged: _______ml_ -or - ____a soil in ______mL H20 -1 ————— —————— ————————————— ! Anal yte: ISpike level (unit) _ ! Reol i cats 1 ! Replicate 2 ! Repl icate 3 ! Reel icate 4 ! Replicate 5 ! Repl icate 6 ! Replicate 7 lAveraae result ! (n-l)sd :MDL* : PQL** !Is spike level <6x ! calculated MDL? !SL GQAP PQL 4.. ————— __ —————————— t i ——————————— EDB _0.020 ug/L 0.017?" 0.01 91 0.0174 0. 184 0.0204 0 . 0 1 94 0.0211 0.0191 0.001361 0.00427 0.0136 ves 0.020 uq/L —————— _. — . — i i ————— .. ——— DBCP 0.020 ug/L 0.0170 0.0230 0.0160 0.0190 0.0180 0 . 0220 0.0230 0.0197 0 . 0029277 0.00919 0.0293 yes 0.020 uq/L #Chl oropic 0.0080ug/L 0.00817 0.00754 0.00817 0 . 008SO 0.00817 0 . 008SO 0 . 0089S 0. OOS37 0.00050444 0. 0015S 0. 00504 ves 0.010 UQ/L ———— — ————— . —————— 4 I ———————————————————— 1, 1-DCPa _ 2.7 ug/L 2.95 3 . 00 3.00 3 . O6 2.89 2.89 2.68 T.- •!•'•• 0 . 1 24 0.290 1.24 no(6.9) 0. 50ua/L i ——— • —— •— — — t tfTh iocyan _ 20.0 ug/L 26. 1 26.7 27.4 26.4 26. 1 27.7 27 . 2 26.8 0.643 2.02 *• .* *"* O • TO no (9. 9) 75.0uq/L *MDL = sdCn-1) x 3.14 **PQL = sd(n-l) x 10 Analyst: Martin Thomas QA Manaoer:' E.L. Schneider Remarks: Results are from DB-5 column. DB-17O1 results are very similar • DBCP on DB-1701 MDL=O.0078f PDL=0.0247 »Chl oropic = Chlorop icr im. 81,1-DCPa = 1, 1-Dic hi ore-prop an e. = methyl isothiocyanate. QA Objectives < Anal yte: 31, 1-DCPa ftThiocvan \nd PQL's to be Ac c ur ac y ( 7.Rec ) added to Table : Precision(7.RPD> j: C'-<mp 1 et enes s ( 7. ) PDL (ug/L) 2.0 20 TUT OO6 O.199 METHOD .VAL ! D.',T I OK Append 1 x A Page Number 34 Date: 05/04/92 Method: 504 Rev. 2.0 Reference: EPA/600/4-88/039 Matrix: water Instrument: Shimadzu 6C-9AM Dual ECD Analytical technique: SC/ECD Single lab validation by SL Division: Tallahassee *•— • ——————— — ' ——— ——————— —— Extr actabl Vol ume ext : —or — Wt . ext . (dry) : Extraction Solvent Final Solvent: Final Volume: es oSmL Q : Hexane Hexane 3.0mL Purgeabl es Amount puraed: mL —or — a so i 1 i n mL H20 - —————————— l. ——— ——————————————— i —————— _. ——————————— u_. ——— . —————— . —— Analyte: Spike level (unit) Replicate 1 Replicate 2 Reel icate 3 Replicate 4 Reol icate 5 Repl icate 6 Repl icate 7 Averaae result (n-l)sd MDL* PQL*-* Is spike leveKGx calculated MDL? SL GQAP PQL ttcis-DCPe ! 0. US uq/L! 0.116 ! 0.110 ; 0. 113 ! 0.114 ! o.io7 : o .108 : o.ii3 : 0.112 ; 0.0033 ! 0.0104 ; 0.0331 !ii no (11. 4) ! 1.0 (total) ! fctrans-DCPe 0.0792 ua/L O.OBS6 0.0866 0.0802 0 . 0802 0.0323 0.0760 0.0887 0 . 0829 0.00454 0.0142 0.0454 yes 1.0(total :> • — *• *MDL = sdCn-l) y, 3. 14 **PQL = sd(n-l) Y. 10 Analyst: Martin Thomas QA Manaqer: E.L. Schneider Remarks: #cis-DCPe = cis-1,3-Dichloropropene #trans-DCPe = trans-1, 3-Dichloropropene QA Objectives « Analyte: 1 , 3-Dichloro- propene (total ) and PQL's to be Ac c ur ac y ( X.Rec ) added to Table 1 PrecisionC/RPD) 5: Compl eteness (.'/.') PQL (ug/LX 1 . 0 TUT 006 0200 >:rr:-:oD VALIDATION Date: 07/09/92 Appendix A Pace Kur.ber 37 Ke~hod: 8330 Mod if iec Reference: SU'S£6 Proposed Undate T I / S L Matrix: varer Instrument: Waters 600;/*66 uv Derocror Analytical technique: ppi.r/i;y validation by SL Division: Tallahassee_____________._____ £>:tr a c tables Volurae ext: -or- Wt. ext.(dry): nl Extraction Solvent: Final Solvent: Final Voluae: nl Purgeables Anount purged: -or- ___g soil in al _:nl H20 Analyte: Snike level (unit) Henlicate 1 Heolicate 2 ' Reolicate 3 • Replicate 4 Reolicate 5 P.eulicate 6 P.eolicate 7 Averaoe result fn-l)sd KDL* PQL** Is soike level<6x calculated KDL? SL GQA? ?QL Nitroglycerir 8.0 U2/1 7.96 6.96 6.96 • 7.96 • 7.96 S.96 7.96 7.S2 0.690 •> •> 6.9 ves . ._., _. _ Analyst: Paul Rvgjel *MDL = sd(n-l) X 3.14 **?QL = sd(n-l) X 10 QA Manager: Elizabeth L. Schneice: Recarks: Sanple preparacion consists of filcracion. The filcered szicale is______ _________injecced direeclv inco the KPLC svscem.__________________________ QA Objectives and PQL's to be added to Table 5: Analyte: Nicrozlvcerin Accuracy (%Rec) 71-121Z Precision (%RPD) 0-22% Completeness (%) ?QL ( Uc/i ) !0 TUT 006 0201 XITHOD VALIDATION Dc'e: 07/Q9/°? Appendix A Pace JCur.ber 3S Method:' 8330 M o d i f i e d Reference: svRAft P^nn^c^ v^s?™ T T ' S L Matrix: yn- Instrument: y?r*r* finnr/^si \\\> ngrgprn" Analytical technique: KPLC/UV Single lab validation by SL Division: Tallahassee Zxtractables Volume ext: ___ -or- Kt. ext.(drv): 2.0 Extraction Solvent: ______ Final Solvent: 1:1 ACN;5c/l CaC12 Final Voluse: 10____-.1 ACN Purceables Araount purged: -cr- ___g soil in _-.i :-:2o Analyte: Soike level (unit) Heolicate 1 Henlicate 2 Heolicate 3 Dedicate 4 P.STlicaze 5 P.eolicate 6 Seolicate 7 Averace result fr.-ilsd HDL* ?QL** Is soi>:e level<6>: calculated KDL? SL GQA? ?QL Kicroglyceri: 250 ug/ke 29t 29A 331 220 40i 257 257 294 60.12 169 601 ves . . - • . Analvst: Paul Rvsiel *MDL = sc(n-l) X 3.14 **?QL = sd(n-l) x 10 QA Manager: Elizabeth L. Sehnelde: Remarks: Mobile phase * 65:55 ACK:uater: uavelenerh - 209nni._______________ QA Objectives and PQL's to be added-to Table 5: Analyte: Hicrozlvcerin Accuracv(%?.ec) 46-190% Precision (%?.?D) 0-72Z Cor:oleceness (%) ?QL ( ,,c/i-c ) i nnn TUT 006 0202 Appendix A Page Number 35 KETEOD VALIDATIOH Date: Julv' 15. 1991 Method: 8330 Reference: SW 846 Proposed Update II Matrix: Water Instrument: Waters/LC Analytical technique: KPLC/UV Extractables Volume ext: ml -or- Wt. ext. (dry): g Extraction Solvent: Final Solvent: Final Volume: ml ————————————————————————————————— -i Purgeables Amount purged: ml -or- a soil in ml K20 n-NDPA = n-Nitrosodiphenylamine DPA = diphenylamine Analyte: . Spike level (unit) Replicate 1 Replicate 2 Replicate 3 Replicate 4 Replicate 5 Replicate 6 Replicate 7 Average result fn-Dsd MDL* PQL** Is spike level<6x calculated MDL? SL GQAP PQL u— . ——— —— . ————————— —— . — .— -i n-NDPA, 10 ug/L 13.3 12.0 12.0 13.3 12.0 13.3 12.0 12.5 0.69 2.17 6.9 YES N/A DPA 10 ug/L 11.2 12.8 10.6 10.1 10.6 10.6 11.2 11.0 0.88 2.75 8.8 YES N/A — __. — . —— ___-: "* *MDL = sd(n-l) X 3.14 **PQL = sd(n-l) x 10 Analyst: /^cd1 —— - R. Driver QA Manager: o(. L. Schneider Remarks: Accuracy & precision targets were derived from 6 mid-level spikes. The range for DPA is extremely small and will be updated when more data points are acquired. QA Objectives c Analyte: n-NDPA DPA ind PQL's to be Accuracy (%Rec) 55-121 65-95 added to Table '. Precis ion (%RPD) 0-20 0-20 5 : Completeness (%) 96-100 96-100 PQL (ug/L) 10 10 TUT OO6 O2O3 XZTHOD VALIDATION Date: 06/23/92 Appendix A Page Number 36 Method:' 6330 Reference: SU846 Proposed Uodare T Matrix^ Instrument: Vacers HPT.c/Kratos fluorescgnceAnalytical technique: detector/Waters UV detector Single lab validation, by SL Division: Tallahassee_________ Zxtractables Volujae ext: ____ lal -or- Wt. ext.(dry): 2.0 q Extraction Solvent: aeetonicrile Final Solvent: acetonicrile Final Voluae:. 10 al. Purgeables Amount purged: -or- ___g soil in nl ttl H20 Analyte: Snike level (unit) Reolicate 1 Reolicate 2 Reolicate 3 Reslicate 4 Reolicate 5 Renlicate 6 Renlicate 7 Average result (n-l)sd MDL* ?QL** Is spike level£6x calculated HDL? SL GQAP PQL D?A* 50.0 ue/ke 62.0 57.0 £6,0 46.0 A2.0 49.0 46.0 46.9 5.113 16.1 51 ves nnDPA** 50.0 ue/ke 60.0 60.0 55.0 40.0 35.0 40.0 47.0 47.0 10.286 32.3 103 ves _ _ _ Analyst: Paul Ryeiel *MDL = sd(n-l) X 3.14 **?QL = sd(n-l) x 10 QA Manager: Elizabeth L. ScWeider____ Renarks : *DPA" diphenylamine; **nnDPA" n-nitrosodiphenylataine_________________— Analysis performed using an isocratie mobile phase of 70Z nechanol/30Z va'ter: Cie column. QA Objectives a Analyte: DPA nnDPA ind PQL's to be Accuracy ( %Rec ) 50-125 3^-158 added to Table f Precision (%?J?D) 0-35 0-35 . 5: Conpleteness (%) - PQL (ue/ke ) 100 inn TUT 006 O204 XTTKOD VALIDATION Appendix A Pace Date: 07/06/92______ Method: 7041/3005 Reference: SWS46 3rd. Ed. ____ Instrument: Varian SpeccrAA-400_______. Analytical technique: GFAA-Zeeman Single lab validation by SL Division: Tallahassee Matrix: vacer Extra Volume ext: -or- Kt. ext. (dry) : Extraction Solv Final Solvent: Final Volume: ctables 100 ent : ml g 100 ml , Purgeables Amount purged: ml -or- g soil in nl H20 Analyte: SDike level (unit) Renlicate 1 Replicate 2 . Reolicate 3 Reolicate 4 Renlicate 5 Reclicate 6 Reolicate 7 Average result (n-l)sd MDL* PQL** Is spike level£6x calculated KDL? SL GQAP PQL Antimony 0.050 ms/1 0.0437 0.0412 0.0454 0.0470 0.0449 0.0430 0.04^5 O.OAi2 0.00185 0.00581 0.0165 no C8.61 0.020 , " *KDL = sd(n-l) x 3.14 **?QL = sd(n-l) x 10 Reaarks: Analyst: Todd Baumearrner______ QA Manager: Elizabeth L. Schneider QA Objectives c Analyte: Antimonv . ind PQL's to be Accuracy (%Rec) 80-120% added to Table : Precision (%RPD) 0-202 5 : Completeness (%) PQL (me/1 ) 0.020 • TUT '-'06 O2O5 VALIDATIOX Date: 07/06/92 Appendix A Pace K ur.be r Matrix: soil Method: 70M/3050 Reference: SW6^6 3rd. Ed.________ ____ Instrument: Varian SoeccrAA-400______ Analytical technique: CFAA-Zeeman Single lab validation by SL Division: Tallahassee___________________ Extractables Volume ext: -or- Wt. ext.(dry): 0.50 Extraction Solven Final Solvent: Final Volume: 100 Ell Purgeables Amount purged: -or- ___g soil in l H20 Analyte: Spike level (unit) Reolicate 1 Reolicate 2 Replicate 3 Reolicate 4 Reolicate 5 Reolicate 6 Renlicate 7 Average result (n-l)sd KDL* ?QL** Is snike level<6x calculated KDL? SL GQAP PQL ' Antimony 10.0 me/ke d 8.56 8.78 9.12 7.80 8 ?n 9.«0 7.72 8.51 0.6i! 2.01 6.M ves 5.0 .* Analvst: Toed *MDL = sd(n-l) x 3.14 **?QL = sd(n-l) x 10 QA Manager: Elizabeth L. Schneider Remarks: Digestion method 3005 is not applicable co soil. The normal 3050 digestion method vas employed. KBS 1633A soil watrix was used. QA Objectives i Analyte: Ant into nv ind PQL's to be Accuracy ( %Rec) 70-1302 • added to Table : Precision (%R?D) 0-30% 5 : Completeness (%) PQL ( W e / V o n v ) s.n TUT 006 0206 Savannah Labs fethod Validation SL Tallahassee APPENDIX A Page Number riethod: B27C Rsference: SW84i Proposed update 1 Katpis: SOIL Technique: GC/HS Dace:07/OS/92 EXTRACTABLES VoluflE/tess EIT; Extraction Method Solvent: Final Voluae; Final Solvent; Instrument Analyst: Cocpound Hare ETHYL CARBAfttTE : 3Cg : sonication : KeC12/Acetone : 1 r.l : feC12 : SfS2 : Teresa Rygiel Spike Level L"nit 333 uo/kg PUR6EABLES: Asount (H20): or Soil amount: in (ols water): For & Rl R2 R3 167 195 215 Bis 0 els Results >ven replicates R4 R5 1 186 206 . H20 tent Digested: Soil Aant Dioested: Final Voluae: ols 9 ols R6 R7 AVE s(n-l) KDL POL Y/N Factor SLFK. 183 194.1 10.9P? 34.226 W.&3 No 9.7 QA Objectives and PQLs to be added to Table 5: Analyse Accuracy Precision Ethyl carbamate 4S-100Z 0-20Z POL (ug/kg dw) 200 * = is spike level </= is calculated KDL? TUT 006 0207 Savannah Labs fethod Validation APPENDIX A Page Number Method: 8276 Reference: SW34A Proposed update 1 Katrix: Groundxater Technique: K/K3 ETTRACTASLES Voluee/Kass ETT: 10313 fils Extraction Method: cent 11 Solvent: HeC12 Final Voluae: 1 Final Solvent: feC12 Cocpound Nauoe ETHYL CARKVttTE Spike Level Unit 10 uo/1 Dace: 06/30/92 Instrument: SHS2 Analyst: Teresa Rygiel PJRSEABLS: Assu-.t (K20J: nls or Soil ajcount: g in (nls water): els Results For Seven replicates METALS: K20 tent Digested: Soil ftsnt Digested: Final Volume: els 9 • is Rl R2 R3 R5 R6 R7 A1^ s(n-l) KL P2L Y/K Factor SL^ 6.31 6.?4 7.22 6.9i 7.35 7.52 6.9 6.555 1.733 5.5?7 Yes 5.7 ^ -/ QA Objectives and PQLs to be added to Table 5: Analyte Accuracy Precision PQL(ug/l) Ethyl carbamate 52-100Z 0-242 10 TUT 006 0208 * = is ssike levsl </= ix ca!c-!l£t?j fiDL?