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1ST SAMPLING REPORT SEPTEMBER 1990 TUTU WELLS SITE QUARTERLY SAMPLING ST. THOMAS, U.S. VIRGIN ISLANDS January 1991 Prepared for Tutu Environmental Investigation Committee Geraghty & Miller, Inc. 290 Vincent Avenue Hackensack, New Jersey 07601 (201) 646-1400 1828 *64429* 64429 CONTENTS Page INTRODUCTION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 SAMPLING AND ANALYTICAL PROCEDURES . . . . . . . . . . . . . . . . . . . . . . . . . . 1 Procedural Deviations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 RESULTS AND DISCUSSION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4 Data Quality Provisions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4 Organic Analytical Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 Inorganic Analytical Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 RECOMMENDATIONS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8 TABLES 1. Summary of Organics Analysis of Ground-Water Samples Collected From Water Supply Wells, September 1990 Sampling Event, Tutu Wells Site, St. Thomas, USVI. 2. Summary of Inorganics Analysis of Ground-Water Samples Collected From Water Supply Wells, September 1990 Sampling Event, Tutu Wells Site, St. Thomas, USVI. 3. Proposed Sampling Effort for the 2nd Sampling Event (February 1991), Tutu Wells Site, St. Thomas, USVI. FIGURE 1. Well Sampling Locations, Tutu Wells Site Sampling, Analysis, and Monitoring Plan, St. Thomas, USVI. APPENDIX A. Data Validation Summary Report for the Tutu Wells Site, September 1990 Quarterly Sampling, St. Thomas, USVI. 1329 GERAGHTY & MILLER. INC. 1ST SAMPLING REPORT SEPTEMBER 1990 TUTU WELLS SITE QUARTERLY SAMPLING ST. THOMAS, U.S. VIRGIN ISLANDS INTRODUCTION The Tutu Wells Site 1st Quarter (September 1990) Sampling Report was prepared by Geraghty & Miller, Inc. for both the Tutu Environmental Investigation Committee (TEIC), which is comprised of Texaco Caribbean Inc. (Texaco) and Esso U.S. Virgin Islands (Esso), and L'Henri, Inc. (O'Henry). This report was prepared in accordance with the requirements detailed in the "Sampling, Analysis, and Monitoring Plan (SAMP) for Wells, Tutu Wells Site, St. Thomas, U.S. Virgin Islands," September 1990, which was approved by the U.S. Environmental Protection Agency (USEPA) in its September 21, 1990 letter to TEIC and the Administrative Order (Order) effective March 22, 1990. The objectives of the SAMP are to identify, quantify, and monitor the occurrence of gasoline constituents and tetrachloroethene (commonly referred to as perchloroethylene and abbreviated as PCE), and its breakdown products, in certain wells in the vicinity of Route 38 within the Tutu Wells Site (Figure 1). SAMPLING AND ANALYTICAL PROCEDURES The sampling was conducted from September 24 through October 3, 1990 by Soil Tech and Geraghty & Miller. USEPA representatives were present for the sampling conducted through September 28, 1990. Additionally, representatives of the USEPA's Monitoring Management Branch (MMB) were present in an audit capacity on September 24 and 25, 1990. A representative of the Virgin Islands Department of Planning and Natural Resources (DPNR) was present throughout the sampling event. TIJI" 002 1830 GERAGHTY & MILLER. INC 2 Sampling and analysis were performed as described in the SAMP, with the exception of the few deviations outlined in the following sectionJn brief, the wells were sampled and analyzed for the Target Compound List (TCL) and Target Analyte List (TAL) constituents, with the exception of polychlorinated biphenyls (PCBs), under the Contract Laboratory Program (CLP). Volatile organic compound (VOC) analyses were performed in accordance with a modified version of EPA Method 524.2 in order to achieve lower detection levels. The modifications to EPA Method 524.2 which were adopted are described in Appendix A of the SAMP. The samples were collected in 23 of the 24 wells sampled for the September 1990 sampling event utilizing the permanent pumps and piping systems. These wells were evacuated prior to sampling by pumping the wells for a minimum of 15 minutes. One well (Gassett), which is not outfitted with a permanent pump, was evacuated and sampled using a peristaltic pump. The analytical data was validated by Geraghty & Miller in accordance with the USEPA Standard Operating Procedures (SOP) No. HW-2, February 1990 for inorganic compounds and the USEPA SOP No. HW-6, March 1990 for organic compounds. The data validation summary and the complete data set (tabulated) are provided in Appendix A. Details of the sampling and analysis procedures, data validation requirements, and reporting requirements are provided in the SAMP. Procedural Deviations Deviations from the scope of work and procedures as presented in the SAMP are outlined below. 1. Four Winds Well No. 1 was not sampled during the September 1990 sampling event when it was discovered that the pump, which was thought to be in good working order, was inoperable at the start of the sampling event. TUT 002 1831 GERAGHTY & MILLER. INC 3 2. The well sampled on the Gassett property (formerly Hartman 1) during the September 1990 sampling event was the same well which was formerly sampled by USEPA and was proposed to be sampled in the SAMP. The well is located near the fence on the north side of the Gassett property. When USEPA and TEIC representatives examined the well in August 1990, it became clear that the integrity of the well had been compromised based on the repon of the USEPA Technical Assistance Team (TAT) member who previously sampled the well. It was decided, and approved by USEPA, to sample a newer well located on the Gassett property, hi its place. The new well is located behind the building and consists of 6-inch diameter PVC which extends several feet above ground surface. However, during the September 1990 sampling event, the old well near the fence was sampled. Additionally, the sample from the well was collected using a peristaltic pump, instead of a Teflon™ bailer. Due to problems associated with sounding and evacuating the well, the well volume could not be determined, and it is unlikely that 3 well volumes were removed prior to sampling. 3. The 1:1 hydrochloric acid (HG) used to acidify the VOC samples was reagent grade and not ultra pure grade. The sampling team attempted to obtain ultra-pure grade HC1, but was unable to do so due to shipping problems. 4. The samples for cyanide analysis were preserved by adding sodium hydroxide (NaOH). However, for some of the samples, the pH was not raised to greater than 12. While this requirement was not stated in the plan, it is recognized as a requirement and will be met in subsequent cyanide analyses. 5. One sample (Smith) was analyzed for VOCs using EPA Method 624, instead of Method 524.2 in order to perform the analysis within the holding time. GERAGHTY & MILLER, INC. 4 6. Although the analysis for PCBs was not required for this project, they were analyzed for; the analytical results are provided in this report. 7. The Tillett well was pumped for a minimum of 15 minutes prior to sampling, as specified in the SAMP. However, due to logistical problems associated with containing the evacuated water, the water was pumped at a low rate and only approximately 110 gallons were removed prior to sampling. Data provided by the U.S. Geological Survey (USGS) indicates that the Tillett wells is 100 feet deep and 6 inches in diameter. Assuming a depth to water of 20 feet, it is calculated that 3 well volumes is equal to approximately 360 gallons. RESULTS AND DISCUSSION A summary of the organic analytical results is provided in Table 1. Table 1 includes only the organic compounds which were detected; the complete organics analytical results are provided in tabulated form in Appendix A. The inorganic analytical results are summarized in Table 2. Data Quality Provisions A discussion of the data validation findings is provided in Appendix A. In general, the overall quality of the data set is acceptable and meets the project data quality objectives. For some data, however, there are some provisions which should be noted. As discussed in USEPA's MMB CERCLA Limited Technical Systems Audit for the September 1990 sampling, air bubbles were found to be present in several of the VOC sample bottles. When the VOC bottles were originally filled, no bubbles were apparent; the bubbles came out of solution later. While every effort was made to avoid this condition, a few of the samples (Eglin 1, LaPlace, Tillett, and Tillett Replicate) analyzed by the laboratory contained air bubbles. In this event, the data validation SOP requires that all GERAGHTY & MILLER. INC. 5 positive detections be assumed to be minimum values and that all non-detections be rejected based on the assumption that all VOCs in the water would diffuse into the air bubble, and consequently escape analysis and detection. In reality, it is likely that any volatile organic compound present would stabilize in both the air and water at concentrations related to the compound vapor pressure. In any event, the compounds which were consistently detected in the four affected samples (PCE, trichloroethene [TCE], and 1,2-dichloroethene [1,2- DCE]) were also consistently detected throughout the data set and comprise the constituents of concern at the site. It is unlikely that the undetected compounds in the four affected samples are present in ground water at the site. Holding time violations resulted in the rejection of some of the mercury analytical results. In most instances, the mercury holding time of 28 days was exceeded by only 1 or 2 days; for one sample the holding time was exceeded significantly. Unsatisfactory instrument calibrations resulted in the rejection of some results. For some samples, non-detection of acetone, 2-butanone, 2-hexanone, trans-l,3-dichloropropene, and vinyl acetate were rejected due to poor instrument response factors and continuing calibration performance. Poor sensitivity for acetone and similar compounds is not unusual at low detection levels. Moreover, these compounds are not constituents of concern at the site. Spike recovery values outside of quality control limits contributed to the rejection of some data. The acid fraction of the Tillett Replicate analysis was rejected because the acid surrogate recoveries were out of control limits, and the thallium data was rejected because the matrix spike recoveries were out of control limits. The laboratory suggested that the thallium recoveries may be affected by the high natural dissolved solids concentrations in site ground water. Additionally, some of the antimony and mercury data was rejected for several samples because the recovery for the laboratory standard for one run was out of control limits. OO2 1834 GERAGHTY & MILLER, INC. 6 Many constituent concentrations are estimated due to quality control inadequacies related to holding times, sample preservation, calibration performance, spike recoveries, and quality control studies. Although many of the constituent concentrations are estimated, their identification and quantitation were subject to strict quality control requirements and therefore, the reported values are likely to be within a reasonable range of the true values. The overall quality of the data set is acceptable; there was good reproducibility between replicate samples and the chief constituents of concern were consistently detected. Organic Analytical Results As indicated in Table 1, VOCs constitute the chief analyte group of concern at the Tutu Wells Site. The compounds which were consistently detected in site samples are PCE, TCE, and 1,2-DCE. All three compounds were detected in the following wells: Eglin 1, 2, and 3; Hartman 2; Smith; Four Winds 2; Four Winds 2 Replicate; Steele; LaPlace; Matthias; Tillet; and the Tillett Replicate. Additionally, one or two of these compounds were detected in wells Hartman 3, Harvey, Ramsey, and VIHA 1. VOC tentatively identified compounds (TICs) were identified in 12 out of the 24 site samples. Eight compounds were tentatively identified and unknown compounds were detected. Total estimated VOC TIC concentrations ranged from 3 to 435 micrograms per liter (ug/L). The presence of methylene chloride and acetone in site and blank samples is attributed to laboratory contamination. Other VOC compounds which were detected in site samples include chloroform in well VIHA 3 (3 ug/L), and vinyl chloride (17 ug/L) and benzene (32 ug/1) in both the Tillett and Tillett Replicate sample. GERAGHTY & MILLER, INC. 7 No semi-volatile (base-neutral and acid extractable organic compounds) or pesticide organic compounds were detected in any of the site samples. One library search semi- volatile compound (penta-chlorofluorobenzene; 4 ug/1) was detected in the Tillett Replicate sample and unknown semi-volatile organic compounds were detected in several samples. In general, the wells in which VOCs were detected are located in the central Tutu valley. No VOCs were detected in wells outside the central valley. The wells in which no VOCs were detected include: the Dimitri and Leonard wells located significantly upgradient of the central Tutu valley; the Bryan well which is located in the next drainage subbasin to the west; and the Devcon 1 and 3, Dench, and Dede wells located significantly downgradient from the central Tutu valley (see Figure 1). Additionally, no VOCs were detected in the Gassett (Hartman 1) or Rodriguez wells which are located at the southern end of the central Tutu valley. Inorganic Analytical Results The inorganics analytical results are provided in Table 2. The inorganic concentrations were within acceptable ranges. While some cation concentrations (calcium, magnesium, potassium, and sodium) were elevated in relation to potable water quality typical of North America, the concentrations were within the range of concentrations commonly detected in ground water pumped from domestic, commercial, and public supply wells in the U.S. Virgin Islands. The heavy metal concentrations detected were all below the Federal Primary Drinking Water Standards, where applicable. Lead concentrations, which were of particular interest due of the possibility of past gasoline releases, were all below the Federal Primary Drinking Water Standard. GERAGHTY & MILLER, INC. 8 RECOMMENDATIONS The 1st Quarter results meet the prescribed objectives of the SAMP. It is recommended to continue to implement the plan with a few minor changes. First, the deviations from the sampling and analysis procedures detailed in the SAMP will be rectified for the remaining quarterly sampling events. Second, it is recommended that the analytical problems associated with the thallium and antimony analyses be reviewed so that subsequent analyses will provide acceptable data. It may be necessary to alter the analytical method in order to achieve this; if so, all revisions will be approved by USEPA before implementation. Furthermore, it is recommended to resample for mercury for the samples which were analyzed after the holding time elapsed. Proposed analyses for the 2nd sampling event, which is tentatively scheduled to begin on February 4, 1991, are based on the results of this report The proposed sampling effort for February 1991 is detailed in Table 3. For VOC analysis, it is proposed to sample only those wells in which VOCs other than laboratory contaminants (methylene chloride and acetone) were detected hi the 1st Sampling Report. Additionally, it is proposed to sample the Gassett well for VOCs because the September 1990 sampling procedure used for this well was not in keeping with the procedures described in the SAMP. It is also proposed to sample for thallium, antimony, mercury, and selenium in the wells for which these data were rejected due to quality control inadequacies. Sampling and analysis T U T GERAGHTY & MILLER, INC. 9 for semivolatile organic compounds, pesticides, and PCBs are not proposed for the 2nd, 3rd, or 4th sampling events because these compounds were not detected in any of the wells. Respectfully Submitted, GERAGHTY & MILLER, INC. MF:gv #PR00801/1STQTR.RPT Marcia Findlay Senior Scientist Daniel A. Nachman Senior Associate GERAGHTY & MILLER, INC. Table 1. Summary of Organic. Analysis of Ground-Water Samples Collected from Water Supply Wells, September 1990 Sampling Event, Tutu Well Site, St. Thomas, USVI. Sample Identification: VOLATILE ORGANIC COMPOUNDS Methylene chloride Chlorometnane Acetone 1,2-Dichloroethene Trichloroetnene Tetrachlorocthene Tentatively Identified VOCs Propane, 2-methoxy-2-methy1 unknown compound SBMIVOLATILE ORGANIC COMPOUNDS Tentatively Identified SVOCs unknown compound PESTICIDE /PCBs Dede ND ND R ND ND ND ND ND 4JN ND Dench ND 1J R ND ND ND 6JN ND ND ND Devcon 1 1NDJ ND R ND ND ND ND ND 4JN ND Devcon 3 8NDJ ND R ND ND ND 2JN ND ND ND Eglin 1 R R R -mm 10 J*te 6JN 3JN ND 12 JN ND Eglin 2 5NDJ ND R *-^Bp!t 22J »«B« 220 JN ND ND ND Eglin 3 10NDJ ND 22J *M 14 «Mi 5JN ND ND ND Hartman 2 \ 1NDJ ND R r 5ju It ?J 3JN ND ND ND Hartman 3 3NDJ ND R 2 ND U 4JN ND ND ND Harvey 1SONDJ ND R ND ND *•» ND ND ND ND Leonard ND ND R ND ND ND ND ND ND ND Rodriguez 1NDJ ND R ND ND ND UN ND ND ND Rodriguez Replicate 2NDJ ND R ND ND ND ND ND ND ND Analytical results are reported in mkrograms per liter (ug/1); equivalent to parts per billion. VOCs Volatile organic compounds. SVOCs Semivolatile organic compounds. ND Compound not detected. J Estimated concentration. For tentatively identified compounds, all concentrations are estimated. For other compounds, this data qualifier indicates that either the compound is present but al concentrations lower than the contract required quantitalion limit, or that due to quality control problems, the data is provisional and therefore the concentrations are estimated. R Data rejected. N Compound is a tentatively identified compound. Pace 2 of 4 Table 1. Summary of Organic! Analysis of Ground-Water Samples Collected from Water Supply Wells, September 1990 Sampling Event, Tutu Well Site, St. Thomas, USVI. V; y Sample Identification: VOLATILE ORGANIC COMPOUNDS Methylene chloride Chloromethane Acetone 1,2-Dichloroethene ' Trichloroelhene Telrachloroethene Total Xylenes Toluene Tentatively Indentified VOCs l,U-Trichloro-lA2-trifluoroetbai»e Propane, 2-methoxy-2-methyi Dichlorobenzene isomer unknown compound SEMIVOLATILE ORGANIC COMPOUNDS Tentatively Identified SVOCs PESTICIDE /PCBs Smith 12NDJ ND 25NDJ* vHftfc ND ND 88 JN ND ND ND Four Winds 2 14NDJ ND R 6J vttsjMP ND ND 15 JN ND ND ND Four Winds 2 Rep. 10NDJ ND R 4J t&JM ND ND 7.5 JN ND ND ND Trip Blank 9/24 25J ND 12 J ND ND ND 8 ND 5JN NA NA NA Trip Blank 9/25 34J ND 42 J ND ND ND 7 1 3JN UN 7JN NA NA NA Trip Blank 9/26 24 J ND 4J ND ND ND ND ND 7JN NA NA NA Steele 140 ND J ND R 130 J ND ND 42 JN ND ND ND Dimilri 2NDJ ND R ND ND ND ND ND ND ND ND ND Bryan 2NDJ ND R ND ND ND ND ND ND ND ND ND Analytical results are reported in micrograms per liter (ug/l); equivalent to parts per billion. VOCs Volatile organic compounds. SVOCs Semivolatile organic compounds. ND Compound not detected. NA Compound not analyzed. J Estimated concentration. For tentatively identified compounds, all concentrations are estimated. For other compounds, this data qualifier indicates that either the compound is present but at concentrations lower than the contract required quantitatioo limit, or that due to quality control problems, the data is provisional and therefore the concentrations are estimated. Rep. Replicate. R Data rejected. N Compound '» a tentatively identified compound. Table 1. Summary of Organic* Analysis of Ground-Water Samples Collected from Water Supply Wells, September 1990 Sampling Event, Tutu Well Site, St. Thomas, USVI. Sample Identification: VOLATILE ORGANIC COMPOUNDS Methylene chloride Acetone 1,2-Dichlofoethene Tricbioroeibene Tetrachloroetbene Vinyl chloride Benzene Chloroform Tentatively Indentifled VOCs l,l,2-Trichloro-l,2£-trifluoroethane Propane, 2-methoxy-2-methyl Aliphatic hydrocarbon C3-Benzene isomer C5H12 isomer C6H12 isomer C9H12 isomer unknown compound Trip Blank 9/27 16 J R ND ND ND ND ND ND ND Trip Blank 10/1 13 J 6J ND ND ND ND ND ND UN Trip Blank 10/2 14 J 7J ND ND ND ND ND ND 3JN Trip Blank 10/3 ND R ND ND ND ND ND ND 1.5 JN Gassett Ramsey Laplace (Hartman 1) 17NDJ R R R ND MM ND ^| 3J Ut ND R ND R ND R 130 JN 2JN 1NDJ R ND ND ND ND ND ND 2JN Matthias VIHA 1 9NDJ 2NDJ R R MM 6J >•*> ND MMfc 5J ND ND ND ND ND ND ND 16 JN VIHA 3 2NDJ R ND ND ND ND ND 3 UN TiUet R ND *& «*r ^^^^^^^ T7J 32 J R 240 JN 6JN 6JN 121 JN 35 JN 6JN 21 JN Tillett Replicate 44NDJ 52NDJ 270J 47 J f 98J 12J 26J R 270 JN 230 JN 39 JN Analytical results are reported in mkrograms per liter (ug/1); equivalent to parti per billion. VOCs Volatile organic compounds. ND Compound not detected. NA Compound not analyzed. J Estimated concentration. For tentatively identified compounds, all concentrations are estimated. For other compounds, this data qualifier indicates that either the compound is present but at concentrations lower than the contract required quantitatkw limit, or that due to quality control problems, the data is provisional and therefore the concentrations are estimated. R Data rejected. N Compound is a tentatively identified compound. Table 1. Summary of Organic* Analysis of Ground-Water Samples Collected from Water Supply Wells, September 1990 Sampling Event, Tutu Well Site, St. Thomas, USVI. Sample Identification: SEMTVOLATTLB ORGANIC COMPOUNDS Tentatively Identified SVOCs Benzene, pentachlorofluoro unknown compound PESTICIDE /PCBs Trip Blank 9/27 NA NA NA Trip Blank 10/1 NA NA NA Trip Blank 10/2 NA NA NA Trip Blank 10/3 NA NA NA Ramsey ND ND ND Laplace ND 42 JN ND Gassett (Hartmanl) Matthias VIHA1 V1HA3 Tillet ND ND ND ND ND ND ND 12 JN 4JN 37 JN ND ND ND ND ND Tillelt Replicate ND 4JN 82 JN ND Analytical results are reported in mkrograou per liter (ug/1); equivalent to parts per billion. SVOCs Semivolatile organic compounds. ND Compound not detected. NA Compound not analyzed. J Estimated concentration. For tentatively identified compounds, all concentrations are estimated. For other compounds, this data qualifier indicates that either the compound is present but at concentrations lower than the contract required quantilatkm limit, or that due to quality control problems, the data is provisional and therefore the concentrations are fttlmtH, N Compound is a tentatively identified compound. ec Table 2. Summary of Inorganic* Analysis of Ground-Water Samples Collected from Water Supply Wells, September 1990 Sampling Event, Tutu Well Site, St. Thomas, USVI. Sample Identification: INORGANIC ANALYTBS Aluminum Antimony Arsenic Barium Beryllium Cadmium Calcium Chromium (Total) Cobalt Copper Iron Lead Magnesium Manganic Mercury Nickel Potassium Selenium Silver Sodium Thallium Vanadium Zinc Cyanide Dede 136 BJ R ND SB 3BJ 5 23500 16 J 60 J 32 43 B 3.7 J 25600 201 ND ND 2000 B 1NDJ 7NDJ 324000 R 21 B 12 BJ ND Dench 278 J R ND 19 B 4BJ 3B 24200 22J 44 BJ 52 163 7.8 J 25000 545 ND 73 1690 B 1NDJ 7NDJ 328000 R 28B 41J 6.8 B Devcon 1 139 BJ R ND 21 B 5BJ ND 41600 4NDJ ND ND 34B 8.2 J 39500 241 ND 13 B 2970 B 1.6 BJ 7NDJ 330000 R 32 B 6BJ 5NDJ Devcon 3 411 R ND 15 B 4BJ ND 43800 4NDJ 59 J 53 40 B 11.8J 41000 91 ND 41 2050 B 1.4 BJ 7NDJ 384000 R 20 B 6BJ 5NDJ Eglin 1 149 B ND ND ND 4B ND 35300 12 ND 14 BJ 20NDJ 2BJ 28700 56 R 26 BJ 920 B 10NDJ ND 190000 R 34 BJ 13 BJ ND Eglin 2 69 BJ R ND 23B 3BJ_ 4TOOO 17 J 32 BJ 36 86B 2.1 BJ 35400 SB ND 67 1620 B 1.2 BJ 7NDJ 247000 R 47 B 75 J 6.8 B Eglin 3 156 BJ R 3ND 57 B 4BJ ND 81400 10 J 30 BJ 9B 56 B 1NDJ 54600 53 ND 24B 2250 B 1.2 BJ 18 J 398000 R 9B 49 J 7.4 B Gassett (Hartman 1) 526 ND ND 7B 4B ND 31200 4B ND 10 BJ 418J 1.4 BJ 26300 853 R ND 880 B 10NDJ 7B 236000 R 26 BJ 5BJ ND Hartman 2 269J R ND 12 B 3BJ 38100 11J 30 BJ 34 23B 10.4 J 33400 ND ND 95 1040 B 1.6 BJ 7NDJ 285000 R 52 9BJ ND Hartman 3 278 R ND 15 B 4BJ ND 41100 11 J 25 BJ 30 31 B 1.8 BJ 28300 3B ND 52 1690 B 1NDJ 7NDJ 217000 R 124 13 BJ ND Analytical results are reported in microgram* per liter (ug/1); equivalent to parts per billion. ND Compound not detected. B Reported value obtained from a reading that was less than the contract required detection limit but greater than the instrument detection limit. j Estimated concentration. R Data rejected. vi/RT 1 Table 2. Summary of Inorganic* Analysis of Ground-Water Sample* Collected from Water Supply Wells, September 1990 Sampling Event, Tutu Well Site, SL Thomas, USVI. Sample Identification: INORGANIC ANALYTES Aluminum Antimony Arsenic Barium Beryllium Cadmium Calcium Chromium (Total) Cobalt Copper Iron Lead Magnesium Manganese Mercury Nickel Potassium Selenium Silver Sodium Thallium Vanadium Zinc Cyanide Smith 234 J R ND 15 B 3BJ ND 50200 14 J ND 13 B 158 10.9 J 45500 41 ND 57 1540 B R 7NDJ 410000 R ND 179 J ND Four Wind* 2 162 BJ R ND 15 B 3BJ 5 46100 32 J 29 BJ 37 55 B 8J 34000 28 ND 36B 2190 B 1.2 BJ 7NDJ 215000 R 75 85 J 8.5 B Four Winds 2 Rep. 304 J R ND 11 B 4BJ 6 54300 14 J 43 BJ 5B 57 B 8.7 J 38800 31 ND 44 2060 B 1NDJ 7NDJ 249000 R 83 88J ND Steele 492 J R ND 27B 3BJ 4B 44000 9BJ 55 J 21 B 26B 13.2 J 40500 23 ND 45 1180 B 1.4 BJ 7NDJ 313000 R 27 B 12 BJ 6.3 B Dimitri 163 BJ 52NDJ 3NDJ 3NDJ 4BJ 3BJ 37500 J 4BJ 18NDJ 17 BJ 115J 2.6 BJ 27800 J 7BJ R 14 BJ 2000 BJ 10NDJ 7NDJ 328000 J R 92 J 4NDJ SNDJ Bryan 149 B ND 3NDJ ND 3B 4BJ 54300 7B ND 17 BJ 63 BJ 4.6 J 49100 2B R ND 1000 B 2NDJ ND 283000 R 37 BJ 30 ND Leonard 93 BJ R ND 11 B 3BJ ND 38300 15 J 37 BJ 31 37 BJ 1.8 BJ 24400 ND ND ND 1210 B 1.4 BJ 17 J 318000 R 135 7BJ 63 B Rodriguez 58 BJ R ND SB 3BJ ND 40000 14 J 34 BJ 22B SOB 2BJ 38700 122 ND 22B 1610 B 1NDJ 7NDJ 281000 R 19 B 17 BJ 21 J Rodriguez Rep. 431 R ND ND 3BJ ND 47400 40 J 39 BJ 29 45 B 12.1 J 41400 129 ND 39B 1730 B 1NDJ 7NDJ 298000 R 8B 16 BJ 5NDJ Analytical mult* are reported In micrograms per liter (ug/1); equivalent to parts per billion. ND Compound not detected. B Reported value obtained from a reading that was less than the contract required detection limit but greater than the instrument detection limit. Rep. Replicate. J Estimated concentration. R Data rejected. Table 2. Summary of Inorganic* Analysis of Ground-Water Sample* Collected from Water Supply Well*, September 1990 Sampling Event, Tutu Well Site, St. Thomas, USVI. Sample Identification: INORGANIC ANALYTBS Aluminum Antimony Anenic Barium Beryllium Cadmium Calcium Chromium (Total) Cobalt Copper Iron Lead Magnesium Manganese Mercury Nickel Potassium Selenium Silver Sodium Thallium Vanadium Zinc Cyanide VIHA1 154 B 54 BJ ND 5B 3B 4BJ 49400 10 ND 10 B 29 BJ 9J 33900 ND R 15 B 2000 B 1.4 BJ 16 J 252000 R 67J 16 B 9.7 B VIHA3 182 BJ R ND 14 B 3BJ ND 43300 5BJ ND 29 149 3.7 J 28000 11 B ND 43 1030 B 1.5 BJ 7NDJ 162000 R 33 B 17 BJ 8BJ Laplace 146 B 57 B ND ND 4B 4BJ 41000 SB ND 49 J 55 BJ 23 BJ 32600 2B R 18 BJ 1140 B 10NDJ ND 250000 R 39 BJ 13 BJ ND Matthias 227 ND 3NDJ 6B 3B ND 36300 5B ND 18 BJ 20NDJ 1.8 BJ 34900 ND R 20 BJ 1410 B 2NDJ ND 379000 R 21 BJ 4BJ ND Ramsey 187 B ND 3NDJ ND 3B 3BJ 43100 11 ND 15 BJ 20 BJ 2.6 BJ 34400 ND R 21 BJ 1140 B 10NDJ ND 209000 R 43 BJ 7BJ ND Harvey 1280 R ND 35B 3BJ ND 53700 18 J 38 BJ 59 3360 32.6 J 46200 191 ND 58 2000 B 1.2 BJ 11 J 233000 R 59 248 J 7.4 B Tiuett 153 BJ 52NDJ 3NDJ 43 BJ 4BJ 4BJ 54800J 8BJ 18NDJ 48J 953 J UBJ 38300 J 1260 J R 33 BJ 760 BJ 10NDJ 7NDJ 192000 J R 25 BJ 162 J 52NDJ Tillcu Replicate 159 B ND 4.4 B 40 B 4B 3BJ 48600 7B ND 32 J 2660 J 8.5 J 34500 1100 R 15 BJ 1190 B 10NDJ ND 169000 R 50J 124J ND Analytical results are reported in micrograms per liter (ug/1); equivalent to parts per billion. ND Compound not detected. B Reported value obtained from a reading that was less than the contract required detection limit but greater than the instrument detection limit. Rstimiitcd conc Data rejected. entration. 1 oO Table 3. Proposed Sampling Effort for the 2nd Sampling Event (February 1991), Tutu Wells Site, St. Thomas, USVI. Well Bryan Dede Dimitri Dench Devcon 1 Devcon 3 Eglin 1 Eglin2 Eglin 3 Four Winds No. 1 Four Winds No. 2 Gassett Hartman2 Hartman 3 Harvey LaPlace Leonard Matthias Ramsey Rodriguez Smith Steele Tillett VIHA1 VIHA3 Proposed Analytes thallium, mercury antimony, thallium thallium, mercury VOCs, antimony, thallium antimony, thallium antimony, thallium VOCs, thallium, mercury VOCs, antimony, thallium VOCs, antimony, thallium VOCs VOCs, antimony, thallium VOCs, thallium, mercury VOCs, antimony, thallium VOCs, antimony, thallium VOCs, antimony, thallium VOCs, thallium, mercury antimony, thallium VOCs, thallium, mercury VOCs, thallium, mercury antimony, thallium VOCs, antimony, thallium, selenium VOCs, antimony, thallium VOCs, thallium, mercury VOCs, thallium mercury antimony, thallium MF:gv #PR00801/lstqtr.rpt IB GERAGHTY & MILLER, INC. ••; —»««<" "Z2&...-- ^5?^X-:vSn;- trS'TSf \\ he^-fSl?^ ^,'T'.^> --^<:^«c4<o -N^uiJI l-V^YiVS LEGEND . • RESIDENTIAL WELL A BRYAN B DEDE C DEMTTRI D DENCH E1 OEVCON 1 E2 DEVCON2 (ALTERNATE) E3 OEVCON 3 F1 EGUN 1 F2 EGUN 2 F3 EGUN 3 G FOUR WINDS No. 1 H FOUR WINDS No2 •«t 11 GASSETT \2 HARTMAN CRUSHER D HARTMAN ESTATE J HARVEY K LaPLACE L LEONARD M LOCKHART (ALTERNATE) N MATTHIAS RAMSEY RODRIGUES SMTTH O P Q R S T1 TILLETT VIHA No.1 T2 VIHANo.2 (ALTERNATE) T3 VIHA No.3 T4 VIHANo.4 (ALTERNATE) WELL SAMPUNG LOCATIONS, TUTU WELLS SITE SAMPUNG ANALYSIS, AND MOMTORMG PLAN, ST. THOMAS, USVI •0* TEIC cc SOURCe USGS QUADRANGLE EASTERN ST.THOMAS.Vi(1954) Gcraghtv filler. Inc. RNOLAY ISCM.C SHOWN 5/90 DATA VALIDATION SUMMARY REPORT for the TUTU WELLS SITE September 1990 Quarterly Sampling USEPA REGION II Standard Operating Procedures HW-2 and HW-6 for the Contract Laboratory Program Organic and Inorganic Data Review Sample Delivery Group 900731 (Dede) January 1991 Prepared for Tutu Environmental Investigation Committee Geraghty & Miller, Inc. International Group 290 Vincent Avenue Hackensack, New Jersey 07601 GERAGHTY & MILLER. INC. SOP NO. B*-6 Revision 17 1 1 CLP CfGANICS DATA FEVIEW AMD FRELUCDQIV REVIEW 1 1 1 1 Date: Lean LazarQs, Environmental Scientist Ibxic and Hs7^rriais Haste Section ONO3RRED BY Date: 1 1 1 , *-> <cf 7 o Gerard F. McKenna, Qiief Monitoring Management Branch 1B41 STANDARD OPERATING PROCEDURE Page: 1 of 36 Date: Marti*. 19SO Revision 7 INTRODUCTION TO DATA VALIDATION .0 1.1 This procedure is applicable to organic data obtained from contractor laboratories working for the Contract Laboratory Piuyiaa (CLP). 1.2 The data validation is based upon analytical and quality assurance requirements specified in the Statement of Work (SOW). • 0 Data reviewers will complete the following tasks as assigned by the Data Review Coordinator: 2.1 Data Assessment - The reviewer must answer every question on the checklist. All response shall be in ink. 2.2 Data Assessment Narrative (Attachment 1) - Data reviewer is required to use these forms and must match the action in the narrative with the action taken on the Form I(s). 2.3 Rejection Surrary Form (Attachment 2) - Fill in the total number of analytes measured by different analyses and the number of analytes rejected or flagged as estimated due to corresponding quality control criteria. Place an "X" in the boxes where analyses were not performed or criteria do not apply. 2.4 Organic Regional Data Assessment - Data reviewer is also required to fill out Organic Regional Data Assessment Fora (Attachment 3). 2.5 Telephone Record Log - The data reviewer should enter the bare facts of inquiry before initiating any authorized telephone conversation with a CLP laboratory. After the case review has been completed, mail the white copy of the Telephone Record Log to the laboratory and the pink copy to SMO. File the yellow copy in the Telephone Record Log folder and attach a photocopy of the Telephone Record Log to the completed Data Assessment Narrative. 2.6 Forwarded Paperwork - Upon completion of the review, the following are to be for*-arded to the Regional Sample Control Center (RSCC) located in the Surveillance and Monitoring Branch: a. data package b. completed assessment checklist c. SMO Contract Compliance Screening (CCS) Forward four (4) copies of the completed Data Assessment Narrative along with four (4) copies of the Organic Data Assessment Form: one each for the appropriate Regional DPO, the Sample Management Office (SMO), and to the last two addresses of the Data Reviewers Mailing List. 2.7 Filed Paperwork - Upon completion of the review, the following are to be filed within the Monitoring and Management Branch (MMB) files: a. Telephone record Log (copy) b. Record of Communication (original) c. Rejection Summary Form STWCARD OPERATING 2 of Date: March 1990 Revision 7 36 r.o Re-iection of te-ba - All values determined to be unacceptable on the Organic Analysis Data Sheet (Form I) must be flagged with an "R". As soon as review criteria causes data to be rejected, that data can be eliminated from any further review or consideration. .0 ______ - In order that the reviews be consistent among reviewers, this Standard Operating Procedure (SOP) should be used. Additional guidance can be found in the Functional Guidelines. intended to aid the reviewer in However, the validation should locating any problens, both be carried out even if CCS is in response to CCS oust be used by the reviewer. «».!led and u not present. UBiiilinlttMi received from the laboratory 1851 STRNDA3D OFSSAIDC Pai 111 igg ftoge: 3 of 36 Due: March 1990 Hevision 7 AOQCZ CSKPLEZaCSS AND DELZVESABTZS CASE tOSSl: 9to 0 73 / gTTF* .0 Data '^"rrrlet-grio"**; *^H T>??, i^^r^^*1* ypg JJQ N/A X 1.1 Have any missing deliverables been received and added f v 1 __ __ ta the- data package. ACTICN: Call lab for explanation / LI inlinirr il of any missing deliverables. If lab cannot provide them, note the effect on review of the package under the "Contract Problems/Sufi i n^linnoe1* «enMm of reviewer narrative. 1.2 Was ac CCS checklist included with package? [__] 2.1 Is the Narrative or Cover Letter present? T ^ 2.2 Are Case R=±er and/or SAS nuaber cantained in the Narrative or Cover Letter? following checklist is divided into three parts. Part A is filled cue if the data package contains any TC& analyses, Part 5 for any SJA analyses and Part C for Pestieide/PC3s. Does this package ccntain: 3A data? * GV data? J^T v icide/PC3 data? AdlCN: C=r=plete carresponding parts of checklist. ur^.-<A—_NG PRCdLTJT Page: 4 of 35 Data: March 1950 Revision 7 YES PART A; TKM. :Q Traffic______________________ 1.1 Are the Traffic Report Poras present for all sasples? f ^ __ ACTION: If no, contact lab for replaoenent of missing or illegible copies. 1.2 Do the Traffic Reports or Lab Narrative indicate any problems with sample receipt, condition of samples, analytical problens or special notations affecting /* the quality of the data? _ r l/i ACnCN: Use professional judgenent to evaluate the effect on the quality of the data. ACTION: If any sample analyzed as a soil contains more than SO* water, all data should be flagged as estimated (J). ACTION: If both VQA vials for a sample have air bubbles, flag all positive results "J" and all nan-detects "R". ire Tl 2.1 Have any VQA holding times, determined froa date of collection to date of analysis, been exceeded? __ If unpreserved, aqueous aroratic volatiles must be analyzed within 7 days of collection and non-aronatic volatiles most be analyzed within 14 days. If preserved with hydrochloric acid and stored at 4°C, then both aromatic and non-aronatic volatiles must be analyzed within 14 days. If uncertain about preservarion, contact the sampler to determine whether the sarnies were preserved. A ten-day holding time for soil samples is recoaserdad. T^hle of HnTcJlnc Time Violations (See Traffic Report) Sarple Date Date Lab Date Sample Matrix Preserved ? Sampled Received Analyzed ACITCN: If holding tines are exceeded, flag' all positive results as estimated ("J") and sairple quantatation limits as estimated ("UJ"), and dccument in the narrative that holding tines were exceeded. OPERATING SROCE3JHE Page: 5 of 36 Date: Hirer. 1990 Revision 7 YES NO N/A" If analyses were done more than 14 days beyond holding time, either on the first analysis or upon reanalysis, the reviewer nust use professional judgement to determine the reliability of the data and the effects of additional storage on the sanple results. The reviewer may determine that nan-detect data are unusable ("R") . ">.0 Surrogate RporTverv (Ftara Til 3.1 Are the V3A Surrogate Recovery Summaries (Form U) present for each of the following matric a. laj Water r 1/1 __ b. Mad Water [__] __ c. l£M Soil [__] __ d. Mad Soil [__] __ 3.2 Are all the TCA sarples listed on the appropriate Surrogate Recovery Sumaries for each of the following natric a. Low Water b. Mad Water c. low Soil [__] __ " d. Med Soil ACTION: Call lab for explanation / resubmittals. If missing deliverables are unavalLeble, document effect on data under "Conclusions" section of reviewer narrative. 3.3 Wera outliers narked correctly with an asterisk? ACTION: Circle all outliers in red. 3.4 Was one or more TC& surrogate recovery outside of contract specifications for any sample or method blank? *^ [__] __ If yes, were sanples reanalyzed? Were method blanks reanalyzed? ACTION: If surrogate recoveries are > 10% but all do not meet SOW specifications: 1. Flag all positive results as estimated ("J"). 2. Flag all non-detects as estimated detection limits ("UT"). rur Page: 6 of J6 Date: March 1990 Revision 7 YES NO If any surrogate has a recovery of <10* : 1. Flag all positive results as estimated ("J"). 2. Flag all nan-detects as unusable ("R"). Professional judgement should be used to qualify data that have method blank surrogate recoveries out of specification in both original and re- analyses. Check the internal standard areas. 3.5 Are there any transcription/calculation errors between raw data and Fora H? __ AdTCH: If large errors exist, rail lab for explanation / resubmittal, make any necessary corrections and note errors under "Conclusions11. 0 Matrix Spik0*5 fFarm TIP 4.1 Is the Matrix Spike Duplicate/Recovery Fora (Form HI) present? 4.2 Were matrix spikes analyzed at the required frequency for each of the following matrices: a. L3w Water b. Med Water c. Lew Soil d. Med Soil ACTION: If any matrix spike data are missing, take the action specified in 3.2 above. 4.3 Kow sary VGA spike recoveries are outside QC limits? 3, out of 10 Un out of 10 4.4 How many RPD's for matrix spiJce and matrix spiJce duplicate recoveries are outside QC limits? Water Soils \ Q out of 5 vl- out of 5 ACTION: If MS and MSD both have less than 10* re- covery for an analyte, negative results for that analyte should be rejected, and positive results should be flagged "J". The above applies only to the sample used for the MS/JSD analysis. Use professional judgement in applying this critericn to other samples in the package. D OPS3AT2C PSOdL!<I Page: 7 of 36 Date: March 1990 Pevision 7 NO N/A ,0 Blanks (Form IV"> 5.1 Is the Method Blank summary (Form IV) present? f/^l __ __ 5.2 Frequency of Analysis: for the analysis of VGA TCL ccnpounds, has a reagent/method blank been analyzed for each set of samples or every 20 samples of similar matrix (low water, med water, low soil, medium soil), whichever is Bare frequent? 5.3 Has a VGA instrument blank been analyzed at least once every twelve hours for each GC/KS system used? ACTION: If any method blank data are missing, «-*ii lab for explanation / resubnittal. If not available, reject all associated positive data ("R"). 5.4 CTiromatography: review the blank raw data - chromat: (KICs), quant reports or data system printouts and spectra. Is the chroratographic performance (baseline stability) for each instrunent acceptable for V3As? ACTION: Use professional judgement to determine the effect on the data. NCflZ: "Water blanks" and "distilled water blanks" are validated like any other sarple and are not used to qualify data. Do not confuse then with the other QC blanks di'«<"itg.«sad below. 6.1 Do anv method/instrunienVreagent blanks have positive results (TCL and/or TTC) for VQAs? «nen applied as described below, the contaminant concentration in these blanks are Multiplied by the sanple Dilution . S* Factcr. ±L I__1 __ 6.2 Do any field/trip/rinse blanks have positive TOA results . ^ (TCL and/or TIC)? JS [__] __ AcnCN: Prepare a list of the saitples associated with each of the contaminated blanks. (Attach a separate sheet.) NOTE: Only field/rinse blanks taken the same day as the sarples are used to qualify data. Trip blanks are used to qualify only those samples with which they wera shipped. Blanks may not be qualified because of contamination in another blank. Blanks may be qualified for surrogate, spectral, tuning or calibration QC problems. r STANDARD QFEttrnC »ut-Vi'gg Page: 8 of 36 Data: March 1990 Revision 7 NO ACTICN: Follow the directions in the table belov to qualify TCL results due to contamination. Use the largest value fron all the nwriate^ blanks. [Sample cone > CRQLjSample cone < CRQL &!Sa&ple cone > CRQL ——— but < lOx blank is < lOx blank value value & >10x blank value Methylene chloride Flag sample result Acetone with a 'U'; Toluene out *B' flag J2-butanone_{ Reject saaple result No qualification and report CRQL; lit out 'B' flag [Sample cone > CRQLjSample cone < CRQL *!Sample cone > CRQL but < 5x blank is < 5x blank value value & > 5 blank value Other {Flag saaple result!Reject sample result No qualification Contaminants with a 'U1; cross and report CRQL; is needed out 'B' flag jcross out 'B1 flag | I. ACTION: For TIC ccnpounds, if the concentration in the sample is less than five times the concentration in the most con- taminated associated blank, flag the sample data "R" (unusable). 6.3 Are there field/rinse/equipment blanks associated with every / • ' sasple? r i \S ACTION: For low level samples, note in data assessment that there is no associated field/rinse/equipment blank. Deception: sanples taken from a drinking water tap do not have associated field blanks. * 0 G?w^^^^ T^^^^^^^ ^nd r^sss CHL!^J3i'8tion i * orrn yj 7.1 Are the GC/tS Tuning and Mass Calibration Forms (Form V) present for Brcrnofluorobenzene (BFB)? 7.2 Are the enhanced bar graph spectrum and mass/charge (m/z) listing for the BFB provided for each twelve hour shift? 7.3 Has a tuning performance cccpound been analyzed for every / twelve hours of sample analysis per instrument? r v •" ACTTCN: If any tuning data are missing, take action specified in 3.2 above. ACTICN: List date, time, instrument ID, and sample analyses for which no associated GC/MS tuning data are available. Page: 9 of 35 Date: March 1990 Revision 7 YES NO N/A UTU.C. - HfH. - •ijvj i ru r^jjiA ——————————————————— ———————————————— ___ aMnriXi nurastro ACTION: If lab cannot provide missing data, reject ("R") *ll data generated outside an acceptable twelve hour calibration interval. 7.4 Have the ion abundance criteria been net for each instrument used? f iXl __ __ ACTION: List all data which do not meet ion abundance criteria (attach a separate sheet). ACTION: If tuning calibration is in error, flag all associated sample data as unusable ("R"). However, if expanded ion criteria are met (See 1933 Functional Guidelines), the data reviewer may accept data with appropriate • qualifiers. ^ 7.5 Are thers any transcription / calculation errors between mass lists and Forz Vs? (Check at least two values but if errors ara found, check more.) 7.6 Have the appropriate nurber of significant figures (two) been reported? (Check at least two values, but if errors are found check more values.) ACTION: If large errors exist, call lab for explanation / resubrJ.ctal, make necessary corrections and note errors under "Conclusions". 7.7 Are the scectra of the mass calibration carpound acceptable? [V 1 ACTION: Use professional judgement to determine whether associated data should be accepted, qualified, or rejected. 3.0 Taroet Prpcund Vft^fc fTT^ ^"^lyfoB? 8.1 Are the Organic Analysis Data Sheets (Form I TOA) present with required header information on each page, for each of the following: a. Samples and/or fractions as appropriate r ^ 1 b. Matrix spikes and matrix spike duplicates c. Blanks STANDARD OFESAT2JG mxULTE Page: 10 cf Date: Marsh 19SO Revision 7 ACTICN: Use professional judgement to determine the ! .t ahn 1 •Jt of the data. 8.5 Are the lab-^generatad standard rass spectra of the identified VCZ. cccpounds present for each sanple? ACHCN: If any rass spectra are missing, take action specified in 3.2 above. If Lab dees net generate their own standard ScjeuLia, make note in "Contract Problens/Non-conpliance'1 . _ NO 8.2 Are the TOA. Reconstructed Ion Chromatograms, the mass bpeuLid for the identified compounds, and the data system printouts (Quant Reports) included in the sample package for each of the following? a. Saqples and/or fractions as appropriate [I/] __ b. Matrix spikes and matrix spike duplicates f tXl __ (Mass sfejecLid. not required} c. Blanks ACTION: If any data are missing, take action specified in 3.2 above. 8.3 Are the response factors shown in the Quant Report? __ 8.4 Is chraratographic performance acceptable with x to: / Baseline stability U^J __ __ Resolution Peak shape Full-scale graph (attenuation) Other: 8.6 Is the FHT of each reported conpound within 0.06 HRT units of the standard RRT in the continuing calibration? 8.7 Are all ions present in the standard mass spectrum at a relative intensity greater than 10* also present in the sanple mass spectrua? f!/__! __ 8.8 Do sarple and standard relative ion intensities agree within 2C%? ACITCN: Use professional judgement to determine acceptability of data. If it is determined that incorrect identifications were made, all such data should be rejected, flagged TUT "N" (presumptive evidence of the presence of the coipcund) or changed to not detected (at the calculated detection limit). STRNDAHD OPERATING PSCdUHE Page: 11 of 36 Date: March 1990 Revision 7 Y E S N O J.Q Terr^tiv^v Identifi'H C'npour^ 9.1 Are all Tentatively Identified expound Forms (Form I, Part B) present; and do listed TTCs include scan number or retention tine, estimated concentration and "J" / qualifier? . f \/\ 9.2 Are the mass bpm-tid for the tentatively identified Goxrpounds and associated "best match" spectra included in the sample package for each of the following: a. Samples and/or fractions as appropriate [ \s] b. Blanks ACTTCN: If any TTC data are missing, take action specified in 3.2 above. ACTTCN: Add "J" qualifier if missing and "N" qualifier to all identified TTC compounds on Fora I, Part B. 9.3 Are any TCL compounds (front any fraction) "H«?«•»* as TTC cccpcunds (exarple: 1,2-dinethylbenzene is xyl a VGA TCL—and should not be reported as a TIC)? ACTTCN: Flag with "R" any TCL conpound listed as a TTC. 9.4 Are all ions present in the reference mass spectrum with a relative intensity greater than 10% also present in the sasple ffv»<t« spectruz? 9.S Do TTC and "best match" standard relative ion intensities >. agree within 20*? flXl __ __ ACITCN: Use professicnal judgement to determine ~ acceptability of TTC identifications. If it is determined that an incorrect identi- fication was made, change identification to "unknown" or to some less specific identi- fication (exanple: "C3 substituted benzene") as appropriate. .0.0 Cuiijjound Qn^nti^^tion and 10.1 Are there any transcription / calculation errors in Fora I results? Check at least two positive values. Verify that the correct internal standard, quantitation ion, and RRF were used to calculate Fora I result. / Were any errors found? __ r V 1 __ 10.2 Are the CSQLs adjusted to reflect sanple dilutions and, for soils, saaple moisture? -A3D OFESATING PROCURE Page: 12 of 26 Date: March 19SO Revision 7 NO ACTION: If errors are large, call lab for explanation / resubmittal, mate any necessary corrections and errors under **<xi«'^*g j^ ACTTCN: Wven a sanple is analyzed at more than one dilution, the lowest CSQLs are used (unless a QC exceadanoe dictates the use of the higher CRQL data from the diluted sample analysis) . Replace concentrations that ?xr~***l the calibration range -in the original analysis by crossing out the "F* value on the original Fora I and substi- tuting it with data from the analysis of dilutad sarple. Specify which Form I is to be used, then draw a red "X" across the entire page of all Fora I's that should not be used, including any in the suanary package. 11.0 gr *,;-«•! a -"ds Data fC 11.1 Are the Reconstructed Ion Ciraratograas, and data system printouts (Quant. Reports) present for initial and continuing calibration? ACTION: If any calibration standard data are missing, take action specified in 3.2 above. ..0 GCVTS Initial Calibration fForr. VD 12.1 Are the Initial Calibration Forrs (Form VI) present and ccqplete for the volatile fraction? f ^ 1 ACTION: If any calibration standard fores are missing, take action specified in 3.2 above. 12 . 2 Are response factors stable for volatiles over the concentration range of the calibration (PSD <30*)? ACTION: Circle all outliers in red. ACTION: When PSD >30*, non-detects may be qualified using professional judgement.^ Flag all positive results "J". When RSD >90%, flag all non-detects as unusable ("R") . (Region H policy.) 12.3 Do any ccrpcunds have an average RRF < 0.05? v ACTION: Circle all outliers in red. ACTION: If any volatile conpound has an average RPJ < 0.05, flag positive results for that --^ ccnpound as estimated ("J") , and flag non- detacts for that ccnpound as unusable ("R") . OFE3AZDC PRCXZX'PZ Page: 13 of 35 Date: March 1990 Revision 7 YES 12.4 Are there any transcription / gi"Tla*im errors in the reporting of average lesponsa factors (RRF} or %RSD? (Check at least two values but if errors are found, check nore.) __ ACXTCN: Circle errors in red. ACITCN: If errors are large, can lab for explanation / resubmittal, make any necessary corrections and note errors under "Conclusions". 13.0 GC/^S (^rirT^r^T^^TT r^llfcration fPuim vm 13.1 Are the Continuing Calibration Foras (Form VTI) present / and ccnplete for the volatile fraction? f 1/1 __ __ 13.2 Has a continuing calibration standard been analyzed for every twelve hours of sanple analysis per / instrument? f y 1 __ __ ACT!OK: List below all sarole analyses that were not within twelve hours of the previous :tinuing calibration analysis. ACTICW: If any for=s are missing or no continuing calibration standard has been analyzed within twelve hours of every sanple analysis, ea.U lab for explanation / resubmittal. If continuing calibration data are not available, flag all associated sanple data as unusable ("R"). 13.3 Do any continuing calibration standard corpourds have / a PPT < 0.05? y ACTICN: Circle all outliers in red. ACTION: If any volatile conpcund has a FRF < 0.05, flag positive results for that compound as estimated ("J"), and flag non-detects for that cccpound as unusable ("R"). 13.4 Do any cccpcunds have a * difference between initial and continuing caiibration RRF > 25\? y [__] __ ACnQN: Circle all outliers in red and qualify associated sarrple data as outlined in the table below: OPERATING Page: 14 of 35 Date: March 1990 Revision 7 YES NO N/A wW ^V | ^^*f ^V 'J1 positive j 'J' positive results, no action results, 'UT1 for nan detects nan detects ! ^^w 'J' positive results, "R" nan detects 13.5 Are there any transcription / calculation errors in the reporting of average response factors (PRF) or diff< (%D) between initial and continuing RRFs? (Check at least two values but if errors are found, check nore.) ACTION: Circle errors in red. ACTION: If errors are large, e»n lab for explanation / resubmittal, make any necessary corrections and note errors under "Conclusions". / __ [ \/i __ 14.0 Inty"* 14.1 Are the internal standard areas (Fora VTH) of every sarple and blank within the upper and lower limits for each continuing calibration? ACTION: List all the outliers below. Sample I Internal Std Area Lower Limit Limit (Attach additional sheets if necessary.) ACTION: If the internal standard area count is outside the upper or lower limit, flag with "J" all positive results and nan- detects (U values) quantitated with this internal standard. If extremely low area counts are reported, or if performance exhibits a major abrupt drop off,'flag all associated nan- detects as unusable ("R"). 14.2 Are the retention times of the internal standards within 30 seconds of the associated calibration standard? ACTION: Professional judgement should be used to qualify data if the retention frjj"*« differ by more than 30 STAJCAHD OFERAHN3 HROCZDLSi Page: 15 of 36 Date: March 19SO Revision 7 NO it/A" 15.1 Were any field (duplicates submitted for VQA analysis? ACITOK: Cccpare the reported results far field duplicates and calculate the relative percent dif fe ACIICN: Any gross variation between field duplicate results sust be addressed in the reviewer narrative. Hawever, if large differences exist, identification of field duplicates should be conf iraed by contacting the sanpler. STANDARD OPSPXHX PROG3SE Page: 16 of 36 Date: March 1990 Revision 7 Y E S N O N / T BART Bt a<A ANAIVS5S ..0 Traf 3fi? P'l'tf'i'l ^i? :M"r3 1.1 Are the Traffic Report Forms present for all samples? ACTICN: If no, contact lab for replacement of missing or illegible copies. 1.2 Do the Traffic Reports or Lab Narrative indicate any problems with sample receipt, condition of samples, analytical problems or «r*^»l notations affecting the quality of the data? ACTTCN: Use professional judgement to evaluate the effect on the quality of the data. ACTICN: If any sample analyzed as a soil contains more than 50% water, all data should be flagged as estimated (J). 2.1 Have any BKn holding tines, determined from date of / collecrion to date of extraction, been exceeded? __ [y 1 __ Samples for BA analysis, both soils and waters, oust be extracted within seven days of the date of collection. Detracts nust be analyzed within 40 days of the date of extraction. ^s Violations (See Traffic Report) Sample Date Date Lab Date Date Sanple Matrix Sanpled Received Extracted Analyzed ACTICN: If holding tiaes are exceeded, flag all positive results as estimated ("J") and sanple quantitation limits as estimated ("UT"), and document in the narrative that holding timr*s were exceeded. OFE2ATDG EROCS3URE Page: 17 of 35 Date: March 1990 Revision 7 s If analyses were done more than 14 days beyond holding tine, either on the first analysis or upon reanalysis, the reviewer oust use professional judgement to determine the reliability of the data and the effects of a*nifrj™-iai storage on the sample results. Hie reviewer may determine that ncn-detect data are unusable ("R") . 3.0 SLSJTTS^r? P**?!Vp'*^ fFora TT1 3.1 Are the a*A Surrogate Recovery Summaries (Form H) present for each of the following matrices: a. Low Water [ J 1 __ b. Mad Water [ __ ] __ / c. Low Soil [ __ ] __ / d. Med Soil 3.2 Are all the ENA sasples listed on the appropriate Surrogate Recovery Surraries for each of the following matric a. latj Water f V} b. Med Water c. TJX Soil __ d. Med Soil [__] __ / ACIICN: Call lab for explanation / resubmittals. If missing deliverables are unavailable, dorunerit effect on data under "Conclusions" section of reviewer narrative. 3.3 Were outliers marked correctly with an asterisk? ACITCN: Circle all outliers in red. 3.4 Were two or nore base-neutral SB acid surrogate recoveries / out of specification for any sample or method blank? __ r v 1 __ If yes, were samples reanalyzed? [__] __ v • Were method blanks reanalyzed? [__] __ _•_ ACnctJ: If all 94& surrogate recoveries are > 10% but two within the base-neutral or acid fraction do not meet SOW specifications, for the affected fraction o^]_y f i.e. base—neu*^^^ T OR acid gunpoury^^ - 1. Flag all positive results as estimated ("J"). 2. Flag all non-detects as estimated detection limits ("UJ"). STANDARD OF5V>T2JG PSDCZXHE Page: 18 of 35 Date: March 19SO Revision 7 "__; _ If any base-neutral or. acid surrogate has a recovery of <10% : 1. Flag all positive results for that fraction (i.e. all acid or. base-neutral compounds) "J". 2. Flag all nan-detects for that fraction "R". Professional judgement should be used to Qualify data that have method blank surrogate recoveries out of specification in both original and re- analyses. Check the internal standard areas. 3.5 Are there any transcription/calculatian errors between raw data and Forn H? __ r V 1 __ AcnCK: If large errors exist, «T1 lab for explanation / resutnittal, make any necessary collections and note errors under "Conclusions". 4.0 Matrix ^iJf***5 fForr. mi •4.1 Is the Matrix Spike Duplicate/Recovery Fora (Form IU.) pn ULJ _ _ 4.2 Wars matrix spikes analyzed at the required frequency for each of the following matric a. Low Water C V / 1 __ b. Mad Water c. Low Soil d. Med Soil ACIxOK: If any matrix spike data are missing, take the action specified in 3.2 above. 4.3 How many EKn spike recoveries are outside QC limits? Water SojJLs Q out of 22 Kjlft out of 22 4.4 Kow many RPD's for matrix spike and matrix spike duplicate recoveries are outside QC limits? Water Soils Q out of 11 fjl out of 11 ACTICN: If MS and M5D both have less than 10% recovery for an analyte, negative results for that analyte should be rejected, and positive results should be flagged "J". The above applies only to the sample used for M5/M5D analysis. Use professional judgement in applying this criterion to other samples. OFE3AT2G PROCEDURE Page: 19 of Date: March 1990 Revision 7 - NO 5.0 Blanks nPora IV) fV/1 __ 5.1 Is the Itethcd Blank Sunsary (Pom IV) present? 5.2 Frequency of Analysis: for the analysis of SNA TCL occpcunds, has a reagent/method blank been analyzed for each set of samples or every 20 sanples of similar matrix (low water, mad water, low soil, / nediuc soil), whichever is acre frequent? r v/1 5.3 Has a SNA instrument blank been analyzed for each OS/MS system used. ACTION: If any oethod blank data are missing, e*n lab for explanation/rest tfmittal . If not available, reject all nvjnri aitfrl positive data ("R") . 5.4 Chroretcgraphy: review the blank raw data - chrccategraas quant reports or data system printouts and spectra. Is the chracatographic perforrance (baseline stability) s for each instruaent acceptable for V3As? C y ] __ __ ACTION: Use professional judgement to determine the effect on the data. 6.0 NCTZ: "Water blanks" and "distilled water blanks" are validated like any other sasple and are not used to qualify data. Do not confuse them with the other QC blanks discussed below. 6.1 Da any Dethod/irstrurient/reagent blanks have positive results (TCL and/or TIC) for BSAs? When applied as described below, the contaminant concentration in these blanks are mltiplied by the sample Dilution / Factor. __ fV 1 __ 6.2 Do any field/rinse blanks have positive ENA results (TCL and/or TIC)? __ ACTICN: Prepare a list of the sanples associated with each of the contaminated blanks. (Attach a separate sheet.) NOTE: Only field/rinse blanks taken the same day as the sacples are used to qualify data. Blanks may not be qualified because of contamination in another blank. Blanks say be qualified for surrogate, spectral, tuning or calibration QC probl .1.868 OFE3AT2C cm1:- i~vr Page: 20 of 36 Date: March 1990 Bevision 7 NO N/A ACTICN: Follow the directions in the table below to qualify TCL results due to contamination. Use the largest value from all the associated blanks. 'SaHple onne > CPQT'S*T*p1« cmf < rPQT. gigarrplq r - n f y > CRQL ' but < lOx blank is < lOx blank value value & >10x blank value CUL~UU Flag sarple result Reject sanple result No qualification Rithalate with a 'U'; cross and I^JIL CPQL; |is needed Esters out 'B1 flag cross cut 'B1 .1. 'Sarple cone > CPCLlSairple cone < CSQL &{Saqple cone > CBQL but < 5x blank is < 5x blank value value & > 5 blank value 11 Other Flag sarple result Pej ect sanple result' No qualification Contaminants with a 'U'; cross and neyui.t OX2L; is needed cut 'E' flax; cross out 'B' flag i ——————————— i ____________ i ACTION: For TIC ccrpcunds, if the concentration in the sarole is less than five t.irres the concentration in the mcst con- tariratad associatad blank, flag the sacple data "K" (unusable) . €.3 Are there field/rinse/eguipment blanks »<»wiva^ with every / satpie? * " C __ ] __ v ACITCK: For low level sazples, note in data assessment that there is no associatad field/rinse/eouiFinent blank. Deception: sanples taken froa a drinking water tap do not have associated field blanks. 7.1 Are the GC/MS Tuning and Mass Calibration Forrs (Form V) / present for Decafluorctriphenylphosphine (DFTP?)?. f v] 7.2 Are the enhanced bar graph spectrum and nass/charge (m/2) listing for the DFTPP provided for each twelve hour shirt? 7.3 Has a tuning perfonrance conpound been analyzed for every twelve hours of sanple analysis per instrument? ACTICN: If any tuning data are missing, take action specified in 3.2 above. ACTTCN: List date, time, instrument ID, and sanple analyses for which no associated GC/MS toning data are available. STANDARD OPERATING Page: 21 of 35 Date: March 1990 Revision 7 NO N/A ——————— ———————————— 1 - ———— ACTION: If lab cannot provide missing data, reject ("R") all data generated outside an acceptable twelve hour calibration interval. 7.4 Have the ion abundance criteria been net for each instrument used? ACITCK: List *ii data which do not meet ion abundance criteria (attach a separate sheet). ACTION: If tuning calibration is in error, flag all associated sanple data as unusable ("R"). However, if expanded ion criteria are met (See 1988 Functional Guidelines), the data reviewer may accept data with appropriate qualifiers. 7.5 Are there any transcription / calculation errors between mass lists and Form Vs? (Check at least two values but if errors are found, check, acre.) 7.6 Have the appropriate number of significant figures (two) been reported? (Check at least two values, but if errors are found check more values.) ACTION: If large errors exist, call lab for explanation / resubrrJLtTEal, make necessary corrections and note errors under "Conclusions". send 7.7 Are the spectra of the mass calibration acceptable? ACTION: Use professional judgement to determine whether associated data should be accepted, qualified, or rejected. 8.0 Oar Tist Analvtes 8.1 Are the Organic Analysis Data Sheets (Form I SNA) present with required header information on each page, for each of the following: a. Sairples and/or fractions as appropriate b. Matrix spikes and matrix spike duplicates c. Blanks STANDARD OPE3KZIX HS'X'UJjRE Page: 22 of 35 Date: March 1990 Revision 7 c. Blanks ACTON: If any data are missing, take action rifled in 3.2 above. v i YES NO 8.2 Are the SNA Peconstructed Ion Qironatogrars, the mass spectra for the identified compounds, and the data system printouts (Quant Reports) included in the sample package for each of the following? a. Sanples and/or fractions as appropriate [ y/ ] __ __ b. Matrix spiXes and matrix spike f^ii/-^^ rv/1 __ __ (Mass bfejeutid not required) 8.3 Are the response factors shown in the Quant Report? 8.4 Is chronatcgraphic performance acceptable with respect to: / Baseline stability r /I __ Resolution Peak shape r v 1 __ __ Full-scale graph (attenuation) C Vj __ __ Other:________________ [__] __ y ACTION: Use professional judgement to determine the acceptability of the data. 8.5 Are the lab-generated standard mass spectra of the / identified StA cccpcunds present for each sample? [__] __ v ACTTCN: If any mass spectra are missing, take action specified in 3.2 above. If lab does not generate their own standard spectra, make note in "Contract Problers/Non-compliance". 8.6 Is the RRT of each reported compound within 0.06 RPT / units of the standard RPT in the continuing calibration? [__] __ v 8.7 Are all ions present in the standard mass spectrum at a relative intensity greater than 10% also present in the sample mass spectrum? 8.8 Do sanple and standard relative ion intensities agree / within 20%? C__] —— -*— ACTION: Use professional judgement to determine acceptability of data. If it is determined that incorrect identifications were made, all such data should be rejected, flagged "N** (presumptive evidence of the presence of the conpound) or changed to not detected (at the calculated detection limit). SLVJCARD OPE3AT3C HcmURZ Page: 23 of 36 Date: March 19SO Revision 7 NO 9.0 Tentatively Tdentif i« f*' TIO 9.1 Are all Tentatively Identified expound Forms (Fora I, Part B) present; and do "Listfrl TICS include scan nunber or retention tine, estimated concentration and "J" qualifier? 9.2 Are the mass bpauLid for the tentatively identified conpounds and associated "best match" t^m.Lid included in the sacple package for each of the following: a. Sacples and/or fractions as appropriate tv b. Blanks [ __ ACTION: If any TIC data are missing, take action specified in 3.2 above. ACITCN: Add "J" qualifier if missing and "N" qualifier to all idantified TIC conpounds on Form I, Part B. 9.3 Are any TCL cccpounds (from any fraction) listed as TIC ccrpounds (exsrple: l,2-di3fithylbenzene is xylene — / a VQA TCL— and should not be reported as a TIC)? __ f \/ 1 __ ACTICN: Flag with "R" any TCL conpound listed as a TIC. 9.4 Are all ions present in the reference mass spectrum with a relative intensity greater than 10* also present in the / sacple TTPISS spectrus? [ __ ] __ y 9.5 Do TIC and "best natch" standard relative ion intensities / agree within 20*? [__] __ V ACTION: Use professional judgement to determine acceptability of TIC identifications, if it is determined that an incorrect identi- fication was made, change identification to "unknown" or to some less specific identi- fication (example: "C3 substituted benzene") as appropriate. 10.0 10.1 Are there any transcription / calculation errors in Form I results? Check at least two positive values. Verify that the correct internal standard, quantitation ion, and FPF were used to calculate Form I result. Were any errors found? 10.2 Are the CRQLs adjusted to reflect sacple dilutions and, for soils, sample moisture? STANDARD OPERATING E«a * *il'.~ Page: 24 of 35 Date: March 1990 Revision 7 NO ACTION: If errors are large, call lab for explanation / resubmittal, make any necessary collections and note errors under •Conclusions". ACTION: When a sample is analyzed at more than one dilution, the lowest CSQLs are used (unless a QC exceedance dictates the use of the higher CPQL data from the diluted sample analysis) . Baplaoe concentrations that exceed the calibration range In the original analysis by crossing out the "E" value on the original Fora I and substi- tuting it with data from the analysis of diluted sample. Specify which Fora I is to be used, then draw a red "X* across the entire page of all Form I's that should not be used, including any in the sunnary package. Ll.O 11.1 Are the Reconstructed Ion Chraratograns, and data system printouts (Quant. Reports) present for initial and continuing calibration? [_•/ ] ACTION: If any calibration standard data are missing, take action specified in 3.2 above. .2.0 GC/T-S Ir_ ti*j ^.liriT^ion fFora 12.1 Are the Initial Calibration Fores (Form VI) present and conplete for the ENA fraction? ACTION: If any calibration standard faros are missing, take action specified in 3.2 above. 12.2 Are response factors stable for BNAs over the / concentration range of the calibration (PSD <30*)? [ __ ] \J __ ACTION: Circle all outliers in red. ACTION: When RSD >30*, non-detects may be qualified using professional judgement. Flag all positive results "J". When RSD >90%, flag all non-detacts as unusable ("R") . (Region H policy.) 12.3 Do any conpounds have a PRF < 0.05? __ tv 1 __ ACTION: Circle all outliers in red. ACTION: If any B1A ccnpound has an average ^— PRF < 0.05, flag positive results for that compound as estimated ("J1*) , and- flag non- detacts for that conpound as unusable ("R") . STANDARD OPERATING PF1X T- H IKE Page: 25 of 36 Date: March 1990 Revision 7 ~ ~ Y E S N O 12.4 Are there any transcription / g*'1'""lviTi errors in the reporting of average mporun factors (RRT) or *RSD? (Check at least two values but if errors are found, check more.) __ ACTION: Circle errors in red. ACTION: If errors are large, «*TL lab for explanation / resubmittal, oak* any necessary aju.m-d.ons and note errors under "Conclusions". 13.0 GC/TC ?J"*il«TWTT T3J iteration CPors VTH 13.1 Are the Continuing Calibration Fbnns (Fbrm VH) present and ccnplete for the BA fraction? 13.2 Has a continuing calibration standard been analyzed for every twelve hours of sairple analysis per instrument? ACTION: List below all sacple analyses that were not within twelve hours of the previous continuing calibration analysis. ACTION: If any forss are missing or no continuing calibration standard has been analyzed within twelve hours of every sanple analysis, call lab for explanation / resubmittal. If continuing calibration data are not available, flag all associated sarple data as unusable ("R"). 13.3 Do any continuing calibration standard compounds have a RRF < 0.05? __ ACTION: Circle all outliers in red. ACTION: If any SNA conpound has a RRF < 0.05, flag positive results for that conpaund as estirated ("J"), and flag nan-detects for that conpound as unusable ("R"). 13.4 Do any oanpounds have a % difference between initial and / continuing calibration I?RF > 25%? v _ [__] —— ACTION: Circle all outliers in red and qualify associated sanple data as outlined in the table below: 1874 STANDARD OFE3AJZNG P5CC3URI Page: 26 of 26 Date: March 1990 Revision 7 ~~ " Fo 25-50 'J' positive results, no action for nan detects 50-90 ! 'J1 positive results, 'HI1 nan detects >90 'J1 positive results, "R" nan detects _________ i 13.5 Are there any transcription / f^Tn^yt-jr^ errors in the reporting of average response factors (RRF) or diffi (%D) between initial and continuing RRFs? (Check at least two values but if errors are found, check more.) ACTION: Circle errors in red. ACTICN: If errors are large, call lab for explanation / resubmittal, make any necessary corrections and note errors under "Conclusions". 14.0 Interr-fli y'^T'iiflrflff ./Fora 14.1 Are the internal standard areas (Fora vm) of every sample and blank within the upper and lower limits for each continuing calibration? fs/ 1 ACTICN: List aOl the outliers below. Sazple I Internal Std Area lower Limit Upper Lisit (Attach additional sheets if necessary.) ACTICN: If the internal standard area count is outside the upper or lower limit, flag with "J" all positive results and non- detects (U values) quantitatad with this internal standard. If extremely low area counts are reported, or if performance exhibits a major abrupt drop off, flag all assnri atari nan- detects as unusable ("R"). 14.2 Are the retention times of the internal standards within / 30 seconds of the associated calibration standard? r v 1 ACTICN: Professional judgement should 06 used to qualify data if the retention timpa differ by more than 30 seconds. .,.,,., ,-„-,,., IB; Page: 27 of 35 Date: March 19SO Revision 7 *0 N/ ,0 Field IS . 1 Were any field duplicates subnittfld for att. analysis? f V] ACITCN: Ccopare the reported results for field duplicates and calculate tb* relative percent difference. ACITCN: Any gross variation between field duplicate results oust be addressed in the reviewer narrative. However, if large differences exist, identification of field duplicates shculd be confirmed by contacting the saspler. I 87t> OPEPAUNG PKXSXPE Page: 23 of 35 Date: March 1990 Revision 7 ___ NO N/A PBKT c: P^'l'iVi^d/ H"** MJoX^^tS 1.0 1.1 Are the Traffic Report Forms present for all samples? ty 1 __ __ AdTCN: If no, contact Lab for replacement of missing or illegible cepies. 1.2 Do the Traffic Reports or T»H Narrative indicate any problems with sample receipt, condition of samples, analytical problems or special notations affecting the quality of the data? __ ACTICN: Use professional judgement to evaluate the effect on the quality of the data. AdlCN: If any sample analyzed as a soil contains more than 50* water, all data should be flagged as estimated (J). 2.0 Wold-ire: TJJT**5 2.1 Have any PEST/PC3 holding times, determined from date of collection to data of extraction, been exceeded? __ f V ] __ ~ Sarnies for FEST/PC3 analysis, both soils and waters, must be extracted within seven days of the date of collection. Extracts must be analyzed within 40 days of the date of extraction. 3.0 ?> V, L ' gate p«=QTvorv f f om IT) 3.1 Are the PEST/PC3 Surrogate Recovery Sumnaries (Form H) present fcr each of the following matrices: ft/ 1 __ __ a. Lew Water b. Mad Water __ c. Lew Soil [ __ ] " __ _VL d. Mad Soil 3.2 Are all the PEST/PCS samples listed on the appropriate Surrogate Recovery Sunraaries for each of the following matrices: • v i a. Low Water b. Had Water c. Low Soil d. Med Soil C——] _- ^ STANDARD OPERATING ERCCEIXJRE Page: 29 of 35 Date: March 1990 Revision 1 ! 5 s S o JVA" ACnON: ea~n lab for explanation / resubmittals. If missing deliverables are unavailable, effect on data under "Conclusions" section of reviewer narrative. 3.3 Were outliers marked correctly with an asterisk? ACTION: circle an outliers in red. 3.4 Was surrogate (DEC) recovery outside of the contract / • _ » . _ * f^L c_] _ _, specification for any sa&ple or blank? ACTION: No qualification is done if surrogates are diluted beyond detection. If recovery is below contract limit (but above zero) , flag all results for that sample "J". If recovery is zero, flag positive results "J" and nan-detects "R". If recovery for the blank is zero, flag nan-detects far all associated sarples "R". If recovery is above contract limit, flag all positive results for that saqple "JT", unless in the reviewers professional judgement the high recovery is due to co eluting interference (check the associated blank - if recovery is high there also, flag the sample data). ^_ 3.5 Are there any transcription/calculation errors between raw / data and Fora IT? __ fv 1 __ ACTION: If large errors exist, call lab for explanation / resubc-dttal, make any necessary corrections and note errors under "Conclusions". 4.0 Matrix Spikes (Tarn Till 4.1 Is the Matrix Spika Duplicate/recovery Fora (Form HI) / present? * __ f vM __ __ /1 4.2 Were matrix spikes analyzed at the required frequency for each of the following matrices: a. low Water b. Mad Water c. low Son d. Med Son C __ ] __ JL ACTION: If any matrix spike data are missing, take the action specified in 3.2 above. 4.3 How many KST/PCB spike recoveries are outside QC limits? Water Sails O out of 12 tWA out of 12 TUT 002 1S7Q STANDARD OFE3A1EC PROCEDURE Page: 30 of Date: March 1990 Revision 7 o N/A 4.4 How many RPD's for matrix spike and natxix spike duplicata recoveries are outside QC limits? Soils D out of 6 K ) f r out of 6 If JG and ISO both have 1«*?3 than zero recovery for an analyte, negative results for that analyte should be rejected, and positive results •should be flagged "J". da above applies only to the sample used for ifi/HSD analysis. Use professional judgement in applying this criterion to other sanples. Blanks fForsi TV] 5.1 Is the Method Blank Suanary (Form IV) present? f / 1 5.2 Frequency of Analysis: for the analysis of Pesticide TCL ccrpounds, has a reagent/method blank been analyzed for each set of samples or every 20 sanples of sinilar matrix (low water, mad water, low soil, / apriiug soil) , whichever is more frequent? [ v } 5.3 Quranatagraphy: review the blank raw data - chzoratogrars, quant reports or data system printouts. Is the chrazatographic performance ^baseline stability) for each instnoent acceptable for PEST/PC3s? ACTION: Use professional judgement to determine the effect on the data. 5.0 NOIZ: "Water blanks" and "distilled water blanks" are validated like any other sample and are not used to cualify data. Do not confuse than with the other QC blanks rf •?*«»<.««*< below. 6.1 Do any method/if &timient/raagent blanks have positive results for PEST/PCBs? When applied as described below, the contaminant concentration in these blanks are multiplied by the sample Dilution Factor. __ f 1 6.2 Do any field/rinse blanks have positive PEST/PCS results? __ C __ ] AdTCN: Prepare a list of the samples associated with each of the contaminated blanks. (Attach a separate sheet.) STANIA3D OFE3ATDG PROCEDURE Page: 31 of Date: Mar±x 1990 Revision 7 36 NOTE: Oily field/rinse blanks taken the saw day as the samples are used to qualify data. Blanks nay not be qualified bnransp of contamination in another blank. Blanks nay be qualified for surrogate, spectral, tuning or calibration QC problems. ACTION: Follow the directions in the table below to qualify TCL results due to contamination. Use the largest value from all the »«*•*••? »»»j blanks. YES NO N/A Sarpla cone > CSQL but < Sx blank flag sample result with a "U"; cross out "B" flag i Sample cone < CSQL &j is < 5x blank value Reject sanple result and report CRQL; cross out "B" flag ________ ' Sample cone > CSQL & > 5x blank value No qualification is needed i 6.3 Are there field/rinse/equianent blanks associated with every sample? ACHCN: For low level sanples, note in data assessment that there is no associated field/rinse/equipnent blank. Exception: sanples taken from a drinking water tap do not have associated field blanks. and GC 7.1 Are the following Gas Chrcratograns and Data System Printouts for both Primary and Confirmation (conf irration standards not required if there - are no positive results above CRQL) column present: a. Evaluation Standard Mix A b. Evaluation Standard Mix B c. Evaluation Standard Mix C d. Individual Standard Mix A e. Individual Standard Mix B f . miti-cccponent Pesticides Toxaphene & Oilordane g. Arcclors 1016/1260 h. Arcclors 1221, 1232, 1242, 1248, and 1254 ACITCN: If no, take action specified in 3.2 above / L'T 00V 1 880 STANDARD OFS3ATUC FBCdLTI Page: 22 of 35 Data: March 1990 Revision 7 YES NO 7.2 Is Fora VEEI Pest-1 present and complete for each GC column (primary and confiraaticn) and each 72 hour of analyses? ACTICN: If no, take action specified in 3.2 above. 7.3 Are there any transcripticn/ralailation errors between raw data and Fora VIU? __ \\/ -\ ACTICN: if large errors exist, call lab for explanation / resubmit±al, sake any necessary corrections and note errors under "Conclusions". 7.4 Has the total breakdown on quantitation or canfiraaticn column exceeded 20% for JU1'? - for Endrin? or if Endrin aldehyde and 4,4'-OCO cc~elute and there is a peak at their retention time, has the combined COT and Endrin breakdown exceeded 20%? ACTICN: a. If COT breakdown is greater than 20% cn quantitation colusn beginning with the sanples following the last in control standard: 1. Flag all positive EOT results "J". 2. If COT was not detected but ECO and/or CCE are positive, flag the COT nan-detect "R". 3. Flag positive DCO and CCE results "JIT1. 4. If COT breakdown is > 20% cn confirmation column and COT is identified on quantitation column but not on confiraation colusn, use professional judgement to determine whether DOT should be reported on Fora I (if reported, flag result "N"). b. If Endrin breakdown is > 20% cn quantitation column, beginning with the sanples following the last in contiul standard: 1. Flag all positive Endrin results "J". 2. If Endrin was not detected, but Endrin Aldehyde and/or Endrin Ketone are positive, flag the Endrin non-detect "R". 3. Flag Endrin Ketone positive results "JN". 4. If Endrin breakdown is > 20% on confiraaticn column and Endrin is identified cn guantitation column but not on confirmation column, use professional judgement to determine whether Endrin should be reported cn Form I (if reported, flag result "N"). c. If the combined breakdown is used (it can only be used if the conditions in 7.4 above are net) and is > 20% on quantitation column beginning with the last in cuitiol standard, take the actions specified in 7.4 a and b above. If the combined breakdown is >20% cn confiraaticn column and Endrin or DOT is identified cn quantitation column but not cn confirmation column, use professional judgement to determine whether Endrin or COT should be reported cn Fora I (if reported, flag result "IT). TUT 002 138: OPSVCIJC JRDdEEE Page: 23 of 36 Date: March 1990 Revision 7 YZS NO N/A four calibration factors <10* for the quantitation column? 7.5 Is the linearity check RSD of all four calibration factors / •\s • ACTICN: If no, flag positive hits for all pesticide and PCS analytes "J" for all »«-«*-•» »r-«j saoqples. Do not flag toxaphene or DOT if they are quantified from a 3-yoint calibration curve. 7.6 Is the * difference between the EVAL A and each analysis (quantitation and confirmation) DBC retention t-i-rm* within QC limits (2% for packed column, 0.3* for capillary [I.D. < 0.32 mm], 1* for Tnpiyihore [0.32 < I.D. < 2 mn]) ? ACTION: DBC retention t-imo cannot be evaluated if BBC is not detected. If it is present and has a retention *••**•» cut of QC limits, then use professional judgement to determine the reliability of the analysis and flag results "R", if appropriate. 7.7 Was the proper analytical sequence followed for each 72 hour period of analyses (page PEST D-36 in 8/87 SOW) ACTION: If no, use professional judgement to determine the severity of the effect on the data and accept or reject it accordingly. Generally, the effect. is negligible unless the sequence was grossly altered or the calibration was out of limits. J.O Pp^ticlde/PT? Sf>*'^a'r^^ Surra ]ry 8.1. Is Form IX present and conplete for each GC column and 72 hr sequence of analyses? ACTICN: If no, take action specified in 3.2 above. 8.2 Are there any transcription/osculation errors between raw data and Form IX? __ Fv 1 ACTICN: If large errors exist, call lab for explanation / resubmittal , make any necessary corrections and note errors under "Conclusions". 8.3 Is DOT retention <""*» for packed columns > 12 nin / (except OV-1 and CV-101 columns)? fv 1 __ __ ACTICN: If no, check that there is adequate resolution between individual components. If not, flag results for ccnpoonds that interfere with each other (co-eluta) "R". 8.4 Do all standard retention tines fall within the windows established for the first IND A and IND B analyses? OPSttTDC HCGZL^l Page: 34 of 35 Date: March 1S90 Revision 7 YES w N/A" ACTICK: Beginning with the samples following the last in control standard, check to see if the chrcmatograns contain peaks within an expanded window surrounding the expected retention times. If no peaks are found and, DBC is visible non-detacts are valid. If peaks are present and cannot be jA»nH*-iod through "pattern recognition" or a consistent shift in standard retention tiaes, flag all affected compound results "R". 8.5 Are the continuing calibration standard calibration factors within 15* (for quantitation colusn) or 20* (for confirmation oolum) of the initial (at beginning of 72 hr sequence) calibration factors? ACTICN: If no, flag all associated positive results "J". Use professional judgement to determine whether or not to flag non-detects. i.O 9.1 Is Fors X cccplete for every sample in which a pesticide or PCS was detected? [__] __ ACTION: If no, take action specified in 3.2 above. 9.2 Are there any transcription errors between raw / data and Fora X? __ [__] \/ ACTION: If large errors exist, call lab for explanation / resutnittal, rake any necessary collections and note errors under "Conclusions". 9.3 Are retention timPB of sairple ocqpounds within the calculated retention tine windows for both quantitation and confirmation analyses? Was GC/JS confirmation provided when required (when / conpcund concentration is > 10 ug/ml in final extract)? [ __ ] __ \/ ACnCN: Reject ("R") an positive results (neeting quantitation column criteria, but missing confirmation by a second column or GC/tS (if appropriate) . Also, reject ("R") all positive results not meeting retention time window criteria unless a«o'-i*'fc^ standard compounds are similarly biased (i.e. base on RRT to DBC) . 9.4 Check chromatograns for false negatives, especially for the multiple peak conponents toxaphene and PCB's. Were there any false negatives? __ [ __ 3 ACTION: If appropriate PCS standards were not analyzed, or if the lab performed no confirmation analysis, flag the appropriate data with an "R". STANDARD OFS3AI3C HOCE3UPZ Page: 35 of 36 Date: March 1990 Revision 7 35 NO . 0 CMmound Quantitation and P***1'^**^ Dst"**, Lion r.iTjtg 10.1 Are there any transcription / calculation errors in Form I results? deck at least two positive values. Were any errors found? __ [__] NOTE: Sizple peak pesticide results can be checked for rough agreement between quantitative results obtained on the two GC columns. The reviewer should use professional judgement to **ri** whether a such larger concentration obtained on one column versus the other indicates the presence of an interfering compound. If an interfering compound is indicated, the lower of the two values should be reported and qualified as presumptively present at an estimated quantity ("JN"). This necessitates a determination of an estimated concentration on the confirmation column. The narrative should indicate that the presence of interferences has obscured the attempt at a second column confirmation. 10.2 Are the CSQLs adjusted to reflect sample dilutions and, for soils, sanple moisture? __ [__] V ACTION: If errors are large, call lab for explanation / resubmirtal, make any necessary con actions and note errors under "Conclusions". ACTION: When a sanple is analyzed at more than dilution, the lowest CBQLs are used (unless a QC exceedance dictates the use of the higher CRQL data from the diluted sample analysis). Replace concentrations that exceed the calibration range in the original analysis by crossing out the "E" value on the original Fora I "and substi- tuting it with data from the analysis of diluted sample. Specify which Fora I is to be used, then draw a red "X" across the entire page of all Form I's that should not be used, including any in the summary package. i 0 ^^U^TftQ^rOCn^STn Q^^^Llvy 11.1 Were baselines stable? w '( __ —— 11.2 Were any electropositive displacement (negative peaks) or unusual peaks seen? __ 11.3 Were early eluting peaks (for early eluting / _ analytes) resolved to baseline? r v/1 __ —— ACTICN: For 11.1 and 11.2, commit only. For 11.3, reject ("R") those analytes that are not , ! l f Oo2 18S4 sufficiently resolved. STANDARD OPERATING HOVI7RE Page: 36 of 36 Date: March 1990 Revision 7 NO N/A 12.1 Were any field duplicates submitted for PEST/PCB analysis? ACTION: Ccopare the reported results for field duplicates and calculate the relative percent difference. ACTION: Any gross variation between field duplicate results oust be addressed in the reviewer narrative. However, if large differences exist, identification of field duplicates should be confiraed by contacting the saspler. SDG # 900731 Dede Tutu Wells Site Contaminated Volatile Method Blanks and Their Associated Samples Method Blank Associated Samples VBLK01 VBLK02 VBLK03 VBLK04 VBLK05 VBLK06 VBLK07 Devcon I, Hartman II, Rodriguez (P) Eglin III, Four Winds II, Harvey, Tutu Smith Rodriguez (PD) Eglin II Hartman III, Leonard, Steele, Trip Blank 9/26, VIHA III, Steele MS, Steele MSD Dede, Dench, Devcon III, Trip Blank 9/24, Trip Blank 9/25 TUT GERAGHTY & MILLER. INC. SDG # 900731 Dede Tutu Wells Site Contaminated Trip Blanks and Their Associated Samples Trio Blank Associated Samples Trip Blank 9/26 (770-15) Trip Blank 9/24 (731-05) Trip Blank 9/25 (731-10) Trip Blank 9/26 (731-18) Eglin II, Eglin III Devcon I, Devcon III, Rodriguez (P), Rodriguez (PD) Dede, Dench, Smith, Steele, Steele MD, Steele MSD Hartman II, Hartman III, Four Winds II, Tutu, Harvey, Leonard, VIHA III 1387 GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE TOTAL REVIEW CLP DATA ASSESSMENT Functional Guidelines for Evaluating Organics Analysis Case No. *?^73/ SDG No . Ttc-fa. LABORATORY CeiHif, S ITE DATA ASSESSMENT: The current functional guidelines (1988) for evaluating organic data have been applied. All data are valid and acceptable except those analytes which have been qualified with a "J" (estimated), "U" (non-detects), "R" (unusable) ,or "JN" (presumptive evidence for the presence of the material at an estimated value). All action is detailed on the attached sheets. Tvo facts should be noted by all data users. First, the "R" flag means that the associated value is unusable. In other words, due to significant QC problems the analysis is invalid and provides no information, as to whether the compound is present or not. "R" values should not appear on data tables because they cannot be relied upon, even as a last resort. The second fact to keep in mind is that no compound concentration, even if it has passed all QC tests, is guaranteed to be accurate. Strict QC serves to increase confidence in data but any value potentially contains error. Reviewer's C\ ^ J? J S i gnature: lAsffVwUis'?(-/ttdcjL,________Date: ol / Verified By; ^~^ }>***^>~- Date; / / -* — * — ATTACHMENT 1 SOP NO. HW-6 PAGE 2 OF 2-4 DATA ASSESSMENT: 1. HOLDING TIME: The amount of an analyte in a sample can change with time due to chemical instability, degradation, volatilization, etc. If the specified holding time is exceeded, the data may not be valid. Those analytes detected in the samples whose holding time has been exceeded with be qualified as estimated, "J". The non-detects (sample quantitation limits) will be flagged as estimated, "UJ", or unusable, "R", if the holding times are grossly exceeded. The following action was taken in the samples and analytes shown due to excessive holding time. The volatile and semivolatile organic compounds and pesticides/PCBs were analyzed within holding times for all samples. n.J'I OO2 .1.889 GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE J OF DATA ASSESSMENT: 2. BLANK CONTAMINATION: Quality assurance (QA) blanks, i.e., method, trip, field, rinse, and water blanks are prepared to identify any contamination which may have been introduced into the samples during sample preparation or field activities. Method blanks measure laboratory contamination. Trip blanks measure cross-contamination of samples during shipment. Field blanks measure contamination of samples during field operations. If the concentration of the analyte is less than 5 times the blank contaminant level (10 times for the common lab contaminants), the analytes are qualified as non-detects, "U". The following analytes in the samples shown were qualified with "U" for these reasons: A) Method blank contamination Volatile Organic Compounds Method blank VBLK01 is reported to contain a tentatively identified compound (TIC) with a retention time (RT) of 3.78 minutes at a concentration of 8.0 micrograms per liter (ug/L). The samples Devcon I, Hartman II, and Rodriguez(P) are associated with this method blank and contain the same TIC contamination. These TIC concentration values are qualified as non-detects because they are less than 5 times the contamination in the method blank and therefore the values are not reported. Method blank VBLK02 is reported to contain methylene chloride at a concentration of 3 ug/L and a TIC with a RT of 3.83 at a concentration of 4 ug/L. The samples Eglin III, Four Winds II, Harvey, and Tutu are associated with this method blank and have methylene chloride concentrations above the CRQL and the same TIC contamination. The methylene chloride concentration values are qualified with "U" because they are less than 10 times the common contaminant concentration in the method blank. The TIC values are not reported for reasons stated above. Method blank VBLK03 is reported to contain methylene chloride at a concentration of 5 ug/L. Sample Smith, which has a dilution factor of 2.5, is associated with this method blank and has a methylene chloride concentration of 11 ug/L. This concentration value is raised to 12 ug/L, the CRQL, and qualified with "U" because the value is less than 10 times the common contaminant concentration in the method blank. Please note that this sample •an GERAGHTY & MILLER. INC. ATTACHMENT 1 SOP NO. HW-6 PAGE ^ OF 2H DATA ASSESSMENT: was analyzed using Method 624 due to high compound concentrations and as a result the CRQL is higher for this sample. Method blank VBLK04 is reported to contain methylene chloride at a concentration of 3 ug/L and a TIC with a RT of 3.83 at a concentration of 4 ug/L. Sample Rodriguez(PD) is associated with this method blank and contains 2 ug/L of methylene chloride and 3 ug/L of the same TIC. The methylene chloride concentration value is qualified with "U" and the TIC value is not reported for reasons previously stated. Method blank VBLK05 is reported to contain 5 ug/L of methylene chloride, 2 ug/L of acetone, and 2 ug/L of a TIC with a RT of 3.78. Sample Eglin II is associated with this method blank and has a 5 ug/L of methylene chloride. This value is qualified with "U". Method blank VBLK06 is reported to contain 5 ug/L of methylene chloride, and 7 ug/L of a TIC with a RT of 3.83. Samples Hartman HI, Leonard, Steele, and VIHA III are associated with this method blank and have methylene chloride concentrations above the CRQL and the same TIC contamination. The methylene chloride concentration values are qualified with "U" and the TIC values are not reported for reasons stated above. Method blank VBLK07 is reported to contain 3 ug/L of methylene chloride and 2 ug/L of a TIC with a RT of 3.83. Samples Dede, Dench, and Devcon in are associated with this method blank and have the same TIC contamination. These TIC values are not reported for reasons stated above. Samples Dede and Devcon III have methylene chloride concentrations above the CRQL. These values are qualified with "U". Semivolatile Organic Compounds No contaminants are detected in the method blank. Pesticides/PCBs No contaminants are detected in the method blank. TUT GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE 5OF 2H DATA ASSESSMENT: B) Field or rinse blank contamination ("water blanks" or "distilled water blanks" are validated like any other sample). All samples were taken directly from a drinking water tap into a collection bottle, therefore no field blanks were necessary. C) Trip blank contamination (VOCs only). Trip blank 9/24 is reported to contain 25 ug/L of methylene chloride, 12 ug/L of acetone, 8 ug/L of xylenes, and 5 ug/L of a TIC with a RT of 3.83. The samples Devcon I, Devcon III, Rodriguez(P), and Rodriguez(PD) are associated with this trip blank. Devcon I and Rodriguez(P) have methylene chloride concentrations above the CRQL and the same TIC contamination. The methylene chloride concentration values are qualified with "U" because they are less than 10 times the concentration in the trip blank. The methylene chloride concentration values are already qualified in Devcon III and Rodriguez(PD) due to method blank contamination. The TIC concentration values for the four samples are already qualified due to method blank contamination. Devcon in and Rodriguez(PD) have acetone concentrations above the CRQL. These values are qualified with "U" because they are less than 10 times the common contaminant concentration in the trip blank. Trip blank 9/25 is reported to contain 34 ug/L of methylene chloride, 42 ug/L of acetone, 1 ug/L of toluene,? ug/L of xylenes, 3 ug/L of a TIC with a RT of 3.82, 7 ug/L of a TIC with a RT of 8.7, and 1 ug/L of a TIC with a RT of 21.52. Samples Steele, Smith, Dede, and Dench are associated with this trip blank. Sample Smith contains 25 ug/L of acetone. This value is qualified with "U" for reasons stated above. All four samples have methylene chloride concentration values above the CRQL which are qualified with "U" for reasons stated above. Samples Steele, Dede, and Dench contain the same TIC contamination. The TIC values are not reported for reasons stated above. Trip blank 9/26 is reported to contain 24 ug/L of methylene chloride, 4 ug/L of acetone, and 7 ug/L of a TIC with a RT of 3.82. The samples Hartman III, Hartman II, Four Winds II, Tutu, Leonard, Harvey, and VIHA III are GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE 6 OF 2H DATA ASSESSMENT: associated with this trip blank. Sample Hartman II contains methylene chloride at a concentration above the CRQL. This value is qualified "U" for reasons stated above. Samples Fourwinds II and Leonard both contain acetone at concentrations above the CRQL. These values are qualified with "U" for reasons stated above. Hartman III, Fourwinds II, Tutu, Leonard, Harvey, and VIHA III have methylene chloride concentration values above the CRQL which are already qualified due to method blank contamination. The TIC concentration values for the above samples are already qualfied due to method blank contamination. Trip blank 9/27 is reported to contain 16 ug/L of methylene chloride. Samples Eglin II and Eglin III are associated with this trip blank and have methylene chloride concentrations at or above the CRQL. These values are qualified as "U" for reasons stated above. GERAGHTY & MILLER. INC. ATTACHMENT 1 SOP NO. HW-6 PAGE 7 OF ZH DATA ASSESSMENT: 3. MASS SPECTROMETER TUNING: Tuning and performance criteria are established to ensure adequate mass resolution, proper identification of compounds, and to some degree, sufficient instrument sensitivity. These criteria are not sample specific. Instrument performance is determined using standard materials. Therefore, these criteria should be met in all circumstances. The tuning standard for volatile organics is bromofluorobenzene (BFB) and for semi-volatiles is decafluorotriphenyl-phosphine (DFTPP). If the mass calibration is in error, all associated data will be classified as unusable, "R". All mass calibrations are acceptable for both the volatile and semivolatile analyses. Two BFB tunes have a sample out of the 12-hour limit by less than 12 minutes. Each succeeding tune is acceptable, therefore, in this reviewer's professional judgement, no qualifiers are necessary. GERAGHTY & MILLER. INC. ATTACHMENT 1 SOP NO. HW-6 PAGE DATA ASSESSMENT: 4. CALIBRATION: Satisfactory instrument calibration is established to ensure that the instrument is capable of producing acceptable quantitative data. An initial calibration demonstrates that the instrument is capable of giving acceptable performance at the beginning of an experimental sequence. The continuing calibration checks document that the instrument is giving satisfactory daily performance. A) RESPONSE FACTOR: The response factor measures the instrument's response to specific chemical compounds. The response factor for the Target Compound List (TCL) must be >_ 0.05 (a ratio of areas) in both the initial and continuing calibrations. A value < 0.05 indicates a serious detection and quantitation problem (poor sensitivity). Analytes detected in the sample will be qualified as estimated, "J". All non-detects for that compound will be rejected ("R"). Volatile Organic Compounds The initial calibration performed on 9/19 has response factors >0.05 for all compounds. Sample Smith is associated with this calibration. No qualifiers are necessary. The initial calibration performed on 9/28 has response factors <0.05 for acetone, 2-butanone, and 2-hexanone. All samples except Smith are associated with this calibration and are qualified with "R" for the compounds stated above. The continuing calibrations performed on 9/29, 10/03, and 10/09 have response factors <0.05 for acetone, 2-butanone, and 2-hexanone. The continuing calibration performed on 10/01 has response factors <0.05 for acetone and 2-butanone. The continuing calibration performed on 10/08 has a reponse factor < 0.05 for 2-butanone and 2-hexanone. These compounds are already qualified in the samples associated with the above continuing calibrations as a result of deficient initial calibration response factors. The continuing calibration performed on 10/06 has a response factor <0.05 for acetone, 2-butanone, vinyl acetate, and 2-hexanone. The associated GERAGHTY & MILLER. INC. ATTACHMENT 1 SOP NO. HW-6 PAGE ^ OF 2 H DATA ASSESSMENT: samples are Devcon III, Trip blank 9/24, Dede, Dench, and Trip blank 9/25. The acetone, 2-butanone, and 2-hexanone concentration values are already qualified as a result of deficient initial calibration response factors. The vinyl acetate concentration values are qualified with "R" based on this continuing calibration. Semivolatile Organic Compounds All response factors are greater than or equal to 0.05 in both the initial and continuing calibrations. GERAGHTY & MILLER. INC. ATTACHMENT 1 SOP NO. HW-6 PAGE 10OF DATA ASSESSMENT: 5. CALIBRATION: A) PERCENT RELATIVE STANDARD DEVIATION (%RSD) AND PERCENT DIFFERENCE (%D): Percent RSD is calculated from the initial calibration and is used to indicate the stability of the specific compound response factor over increasing concentration. Percent D compares the response factor of the continuing calibration check to the mean response factor from the initial calibration. Percent D is a measure of the instrument's daily performance. Percent RSD must be <30% and %D must be <25%. A value outside of these limits indicates potential detection and quantitation errors. For these reasons, all positive results are flagged as estimated, "J" and non-detects are flagged "UJ" (if %D or RSD > 50%). If there is a gross deviation of %RSD and %D, the non-detects may be rejected ("R"). For the PCB/PESTICIDE fraction, %RSD for aldrin, endrin, DDT, and dibutylchlorendate must not exceed 10%. Percent D must be within 15% on the quantitation column and 20% on the confirmation column. Volatile Organic Compounds The initial calibration performed on 9/19 has a %RSD greater than 30% for chloromethane(35%). Smith is the only sample associated with this initial calibration. Chloromethane is a non-detect in this sample, therefore no action is necessary. The initial calibration performed on 9/28 has a %RSD greater than 30% for methylene chloride(66.948%) and acetone(71.280%). All samples except Smith are associated with this initial calibration. The methylene chloride concentration values are qualified with "J" for all positive hits and "UJ" for all non-detects. The acetone concentration values are already qualified as a result of deficient response factors. TUT GERAGHTY & MILLER. INC ATTACHMENT 1 SOP NO. HW-6 PAGE 11 OF DATA ASSESSMENT: The continuing calibration performed on 10/02 has a %D greater than 25% for the following compounds: Compound %D Methylene Chloride -52.4 2-Butanone 44.4 Vinyl Acetate -36.7 trans-l,3-Dichloropropene .999 4-Methyl-2-pentanone 39.1 2-Hexanone -58.0 Sample Smith is associated with this calibration. The trans-1,3- dichloropropene concentration is qualified with "R" because it is a non-detect and the %D is is greater than 90%. The 2-butanone, vinyl acetate, and 4- methyl-2-pentanone are non-detects, therefore no qualifiers are necessary. 2- Hexanone is a non-detect, but the %D is greater than 50%, therefore the quantitation limit is qualified with "UJ". The methylene chloride concentration is already qualified due to deficient initial calibration %RSD. The continuing calibration performed on 9/29 has a %D greater than 25% for the following compounds: Compound %D Methylene Chloride 43.38 Acetone 27.13 Carbon Tetrachloride 28.68 Bromoform 25.15 The samples Devcon I, Rodriguez(P), and Hartman II are associated with this calibration. Carbon tetrachloride and bromoform are not detected in these samples, therefore no action is necessary. Methylene chloride concentration values are already qualified due to a deficient initial calibration %RSD. Acetone is already qualified due to a deficient response factor. TUT 002 1898 GERAGHTY & MILLER. INC. ATTACHMENT 1 SOP NO. HW-6 PAGEI20FZM DATA ASSESSMENT: The continuing calibration performed on 10/01 has a %D greater than 25% for the following compounds: Compound %D 1,2-Dichloroethane 42.31 2-Butanone 47.03 Bromodichloromethane 25.24 trans-l,3-Dichloropropene 28.28 Dibromochloromethane 41.51 1,1,2-Trichloroethane 39.96 Bromoform 26.97 2-Hexanone 34.13 4-Methyl-2-Pentanone 56.49 1,1,2,2-Tetrachloroethane 39.33 Rodriguez(PD) is the only sample associated with this calibration. 4-Methyl-2 -pentanone concentration value is qualified with "UJ" because it is a non- detect and the %D is greater than 50%. The 2-butanone and 2-hexanone concentration values are already qualified due to deficient response factors. The remaining compounds are non-detects and have %Ds less than 50%, therefore no qualifiers are necessary. The continuing calibration performed on 10/03 has a %D greater than 25% for the following compounds: Compound %D Chloromethane 26.36 Methylene Chloride 39.16 Acetone 34.95 2-Hexanone 29.35 Samples Four Winds II, Tutu, Harvey, and Eglin III are associated with this calibration. Chloromethane is not detected in any of these samples, therefore no action is necessary. Methylene chloride concentration values are already qualified due to deficient initial calibration %RSD. Acetone and 2-hexanone concentration values are already qualified due to deficient initial calibration rUT 002 1899 GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE 13OF 2-H DATA ASSESSMENT: response factors. The continuing calibration performed on 10/06 has a %D greater than 25% for the following compounds: Compound %D Vinyl Chloride 33.45 Methylene Chloride 44.78 Acetone 48.44 Vinyl Acetate 66.87 1,1,2,2-Tetrachloroethane 30.11 Samples Devcon III, Trip blank 9/24, Dede, Bench, and Trip blank 9/25 are associated with this calibration. Vinyl chloride and 1,1,2,2-Tetrachloroethane are not detected in these samples, therefore no qualifiers are necessary. The methylene chloride concentration values are already qualified due to a deficient initial calibration %RSD. Acetone and vinyl acetate are already qualified due to deficient initial response factors. The continuing calibration performed on 10/08 has a %D greater than 25% for the acetone(93.97) and 2-butanone(82.37). Samples Steele, Hartman III, Leonard, VIHA III, and Trip blank 9/26 are associated with this calibration. These compounds are already qualified as a result of deficient initial calibration response factors. The continuing calibration performed on 10/09 has a %D greater than 25% for the following compounds: Compound %D Chloromethane 28.83 Bromomethane 27.13 Methylene Chloride 33.67 2-Butanone 75.79 Vinyl Acetate 46.25 4-Methyl-2-Pentanone 38.55 GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE flOF 2-H DATA ASSESSMENT: Sample Eglin II is associated with this calibration. Methylene chloride is already qualified due to deficient initial calibration %RSD. 2-Butanone is already qualified due to a deficient initial calibration response factor. The remaining compounds are non-detects and have %Ds less than 50%, therefore no qualifiers are necessary. Semivolatile Organic Compounds No semivolatile organic compounds were detected in any of the samples. Therefore, the CRQLs will be qualified with "UJ" only when calibrations have %RSDs or %Ds greater than 50%. The continuing calibration performed on 10/13 has a %D greater than 25% for 2,4-dinitrophenol(61.8%). The sample Steele is associated with this calibration. The non-detect value is qualified with "UJ". Pesticides/PCBs The %RSD for aldrin, endrin, DDT, and dibutylchlorendate did not exceed 10%. The %D was within 15% on the quantitation column. TUT 002 1901 GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 DATA ASSESSMENT: 6. SURROGATES: All samples are spiked with surrogate compounds prior to sample preparation to evaluate overall laboratory performance and efficiency of the analytical technique. If the measured surrogate concentrations were outside contract specifications, qualifications were applied to the samples and analytes as shown below. Volatile Organic Compounds For the Method 624 analysis, all surrogate recoveries are within quality (QC) limits. As specified in Method 524.2, only two surrogate compounds were used, bromofluorobenzene (BFB) and trans-l,2-dichlorobenzene-d4 (t-DCB). The recovery of BFB is outside the QC limits (86-115%) in the following sample analyses: Sample %BFB Recovered Dench 60 Eglin II 84 Four Winds II 128 Leonard 118 Rodriguez(PD) 68 TUTU 126 VBLK01 84 VBLK04 68 VBLK06 120 These samples were not re-analyzed. For each affected sample, the concentration values for all compounds are qualified "J" for positive hits, and "UJ" for all non-detects. No QC limits are established for the recovery of t-DCB; however, when the BFB recovery is within QC limits, the t-DCB recovery is in the range of 84% to 122%. GERAGHTY & MILLER. INC. ATTACHMENT 1 SOP NO. HW-6 PAGE DATA ASSESSMENT: Semivolatile Organic Compounds The surrogate compound 2-fluorophenol is out of QC limits (21-100%) in the sample analysis of Dench. No action is necessary when only one surrogate is out of QC limits. Pesticides/PCBs The Dibutylchlorandate (DEC) recovery was high for all samples except Leonard. No pesticides or PCBs were found in any of the samples, therefore no qualifiers are necessary. GERAGHTY & MILLER. INC. ATTACHMENT 1 SOP NO. HW-6 PAGE n OF 2H DATA ASSESSMENT: 7. INTERNAL STANDARDS PERFORMANCE: Internal standards (IS) performance criteria ensure that the GC/MS sensitivity and response are stable during every experimental run. The internal standard area count must not vary by more than a factor of 2 (-50% to +100%) from the associated continuing calibration standard. The retention time of the internal standard must not vary by more than +_ 30 seconds from the associated continuing calibration standard. If the area count is outside the (-50% to +100%) range of the associated standard, all of the positive results for compounds quantitated using that IS are qualified as estimated, "J", and all non-detects as "UJ", or "R" if there is a severe loss of sensitivity. If an internal standard retention time varies by more than 30 seconds, the reviewer will use professional judgement to determine either partial or total rejection of the data for that sample fraction. All internal standard area counts and retention times are within QC limits for both volatile and semivolatile compound analyses. 1904 \\\\ *-•-•-• GERAGHTY & MILLER. INC. ATTACHMENT 1 SOP NO. HW-6 PAGE//OF 24 DATA ASSESSMENT: 8. COMPOUND IDENTIFICATION: A) VOLATILE AND SEMI-VOLATILE FRACTIONS: TCL compounds are identified on the GC/MS by using the analyte's relative retention time (RRT) and by comparison to the ion spectra obtained from known standards. For the results to be a positive hit, the sample peak must be within +_ 0.06 RRT units of the standard compound and have an ion spectra which has a ratio of the primary and secondary m/e intensities within 20% of that in the standard compound. For the tentatively identified compounds (TIC) the ion spectra must match accurately. In the cases where there is not an adequate ion spectrum match, the laboratory may have provided false positive identifications. Volatile organic compounds are properly identified on the GC/MS and all TICs accurately match their ion spectra. No semivolatile target compounds were found in any sample. B) PESTICIDE FRACTION: The retention times of reported compounds must fall within the calculated retention time windows for the two chromatographic columns and a GC/MS confirmation is required if the concentration exceeds 10 nanograms per liter (ng/ml) in the final sample extract. No pesticides or PCBs were found in any sample. GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE HOP 2L4 DATA ASSESSMENT: 9. MATRIX SPIKE/SPIKE DUPLICATE, MS/MSD: The MS/MSD data are generated to determine the long-term precision and accuracy of the analytical method in various matrices. The MS/MSD may be used in conjunction with other CC criteria for some additional qualification of the data. All MS/MSD % recoveries are within QC limits for volatile, semivolatile organic compounds and pesticides and PCBs. GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE20OFZH DATA ASSESSMENT: 10. OTHER QC DATA OUT OF SPECIFICATION: A) Method Detection Limit Study Method 524.2 state that a method detection limit (MDL) study must be performed prior to sample analyses. The MDL study consists of seven repeat analyses of target compounds at concentrations of 1 ppb. The QC limits for mean accuracy (% recovery) and %RSD are 80-120% and 20%, respectively. The MDL study must be repeated if these standards are not met. The MDL study associated with SDG Dede results was performed in April 1990 and has the following deficiencies (*): Mean Compound Aceuracy.% % RSD 1.1-Dichloroethene 72* 7.2 Methylene Chloride 148* 12.0 1.2-Dichloroethane 121* 7.9 Tetrachloroethene 76* 9.5 Bromoform 88 28.0 * 1,1,2,2-Tetrachloroethane 122* 7.3 In addition, the following compounds were not included in the MDL study: acetone, carbon disulfide, 2-butanone, vinyl acetate, 4-methyl-2-pentanone, 2- hexanone. The above compounds are flagged "J" for all samples, except where compounds are qualified "R" for other deficiencies. B) Laboratory Fortified Blanks QC requirements established in Method 524.2 and the Sampling, Analysis, and Monitoring Plan (Appendix A) state that laboratory fortified blanks (LFBs) must be analyzed immediately following each continuing calibration and the accuracy must be between 80% to 120% recovery. The provided data indicate that the recoveries were out of QC limits for volatile compounds in each LFB. The LFBs were not always analyzed immediately after the calibrations. The affected samples and compounds are qualified "J" to reflect these deficiencies. GERAGHTY & MILLER. INC. TU > ATTACHMENT 1 SOP NO. HW-6 PAGE21QFZ4 DATA ASSESSMENT: 11. SYSTEM PERFORMANCE AND OVERALL ASSESSMENT The compounds of primary importance in this project are the volatile organics. SDG Tutu has several QC criteria out of specification. The MDL study had % recoveries out of QC limits as well as compounds which were not included in the study at all. The FLBs also had several compounds out of QC Limits and twice was not run immediately after the continuing calibrations. All target compounds were present in the FLBs. These MDL and FLB deficiencies indicate that the laboratory instrumentation has difficulties recovering certain compounds at such low concentrations (1 ppb). As a result, the affected compounds are qualified with "J" in the associated samples. The volatile surrogate recoveries are out of QC limits in several samples as well as three (out of seven) method blanks. For the affected samples, the identification of the compounds is acceptable, but for positive hits and non- detects the quantitation must be considered as estimated only. The concentration values and quantitation limits for the six affected samples have been qualified as such. The volatile calibrations are deficient for compounds which were either common lab contaminants or compounds not detected in any sample. The majority of the data is not seriously affected by these deficiencies. During the process of validation, the compound quantitation performed by the reviewer did not agree with the quantitation performed by the lab. The lab was notified and the laboratory personnel determined that the incorrect response factors were used to quantitate the compound concentrations for samples Hartman III, Leonard, Steele, and VIHA III. The lab corrected the problem and sent revised Form I(s) and quant Hation reports. These revisions are included with the data package. Overall, the volatile organic data is consistent although QC problems do exist as discussed above. The semivolatile data is acceptable. One qualifier was needed due to calibration deficiencies. TUT GERAGHTY & MILLER. INC ATTACHMENT 1 SOP NO. HW-6 PAGE2ZOF2M DATA ASSESSMENT: The pesticide/PCB data is acceptable. The surrogate recovery was high for all but one sample, but no pesticides or PCBs were found, therefore it has no effect on the data. TUT OO2 19O9 GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 DATA ASSESSMENT: 12. CONTRACT PROBLEMS The MDL study failed to include six target compounds. Several results were out of QC limits established in Method 524.2 and the Sampling, Analysis, and Monitoring Plan. The LFBs were not analyzed immediately after the calibrations and many % recoveries are not within QC limits. The volatile organic analyses have several samples and three blanks with the surrogate BFB out of QC limits. The lab has failed to perform satisfactorily because there is no evidence of reanalysis for any sample or blank. Sample Smith was originally analyzed using Method 524.2. The compound concentration values were not within the calibration range of the instrumentation. In order to analyze the sample within holding time the laboratory defaulted to Method 624. This was a breach of contract. The Sampling, Analyses, and Monitoring Plan calls for all samples to be analyzed using Method 524.2 in order to reach low detection limits. T U T GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 DATA ASSESSMENT: 13. This package contains sample re-extractions, re-analyses or dilutions. Upon reviewing the OA results, the appropriate following form I(s) have been used. Form I(s) for sample re-extraction, re-analysis, or multiple dilutions are not included in this package because all original analyses were accepted. GERAGHTY & MILLER. INC. SOP NO. itt-2 Evaluation of Metals Data for the Contract Laboratory Ptoyrau (CLP) based on SOW. 7/88 REV. 2/89 1 1 ^ (SOP Revision X) V / *• PP£?*P£3 BY; ^ Jj^'~ ^ *" / *^ A^ •* /»' O_______..__ EME: A"" /c* •— /O m Hanif aieikn, Quality Assurance Cnentist Toxic and Hazardous Waste Section 1 BY; (SF-t-i1-* f%lt*-4*-'-rm<'— ——— ERIE: Louis Beviiaqoua, Section" Chief ~ ' " Hazafoous Waste ~ Gerard F. Md^rma. Oiief ^ Morrrtoring Management Branch 1 1 T 1 1912 OPERATING PKJCDU?.£ Page 1 o: 35 Title: Evaluation of Inorganic Data for the Date: Feb. i??:- Contract Laboratory Program Number: K-.-2 Revision: 10 1.0 Scope 1.1 This procedure is applicable to inorganic data obtained from contractor laboratories wsrking for Hazardous Waste Site Contract Laboratory Program (CLP). 1.2 Tne data validation is based upon analytical and quality assurance requirements specified in Statanent of Work (SOW) 7/88. 2.0 Responsibilities - Data reviewers vill complete the following tasks as assigned by the Dat Review Coordinator: 2.1. For a 2.1.1 Tta^a ^-^TffrfjTg'it ~ *TVirai Review-InmutmJi"^* CTBCXIifTL PiTFTTliX (A..1) Tne reviewer nust answer every question on the checklist. 2.1.2 DfTM PtfTiyyiilH H ~* I?Btfl ftSfittmmU HBtrnifrive (AiiJaitl'ifl ft, 2) Tlie answer on the checklist nust match the action in the narrative (appendix A. 2) and on Form I's. Do not use pencil to write the narrative. 2.1.3 Qntr^fiTt yon-ffnpl lance - ffp RfiEflTT This repom is to be completed only when a serious contract violation is encountered, or upon the request of the Data Review Manager or Deputy Project Officer (DPO). Forward 5 copies: one each for internal files, appropriate Regional DPO, Sample Management Office (SMD) and last two addresses of Mailing List for Data Reviewers (Appendix A. 4). In other cases, all contract violations should be appended to end of Data Assessment Narrative (Sec. A. 2. 2) 2 1.4 PBtva Supxparv ^**^f •• StUBHTV of incTpmnic QtialitTY CmtJPl DP^^ (Amfpjlx A. 5). Enter in ink on Data Summary Sheet required QC values from Forms I through IX. Circ all values that require data qualification "Action". 2.1.5 CTJP TifttVl ?^VrtiiVirmt'i I?lITna'rY 2.1.5.1 Appendix A. 6 Fill in the total nunter of analytes analyzed by different analyses and tne number of analytes rejected or flagged as estimated due to corresponding quality control criteria. Place an "X" in boxes where analyses were not performed, or criteria do not apply. 2.1.5.2 __ Data reviewer is also required to fill out Inorganic Regional Data Assessment form (Appendix A. 7) provided by EPA Headquarters. Codes listed on the form vill be used to describe the Data Assessment Summary. TUT 002 1913 SIWCftSD OFS3ATZN3 PPQdXJRE Page 2 o: 35 Title: Evaluation of Inorganic Data for the Date: Feb. 19?0 Contract. Laboratory Program Number: Hri-2 Revision: 10 2.1.6 Data Review Log: it is reoormended that each data reviewer should maintain a ice cf reviews completed to include: a. date of start of case reviev b. date of completion of case review c. site d. case number e. contract laboratory f. number of samples g. matrix h. hours uorked i. reviewer's initials 2.1.7 Telephone Rapprd Log - the data reviewer should enter the bare facts of inquiry, before initiating any pane conversation with CLP laboratory. After the case reviev has been completed, mail white copy of Telephone Record Log to the laboratory and pink copy to SC. File yellow copy in the Telephone Record Log folder, and attach a xerox copy of the Telephone Record Log to the completed Data Assessment Narrative (Appendix A. 2). 2.1.8 ... 1.8.1 Upon completion of reviev, the following are to be forwarded to the Regional Sample Control Center (RSCC) located in the Surveillance and Monitoring Branch: a. data package b. completed data assessment checklist (Appendix A.I,original) c. S-O Contract Compliance Screening (CCS) d. Data Summary Sheet (Appendix A. 5) along with completed Data Assessment Narrative (Appendix A.2) e. Record of Communication (copy) f. CLP Reanalysis Request/Approval Record (original + 3 copies) g. Appendix A.7 (original). ..1.8.2 Forward 4 copies of completed Data Assessment Narrative (Appendix A.2) along with 2 copies of the Inorganic Data Assessment Form (Appendix A.7) and Telephone Record Log , if any,: one each for appropriate Regional DPO, Sample Management Office (SMD), and last two addressees of Mailing List for Data Reviewers (Appendix A. 4) (the Inorganic Data Assessment form does not go to the last two addressees). STXCR3D OPERATING PROCEDURE Pace 3 c: 35 Title: Evaluation of Inorganic Data for the Date: Feb. 19?-: Contract Laboratory Program Number: H.-:-2 Revision: 10 2.1.9 Filed P^PflT-^rfr ~ Upcrv completion of review, the following are to be filed within M-3 files: a. Four copies of completed Data Assessment Narrative (Appendix A. 2) each carrying Appendix A.7. b. Telephone Record Log (copy) c. S-D Report (copy Appendix A-3) d. CLP Data Assessment Summary Form (Appendix A. 6 > . e. CLP Reanalysis Request/Approval Record (copy) Indicate incomplete data pacJcage on the computer tracking sheet located in M-3 office. Authorized contractor personnel may contact the laboratory after discovery of an incomple- data pacJcage. If a laboratory win not return phone calls or does not respond to request: notify M-3 coordinator of Region II for resolution. 4.0 Rejection of Data - All values determined to be unacceptable on the Inorganic Analysis Da- Sheet (Form I) must be lined over with a red pencil. As soon as any review criteria caus^ data to be rejected, that data can be eliminated from any further review or consideratia L 5.0 Accept^nr*? f^iteria ~ In order that reviews be consistent among reviewers, acceptance criteria as stated in Appendix A.I (pages 4-25) should be used. Additional guidance c be found in the National Inorganic Functional Guidelines of October 1, 1989. Screening (CCS) - This is intended to aid reviewer in locating a probisns, both corrected and uncorrected. However, the validation should be carried o €"/en if CCS is not present. Resutmittals received from laboratory in response to CCS mu be used by the reviewer. 7.0 PcrjuidBr f^r ^aanaiysig - Data reviewers must note all items of contract non-compliancs within Data Assessment Narrative. If holding times and sample storage times have not be exceeded, DPO may request reanalysis if items of non-compliance are critical to data assessment. Requests are to be made on "CLP Re-Analysis Request/Approval Record". 8.0 Rnrart flf carmjnieat.iqi - Provided by the Regional Sample Control Center (RSCC) to indicate which data packages have been received and are ready to be reviewed. nfr renters - The data reviewer will follow the standard practice. UT 002 19 SIMOVSD OF53AHIC aati -.itae- o: 35 Title: Evaluation of Metals Data for tne Date: Feb. I9?v Contract Laboratory Piutjiam Nustter: H/;-2 Appendix A.l: Data Assessnent - Contract Revision: 1C Compliance (Total Review - Inorganics) : if no, prepare Telephone Record Log,. and contact laboratory. Do numbers of samples correspond to nutters on Record of Communication? A. 1.1 Contract o-flTpl^pee SeraeniTyp RfflprT (CCS) - Present? [__] :: If no, contact RSCC. A. 1.2 P^rW'Q f* Q'iUmniTTfffJgn (fron Rgon - Present? [ __ ] ^ aCUn;: if no, request from RSCC. A. 1.3 Trip Report - Present and complete? [ _ ] _ _ \/ :: if no, contact RSCC for trip report. A. 1.4 sapp^f Traffic P°c"TT ~ Present or on file? [ Vj Legible? [ \/} Ama:: If no, request from Regional Sanple Control Center (RSCC). A.I. 5 CQVBT Pace - Present? [ ^ ] Is cover page properly filled in and signed by the lab / manager or tne manager's designee? C v ] / t____] __ — Do sample numbers on cover page agree with sample numbers on: (a) Traffic Report Sheet? <b) Fora I's? CJ^J ACTI CM-. If no for any of the above, contact RSCC for clarification. TUT 002 1.916 STANDARD OPERATING P»<rv:irar c: 3= Title: Evaluation of Metals Data for the Daze: Feb. 19?: Contract Laboratory Program Number: w.>-2 Appendix A.l: Data Assessment - Contract Revision: 10 Ccrpliance (Ibtal Review - Inorganics) __ -^ r; 5, A. 1.6 Form I frinai Pat-a) - Are all Form I's present and corplete? [J^_] _ _ _ ACTK3J: If no, prepare telephone record log and contact laboratory for submittal. Are correct units (ug/1 for waters and mg/Tcg for soils) / indicated on Fora I's? [J^J _ Are soil sample results for each parameter corrected for percent solids? (__] _ Are E?A sanple # s and corresponding laboratory sanple ID * s the same as on the Cover Page, Form I's and / in the raw data? [J£j _ _ Are computation/transcription errors less than 10% s of reported values? CJ_J _ _ Are all "less than IDL" values properly coded with "U"? (_J _ _ was a brief physical description of samples given on Form I's? C _ J _ _ Were the result qualifiers used correctly with final data? . _ _ ACTTQJ: If no for any of the above, prepare Telephone Record Log, and contract laboratory for corrected data. Were any samples diluted beyond requirements of contract? __ (__J __ If yes, vere dilutions noted on Form I's? [ _ ] _ J_ ACH2J: If no, note under QrttraCT-ProblenVNan-Ccnpliance of the"Data Assessment Narrative". A. 1.7 H?1flSrP Time's - (aqueous and soil sanples ) (Examine sample traffic reports and digestion/distillation logs. ) Mercury analysis (23 days). ...... exceeded? — C — cyanide distillation (14 days). . . -. • exceeded? — tjl — TUT OO2 1917 SIA'CKD OF-SAITC PROGDURT Page 6 c: 35 Title: Evaluation of Metals for the Contract Date: Feb. !??•;• Laboratory Program Number: Hf:-2* Appendix A.l: Data Assessment - Contract Revision: 10 Compliance (itotal Review - Inorganics) YES HQ Other Metals analysis (6 months). . . . exceeded? __ [ v\ _ Prepare a list of all samples and analytes for which holding times have been exceeded. Specify the number of days from date of collection to the date of preparation (from raw data). Attach to checklist. If yes, reject (red-line) values less than Instrument Detection Limit (HO and flag as estimated (J) the values above HJL even though sanple(s) was preserved properly. A.1.8 Raw Data A. 1.8.1 Digestion Log- for flame AVIC? (Form XIII) present? C v 1 _ _ Digestion Log for furnace AA Form XIII present? [ \s\ _ , _ Distillation Log for mercury Form XIII present? [ V] __ _ _ Distillation Log for cyanides Form XIII present? [ v\ __ _ Are pH values (pH<2 for all metals. pH>12 for cyanide) / present in Digestion/Distillation Logs? [_] ^__ _ •Weights, dilutions and volumes used to obtain values. Percent solids calculation present for soils/sediments? [__] _ Are preparation dates present on Digestion Log? t_^J __ A. 1.8.2 Measurement read out record present? ICP [J^J __ Flame AA [_] __ Furnace AA [_v/] __ Mercury [J/J __ Cyanides [J^J _ - !"l" O02 .1.9.18 CPSRAIHC FROGZL3E Page 7 o: 35 Title: Evaluation of Metals Data for the Date: Feb. 19?: Contract laboratory Program Number: H«-2 Appendix A.I: Data Assessment - Contract Revision: 10 Corrpiiance (Total Review - Inorganics) __ -^ A. 1.8.3 Are all raw data to support all sample analyses and QC operations present? Legible? • [ l\ Properly Labeled? [ l/\ ACnCN: If no for any of the above, write Telephone Record Log and contact laboratory. Flag metal data as estimated if pH of sample is greater than 2. Flag cyanide data as estimated if pH sarple is less than 12. A. 1.9 rtata Validation and Veri A . 1 . 9 . 1 A. 1.9. 1.1 Is record of at least 2 point calibration present for 1C? analysis? Is record of 5 point calibration present for Hg analysis? ACTigi: If no for any of the above, write in the Contract Problem/Ttan-Ccnpliance section of the "Data Assessment Narrative". " 1.9.1.2 Is record of 4 point calibration present for: Flame AA? [ __ ] Furnace AA? [ ^ __ _ Cyanides? C ^1 _ _ M7TT: 1. if less than 4 standards are measured in absorbance mode, then the regaining standards in concentration mode must be run inmediately after calibration and be within ±10% of true value. 2. For all AA (except Hg) and Cyanide analyses, one calibration standard is at CRDL level. If not, write in the Contract-F^oblaivWon-Compliance section of the "Data Assessment Narrative". OO2 1919 QFERAT2G PROCSDURI Fags S o: 35 Title: Evaluation of Metals Data for the Date: Feb. 19?: Contract Laboratory Program Number: K<-2 Appendix A.l: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) ED Flag associated data as estimated if standards are net within +10% of true values (except CRDL calibration standard). Do not flag the data as estimated in linear range indicated by good recovery of standard. A. 1.9.1.3 Is correlation *coefficient less than 0.995 for: Mercury Analysis? __ Cyanide Analysis? __ Atonic Absorption Analysis? _ [ *"" ] _ LJ: If yes, flag the associated data as estimated. A.1.9.2 Form II A (Initial and rnnyjrf^na Ca_______ A. 1.9.2.1 Present and conplete for every metal and cyanide? [ ^j Present and conplete for AA and 1C? vhen both are used for same analyte? (__J ACTTCN: If no for any of the above, prepare Telephone Record Log and contact laboratory. A. 1.9.2.2 Circle all values on data summary sheet that are outside contract windows. Are all calibration standards (initial and continuing) within 'control limits? Metals 90-110% [_ Hg - 80-120% [ 1 Cyanides 85-115% reviev^er will calculate correlation coefficient. STANDARD OPERATIC PROCZ3URE Title: Evaluation of Metals Data for the Date: Feb. 1990 Contract Laboratory Program Number: Hw-2 Appendix A.l: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) & Flag as estimated (J) all positive data (not flagged with a "U") analyzed between a calibration standard with %R between 75-89% (65-79% for Hg; 70-84% for CN) or 111-125% (121-135% for Hg; 116-130% for CN) recovery and nearest good calibration standard. Qualify results <IDL as estunated (UJ) . if the ICV or CCV %R is 75-89% (CN, 70-84% ; HG, 65-79%). Reject (red-line) as unacceptable data if recovery of the ICV or CCV is outside the range 75-125% (CN, 70-130%; Hg, -65-135%). Qualify five samples on either side of verification standard out of control limits. Was continuing calibration performed every 10 samples .^ or every 2 hours? t_J ACTTCK: If no, flag the excess samples (eleventh and up) data as estimated (J). Was ICV for cyanides distilled? If no, write in the Contract -Problem/Non-compliance section of the "Data Assessment Narrative". A. 1.9. 3 Form II B (CPir. "a-af^-arfte for AA and ICP) - A. 1.9. 3.1 was a CRDL standard (CRA) analyzed after initial calibration for all AA metals (excecc Ho)? *Was a mid-range calib. verification standard distilled and analyzed for cyanide analysis? IJL-l Was a ZxCRDL ( or 2xJDL when IDLX7DL) analyzed (CRT) for each ICP run? (Note: CHI for AL,BafCa,Fe,Mg,Naror K is not required.) ACTT CM: If no for any of the above, flag as estimated all data falling within the affected ranges. Hie affected ranges are: __ AA Analysis - **True Value ± CRDL ICP Analysis - **True Value * 2CRDL CN Analysis - **True Value ± 0.5 x True Value. ."ind the results of mid-range standard in the raw data. ••True value of CRA, CRI or mid-range standard. 'Substitute IDL for CRDL when IDL > CRDL. 1921 OPERATIC PROCEDURE Page 10 of 3: Title: Evaluation of Metals Data for the Date: Feb. 199: Contract Laboratory Program Number: hv;-2 Appendix A.l: Data Assessment - Contract Revision: 10 Compliance (Itotal Review - Inorganics) XES C D • ' • ~ A. 1.9.3.2 Was CRI analyzed after ICV/IC3 and before the final CCV/CCB, and for every four hours of ICP run? Ad2J: If no, write in Contract Problem/Non-Compiiance Section of the "Data Assessment Narrative". •..1.9.3.3 Circle all values on summary sheet that are outside acceptance windows. Are CRA and CRI standards within control limits: Metals 80 - 120%R? [_] \/_ __ Is mid-range standard within control limits: Cyanide 80 - 120%R? (_^j _ _ Flag as estimated all data within the affected ranges if the recovery of the standard is between 50-79%; flag only positive data if the recovery is between 121-150%; reject (red line) all data if the recovery is less than 50%; reject only positive data if the recovery is greater than 150%. A. 1.9. 4 Form III (Initial and ftnf.Jni''ng ra11*)rfffi1m A.1.9.4.1 Present and complete? C For both AA and ICP when both are used for same analyte? [ *""] Was an initial calibration blank analyzed? Was a continuing calibration blank analyzed after every 10 s frequent)? every 10 samples or every 2 hours (whichever is more >/ am CM: If no, prepare Telephone Record Log, contact laboratory and write in the contract-problems/ non-compliance section of the Data Assessment Narrative. OPERATING PROCZ3UFZ Pace 11 of 35 Title: Evaluation of Metals Data for the Date: Feb. 19?: Contract Laboratory Program Number: K-.*-2 Appendix A. l: Data Assessment - Contract Revision: 10 Ccrpiiance (Total Review - Inorganics) ™_ ._ A. 1.9. 4. 2 Circle all calibration blank values on Data Sunmary Sheet that are above CRDL (or 2 x IDL when KL > CRDL) . Are all calibration blanks (when IDL<CRDL) less than or equal to Contract Required Detection Limits (CRDL)? C *•* Are all calibration blanks less than two times Instrument Detection Limit (when IDLXZRDLJ? [ _ ] _ ^_ ACTION: if no for any of the above, flag as estimated (J) all positive data less than or equal to calibration blank values analyzed between calibration blank with value over CRDL (or 2xH2L) and nearest good calibration blank. Flag five samples on either side of the calibration blank. A. 1.9. 5 FCC94 III (Preparation, BlflTlK) ~ (Note: The preparation blank for mercury is the same as the calibration blank. ) A. 1.9. 3.1 Was one prep, blank analyzed for: each 20 samples? [J_] each batch? [J^J each matrix type? [ _ ] -n AA and 1C? wnen both are used for same analyte? ACTTCK: If no for any of the above, flag- as estimated (J) all associated positive data <10 x ULs for which prep, blank was not analyzed. If only one blank was analyzed for more than 20 samples, then first 20 samples analyzed 00 not have to be flagged as estimated ( J) . A. 1.9. 5. 2 Is concentration of prep, blank greater than CRDL when IDL is less than or equal to CRDL? If yes, is the concentration of the sample with the least concentrated analyte less than 10 times the prep, blank value? OPS3AHTC fcKJLsJURE Pace 12 of 35 Title: Evaluation of Metals Data for the Date: Feb. 1990 Contract Laboratory Program Number: »:-2 Appendix A.I: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) Am CM: if yes, reject(red-line) all associated data greater than CRDL concentration but less than ten times the prep, blank value found in the raw data. A. 1.9.5.3 Do concentrations of prep, blank fall below two times HL when IDL is greater than CRDL? [_] _ ACTTCFJ: if no, reject (red-line) all positive data that has a concentration less than 10 times the prep, blank value in the raw data. A. 1.9.5.4 Is concentration of prep, blank below the negative CRDL? __ [ *"j _ If yes, reject (red-line) all associated data that has a concentration less than lOxCRDL. A.1.9.6 Form IV (1C7 Interference 1.9.6.1 Present and complete? [J^J (ICTE: Not required for furnace AA, flame AA, mercury, cyanide and Ca, MS, -K and Na.) Was ICS analyzed at beginning and end of run (or at least twice every 8 hours)? If no. flag as estimated (J) all samples for which AL, Ca, Fe, or Mg is higher than in ICS. A. 1.8.6.2 Circle all values on Data Summary Sheet that are more than * 20% of true or established mean value. Are all Interference Check Sample results inside of control limits (•»• 20%)? [_1 If no, is concentration of Al, Ca, Fe, or Mg lower than in ICS? t_1 ,. If no, flag as estimated (J) those positive results for which ICS recovery is between 121-150%; flag all sample results as estimated if ICS recovery falls within 50-79%; reject (red-line) those sample results for which ICS recovery is less than 50%; if ICS recovery is above 150%, reject positive results only (not flagged with a "U"). OPZPATZC PSCCiHJrZ Paga 13 o: 35 Title: Evaluation of Metals Data for the Date: Feb. 199-1' Contract Laboratory Program Number: K%-2 Appendix A.I: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) _ A.l.9.7 Form V A ( Note: Not required for Ca, Mg, K, and Na (both matrices) , AI, and Fe (soil only. ) *-..!. 9.7.1 Present and complete for: each 20 samples? each matrix type? [_] each cone, range (i.e. low, med., high)? [_] For both AA and 1C? when both are used for sane analyte? (_1 ama:: If no for any of the above, flag as estimated (J) all positive data less than four times spiking level for which spiked sample was not analyzed. NC7TT: If one spiked sample was analyzed for more than 20 samples, then first 20 samples analyzed do not have to be flagged as estimated (J). A.I.9.7.2 Was field blank used for spiked sample? _ If yes, flag all positive data less than 4 x spike added as estimated (J) for which field blank was used as spiked sample. Matrix spike analysis should be performed on a field blank when it is the only aqueous sample in SDG. A. 1.9.7.3 Circle all values on Data Summary Sheet that are outside control limits (75% to 12S%). Are all recoveries .^ within control limits? t——J -£- — If no, is sample concentration greater than or equal ^^ to four times spiXe concentration? l——1 —— — If yes, disregard spike recoveries for analytes whose concentrations are greater than or equal to four tires spiXe added. If no, circle those analytes on Form V for which sample concentration is less than four times the spike concentration. TUT' 007 OPERATING PROCZDCFZ Page 14 o: 25 Title: Evaluation of Metals Data for the Date: Fes. 19?- Contract Laboratory Program Number: 'KW-Z Appendix A. 1: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) IES CB Are results outside the control limits (75-125%) flagged with "N" on Form I 's and Form VA? Acrrcr:: if no, write in the Contract - Problem/Nan - Compliance section of "Data Assessment Narrative". A.I. 9. 7. 4 Aqueous Are any spike recoveries: (a) less than 30%? ±_ [__] (b) between 30-74%? ^ [ _ ] (c) between 126-150%? __ (d) greater than 150%? __ If less than 30%, reject all associated aqueous data; if between 30-74%, flag all associated aqueous data as estimated ( J) ; if between 126-150%, flag as estimated (J) all associated aqueous data not flagged with a "IT; if greater than 150%, reject (red-line) all associated aqueous data not flagged with a "IT. NCTZ: if pre-digestion spike result is rejectable due to coefficient of correlation of MS»i, analytical spiJce recovery, or duplicate injections criteria, disregard spike recovery on Form V. Flag the associated data as estimated(J) . 1.9.7.5 Soil/Sedijnent Are any spike recoveries: (a) less than 10%? _ [ __ ] (b) between 10-74%? _ [ __ ] Jl (c) between 126-200%? __ [ _ ] _ (d) greater than 200%? __ [ _ 1 J^L ACTTCTJ.- If less than 10%, reject all associated data; if between 10-74%, flag all associated data as estimated; if between 126-200%, flag as estimated all associated data was not flagged with a "IT; if greater than 200%, reject all associated data not flagged with a "U". .tie: Evaluation of Mexais Data for the Contract Laboratory Program Appendix A. 1: Data Assessnent - Contract Conpliance Cltotal Review - Inorganics) Pa=S 15 CJ 3: Date: Feb. 19?: Revision: 10 ..1.9.8 ~1. 9.8.1 FOnn VI Present and complete for: each 20 sanples? 22 I each matrix type? [__1 each concentration range (i.e. low, med., high)? (__] both AA and 1CP when both are used for same analyte? [_] If no for any the above, flag as estimated (J) all data X3DL* for which duplicate sanple was not analyzed. 1. If one duplicate sanple was analyzed for ncre than 20 sanples, then first 20 sanples do not have to be flagged as estimated. 2. If percent solids for soil sanple and its duplicate differ by nore than !»., prepare a Form VI for each duplicate pair, report concentrations in Hg/L on vet weight basis and calculate RPD or Difference for each analyte. A. 1.9.8.2 Was field blank used for duplicate analysis? If yes, flag all data >CRDL* as estimated (J) for which field blank was used as duplicate. Duplicate analysis should be performed on a field blank when it is the only aqueous sanple in SDG. .8.3 Are all values within control limits (RPD. 20\ or difference < +CRDL)? If no, are all results outside the control limits flagged with an * on Form I's and VI? AdlQj*. If no* write in the Contract - Problems/Non- Conpliance section of "Data Assessment Narrative". 1. RPD is not calculable for an analyte of the sanple - duplicate pair when both values are less than IDL. Substitute IDL for CUDL when IDL > CRDL. __ t.VCl __ [_J XL __ OPERATING PROCEDURE Page 16 c: 35 Title: Evaluation of Metals Data for the Date: Feb. 19?: Contract Laboratory Program Number: W.-.:-2 Appendix A.I: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) 2. If lab duplicate result is rejectable due to coefficient of correlation of MSA, analytical spite recovery, or duplicate injections criteria, do not apply precision criteria. 1.9.8.4 Is any value for sanple duplicate pair less than CRDL* and other value greater than or equal to 10 x *CRDL? Acnctj: If yes, flag the associated data as estimated (J). A. 1.9.8.5 Acueous Circle all values on Data Summary Sheet that are: RPD > 50%, or Difference > ± CRDL* Is any RPD greater than 50% where sanple and^duplicate are both greater than or equal to 5 tines *CRDL? Is any **difference between sanple and duplicate greater than *CRDL where sample and/or duplicate is less than 5 f.-nes *CRDL? f^ [.. J __ ACTIQ:: If yes, flag the associated data as estimated. A. 1.9,8.6 Soil/Sediment Circle all values on Data Summary Sheet that are: RPD > 100%, or Difference > 2 X CRDL* Is any RPD (where sanple and duplicate are both greater than or equal to 5 tines *CRDL) : > 100%? Is any **difference between sanple and duplicate (where sanple and/or duplicate is less than 5x*CRDL> : > 2x*CRDL? * Substitute IDL for CRDL when HL > CRDL. ** Use absolute values of sanple and duplicate to calculate the difference. CFESATOC FTOC-HJKZ Page 17 oi 35 Title: Evaluation of Metals Data for the Date: Feb. 19?: Contract Laboratory Program Wjmoer: K<-2 Appendix A.I: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) its kf~" £Cna;: If yes, flag the associated data as estimated. A. 1.9. 9 Field A. 1.9. 9.1 Were field duplicates analyzed? [ \f } If yes, prepare a Form VI for each aqueous field duplicate pair. Prepare a Form VI for each soil duplicate pair, if percent solids for sanple and its duplicate differ by more than 1%; report concentrations of soils in ug/1 on vet veight basis and calculate RPDs or Difference for each analyte. I- Do not calculate RPD when both values are less than IDL. 2. Flag all associated data only for field duplicate pair. A. 1.9.9.2 Is any value for sample duplicate pair less than *<3BL and other value greater than or equal to 10 x *CRDL? . _ If yes, flag the associated data as estimated. A. 1.9.9.3 Aaugo'-is Circle all values on Form VI for field duplicates that are: RPD > 50%, or Difference > ± CRDL* Is any RPD greater than 50% where sanple and duplicate are both greater than or equal to 5 times *CRDL? __ tj/J _ Is any **difference between sanple and duplicate greater than *CRDL where sanple and/or duplicate is less than 5 times *CRDL? __ ACTTCN: If yes, flag the associated data as estimated. * Substitute IDL for CRDL when IDL > CRDL. ** Use absolute values of sanple and duplicate to calculate the difference. QPSSAT2C PPOGH.P.Z Page 18 o: 3: Title: Evaluation of Metals Data for the Date: Feb. 19?-: Contract Laboratory Program Number: H>:-2 Appendix A.I: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) t A. 1.9. 9. 4 Circle all values on Fonn VI for field duplicates that are: RPD >100%, or Difference > 2 x CRDL* Is any RPD (where sample and duplicate are both greater than 5 times *CRDL) : >100\? Is any **difference between sanple and duplicate (utiere sanple and/or duplicate is less than 5x *C3DL ) : >2x *CRDL? 2£Ha;: If yes, flag the associated data as estimated. A. 1.9.10 Form VJT (T-'tfPnTT'prv ^^TrtTPl f^TPlft) <Note: LC5 - not required for aqueous Hg and cyanide analyses.) A. 1.9.10.1 Was one LCS prepared and analyzed for: ^^t every 20 water sanples? [ ] every 20* solid sanples? [ _ ] both AA and 1C? when both are used for same analyte? [ __ ] ACTICK: If no for any of the above, prepare Telephone Record Log and contact laboratory for sudmittal of results of LCS. Flag as estimated (J) all data for which LCS was not analyzed. NOTE: If only one LCS was analyzed for more than 20 samples, then first 20 samples close to LCS do not have to be flagged as estimated. * Substitute IDL for CPDL when IDL > CRDL. **Use absolute values of sample and duplicate to calculate the difference. STANZKQ GFEEATHC PROCEHURE Page 19 o: 35 Title: Evaluation of Metals Data for the Contract laboratory Program Appendix A. 1: Data Assessment - Contract Compliance (Total Review - Inorganics) Date: Feb. 19?C Number: HA-2 Revision: 1C 2SS CLo A.I.9.10.2 Circle all LCS values outside control limits (80 - 120V except aqueous Ag and Sb). Is any LCS recovery: less than S0%? between 50% and 79%? between 121% and 150%? greater than 150%? ACTIcr:: Less than 50%, reject (red-line) all data; between 50% and 79%, flag all associated data as estimated (J); between 121% and 150%, flag all positive (not flagged with a "U") results as estimated; greater than 150%, reject all positive results. _ [_<r _. _ tJ^T _ J^ _ A.I.9.10.3 Solid ITS 1. If "Found" value of LCS is rejectable due to duplicate injections or analytical spixe recovery criteria, regardless of LCS recovery, flag the associated data as estimated (J). 2. If IDL of an analyte is equal to or greater than true value of LCS, disregard the "Action" below even though LCS is out of control limits. Is LCS "Found" value higher than the control limits on Form VII? ACTION: if yes, qualify all associated positive data as estimated. Is LCS "Found" value lower than the Control limits on Form VII? ACTION: If yes, qualify all associated data as estimated. __ (_.} _ __ [_ J __ GPESA73IG PROCEXai Page 20 OJ 35 Title: Evaluation of Metals Data for the Date: Feb. 199! Contract Laboratory Program Number: liv'.-z Appendix A.I: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) as A.1.9.11 Form IX. (ICP Serial Dilution) - MTT-I: Serial dilution analysis is required only for initial concentrations equal to or greater than 10 x EL. A. 1.9.11.1 Was Serial Dilution analysis performed for: s* each 20 samples? [ J_] _ _ each matrix type? [__] ___ __ each concentration range (i.e. low, med.)? [_] __ ±L ACTia:: If no for any of the above, flag all positive data greater than or equal to lOxIDLs as estimated (J) for which Serial Dilution Analysis was not performed, and sumnai^e the deficiency on the DPO report. A.I.9.11.2 Was field blanx(s) used for Serial Dilution Analysis? __ L^J — Acna:: If yes, flag all associated data > 10 x IDL as estimated (J). NOTE; Serial dilution analysis should be performed on a field blank when it is the only aqueous sample in SDG. A. 1.9.11.3 Are results outside control limit flagged with an "E" on Form I's and Form IX when initial concentration on Form IX is equal to 50 times IDL or greater. [__] —— — ACTICM; If no, write in the contract-problem/non- compliance section of the "Data Assessment Narrative". A 1 9.11.4 Circle all values on Data Summary Sheet that are outside control limit for initial concentrations equal to or greater than 10 x TTT-S only. Are any % difference values: , > 10%? IS^ i__1 > 100%? __ (.^\ TUT 002 SINCARD CPERAIHC PROCZZURE Page 21 cf 35 Title: Evaluation of Metals Data for the Date: FeS. 1990 Contract laboratory Program Number: K.-:-2 Appendix A.I: Data Assessment - Contract Revision: 10 Compliance (Ttotal Review - Inorganics) 25 Flag as estimated (J) all associated equal to or greater than lOxULs for which percent difference is greater than 10% but less than 100%. Reject (red-line) all associated sanple results equal to or greater than IQxTDLs for which PD is greater than or equal to 100%. A. 1.9. 12 Fumflc^i Atgruc fttffflrfrt-ic'rc (AA) CK A. 1.9.12.1 Are duplicate injections present in furnace raw data (except during full Method of Standard Addition) for each sarple analyzed by GFAA? A£Ha«: If no, reject the data on Form I's for which duplicate injections were not performed. A. 1.9.12.2 Do the duplicate injection readings agree within 20% Relative Standard Deviation (RSD) or Coefficientpf ^ Variation (CV) for concentration greater than CRDL? [ _ ] Was a dilution analyzed for sample with post digestion spike recovery less than 40%? [ _ ] ACT! CM: If no for any of the above, flag all the associated data as estimated ( J) . A. 1.9. 12.3 Is *post digestion spike recovery less than 10% or greater than 150% for any result? __ ACTI CM: If yes, reject (red-line) the affected data if recovery is <10%; reject data not flagged with "U* if spike recovery is >150%. NOTE: Reject the data only if the affected sanple was not subsequently analyzed by Method of Standard Addition. * Post digestion spike is not required on the pre-digestion spiked sanple when predigest: spike recovery is within control limits of 75-125% or when SR>4xSA. OFZPAJU'C PRQC3UEE Page 22 c: 35 Title: Evaluation of Metals Data for the Date: Feb. 199" Contract Laboratory Program Number: h'.-:-2 Appendix A. i: Data Assessment - Contract Revision: 10 Coiipiiance (Total Review - Inorganics) A.l.9.13 Ftonn VIII (Method of St-.arr*.arrt A. 1.9. 13.1 Present? [_f^J _ If no, is any Form I result coded with "S" or a "+"? _ [_ ] 2CCt£L7: If yes, write request on Telephone Record Log and contact laboratory for sutruttal of Form VIII. A. 1.9. 13. 2 Is coefficient of correlation for MSA less than 0.990 for .^ any sarple? r (_ ] _ A£Ha;: If yes, reject (red-line) affected data. A. 1.9. 13. 3 Was *>Sk required for any sanple but not performed? _ l.^] _ Is coefficient of correlation for M^i less than 0.995? _ [_ .] Are MS^ calculations outside the linear range of the calibration curve generated at the beginning of the analytical run? _ [_ _] ACTTCt:: If yes for any of the above, flag all the associated data as estimated (J). A. 1.9.13.4 Was proper quantitation procedure followed correctly as outlined in the SOW on page E-16 through E-17? Acng;: If no, note exception under contract problem/ non-carpliarce of data assessment narrative, or prepare a separate list. A.I.9.14 Dj A. 1.9.14.1 Were any analyses performed for dissolved as well as total analytes on the same sample(s). __ [ Were any analyses performed for inorganic as well as total ,^- (organic * inorganic) analytes on the same sample(s)? __ [.£_] — * MS>> is not required on LCS and prep. blanJc. TUT OU2 1934 PKX3U?£ Page 23 c: 35 Title: Evaluation of Metals Data for the Date: Feb. I9?v Contract Laboratory Program Nunber: tt-.'-z" Appendix A.I: Data Assessment - Contract Revision: 10 Ccnpiiance (Total Review - Inorganics) 1. If yes. prepare a list comparing differences between all dissolved (or inorganic) and total analytes. Compute tne differences as a percent of the total analyte only when dissolved concentration is greater than CKDL as well as total concentration. 2. Apply the following questions only if in- organic (or dissolved ) results are (i) above CRDL, and (ii) greater than total constituents. 3. At least one preparation blank, ICS, and LCS should be analyzed in each analytical run. A. 1.9.14.2 Is the concentration of any dissolved (or inorganic) analyte greater than its total concentration by nore than io%? A. 1.9.14.3 Is the concentration of any dissolved (or inorganic) analyte greater than its total concentration by . nore than 50»0? _ [. _] r Acna:: If more than 10%, flag both dissolved (or inorganic) and total values as estimated (J) ; if more than 50%, reject (red-line) the data for both values. A.I.9.15 Form I to DC A. 1.9.15.1 Are all the Form I through Form DC labeled with: Laboratory name? [ 1 Case/S^S number? {_} __ _ EPA sample No.? tJ^J __ __ SDG No.? Contract No.? [ ^ Correct units? [ ^J Matrix? j: If no for any of the above, note under contract problemAion-compliance section of the "Data Assessment Narrative". QFOATDC PROCEDURE Page 24 0: 35 Title: Evaluation of Metals Data for the Date: Feb. I9?c> Contract Laboratory Program Number: H-i~2 Appendix A. l: Data Assessment - Contract Revision: 10 Corpiiance (Total Revie.- - Inorganics) A. 1.9.15.2 Do any computation/transcription errors exceed 10% of reported values on Forms I-DC for: (NOTE: Check all forms against raw data.) (a) all analytes analyzed by ICP? _ [ 1^] _ (b) all analytes analyzed by GFAA? _ (c) all analytes analyzed by AA Flame? _ C__] ^ (d) Mercury? _ (e) Cyanide? _ A£2£U: If yes, prepare Telephone Log, contact laboratory for corrected data and correct errors with red pencil and initial. A. 1.9.16 Form I (Fie.Id. B^jP"1^) ~ Circle all field blank values on Data Summary Sheet that are greater than CRDL, 2 x IDL when IDL > CRDL. Do concentrations of field blank(s) fall below CRDL (or 2 x IDL when IDL > CRDL) for all parameters of associated aqueous and soil samples? [__] If no, was field blank value already rejected due to other QC criteria? [_] If no, reject (except field blank results) all associated positive sample data less than or equal to five times the field blank value. S3XZFJ® OPERATING PROdURZ Title: Evaluation of Metals Data for the Date: Feb. 199 :• Contract Laboratory Program Number: Hi-;-2 Appendix A.l: Data Assessment - Contract Revision: 10 Carpiiance (Total Review - Inorganics) __ ffl~ A. 1.9.17 Ftonn X. 3Q . XII (Verification Q A.l.9.17.1 is verification report present for: Instrument Detection Limits (quarterly)? [ 1 ICP Interelement Correction Factors (annually)? [_] 1CP Linear Ranges (quarterly)? ACT! CM: If no, contact DPO of the lab. A.l.9.17.2 Form X (Instrument Detection Limitis) - (Note: TTIL is not required for Cyanide.) Are IDLs present for: all the analytes? all the instruments used? _ For both AA and 1C? when both are used for same analyte? I_1 AcnaJ: If no for any of the above, prepare Telephone Record Log and contact laboratory. Is IDL greater than CRDL for any analyte? _ If yes, is the concentration on Form I of "'the sample analyzed on the instrument whose IDL exceeds CRDL, greater than 5 x IDL? [__1 —_ ACTICN: If no, flag as estimated all values __ less than five times HL of the instrument whose IDL exceeds CRDL. TUT SEVGRRD OP5WZ2C PROCEDUFZ Title: Evaluation of Metals Data for the Date: Feb. 199: Contract Laboratory Program Njmber: K-:-2 Appendix A.I: Data Assessment - Contract Revision: 10 Corpliance (Total Review - inorganics) YES tc LL3 A. 1.9. 17. 3 Form XI (Lir^ar Ponces) A.I. 9. 18 percerft If yes, qualify as estimated all data not previously rejected or flagged due to other QC criteria. Was any sample result higher than high linear range of ICP. _ Was any sample result higher than the highest calibration standard for non-ICP parameters? __ [ _ ] _ If yes for any of the above, was the s sample diluted to obtain the result on Form I? [ _ J _ _ \/_ If no, flag the result reported on Form I as estimated (J). Is soil content in sediment(s) less than 50%? _ C _ J J^i U.S. EPA - CLP DUPLICATES EPA SAMPLE NO. Lab Name: Lab Code: CeiMtC, Matrix (soil/water): * Solids for Sample: Case No. Contract: 1£>oo73>i SAS No.: SDG No. : Level (low/med): ^>w Solids for Duplicate: g-o Concentration Units (ug/L or mg/kg dry weight) : \ 1 I Analy te 1| Aluminum | Antimony I Arsenic 1 Barium | Beryllium I Cadmium I Calcium j Chromium 1 Cobalt I Copper (Iron ILead | Magnesium | Manganese 1 Mercury 1 Nickel j Potassium | Selenium 1 Silver j Sodium j Thallium | Vanadium (Zinc j Cyanide 1 Control Limit 1 1 I I Sample (S) C] j Duplicate (D) C I I Sg-oo \A\ \ 43/-00 1 £-3-00 1^1 1 ttoO \& A. 00 \(J\ 1 3.00 \<J X.ao l&l 1 S.oo \(J 3>.oo l£l 1 a. oo I./J •&-00 ll^l 1 ^.00 1^ HOOOO.OO 1 1 1 HViOD.OO \ 1^.00 \ \ \ HO- 00 \ St.oo I / I l l ,3^.^Q \A J^.,00 1^1 1 ifl.Ort I SQ.OO 1^1 1 V5-.A« l£ £t.oe> (A\ 1 l^.lo 1 387oo, ot> 1 II m'Joo.oo I I^A.oo 1 1 1 ta-l.oo \ O.=IA \[)\\ o.Jo IL/ / f c / o . o < - > lAl 1 112,0. cxp 1^ /.£3<3 I ( J | 1 /• 00 \U -7.0r> IUI 1 7.oo \(J J.*loao.oo 1 II «A^g'o£X).oo 1 /S~.QO lu'U /^:<oe Ib1 11.60 \A 1 f ST,<3o IX /-7./9/D l/^l 1 /fe.oo l£ J./'<5n 1 1 1 ff.rto l i v : I I I 1 1 1 1 I I RPD I I _ _ 1 <TlS2..^ \ \ ————— I I 1 1 I I I I 1 /fc.«? i r^.3^ i - —— - 1 Z-7..5- 1 ^=»^ 1 (H3.Z) 1 ^-^r-7 1 5.6 1 1 1 1 1 I .s-.q 1 1 1 1 1 Q M FORM VI - IN 193' 7/88 STANDARD OPERATING PROCEDURE Page I of 3 Tide: Case# SDG# Contractor Evaluation of Metals Data for the Contract Laboratory Program Appendix A. 1 : Data Assessment - Contract Compliance (Total Review - Inorganics) 900731 Site Tutu Well Site Dede Lab Ceimic Geraghty & Miller Reviewer Donna Lesch Date: Number: Revision: Matrix: Feb. 1990 HW-2 10 Soil Water X Other A.2.1 The case description and exceptions, if any, are noted below with reason(s) for rejection or qualification as estimated values(s) J. This data package includes the analysis of the samples for SDG Dede. These samples originated from St. Thomas on the 24, 25, 26 and 27 of September, 1990. There are seventeen low level water samples for metals analysis including one duplicate and one matrix spike QC sample._____________________ Cyanide concentration values for samples Devcon I, Devcon III, Rodriguez (P), Rodriguez (PD), and VIHA III are flagged "J" because the pH of the samples was less than 12._____________________________________ Thallium concentration values for all samples are flagged "R" because the matrix spike recovery is less than 30% (10.5%). Aluminum, Lead and Selenium____ concentration values are flagged as estimated ("J") because the spike_______ recoveries are between 30-74% (Al 70.6%, Pb 72.0%, Se 54.0%).________ The post digestion spike recoveries are low for Selenium and Thallium in all___ samples. These concentration values are already qualified due to poor______ recovery in the matrix spike. __ ———————————————————————————— TUT Oi">7 1 94o GERAGHTY & MILLER, INC. STANDARD OPERATING PROCEDURE Title: Evaluation of Metals Data for the Date: Feb. 1990 Contract Laboratory Program Number: HW-2 Appendix A.I: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) A.2.1 (continuation) For sample Smith, the Selenium concentration value is qualified with "R" because the coefficient of correlation for the Method of Standard Additions is less than 0.990. This qualifier supercedes all others._____________ The sample Steele was used for the sample duplicate analysis. The % Difference is out for QC limits for Aluminum, Chromium, and Lead, therefore all sample data are qualified with "J" for all positive values and "UJ" for all non-detccts. The % Difference for Aluminum, Chromium, and Lead are also out of QC h'mits in the field duplicate; the sample concentration values are already qualified for ____ these analytes. _____________________________________ One CRDL standard has several metals with recoveries out of control limits ____ (80-120 % recovery). The CRI run on 10/11 has the following deficiencies: ____ ______________ Metal ______________ % Recovery _________ ______________ Antimony ____________ 49.2 _____________ _____________ Beryllium ___________ 130.0 ____________ _____________ Cobalt _____________ 121.0 ____________ _____________ Silver _____________ 60.0 ____________ _____________ Zinc ______________ 135.0 ___________ All samples are associated with the above deficiences. All Antimony concentration values are rejected because the recovery is less than rm- f'02 i941 GERAGHTY & MILLER. INC. L STANDARD OPERATING PROCEDURE Page -3 of 3 Title: Evaluation of Metals Data for the Date: Feb. 1990 Contract Laboratory Program Number: HW-2 Appendix A.I: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) Positive hits for Cobalt, Beryllium and Zinc are qualified with a "J". Silver concentration values are qualified "J" for positive hits and "UJ" for non-detects. In the ICP serial dilution analysis, the initial concentration of Aluminum is___ greater than 10 times the IDL and the % Difference is out of QC limits. As a result, all Aluminum concentration values are qualified with "J"._________ A.2.2 Contract Problems/Non Compliance:_______________________ There were 2-hours and six minutes between independent check samples for the ICAP run on October 11, 1990. This is six minutes greater than the two hour required maximum.__________________________________ Devcon I, Devcon III, Rodriguez (P), Rodriguez (PD), and VIHA III were not correctly preserved for Cyanide.____________________________ MMB Reviewer: Date: Signature Contractor Reviewer: \/(JffwiAAs w- /y&44LzL>_______ Date: <> //»?/?/ Signature Verified by: bus#**A- Mat' J*+iArffaJt***'£'j~J Date: ______ " " " ' ' " r " . 1942 Tl IT OO-t- GERAGHTY & MILLER. INC. STWZARD OFEBATHC PROCEDURE Pace 30 c: 35 :le: Equation of Metals Data for the Date: Feb. 199: Contract Laboratory Prograin Number: Hi-:-2 Appendix A. 2: Data Assessment Narrative Revision: 10 A. 2.2 Contract-Problens/Non-Corrpliance Contractor Reviewer: TUT OO2 194? Page J of 13 Table 2. Tutu Residential Wells Sampling Results, September 1990, Sample Delivery Group 900731 Sample Identification: tile Organic Compounds (VOCs) Chloromethane Bromomethane Vinyl Chloride Chlorocthane Methylene Chloride Acetone Carbon Disulflde 1,1-Dichloroethene 1 , 1 -Dkhloroethane 1,2-Dkhloroethene (total) Chloroform 1,2-Dkhloroethane 2-Butanone 1,1,1 -Trichloroethane Carbon Tetrachloride Vinyl Acetate Bromodichloromethane 1 ,2-Dichloropropane cis-1 ,3-Dichloropropene Trichloroethene Dibroraochloromethane ' ' 2-Trichloroethane ^^iene trans-1 ,3-Dichloropropene Bromoform 4-Methyl-2-Pentanone 2-Hexanone Tetrachloroethene 1 , 1 ,2,2-Tetrachloroethane Toluene Chlorobenzene Ethylbenzene Styrene Total Xylencs Tentatively Identified VOCs Ethane, 1 , 1 ,2-Trichloro- 1 ,2, 2-trifluoro Unknown Propane-2-Methoxy-2-Methyl Dichlorobenzene isomer 731-01 Devcon I 2UJ 2 U 2 U 2UJ 1 UJ R 1UJ 1 UJ 1 UJ 1 U 1 UJ 1 UJ R 1 UJ 1 UJ 2UJ 1 U 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 2UJ R 1 UJ 1 UJ 1 UJ 1 UJ 1 U 1 U 1 U 731-02 Devcon HI 2 U 2 U 2U 2 U 8UJ R 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1UJ R 1 UJ 1 UJ R 1 U 1 UJ 1 U 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 2UJ R 1UJ 1 UJ 1 U 1 UJ 1 U 1 UJ 1 U 2JN 731-03 Rodriguez (P) 2UJ 2 U 2U 2UJ 1 UJ R 1 UJ 1 UJ 1 UJ 1 U 1 UJ 1 UJ R 1 UJ 1 UJ 2UJ 1U 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ- 1 UJ 1 UJ 2UJ R 1UJ 1 UJ 1 UJ 1 UJ 1 U 1 U 1 U 1 JN 731-04 Rodriguez (PD) 2UJ 2UJ 2UJ 2UJ 2UJ R 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ R 1 UJ 1 UJ 2UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 2UJ R 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 731-05 9/24 Trip Blank 2U 2U 2U 2U 25J 12 J IUJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ R 1 UJ 1 UJ R 1 U 1 UJ 1 U 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 2UJ R 1 UJ IUJ 1 U I UJ 1 U 1 UJ 8 5JN 731-06 Dede 2 U 2U 2U 2U 2UJ R 1 UJ IUJ 1 UJ 1 UJ IUJ 1 UJ R 1 UJ t UJ R 1 U 1 UJ 1 U IUJ 1 UJ IUJ 1 UJ IUJ 1 UJ 2UJ R 1 UJ 1 UJ 1 U 1 UJ 1 U 1 UJ 1 U All concentrations are reported in micrograms per liter (ug/L). J - Value is estimated. U - Compound is not detected. R - Value is rejected. N - Compound is a tentatively identified compound. GERAGHTY & MILLER, INC. Table 2. Tutu Residential Wells Sampling Sample Identification: itile Organic Compounds (VOCs) Chloromethane Bromomethane Vinyl Chloride Chloroethane Methylene Chloride Acetone Carbon Disulfide 1 , 1 -Dichloroethene 1 , 1 -Dichloroethane 1 ,2-Dichloroethene (total) Chloroform 1 ,2-Dichloroethane 2-Butanone 1,1,1 -Trichloroethane Carbon Tetrachloride Vinyl Acetate Bromodichloromcthane 1 ,2-Dichloropropane cis-l ,3-Dichloropropene Trichloroethene Dibromochloromethane 2 -Trichloroethane •w-dzene trans- 1 ,3-Dichloropropene Bromoform 4-Methyl-2-Pentanone 2-Hexanone Tetrachloroethenc 1 , 1 ,2,2-Tetrachloroethane Toluene Chlorobenzene Ethylbenzene Styrene Total Xylenes Tentatively Identified VOCs Ethane, 1 , 1 ,2-Trichloro- 1,2, 2-trifluoro Unknown Propane,2-Methoxy-2-methyl Dichlorobenzene isomer Results, September 1990, Sample Delivery Group 900731 731-07 Dench 1 J 2UJ 2UJ 2UJ 1 UJ R 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ R 1UJ 1 UJ R 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 2UJ R 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 6JN 731-08 Smith 25U 25U 25U 25U 12 UJ 25 UJ 12 UJ 12 UJ 12 U 58 12 U 12 UJ 25 UJ 12 U 12 U 25 UJ 12 U 12 U 12 U 20 12 U 12 U 12 U R 12 UJ 25 UJ 25 UJ 330 J 12 UJ 12 U 12 U 12 U 12 U 12 U 88 JN 731-09 Steele 17 UJ 17 UJ 17 UJ 17 UJ 140 UJ R 8UJ 8UJ 8U 120 8UJ 8UJ R 8UJ 8U 17 UJ 8U 8U 8UJ 48 8U 8U 8U 8UJ 8UJ 17 UJ R 130J 8UJ 8 U 8U 8U 8UJ 8UJ 42 JN 731-10 9/25 Trip Blank 2U 2 U 2U 2 U 34J 42 J 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ R 1 UJ 1 UJ R 1 U 1 UJ 1 U 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 2UJ R 1 UJ 1 UJ 1 J 1 UJ 1 U 1UJ 7 3JN 7JN UN 731-11 Hartman II 2UJ 2U 2U 2UJ 1 UJ R 1 UJ 1 UJ 1 UJ 5J 1 UJ 1UJ R 1 UJ 1 UJ 2UJ 1 U 1 UJ 1 UJ 1 J 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 2UJ R 7J 1 UJ 1 UJ 1 UJ 1 U 1U 1 U 3JN Page2of 13 731-12 Hartman III 2UJ 2UJ 2UJ 2UJ 3UJ R 1UJ 1UJ 1U 2 1 UJ 1UJ R 1UJ 1 U 2UJ 1 U 1 U 1 UJ 1 U 1 U 1 U 1 U 1 UJ 1UJ 2UJ R 1 J 1 UJ 1 U 1 U 1 U 1 UJ 1 UJ 4JN All concentrations are reported in micrograms per liter (ug/L). J - Value is estimated. U - Compound is not detected. R - Value is rejected. N Compound is a tentatively identified compound. GERAGHTY & MILLER. INC. Page3of 13 Table 2. Tutu Residential Wells Sampling Results, September 1990, Sample Delivery Group 900731 Sample Identification: 'atile Organic Compounds (VOCs) "~ Chloromethane Bromomethane Vinyl Chloride Chloroethane Methylene Chloride Acetone Carbon Disulfide 1 , 1 -Dichloroethcne 1 , 1 -Dichloroethane 1,2-Dichloroethene (total) Chloroform 1 ,2-DicKloroethane 2-Butanone 1,1,1 -Trichloroethane Carbon Tetrachloride Vinyl Acetate Bromodichloromethane 1 ,2-Dichloropropane cis- 1 ,3-Dichloropropene •hloroethene tJibromochloromethanc 1 , 1 ,2-Trichloroethane Benzene trans-1 ,3-Dichloropropene Bromoform 4-Methyl-2-Pentanone 2-Hexanone Tetrachloroethene 1 , 1 ,2,2-Tetrachloroethane Toluene Chlorobenzene Ethylbenzene Styrene Total Xylenes Tentatively Identified VOCs Ethane, 1 , 1 ,2-Trichloro- 1 ,2,2-trifluoro Unknown Propane, 2-Methoxy-2-methyl 731-13 Four Winds II 5UJ 5UJ 5UJ 5UJ 14 UJ R 2UJ 2UJ 2UJ 75 J 2UJ 2UJ R 2UJ 2UJ 5UJ 2UJ 2UJ 2UJ 6J 2UJ 2UJ 2UJ 2UJ 2UJ 5UJ R 25 J 2UJ 2UJ 2UJ 2UJ 2UJ 2UJ 15 JN 731-14 Tutu (Four Winds II Replicate) 5UJ 5UJ 5UJ 5UJ 10 UJ R 2UJ 2UJ 2UJ 61J 2UJ 2UJ R 2UJ 2UJ 5UJ 2UJ 2UJ 2UJ 4J 2UJ 2UJ 2 UJ 2UJ 2UJ 5UJ R 18 J 2UJ 2UJ 2UJ 2UJ 2UJ 2UJ 7.5JN 731-15 Harvey 100 U 100 U 100 UJ 100 U 150 UJ R 50 UJ 50 UJ SOU 50 UJ SOU 50 UJ R SOU sou 100 UJ 50 UJ sou 50 UJ SOU SOU sou sou sou 50 UJ 100 UJ R 890 J 50 UJ SOU SOU SOU SOU 50 UJ 731-16 Leonard 2UJ 2UJ 2UJ 2UJ 2UJ R 1 UJ 1 UJ 1 UJ 1UJ 1 UJ 1 UJ R 1 UJ 1 UJ 2UJ 1 UJ 1 UJ 1 UJ 1 UJ 1UJ 1 UJ 1 UJ 1 UJ 1 UJ 2UJ R 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 731-17 VIHA III 2UJ 2UJ 2UJ 2UJ 2UJ R 1UJ 1UJ 1U 1 U 3 J 1 UJ R 1 UJ 1 U 2UJ 1 U 1 U 1 UJ 1 U I U 1 U 1 U 1 UJ 1 UJ 2UJ R 1 UJ 1UJ 1 U 1 U I U 1 UJ 1 UJ UN 731-18 9/26 Trip Blank 2UJ 2UJ 2UJ 2UJ 24J 4J 1UJ 1UJ 1U 1 U 1 UJ 1 UJ R 1 UJ 1 U 2UJ 1 U 1 U 1 UJ 1 U 1 U 1 U 1 U 1 UJ 1 UJ 1 UJ R 1 UJ I UJ 1 U I U 1 U 1 UJ 1 UJ 7JN All concentrations are reported in micrograms per liter (ug/L). J - Value is estimated. U - Compound is not detected. r Value is rejected. N— compound is a tentatively identified compound. 'U T GERAGHTY & MILLER, INC. Table 2. Tutu Residential Wells Sampling Results, September 1990, Sample Delivery Group 900731 Sample Identification: Volatile Organic Compounds (VOCs) ioromethane Bromomethane Vinyl Chloride Chloroethane Methylene Chloride Acetone Carbon Disulfide 1 , 1 -Dichloroethene 1 , 1 -Dichloroethane 1,2-Dichloroethcne (total) Chloroform 1 ,2-Dkhloroethane 2-Butanone 1,1,1 -Trichloroethane Carbon Tetrachloride Vinyl Acetate Bromodichloromethane 1 ,2-Dichloropropane cis- 1 ,3-Dichloropropene Trichloroethene Dibromochloromethane 1 , 1 ,2-Trichloroethane "•wzene s _ j»-l ,3-Dichloropropene Bromoform 4-Methyl-2-Pentanone 2-Hexanone Tetrachloroethene 1 , 1 ,2,2-Tetrachloroethane Toluene Chlorobenzene Ethylbenzene Styrene Total Xylenes Tentatively Identified VOCs Ethane, 1 , 1 ,2-Trichloro- 1 ,2,2-trifluoro Unknown Propane, 2-Methoxy-2-methyl All concentrations are reported in micrograms J - Value is estimated. U - Compound is not detected. R - Value is rejected. 731-19 Eglinll 10 UJ 10 UJ 10 UJ 10 UJ 5UJ R 5UJ 5UJ 5UJ 120 J 5UJ 5UJ R 5UJ 5UJ 10 UJ 5UJ 5UJ 5UJ 22 J 5UJ 5UJ 5UJ 5UJ 5UJ 10 UJ R 71 J 5UJ 5UJ 5UJ 5UJ 5UJ 5UJ 220 JN per liter (ug/L). 731-20 Eglinin 10 UJ 10 UJ 10 UJ 10 UJ 10 UJ 22 J 5UJ 5UJ 5 U 52 J 5U 5UJ R 5U 5U 10 UJ 5UJ 5UJ 5UJ 14 5UJ 5UJ 5UJ 5UJ 5UJ 10 UJ R 44J 5UJ 5UJ 5UJ 5UJ 5UJ 5UJ 5JN N - Compound is a tentatively identified compound. GERAGHTY & MILLER. INC. (3 Table 2. Tutu Residential Wells Sampling Results, September 1990, Sample Delivery Group 900731 Sample Identification: Semivolatile Organic ipounds (SVOCs) Phenol bis(2-Chloroethyl)Ether 2-Chlorophenol 1 ,3-Dichlorobenzene 1 ,4-Dichlorobenzene Benzyl Alcohol 1 ,2-Dichlorobenzene 2-Methylphenol N-Nitroso-Di-n-Propylamine Hexachloroethane Nitrobenzene Isopoorone 2-Nitrophenol 2 ,4-Dimethy Iphenol Benzoic Acid bis(2-Chloroethoxy)Methane 2,4-Dichlorophenol 1 ,2,4-Trichlorobenzene Naphthalene 4-Chloroaniline Hexachlorobutadiene f "hloro-3-Methylphenol K _ ..ethylnaphthalene Hexachlorocyclopentadiene 2 ,4 ,6-Trichlorophenol 2,4,5-Trichlorophenol 2-Chloronaphthalene 2-Nitroaniline Dimethyl Phthalate Acenaphthylene 2, 6-Dinitrotol uene 3-Nitroaniline Acenaphthene 2,4-Dinitrophenol 4-Nitrophenol Dibenzofuran 2,4-Dinitrotoluene Diethylphthalate 4-Chlorophenyl-phenylether Fluorene 4-Nitroaniline 4,6-Dinitro-2-Methylphenol N-Nitrosodiphenylamine 4-Bromophenyl-phenylether H""«chlorobenzene 731-01 Devcon I 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 10 U 731-02 Devcon III 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 10 U 731-03 Rodriguez (P) 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 10 U 731-04 Rodriguez (PD) 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 10 U 731-06 Dede 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 10 U 731-07 Deficit 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 10 U Alrtoncentrations are reported in micrograms per liter (ug/L). U - Compound is not detected. 94 GERAGHTY & MILLER. INC. Page6of 13 Table 2. Tutu Residential Wells Sampling Results, September 1990. Sample Delivery Group 900731 Sample Identification: Semivolatile Organic npounds (SVOCs) Pentachlorophenol Phenanthrene Anthracene Di-n-Butylphthalate Fluoranthene Pyreoe Butylbenzylphthalate 3,3-Dichlorobenzidine Benzo(a)Anthracene Chrytene bis(2-Ethylhexyl)Phthalate Di-n-Octyl Phthalate Benzo(b)Fluorantheiie Benzo(k)Fluoranthene Benzo(a)Pyrene Indeno( 1 ,2,3-cd)Pyrene Dibenz(a,h) Anthracene Benzo(g,h,i)Perylene Tentatively Identified SVOCs No tentatively identified compounds found. 731-01 Devcon I SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 731-02 Devcon HI SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 731-03 Rodriguez (P) SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 731-04 Rodriguez (PD) SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 731-06 Dede SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 731-07 Dench SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U concentrations are reported in raicrograras per liter (ug/L). ^T - Compound is not detected. TUi 002 1949 GERAGHTY & MILLER, INC. Table 2. Tutu Residential Wells Sampling Results, September 1990, Sample Delivery Group 900731 Sample Identification: Semivolatile Organic ipounds (SVOCs) Phenol bis(2-Chloroethyl)Ether 2-Chlorophenol 1 ,3-Dichlorobenzene 1 ,4-Dichlorobenzcne Benzyl Alcohol 1 ,2-Dichlorobenzene 2-Methylphenol N-Nitroso-Di-n-Propylamine Hexachloroethane Nitrobenzene Isophorone 2-Nitrophenol 2,4-Dimethylphenol Benzoic Acid bis(2-Chloroethoxy)Methane 2 ,4-Dichlorophenol 1 ,2,4-Trichlorobenzene Naphthalene 4-Chloroaniline Hexachlorobutadiene * "hloro-3-Methylphenol s _ ^ethylnaphthalene Hexachlorocyclopentadiene 2,4,6-Trichlorophenol 2,4,5-Trichlorophenol 2-Chloronaphthalene 2-Nitroaniline Dimethyl Phthalate Acenaphthylene 2 ,6-Dinitrotoluene 3-Nitroaniline Acenaphthene 2 ,4-Dinitrophenol 4-Nitrophenol Dibenzofuran 2,4-Dinitrotoluene Diethylphthalate 4-Chlorophenyl -pheny 1 ether Fluorene 4-Nhroaniline 4,6-Dinitro-2-Methylphcnol N -Nitrosodiphenylamine 4-Bromophenyl-phenylether H'xachlorobenzene 731-08 Smith 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 10 U 731-09 Steele 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 UJ 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U 50 UJ sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 10 U 731-11 Hartman II 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 10 U 731-12 Hartman III 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 10 U Page7of 13 731-13 Four Winds II 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 10 U Arrtoncentrations are reported in micrograms per liter (ug/L). J - Value is estimated. U - Compound is not detected. 1950 GERAGHTY & MILLER, INC. Table 2. Tutu Residential Wells Sampling Results, September 1990, Sample Delivery Group 900731 Sample Identification: Semivolatile Organic (pounds (SVOCs) Pentachlorophenol Phenanthrene Anthracene Di-n-Butylphthalate Fluoranthene Pyreoe Butylbenzylphthalate 3,3-Dichlorobenzidine Benzo(a)Anthracene Chrysene bis(2-Ethylhexyl)Phthalate Di-n-Octyl Phthalate Bcnzo(b)Fluoranthene Benzo(k)Fluoranthene Benzo(a)Pyrene Indeno( 1 ,2,3-cd)Pyrene Dibenz(a.h) Anthracene Benzo(g , h , i)Perylene Tentatively Identified SVOCs No tentatively identified compounds found. 731-08 Smith SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 731-09 Steele SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 731-11 Hartman II SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 731-12 Hartman III SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 731-13 Four Winds II SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U All concentrations are reported in micrograms per liter (ug/L). /alue is estimated. U - Compound is not detected. GERAGHTY & MILLER, INC. Table 2. Tutu Residential Wells Sampling Results. September 1990, Sample Delivery Group 900731 Sample Identification: Semivolatile Organic npounds (SVOCs) Phenol bis(2-Chloroethyl)Ether 2-Chlorophenol 1 ,3-Dichlorobenzene 1 ,4-Dichlorobenzene Benzyl Alcohol 1 ,2-Dichlorobenzene 2-Mcthylphenol N-Nitroso-Di-n-Propylamine Hexachloroethane Nitrobenzene Isophorone 2-Nitrophenol 2,4-Dimcthylphenol Benzole Acid bis(2-Chloroethoxy)Methane 2,4-DichloTophenol 1 ,2,4-Trichlorobenzene Naphthalene 4-Chloroaniline T" 'xachlorobutadiene , _ ^hloro-3-Methylphenol 2-Methylnaphthalene Hexachlorocyclopentadiene 2,4,6-Trichlorophenol 2,4,5-Trichlorophenol 2-Chloronaphthalene 2-Nitroaniline Dimethyl Phthalate Acenaphthylene 2,6-Dinitrotoluene 3-Nitroaniline Acenaphthene 2,4-Dinitrophenol 4-Nitrophenol Dibenzofuran 2,4-Dinitrotoluene Diethylphthalate 4-Chlorophenyl-phenylether Fluorene 4-Nitroaniline 4,6-Dinitro-2-Methylphenol N-Nitrosodiphenylamine <* ''romophenyl-phenylether 731-14 Tutu (Four Winds II Replicate) 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 731-15 Harvey 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 731-16 Leonard 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 731-17 VIHA1II 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 731-19 Eglinll 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U Page*) of 13 731-20 Eglinlll 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U Xtf concentrations are reported in micrograms per liter (ug/L). U - Compound is not detected. GERAGHTY & MILLER, INC. Pagetfof/3 Table 2. Tutu Residential Wells Sampling Results, September 1990, Sample Delivery Group 900731 Sample Identification: Semivdatilc Organic npounds (SVOCs) ^ - Hexachlorobenzene Pentachlorophenol Phenan throne Anthracene Di-n-Butylphthalate Fluoranthene Pyrene Butylbenzylphthalate 3 ,3-Dichlorobenzidine Benzo(a)Anthracene Chrysene bis(2-Ethylhexyl)Phthalate Di-n-Octyl Phthalate Benzo(b)Fluoranthene Benzo(k)Fluoranthene Benzo(a)Pyrene Indeno(l,2(3-cd)Pyrene Dibenz(a,h)Anthraccne Benzo(g,h,i)Perylene ^-ntatively Identified SVOCs ^__ tentatively identified compounds found. 731-14 Tutu (Four Winds II Replicate) 10 U SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 731-15 Harvey 10 U SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 731-16 Leonard 10 U SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 731-17 VIHAI1I 10 U SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 731-19 Eglin II 10 U SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 731-20 Eglin in 10 U SOU 10 U 10 U 10 U 10 U 10 U 10 U 20U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U All concentrations are reported in micrograms per liter (ug/L). U - Compound is not detected. GERAGHTY & MILLER, INC. rUT 1953 Table 2. Tutu Residential Wells Sampling Sample Identification: Pesticide/PCBs ^ja-BHC beta-BHC delU-BHC garama-BHC Heptachlor Aldrin Heptachlor epoxide Endosulfan I Dieldrin 4,4-DDE Endrin Endosulfan II 4,4-DDD Endosulfan sulfate 4,4-DDT Methoxychlor Endrin ketone alpha -Chlordane gamma-Chlordane Toxaphene Aroclor-1016 Aroclor-1221 1 -iclor-1232 ^jelor-1242 Aroclor-1248 Aroclor-1254 Aroclor-1260 Results, September 731-01 Devcon I 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.10U 0.10U 0.10U 0.10U 0.10U 0.10U 0.10U 0.50 U 0.10U 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U 1990, Sample 731-02 Devcon III 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.10U 0.10U 0.10U 0.10U 0.10U 0.10U 0.10U 0.50 U 0.10U 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U Delivery Group 900731 731-03 Rodriguez (P) 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.10U 0.10U 0.10U 0.10U 0.10U 0.10U 0.10U 0.50 U 0.10U 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U 731-04 Rodriguez (PD) 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.10U 0.10U 0.10U 0.10U 0.10U 0.10U 0.10U 0.50 U 0.10U 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U 731-06 Dede 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.10U 0.10U 0.10U 0.10U 0.10U 0.10U 0.10U 0.50 U 0.10U 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U Page/lof 13 731-07 Dench 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.10U 0.10U 0.10U 0.10U 0.10U 0.10U 0.10U 0.50 U O.IOU 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U All concentrations are reported in micrograms per liter (ug/L). U - Compound is not detected. 1954 GERAGHTY & MILLER. INC. Table 2. Tutu Residential Wells Sampling Results, September 1990, Sample Delivery Group 900731 Sample Identification: Pesticide/PCBs ^na-BHC beta-BHC ddta-BHC gamroa-BHC Heptachlor Aldrin Heptachlor epoxide Endosulfan I Dieldrin 4,4-DDE Endrin Endosulfan II 4,4-DDD Endosulfan sulfate 4,4-DDT Methoxychlor Endrin ketone alpha -Chlordane gamma -Chlordane Toxaphene Aroclor-1016 Aroclor-1221 A'oclor-1232 N_jclor-1242 Aroclor-1248 Aroclor-1254 ArocIor-1260 731-08 Smith 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.10U 0.10U 0.10U 0.10U 0.10U 0.10U O.IOU 0.50 U O.IOU 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U 731-09 Steele 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU 0.50 U O.IOU 0.50 U 0.50U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U 731-11 Hartman II 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU 0.50 U O.IOU 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50U 1.0 U 1.0 U 731-12 Hartman III 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU 0.50 U O.IOU 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U Page(2of 13 731-13 Four Winds II 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU 0.50 U O.IOU 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U All concentrations are reported in micrograms per liter (ug/L). U - Compound is not detected. GERAGHTY & MILLER, INC. 1955 Page/30f)3 Table 2. Tutu Residential Wells Sampling Results, September 1990, Sample Delivery Group 900731 Sample Identification: Pesticide/PCBs ~~-" alpha-BHC beta-BHC delta-BHC garama-BHC Heptachlor Aldrin Heptachlor epoxide Endosulfan I Dicldrin 4,4-DDE Endrin Endosulfan II 4,4-DDD Endosulfan sulfate 4,4-DDT Methoxychlor Endrin ketone alpha -Chlordane gamma-Chlordane Toxaphene :lor-1016 Aroclor-1221 Aroclor-1232 Aroclor-1242 Aroclor-1248 Aroclor-1254 Aroclor-1260 731-14 Tutu (Four Winds II Replicate) 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.10U 0.10U 0.10U 0.10U 0.10U O.IOU 0.10U 0.50 U O.IOU 0.50 U 0.50 U i.O U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U 731-15 Harvey 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU 0.50 U O.IOU 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U 731-16 Leonard 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU 0.50 U O.IOU 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U 731-17 VIHA III 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU 0.50 U O.IOU 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U 731-19 Eglinll 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU 0.50 U O.IOU 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U i.O U 1.0 U 731-20 Eglin ID 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU 0.50 U O.IOU 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U All concentrations are reported in micrograms per liter (ug/L). U - Compound is not detected. GERAGHTY & MILLER, INC. Table 2. Tutu Residential Wells Sampling Results, September 1990, Sample Delivery Group 900731 Sample Identification: Inorganic Analyses Aluminum Antimony Arsenic Barium Beryllium Cadmium Calcium Chromium Cobalt Copper Iron Lead Magnesium Manganese Mercury Nickel Potassium Selenium Silver Sodium Thallium Vanadium Zinc Cyanide 731-01 Devcon I 139 R 3 21 5 3 41600 4 18 4 34 8.2 39500 241 0.2 13 2970 1.6 7 330000 R 32 6 5 BJ U B BJ U UJ U U B J U B B BJ UJ B BJ UJ 731-02 Devcon III 411 R 3 15 4 3 43800 4 59 53 40 11.8 41000 91 0.2 41 2050 1.4 7 384000 R 20 6 5 J U B BJ U UJ J B J U B BJ UJ B BJ UJ 731-03 Rodriguez (P) 58 R 3 8 3 3 40000 14 34 22 50 2 38700 122 0.2 22 1610 1 7 281000 R 19 17 21 BJ U B BJ U J BJ B B BJ U B B UJ UJ B BJ J 731-04 Rodriguez (PD) 431 R 3 3 3 3 47400 40 39 29 45 12.1 41400 129 0.2 39 1730 1 7 298000 R 8 16 5 J U U BJ U J BJ B J U B B UJ UJ B BJ UJ 731-06 Dede 136 R 3 8 3 5 23500 16 60 32 43 3.7 25600 201 0.2 11 2000 1 7 324000 R 21 12 5 BJ U B BJ J J B J U U B UJ UJ B BJ U 731-07 Dench 278 R 3 19 4 3 24200 22 44 52 163 7.8 25000 545 0.2 73 1690 1 7 328000 R 28 41 6.8 J U B BJ B J BJ J U B UJ UJ B J B 731-08 Smith 234 R 3 15 3 3 50200 14 18 13 158 10.9 45500 41 0.2 57 1540 R 7 410000 R 5 179 5 J U B BJ U J U B J U B UJ U J U 731-09 Steelc 492 R 3 27 3 4 44000 9 55 21 26 13.2 40500 23 0.2 45 1180 1.4 7 313000 R 27 12 6.3 J U B BJ B BJ J B B J U B BJ UJ B BJ B All concentrations are reported in micrograms per liter (ug/L). J - Value u estimated. U - Analyte is not detected. R - Value i» rejected. B - Value is between instrument detection limit and contract required detection limit. GERAGHTY & MILLER. INC. Table 2. Tutu Residential Wells Sampling Results, September 1990, Sample Delivery Group 900731 Sample Identification: Inorganic Analyses Aluminum Antimony Arsenic Barium Beryllium Cadmium Calcium Chromium Cobalt Copper Iron Lead Magnesium Manganese Mercury Nickel Potassium Selenium Silver Sodium Thallium Vanadium Zinc Cyanide 731-11 Hartman 2 269 R 3 12 3 8 38100 11 30 34 23 10.4 33400 2 0.2 95 1040 1.6 7 285000 R 52 9 5 J U B BJ J BJ B J U U B BJ UJ BJ U 731-12 Hartman 3 278 R 3 15 4 3 41100 11 25 30 31 1.8 28300 3 0.2 52 1690 1 7 217000 R 124 13 5 J U B BJ U J BJ B BJ B U B UJ UJ BJ U 731-13 Four Winds II 162 R 3 15 3 5 46100 32 29 37 55 8 34000 28 0.2 36 2190 1.2 7 215000 R 75 85 8.5 BJ U B BJ J BJ B J U B B BJ UJ J B 731-14 731-15 Tutu Harvey (Four Winds II Replicate) 304 J R 3 U 11 B 4 BJ 6 54300 14 J 43 BJ 5 B 57 B 8.7 J 38800 31 0.2 U 44 2060 B 1 UJ 7 UJ 249000 R 83 88 J 5 U 1280 J R 3 U 35 B 3 BJ 3 U 53700 18 J 38 BJ 59 3360 32.6 J 46200 191 0.2 U 58 2000 B 1.2 BJ 11 J 233000 R 59 248 J 7.4 B 731-16 Leonard 93 R 3 11 3 3 38300 15 37 31 37 1.8 24400 2 0.2 11 1210 1.4 17 318000 R 135 7 6.3 BJ U B BJ U J BJ BJ BJ U U U B BJ J BJ B 731-17 VIHA HI 182 BJ R 3 U 14 B 3 BJ 3 U 43300 5 BJ 18 U 29 149 3.7 J 28000 11 B 0.2 U 43 1030 B 1.5 BJ 7 UJ 162000 R 33 B 17 BJ 8 BJ All concentrations are reported in micrograms per liter (ug/L). J - Value is estimated. U - Analytc is not detected. R - Value U rejected. B - Value i* between instrument detection limit and contract required detection limit. GERAGHTY & MILLER, INC. Table 2. Tutu Residential Wells Sampling Results, September 1990, Sample Delivery Group 900731 Sample Identification: Inorganic Analyses Aluminum Antimony Arsenic Barium Beryllium Cadmium Calcium Chromium Cobalt Copper Iron Lead Magnesium Manganese Mercury Nickel Potassium Selenium Silver Sodium Thallium Vanadium Zinc Cyanide 731-19 Eglin 11 69 BJ R 3 U 23 B 3 BJ 11 47900 17 J 32 BJ 36 86 B 2.1 BJ 35400 8 B 0.2 U 67 1620 B 1.2 BJ 7 UJ 247000 R 47 B 75 J 6.8 B 731-20 Eglin HI 156 BJ R 3 U 57 B 4 BJ 3 U 81400 10 J 30 BJ 9 B 56 B 1 UJ 54600 53 0.2 U 24 B 2250 'B 1.2 BJ 18 J 398000 R 9 B 49 J 7.4 B All concentrations are reported in micrograms per liter (ug/L). J - Value it estimated. U - Analyte is not detected. R - Value is rejected. B - Value U between instrument detection limit and contract required detection limit. 6 '-•', /-, T •• *• .•• f >/ * GERAGHTY & MILLER. INC. DATA VALIDATION SUMMARY REPORT for the TUTU WELLS SITE September 1990 Quarterly Sampling USEPA REGION II Standard Operating Procedures HW-2 and HW-6 for the Contract Laboratory Program Organic and Inorganic Data Review Sample Delivery Group 900770 (VIHA I) January 1991 Prepared for Tutu Environmental Investigation Committee Geraghty & Miller, Inc. International Group 290 Vincent Avenue Hackensack, New Jersey 07601 GERAGHTY & MILLER. INC. 1 1 1 1 1 • . -r • 1 SOP NO. Sf-S Havision f 7 1 1 CLP CRONICS DMA REVIEW "I 1 1 AND EREUMXNMQf KLVltW Laon TflrarGs, Bwironaentad Scientist Ibxic and Hazardous Kasta Data: Data BavaO[^jMJ 01 and MLzardoua- wasta ; ^ ^ ____ Gerard F. McKenna, Monitoring Managemtnt Btancb STANDARD OPERATING PRDCZDORE Page: 1 of 36 Date: March 1990 Revision 7 BTCOCUCTXCN TO DATA VAUDR1TON .0 1.1 This procedure is applicable to organic data obtained tram contractor laboratorie working for the Contract Laboratory Piuyiam (CXP). 1.2 The data validation is based upon analytical and Quality assurance requirements specified in the Statement of Work (SOW). vUl complete the following tasks as assigned by the Data Review Coordinator: 2.1 Data Assessment - The reviewer gust answer every question on the checklist. All response shall be in ink. 2.2 Data Assessment Narrative (Attachment 1) - Data reviewer is required to use these forms and most natch the action in the narrative with the action taken on the Form I (s). 2.3 Rejection Surrary Form (Attachment 2) - Fill in the total number of analytes measured by different analyses and the number of analytes rejected or flagged as estimated due to corresponding quality control criteria. Place an "X" in the boxes where analyses were not performed or criteria do not apply. 2.4 Organic Regional Data Assessment - Data reviewer is also required to fill out Organic Regional Data Assessment Fora (Attachment 3). 2.5 Telephone Record Log - The data reviewer should enter the bare facts of inquiry before initiating any authorized telephone conversation with a CLP laboratory. After the case review has been completed, mail the white copy of the Telephone Record Log to the laboratory and the pink copy to SMO. File the yellow copy in the Telephone Record Log folder and attach a photocopy of the Telephone Record Log to the completed _Data Assessment Narrative. 2.6 Forwarded Paoerwork - Upon completion of the review, the following are to be forwarded to the Regional Sample Control Center (RSCC) located in the Surveillance and Monitoring Branch: a. data package b. completed assessment checklist c. SMO Contract Compliance Screening (CCS) Forward four (4) copies of the completed Data Assessment Narrative along with four (4) copies of the Organic Data Assessment Form: one each for the appropriate Regional DPO, the Sample Management Office (SMO), and to the last two addresses of the Data Reviewers Mailing List. 2.7 Filed Paperwork - Upon completion of the review, the following are to be filed within the Monitoring and Management Branch (MMB) files: a. Telephone record Log (copy) b. Record of Comunication (original) c. Rejection Surmary Form SEACARD OPERATING PROCEDURE Page: 2 cf 36 Date: March 1990 Revision 7 i.O Reiection of te^a - All values determined to be unacceptable on the Organic Analysis Data Sheet (Form I) oust be flagged with an "R". As soon as review criteria causes data to be rejected, that data can be eliminated from any further review or consideration. -.0 Acceptance Cri-t?r1fl * In order that the reviews be consistent among reviewers, this Standard Operating Procedure (SOP) should be used. Additional guidance can be found in the Functional Guidelines. ..0 SMD Contract Canclianoe Screening fCCSI - This is intended to *ta the reviewer in locating any problens, both corrected and utijua.ieu.tad. However, the validation should be carried out even if OS is not present. Resubmittals received from the laboratory in response to CCS oust be used by the reviewer. TUT •I 9,c STANDARD OPERATING PROCEDURE Page: 3 of 36 Date: March 1990 Revision 7 •AOOGE COMPLETENESS AND DELIVERABLES CASE NUMBER; # °f'00 770 IAB: (Let MIC. "Tv-ru li/eu-s, , • 0 Data OTcleter*31^ and Deliverable ypg jo N/A 1.1 Have any missing deliverables been received and added to the data package. ACITCN: 0*11 lab for explanation / resufcmittal of any missing deliverables. If lab cannot provide them, note the effect on review of the package under the "Contract Problens/Non-oecpliance" section of reviewer narrative. 1.2 Was SMD OCS checklist included with package? .0 ^ 2.1 Is the Narrative or Orver Letter present? - 2.2 Are Case Number and/or SAS number contained in the Narrative or Cover Letter? .0 Data Validation Checklist The following checklist is divided into three parts. Part A is filled out if the data package contains any VQA analyses, Part B for any ENA analyses and Part C for Pesticide/PCBs. Does this package contain: . IA data? __ BNA data? J^_ Pesticide/PCB data? JL. ACITCN: Conplete corresponding parts of checklist. STANDARD OPERATIC PROCSCTZ Page: 4 of 35 Date: March 1990 Revision 7 Y E S N O N/A" PART A: " . o Tidffic P jyii'. l'fT? yr^ TftL'Ji ^jrt^rv K*7**___ 1.1 Are the Traffic Report Foras present for all samples? ACTION: If no, contact lab for replacement of missing or illegible copies. 1.2 Do the Traffic Reports or lab Narrative indicate any problems with sample receipt, condition of samples, analytical problems or special notations affecting the quality of the data? \/ [__] __ ACTION: Use professional judgement to evaluate the effect on the quality of the data. ACTION: If any sample analyzed as a soil contains than 50* water, all data should be flagged as estimated (J). ACTION: If both VGA vials for a sarple have air bubbles, flag all positive results "J" and all nan-detects "R". 2.1 Have any VGA holding times, determined fron date of collection to date of analysis, been If urrreserved, aqueous aroratic volatiles must be analyzed within 7 days of collection and non-arcnatic volatiles must be analyzed within 14 days. If preserved with hydrochloric acid and stared at 4°C, then both aromatic and non-aromatic volatiles must be analyzed within 14 days. If uncertain about preservation, contact the sacpler to determine whether the saroles were preserved. A ten-day holding time for soil samples is racaraended. - IP1??!* n1T ff r>^i'rU-no' Time Violations (See Traffic Report) Sample Date Date lab Date _ Sacple Matrix Preserved ? Sampled Received Analyzed 'rrp8/*»f h _ _ «4 a^ _. _ **-• /I _ I • I I. II . ^ f , I ^ > _ . ^ 1 — ~. I JK. >k to ACTION: If holding trnes are exceeded, flag' all positive results as estimated ("J"} and saqple quantitation limits as estimated ("UJ"), and document in the narrative that holding were exceeded. OFDVC3JC PROCEDURE Page: 5 of 36 Date: March 1990 Revision 7 s o N/A~ If analyses were done acre than 14 days beyond holding time, either on the first analysis or upon reanalysis, the reviewer must use professional judgement to determine the reliability of the data and the effects of ~v4jfigr»»T storage on the sample results. The reviewer may determine that ncn data are unusable ("R") . "• • 0 ff 3.1 Are the VQA Surrogate Recovery Suoaaries (Fora H) present for each of the following matrices; a. low Water [ y } _ ^ __ b. Med Water [ __ ] __ y c. la* Soil [ __ ] __ d. Med Soil [ __ ] __ 3.2 Are all the VQA sazples listed on the appropriate Surrogate Recovery Sucsraries for each of the following matrices: a. low Water r \/' 1 __ __ b. Med Water [ __ ] __ c. low- Soil [ __ ] __ d. Med Soil [ __ ] __ \/ ACIICN: CBll lab for explanation / resubmittals. If missing deliverables are unavailable, effect on data under "Canclusicns" section of reviewer narrative. 3.3 Were outliers carted correctly with an asterisk? ACTION: Circle all outliers in red. 3.4 Was one or acre VDA surrogate recovery outside of contract / \/ specifications for any spmplf or method blank? If yes, were samples reanalyzed? [ __ ] ^_ Were method blanks reanalyzed? [ __ ] ACTICN: If surrogate recoveries are > 10% but all do not meet SOW specifications: 1. Flag all positive results as estimated ("J") . 2. Flag all non-dctects as estimated detection limits ("11:"). STANDARD OPERATED PRQ2TLKE Page: 6 of 33 Data: March 1990 Revision 7 NO If any surrogate has a recovery of <10* : 1. Flag an positive results as estimated ("J"). 2. Flag an non-detects as unusable ("R"). Professional judgement should be used to qualify data that have method blank surrogate recoveries out of specification in both original and analyses. Check the internal standard 3.5 Are there any tidiaeription/calculation errors between raw / data and Form H? __ [ \/\ __ ACTICN: If large errors exist, call lab for explanation / resubmittal, make any necessary corrections and note errors under "Conclusions". 4.1 Is the Matrix Spike Duplicate/Recovery Form (Form HI) present? 4.2 Were matrix spikes analyzed at the required frequency for each of the following matrices: v i out of 5 ACTION: If MS and MSD both have less than 10* covery for an anaiyte, negative results for that analyte should be rejected, and positive results should be flagged' "J*. Ins above applies only to the sample used for the MS/MSD analysis. Use professional judgement in applying this criterion to other samples in the package- a. Low Water b. Med Water __ __ c. Low Soil [ __ ] __ * d. Med Soil r •• * ACITCN: If any matrix spDoa data are missing, take the action specified in 3.2 above. 4.3 How many VGA spike recoveries are outside QC limts? v»teT Soils Q out of 10 M/t» out of 10 4.4 How many RPD's for matrix spike and matrix spike duplicate recoveries are outside QC limits? OPERATIC FROCHURE Page: 7 of 36 Date: March 1990 Revision 7 NO N/ f.O Blanks fForr?. nn 5.1 Is the Method Blank Stannary (Form IV) present? 5.2 Frequency of Analysis: for the analysis of VGA TCL ccqpounds, has a reagent/method blank been analyzed for each set of samples or every 20 samples of similar matrix (low water, med water, low soil, medium soil), whichever is mare frequent? r ^ 1 5.3 Has a TCA instrument blank been analyzed at *«•»!. * once every twelve hours for each OC/MS system used? CVl __ __ ACTION: If any method blank data are missing, ^»T1 lab for explanation / resubmittal. If not available, reject all associated positive data ("R"). 5.4 Chraratograpny: review the blank raw data - chronatc; (RIGS) , quant reports or data system printouts and spectra. Is the chromatographic performance (baseline stability) for each instrument acceptable for VQ&s? ACITCN: Use professional judgement to determine the effect on the data. '.0 Corr^^TTLLrja t i on NOTE: "Water blanks" and "distilled water blanks" are validated like any other sample and are not used to qualify data. Do not confuse them with the other QC blanks d.i.qr»s.sflri below. 6.1 Do any method/ instrumenVreagent blanks have positive results (TCL and/or TIC) for VQAs? When applied as described below, the contaminant concentration in these blanks are multiplied by the sample Dilution / Factor. JL_ [ __ ] 6.2 Do any field/trip/rinse blanks have positive VGA results (TCL and/or Tiq ? ACTION: Prepare a list of the samples associated with each of the contaminated blanks. (Attach a separate sheet.) NOTE: Only field/rinse blanks taken the same day as the sanples are used to qualify data. Trip blanks are used to qualify only those samples with which they wera shipped. Blanks may not be qualified because of contamination in another " blank. Blanks may be qualified for surrogate, spectral, tuning or calibration QC problc SSNDARD OPS^ATD^G «g» ••- ITT Page: 8 of 35 Date: March 1990 Revision 7 ~ ~ ~ " ~ ~ 5 5 5 5 ACTICN: Follow the directions in the table below to qualify TCL results due to contamination. Use the largest value from *"n the associated blanks. !Sample ccnc > CRQL [Sample ccnc < CRQL fc!Sanple ccnc > CRQL but < lOx blank is < lOx blank value value £ >10x blank value i Methylene chloride Flag saqple result!Reject sample result{No qualifies^im Acetone with a 'U1; cross and MUMLt CRQL; is Toluene out 'B1 flag cross out •B1 flag _2-butanone_{ {Sanple ccnc > CRQL! Sample ccnc < CRQL t!Sample ccnc > CRQL but < 5x blank is < 5x blank value value 4 > 5 blank value Other 1^*5 sa^P1* result Reject sample result!No qualification Contaminants with a 'U1; cross and lepart CRQL; u cut 'B' flag cross out 'B* flag i———.________i_____________i________.—.______.t ACTION: For TIC cenpounds, if the concentration in the sanple is less than five times the concentration in the most con- taminated associated blank, flag the sample data "R" (unusable). 6.3 Are there field/rinse/equipment blanks associated with every / sample? ^ [__] __ V AdTCN: For lew level sarples, note in data pJiSffnffTTgnt. that there is no associated f ield/rinse/equicnent blank, deception; sarples taken fran a drinking water tap do not have associated field blanks. 0 GC/MS? Tw^"*7 y^ Msss_^alibration fForrn v^ 7.1 Are the GC/KS Tuning and Mass calibration Forms (Fora V) present for Brcmofluorobenzene (BFB)? 7.2 Are the enhanced bar graph spectrum and mass/charge (m/z) listing for the BF3 provided for each twelve hour shift? 7.3 Has a tuning performance cccpound been analyzed for every / twelve hours of sample analysis per instrument? r V 1 __ __ ACTION: If any tuning data are missing, take articn specified in 3.2 above. ACTICN: List date, time, instrument ID, and sample analyses for which no asvnintfri GC/KS tuning data are available. 1 UT STANDARD OPERATING Page: 9 of 36 Date: March 1990 Revision 7 NO N/A — ———— ———— jg» 1 1 r^amtj. ——————————————————— •anfif^f, r*JTlBC*K3 ACTION: If lab cannot provide aissing data, reject ("R") all data generated outside an acceptable twelve hour calibration interval. 7.4 Have the ion abundance criteria been net for each if is! pinianit used? ACTION: List all data which do not neet ion abundance criteria (attach a separate sheet). ACTION: If tuning calibration is in error, flag all associated sacple data as unusable ("R"). However, if expanded ion criteria are net (See 1988 Functional Guidelines), the data reviewer nay acoeut data with appropriate qualifiers. 7.5 Are there any transcription / calculation errors between ness lists and Form Vs? (Check at least two values but if errors are found, check nore.) 7.6 Have the appropriate nusber of significant figures (two) been reported?* (Check at least two values, but if errors are found check nore values.) ACTION: If large errors exist, e»n lab for explanation / resubnittal, make necessary corrections and note errors under "Conclusions". 7.7 Are the bLHt-'—a of the acceptable? calibration pound ACTION: Use professional judgement to determine whether Vry^i?1!*-"* data shaU.fi be accepted, qualified, or rejected. 8.1 Are the Organic Analysis Data Sheets (Fora I VDA) present with required header information on each page, for each of the following: a. Sasples and/or fractions as appropriate b. Matrix spikes and matrix spike duplicates c. Blanks ;l970 v/i SIMJDMO QESWIUC HOCEILKE Page: 10 of 36 Date: Marsh 1990 Revision 7 8.2 Are the vQA RaunurtTUCtud Ton Q<>t^M*i'»jj j»me a the mass li^jeuLia for the identified compounds, and the data system printouts (Quant Reports) included in sanple pvtotfF for each of the following? b. Matrix spikes and matrix spike (Mass spectra not required) c. Blanks * ACTION: If any data are missing, take action a_Cied in 3.2 above. 8.3 Are the a. frrples and/or fractions as appropriate f y/1 __ __ factors shown in the Quant Report? [__] \/ __ 8.4 Is chrccatccraphic performance acceptable with respect to: / Baseline stability r vM __ __ Resolution f x/1 __ __ Peak shape r i/1 __ __ Full-scale graph (attenuation) r \/1 __ __ Other:________________ [__] __ \S ACTION: Use professional judgement to determine the acceptability of the data. 8.5 Are the lab-generated standard mass spectra of the / identified VQA a'Linings present far each sample? f Vj __ __ ACTICN: if any mass spectra are missing, take action specified in 3.2 above. If lab does not generate their own standard spucLta, make note in "Contract Problems/Non-compliance11. f 8.6 Is the RRT of each reported mn.nTrd within 0.06 RRT / units of tte standard RRT in the continuing calibration? f Y1 __ __ 8.7 Are all ions present in the standard mass speu.t-i.um at a relative intensity greater than 10% also prejant in the / sample mass spectrum? F Vj __ __ 8.8 Do sanple and standard relative ion intensities agree within 20%? ACTICN: Use professional judgement to determine acceptability of data. If it is determined that incorrect identifications were made, all such data should be rejected, flagged "IT* (presumptive evidence of the presence of r,, , the ccnpound) or changed to not detected (at TUT °°'-'•'• the calculated detection limit). STANDARD OPERATING PROCEDURE Page: 11 Of 36 Date: March 1990 Revision 7 - " " YES NO N/T j.O Terrfr^jvfllY Id/gitifi**^ f^'"i"jndff 9.1 Are all Tentatively Identified Compound Forms (Form I, Part B) present; and do listed TTCs include scan number or retention time, estimated concentration and "J" V qualifier? r V] __ __ 9.2 Are the mass hpauUd for the tentatively identified compounds and »««^"1»^yl "best match" spectia included in the sample package for each of the following: a. Samples and/or fractions as appropriate r ^^1 __ __ b. Blanks r %/1 __ __ ACTION: If any TIC data are missing, take action specified in 3.2 above. ACTION: Add "J" qualifier if missing and "N" qualifier to all identified TIC compounds on Form I, Part B. 9.3 Are any TCL ccrpounds (from any fraction) listed as TIC compounds (exaqple: 1,2-dimethylbenzene is xyl a VCA TCL—and should not be reported as a ACTION: Flag with "R" any TCL compound listed as a TIC. 9.4 Are all ions present in the reference mass spectrum with a relative intensity greater than 10% also present in the sample ™»« spectrum? r vl __ __ 9.5 Do TTC and "best match" standard relative ion intensities agree within 204? ACTION: Use professional judgement to determine acceptability of TIC identifications. If it is determined that an incorrect identi- fication was made, change identification to "unknown1* or to some less specific identi- fication (example: "C3 substituted benzene") as appropriate. 0.0 O ^iiucund Q.^anti^-^tion and Reooi^ri 10.1 Are there any transcription / calculation errors in Form I results? Check at least two positive values. Verify that the correct infernal standard, quantitation ion, and RRF were used to calculate Fora I result. Were any errors found? * 10.2 Are the CPQLs adjusted to reflect sanple dilutions and, for soils, sanple moisture? STANDARD OTSttTD'C PH X 'Li.I.iHZ Page: 12 of 36 Date: March 1990 Revision 7 YES NO N/A ACTION: If errors are large, call lab for explanation / resubmittal, mate an/ necessary corrections and ACTION: When a sample is analyzed at sore than dilution, the lowest CRQLs are used (unl< a QC exceedance dictates the use of the higher GRQL data from the diluted sample analysis). Replace concentrations that exceed the calibration range -in the original analysis by crossing out the "E" value on the original Form I and substi- tuting it with data from the analysis of rtllnrerl sample. Specify which Farm I is to be used, then draw a red "X" across the entire pege of all Porn I's that should not be used, including any in the sunxnary package. 11.0 S*xrAj)£t*£ Pyta fGC/MSl 11.1 Are the Reconstructed Ion Chronatograins, and data system printouts (Quant. Reports) present for initial S and continuing calibration? [ \/l ACTION: If any calibration standard data are missing, take action specified in 3.2 above. -.0 GOT*S Initial c&\ ^ration (Form 12.1 Are the Initial Calibration Forms (Form VI) present / and cccplete for the volatile fraction? { v 1 __ __ ACTION: if any calibration standard forms are missing, take action specified in 3.2 above. 12.2 Are response factors stable for volatiles over the / concentration range of the calibration (RSD <30*)? [ __ ] v __ ACIICN: Circle all outliers in red. ACnOK: When RSD >30%, nan-detects may be qualified using professional judgement. Flag all positive results "J". When RSD >90%, flag all nan-detects as unusable ("R") . (Region n policy.) 12.3 Do any cotpounds have an average RRF < 0.05? ^__ AdlOK: Circle all outliers in red. ACTION: If any volatile compound has an average _^ RRF < 0.05, flag positive results for that conpound as estimated ("J") , and flag non- detects for that conpound as unusable ("R") . *in OPERATING ERCCZHJKE Page: 13 of 36 Date: March 1990 Revision 7 YES NO N/A 12.4 Are there any EiAi&qri|?*'iHri / p*1r*ilyt'im errors in the reporting of average respmse factors (ERF) or %PSO? (Check at least two values but if errors are / found, check oore.) __ f V/1 __ AdlCN: Circle errors in red. ACTION: If errors are large, can lab for explanation / i r ii il ml it 'il. sake any necessary corrections and note errors under "Conclusions". 13.0 GC/MS ^ "'tUTUjUTT CSll^Lfltion fPonn vm 13.1 Are the Continuing Calibration Paras (Para VH) and complete for the volatile fraction? 13.2 Has a continuing calibration standard been analyzed for every twelve hours of sample analysis per instruaent? ACTICK: List below all sanple analyses that were not within twelve hours of the previous continuing calibration analysis. ACTION: If any foras are missing or no continuing calibration standard has been analyzed within •twelve hours of every sample analysis, call lab for explanation / resubmittal. If continuing calibration data are not available, flag «T1 ^ yyn1;jj**JT^ sample *^*fr* as unusable ("R"*) • 13.3 Do any continuing calibration standard compounds have / a RST < 0.05? v7 ACTICK: Circle an outliers in red. ACTION: If any volatile compound has a RRF < 0.05, flag positive results for that ocnpound as estimated ("J1*), and flag nan-detects for that compound as unusable ("R"). 13.4 Da any compounds have a % difference between initial and / continuing calibration RRF > 25%? J^L t__1 ACTICN: Circle all outliers in red and qualify associated sample data as outlined in the table below: UO-: 19/4 STMJDf&D OF5WIHG rage: 14 of 36 Date: March 1990 Revision 7 YES NO ±^—j*j 1 jAj—rv ' J1 positive | «J« positive results, no action results, 'UP for non detects jnon detects <^yw 'J' positive results, "R" nan detects 13.5 Are there any transcription / errors in the 14.0 «frwrting of average response factors (KRF) or (%0) between initial and continuing RRFs? (Check at least two values but if eiiuis are found, check more.) AdTCN: Circle errors in red. ACTION: If errors are large, call lab for explanation / resurcittal, make any necessary corrections and note errors under "Conclusions". ("FoTJfi VI' II / Fv 1 __ 14.1 Are the internal standard areas (Form vm) of every sacplc and blank within the upper and lower limits / for each continuing calibration? f\/ 1 __ ACTION: List all the outliers below. Sacple « Internal Std Area Lower Limit. Upper Limit (Attach additional sheets if necessary.) If the internal standard area count is outside the upper or lower limit, flag with "J*1 all positive results and non- detects (U values) quantitatad with this internal standard. If extremely low area counts are reported, or if performance exhibits a major abrupt drop off, flag all associated nan- detects as unusable ("R"). 14.2 Are the retention tines of the internal standards within 30 seconds of the associated calibration standard? ACTXCH: Professional judgement should be used to qualify data if the retention timns differ by more than / rv 1 __ __ 30 ~n IT STANDARD OH3A1BC EROCEDEIFE * Page: 15 of 36 Date: torch 1990 Revision 7 £g 55——j^- 15.0 15.1 Here any field duplicates submitted for TOA analysis? f/ 1 ACTICN: Ocopare the injected results for field end calculate the relative percent dif* ACTICN: Any gross variation bftrean field duplicate results must be addressed in the reviewer narrative. However, if large differences exist, identification of field *"r'"-**•*« should be confirmed by contacting the saspler. STANDARD OPERATING PROCEDURE Page: 16 of 36 Date: Marda 1990 Revision 7 5 5 N O N/A" PART B: HtA ANALYSES ..0 Traffic RtfLVi tiff and Tft]n'» liflt <?rv T^ii ifltivff 1.1 Are the Traffic Report Paras p. mint for all samples? ACTION: If no, contact lab for replacement of missing or illegible copies. 1.2 Do the Traffic Reports or Lab Narrative indicate any problems with sasple receipt, "'^ifim of samples, analytical problems or *perinl notations affecting the quality of the data? ACTION: Use professional judgement to evaluate the effect on the quality of the data. ACIICK: If any sazple analyzed as a soil contains than 50% water, all data should be flagged as estisated (J). 7 TJ 2.1 Have any 5\n. holding tines, determined from date of collection to date of extraction, been exceeded? Samples for !NA analysis, both soils and waters, must be extracted within seven days of the date of collection. Extracts most be analyzed within 40 days of the date of extraction. Table qf, ffQJd-iTrf TI'M Violations (See Traffic Report) Sasple Date Date Lab Date Date Sarple Matrix Sampled Received Extracted Analyzed A^.^CLS 10 103-1tJD I I ACTION: If holding tires are exceeded, flag all positive results as estimated ("J") and sample quantitation limits as estimated ("UJ"), and document in the narrative that holding were exceeded. STANDARD OPERATING PRDCSUKE Page: 17 of 36 Bate: March 1990 Revision 7 : 35 NO N/A~~ If analyses were done sore than 14 days beyond holding time, either on the first analysis or upon reanalysis, the reviewer Bust use professional judgement to determine the reliability of the data and the effects of additional storage on the sample results. One reviewer may determine that nan data are unusable ("R") . 3.0 3.1 Are the atA Surrogate Recovery Summaries (Tom U) pieaeiiL for each of the following matrices: a. lau Water f V"\ __ __ b. Med Water [__] __ V c. Lew Soil [__] J/ ~ / d. Med Soil [__] __ / 3.2 Are all the SNA samples listed on the appropriate Surrsgate Recovery Susraaries for each of the following matrices: a. low Water f VI __ __ b. Med Water [ .._] v c. Lew Soil d. Mad Soil ACTION: Call lab for explanation / resubmittals. If missing deliverables are unavailable, da.mnpnL effect on data under "Conclusions'1 section of reviewer narrative. 3.3 Were outliers marked correctly with an asterisk? r v 1 ACTION: Circle all outliers in red. 3.4 Were two or more base-neutral ££ acid surrogate cut of specification for any sample or method blank? V [ _ .J __ If yes, were samples reanalyzed? f\/1 __ __ Were method blanks reanalyzed? [ __ ] __ \X ACTICN: If all BO surrogate recoveries are > 10% but two within the base-neutral or acid fraction do not meet SOW specifications, for the affected fraction bas *'^ UP^*^ * 1. Flag all positive results as estimated ("J") 2. Flag all nan-detects as estimated detection limits ("UJ"). OPERATING IRXH1SZ Page: 18 of 36 Data: March 1990 Revision 7 YES NO If any base-neutral or. acid surrogate has a recovery of <10% : 1. Flag all positive results for that fraction (i.e. all acid or base-neutral compounds) *J". 2. Flag all nan-detects for that fraction "R". Professional judgement should be used to qualify data that have method blank surrogate red cut of specification in both original and analyses. Check the internal standard 3.5 Are there any trarscriptiorv/calculatian errors between raw data and Fora U? ACTION: If large errors exist, call lab for explanation / resubnuttal, make any necessary corrections and note errors under "Conclusions'1. 4.0 Matrix 4.1 Is the Matrix Spike Duplicate/Recovery Form (Fora HI) . present? \ V 1 __ __ 4.2 Were matrix spikes analyzed at the required frequency for each of the following matric a. Low Water r vM __ __ b. Med Water [__] __ / c. Low Soil [__] __ _/_ d. Med Soil [__] __ / ACTION: If any matrix spike data are missing, take the action specified in 3.2 above. 4.3 How carry B& spike recoveries are outside QC limits? out of 22 mft out of 22 4.4 How many RFD's for matrix spike and matrix spike duplicate recoveries are outside QC liaits? sails O cut of 11 t^\\k cut of 11 ACTICN: If MS and MSD both have less than 10% recovery for an analyte, negative results for that analyte should be rejected, and positive results should be flagged "J". The above !UT °02 19': applies only to the sample used for MS/MSD analysis. Use professional judgment in applying this criterion to other samples. STANDARD OPERATING PROCEDURE Page: 19 of 36 Date: March 1990 Revision 7 YES NO 5.0 planks (Form TV! 5.1 Is the Method Blank summary (Farm IV) present? T Vi __ __ 5.2 Frequency of Analysis: for the analysis of BNA TCL compounds, has a reagent/method blank been analyzed for each set of samples or every 20 samples of similar matrix (low water, mad water, low soil, / medium soil), %4iicnever is more frequent? r v 1 __ __ 5.3 Has a BNA instrument blank been analyzed for each GS/MS , system used. f y 1 __ __ ACTICN: If any nethod blank data are missing, call lab for explanation/resuianittal. If not available, reject all associated positive data ("R"). 5.4 Chrarnatography: review the blank raw data - chranatograms .. . (RICs), quant reports or data system printouts and Is the chromatcgraphic performance (baseline stability) / for each instrument acceptable for VQAs? f v ] __ __ ACTICN: Use professional judgement to determine the effect on the data. 5.0 NOTE: "Water blanks" and "distilled water blanks" are validated like any other sample and are not used to qualify data. Do not confuse them with the other QC blanks discussed below. 6.1 Do any method/instrumenVreagent blanks have positive results (TCL and/or TIC) for ENAs? When applied as described below, the contaminant concentration in these blanks are multiplied by the sample Dilution / Factor. __ r *! __ 6.2 Do any field/rinse blanks have positive BNA results / (TCL and/or TIC)? __ [__] JL. ACTION: Prepare a list of the samples assnriafart with each of the contaminated blanks. (Attach a separate sheet.) NOTE: Only field/rinse blanks taken the same day as the samples are used to qualify data. Blanks may not be qualified because of contamination in another blank. Blanks may be qualified for surrogate, spectral, tuning or calibration QC TI...IT problems. QF5WHNS FRDCUJrE Page: 20 of 36 Date: March 1990 Revision 7 __ HO N/A ACnCN: Follow the directions in the table below to qualify TCL results due to contamination. Use the largest value from all the associated blanks. j Sample oarig > CBQT ' Sampl • rrrv < fPgr. tj gar-pi o fray > CRQL ! but < lOx blank is < lOx blank value value £ >10x blank value n,iij.im Flag sarple result Reject sample fnthalate with a 'U'; cross and i"i"V' CRQL; Esters out 'B1 flag cross out 'B' flag Sample cone > CRQLjSample cone < CRQL fi.'Sarple cone > CRQL but < 5x blank is < 5x blank value value 6 > 5 blank value Other ContaiBinants Flag sarple result Reject sample result No qualification • with a 'U1; cross and iqjuit CRQL; is {out 'B' flag cross cut 'B' flag i. ACTION: For TIC expounds, if the concentration in the sample is less than five fi**** the concentration in the most con- taminated assoriatnd blank, flag the sarple data "R" (unusable). €.3 Are there field/rinse/equipment blanks assoriatari with every / sarple? [__] __ ^L. ACITCN: For low level samples, note in data assessment that there is no associated field/rinse/equipment blank. Deception: samples taken from a drinking water tap do not have associated field blanks. GC/MS i T r f 7.1 Are the GC/M5 Tuning and Mass Calibration Foncs. (Fora V) / present for Decafluorotriphenylphosphine (UtTWj ? C V^J __ __ 7.2 Are the enhanced bar graph spectrum and mass/charge (m/z) listii hour shirt? (m/z) listing for the DFUP provided for each twelve / 7.3 Has a tuning performance compound been analyzed for every / twelve hours of sacple analysis per instrument? f\/ 1 ACTION: If any tuning data are missing, take action specified in 3.2 above. ACTION: List date, time, instrument ID, and sample analyses for which no associated GC/MS tuning data are available. 1981 STTANCftRD OPERATING Page: 21 of 36 Date: March 1990 Revision 7 YES NO N/A DATE TIME — ——— " ACTION: If lab cannot provide missing data, reject ("R") all data generated outside an acceptable twelve hour calibration interval. 7.4 Have the ion abundance criteria instrument used? net for each ACTION: List all data which do not meet ion abunda criteria (attach a separate sheet). ACTION: If tuning calibration is in error, flag all associated sanple data as unusable ("R"). However, if expanded ion criteria are met (See 1933 Functional Guidelines), the data reviewer may accept data with appropriate qualifiers. 7.5 Are there any transcription / calculation errors between mass lists and Fora Vs? (Check at least two values but if errors are found, check more.) 7.6 Have the appropriate number of significant figures (two) rted? (Check at least two values, but if errors are found check acre values.) ACTION: If large errors exist, call lab for explanation / resubndttal, rake necessary corrections and note errors under "Conclusions". tra of the mass calibration conpound 7.7 Are the jx « •»*[ iKaihl»? ACTION: Use professional judgement to determine whether associated data should be 1, qualified, or rejected. 8.0 Tamet Cor Are the Organic Analysis Data Sheets (Form I 9A) present with required header inf oznation on page, for each of the following: a. Samples and/or fractions as appropriate b. Matrix spikes and matrix spike duplicates c. Blanks 8.3 Are the response factors shown in the Quant Report? [__] 8.4 Is chrcmatographic performance acceptable with to: / Baseline stability r v 1 STANDARD OPERATING PRCCSUFZ Page: 22 of 36 Date: March 1990 Revision 7 YE 55 8.2 Are the ENA Reconstructed Ion Chramatagrams, the mass speuLia for the identified conpounds, and the data system printouts (Quant Reports) included in the sanplc package for each of the following? a. Sanples and/or fractions as appropriate £v/] __ b. Matrix spiJces and matrix spike duplicates fv 1 __ (Mass hpuctra not required) c. Blanks ACIICN: If any data are missing, take action rifled in 3.2 above. Resolution f \/l __ __ Peak shape r s/1 __ __ Pull-scale graph (attenuation) r V 1 __ __ Other:_________________ [__] __ V ACTION: Use professional judgement to determine the acceptability of the data. 8.5 Are the lab-generated standard mass s^ectna of the / identified ENA compounds present for each sanple? [__] __ v ACITCN: If any rm«s spectra are missing, take action specified in 3.2 above. If lab does not generate their own standard spectra, make note in "Contract Problems/Non-acqplianaeN. B.6 Is the EFT of each reported ccopound within 0.06 HKT • , units of the standard KRT in the continuing calibration? [__] __ v 8.7 Are all ions pi mint in the standard BBSS spectrum at a relative intensity greater than 10% also present in the / sanple mass spectrum? r ^ ^ 8.8 Do saaple and standard relative ion intensities agree / unt-h-in •><•»*? r i y within 20%? ACTION: Use professional judgement to determine acceptability of data. If it is determined that incorrect identifications were made, T all such data should be rejected, flagged ~" '-"-^ 1903 "N" (presunytive evidence of the presence of the cuipuund) or changed to not detected (at the calculated detection limit). STANDARD OPERATING PROCEDURE Page: 23 Of 36 Dete: March 1990 Revision 7 Y E S N O " 9.0 Tentatively Tdentifl 9.1 Are «ll Tentatively Identified r^fjmri Tarns (Poem I, Part B) present; and do *<«*••* TICs include scan number or retention time, estimated conoentration and "J" qualifier? 9.2 Are the mass H.ML.LLA for the tentatively identified Bpounds and associated "best natch" hpectia included in the sample package for each of the following: a. Samples and/or fractions as appropriate r V 1 __ __ b. Blanks [__] __ \f ACTION: If any TIC data are missing, take action specified in 3.2 above. ACTION: Add "J" qualifier if missing and "N" qualifier to all identified TIC compounds on Fora I, Part B. 9.3 Are any TCL expounds (from any fraction) li***^ as TIC compounds (exszple: 1,2-dimethylbenzene is xylene— / a VQA TCL—and should not be reported as a TIC)? __ f v 1 __ ACTICN: Flag with "R" any TCL compound listed as a TIC. 9.4 Are all ions present in the reference mass spectrum with a relative intensity greater than 10% fljg" present in the / sample mass spectrum? Iv ] __ __ 9.5 Do TIC and "best match" standard relative ion intensities / agree within 20%? r V 1 __ __ ACTICN: Use professional judgement to determine acceptability of TIC identifications. If it is determined that an incorrect identi- fication was made, change identification to "unknown" or to some less specific identi- fication (exanple: "C3 substituted benzene") as y],'y*"'^'"'i f*"*- 1Q O AW.W 10.1 Are there any transcription / calculation errors in Form I results? Check at least two positive values. Verify that the correct internal standard, guantitation ion, and PJIT were used to calculate Form I result. / __ L*J —— Were any errors found? Are the OQIs adjusted and, for soils, sample moisture? [__} 10.2 Are the CRQIs adjusted to reflect sacple dilutions / STANDARD QFE3ATBC ERDdLTZ Page: 24 of 36 Data: March 1990 Revision 7 NO ACHCN: If errors are large, call lab for explanation / resubmittal, make any necessary collections and not* errors under "Conclusions". ACTION: When a sample is analyzed at acre than one dilution, the lowest CRQEs are used (unless a QC exoeedance dictates the use of the higher CRQL data from the diluted sample analysis) . Replace ccncentratiens that exceed the calibration rang* in the original analysis by crossing cut the T" value on the original Farm I and substi- tuting it with data frcn the analysis of *"'*•-* sample. Specify «hich Form I is to be used, then draw a red "X* across the entire page of all Fora I's that should not be used, including any in the smsnary package. 11. 0 S*~*rr**TJF [^ta (GC/V5) 11.1 Are the Reconstructed Ion Chranatcgrams, and data system printouts (Quant. Reports) present for initial and continuing calibration? ACTICN: If any calibration standard data are missing, v_ taJce action specified in 3.2 above. J2.0 GC/?S Initial CS^ibrsition fTom 12.1 Are the Initial Calibration Forms (Fora VI) present / and conplete for the ENA fraction? ["^ 1 ACTION: If any calibration standard forms are missing, take action specified in 3.2 above. 12.2 Are response factors stable for ENAs over the concentration range of the calibration (RSD <30%)? [__] ACnCN: Circle all outliers in red. ACTION: When RSD >30%, nan-detects nay be qualified using professional judgement. Flag all positive results "J". When RSD >90t, flag all nan-detects as unusable ("R"). (Region H policy.) 12.3 Do any conpcunds have a FRF < 0.05? __ r V"\ __ ACnCN: Circle an outliers in red. ACTION: If any ENA cotpound has an average ^ RRF < 0.05, flag positive results for that cccpcund as estimated ("J"), and- flag nan- detects for that ccnpound as unusable ("R"). SEWDAPD OPERATING FRXEDGKE Page: 25 of 36 Date: March 1990 Revision 7 25 55 5y3T 12.4 Are there any transcription / p^'|<'"TV"im errors in thereporting of average mponaa factors (RRF) or %RSD? (Check at least two values but if errors are found, check nore.) ___ ACTICN: Circle errors in red. ACTION: If errors are large, «U lab for explanation / resubnittal, sake any necessary corrections and note errors under MCanclusiensN. i3.o cc/?s 13.1 Are the Continuing Calibration Fbnns (Fora VU) present / and conplete for the BNA fraction? r v'\ __ __ 13.2 Has a continuing calibration standard been analyzed for every twelve hours of sanple analysis per / mstruBent? f \/ 1 ^^^ ACTION: List below all sasple analyses that were not within twelve hours of the previous continuing calibration analysis. ACTICN: If any foras are missing or no continuing calibration standard has been analyzed within twelve hours of every sanple analysis, **i.\ lab for explanation / resubmittal. If continuing calibration data are not available, flag all associated sazple data as unusable ("R"). 13.3 Do any continuing calibration standard compounds have a RR? < 0.05? __ ACTICN: Circle all outliers in red. ACTICN: If any ENA conpound has a RRF < 0.05, flag positive results for that conpound as estimated ("J"), and flag nan-detects far that: ccnpound as unusable ("R"). 13.4 Do any compounds have a % difference botvaeen initial and / continuing calibration HRF > 25*? v [__] —— ACTICN: Circle all outliers in red and qualify associated sasple data as outlined in the table below: TUT 002 1986 STANDARD OPERATING 26 of 36 Date: March 1990 Revision 7 YES N/A ^w ww i ww ^w •J1 positive j «j» positive results, no action 'results, 'UT' for ncn detects jnon detects ^•^w 'J1 positive results, "R" ncn detects 13.5 Are there any tr iption / e^l' in the (BRF) or difference reporting of average response (%O) be tr i«an initial and continuing RRFs? (Check at least two values but if eu.ui> are found, check norm.) ACTICN: Circle errors in red. ACTICN: If errors are large, call lab for explanation / resucoittal, make any necessary corrections and note errors under "Conclusions". 14.0 int^r^ Vim 14 . 1 Are the internal standard areas (Form VHI) of every sanple and blank within the upper and lower liaits for each cent inning calibration? ACTION: list an the outliers below. Sazple I Internal Std Area Lower Limit Upper Limit (Attach sheets if ACTICN: If the internal standard area count is outside the upper or lower limit, f*g with MJ" all positive results and nan- detects (U values) ouantitated with this internal standard. If extremely low area counts are reported, or if performance exhibits a major abrupt drop off, flag all assocj detects as unusable ("R"). 14.2 Are the retention times of the internal standards within 30 seconds of the a«™~»'»*•••* calibration standard? non- ACriCK: Professional judgement should be used to qualify data if the retention +*•*** differ by more than 30 •in STANDARD OPERATING PROCEDURE Page: 27 of 36 Date: March 19SO Revision 7 ~"" Y E S 5 5 N/A" w. 0 Field 15.1 Here any field ^T*1-*"1'*'^ submitted for BKA analysis? AdlCN: Ccopare the reported results far field duplicates and calculate tbe relative percent diffe ACZTCK: Any gross variation between field triplicate results oust be addressed in the reviewer narrative. However, if large differences exist, identification of field duplicates should be confirmed by contacting the sanpler. ^ STANDARD OPERATING HOCZZL3Z Page: 28 Of 36 Date: March 1990 Revision 7 T^..... **** * ° * ^ * " 1.0 Traffic P<r,'»'gf5 and 1 1.1 Are the Traffic Report Forms present for all sanples? AdTCN: If no, contact l»*i for replacement of missing or illegible 1.2 Do the Traffic Reports or Lab narrative indicate any probles with sasple receipt, condition of sanples, analytical problems or «r"~i*l natations affecting the quality of the data? AdTCN: Use professional judgement to evaluate the effect on the quality of the data. AdlCN: If any sample analyzed as a soil curtains more than 50% water, all data should be flagged as estimated (J). 2.0 2.1 Have any PEST/PC3 holding times, determined from date of / collection to date of extraction, bisen exceeded? __ tv 1 Sarples for JEST/PCS analysis, bach soils and waters, oust be extracted within seven days of the date of collection. Detracts oust be analyzed within 40 days of the date of extraction. 3.0 3.1 Are the PEST/FC3 Surrogate Recovery Stannaries (Fans H) present for each of the following matrices: a. Low Water " I" \/l __ __ b. Med Water c. Low Soil [__] *". d. Med Soil C__] __ J^L 3.2 Are all the FEST/FCB sanples li^erl on the appropriate Surrogate Recovery Sunsnaries for each of the following natric o^ _ _ a. low Mater b. Med Mater c. Low Soil • d. Med Soil C——3 —— -fc— STANDARD OFERATOC I50CSURE Page: 29 Of 36 Date: March 1990 Revision 7 YES NO N/A f>11 lab for explanation / resubnittals. If atissing deliverables are unavailable, document effect on data under "Conclusions" section of narrative. 3.3 Were outliers marked correctly with an asterisk? r \/1 __ __ ACTION: Circle all outliers in red. 3.4 Was surrogate (DEC) recovery outside of the ujuU.au. / specification for any sample or blank? v ACTION: Kb qualification is done if surrogates are detection. If recovery is below contract limit (but above zero) , flag all results for that sample "J". If recovery is zero, flag positive results "J" and nan-detects "R". If recovery for the blank is zero, flag nan-detects for all associated samples "R". if recovery is above contract limit, flag all positive results for that sample "J™, unless in the reviewers professional judgement the high recovery is due to co-«luting interference (check the associated blank - if recovery is high there also, flag the sample data). 3.5 Are there any transcription/calculation errors between raw / data and Fora H? __ r y 1 __ ACTION: If large errors exist, call lab for explanation / resutcirtal, sake any necessary corrections and note errors under "Conclusions". 4.0 Matrix 4.1 Is the Matrix Spike Duplicate/Recovery Porn (Fora HI) / present? " - fv 1 __ __ 4.2 Were matrix spikes analyzed at the required frequency for each of the following matrices: a. Low Watar r v 1 __ __ b. Med Water c. Low Soil d. Med Soil C __ 3 __ ^L ACITCN: If any matrix ^pike data are missing, take the action specified in 3.2 above. 4.3 How many PE5T/PCB spike recoveries are outside QC limits? Water Soils OO'.Z 199O out of 12 NJJA- out of 12 OFERATOG ERDdXJPE Page: 30 of 36 Date: March 1990 Revision 7 YES NO N/A 4.4 How many PFD's for matrix spike and matrix spike duplicate recoveries are outside QC limits? Soils A/ /A out of 6 ACTICN: If MS and USD both have less than zero recovery for an analyte, negative results for that analyte should be rejected, and positive results should be flarjud "J". Ihe above applies only to the sample used for MS/MSD analysis. Use professional judgement in applying this criterion to other samples. Blanks (Form IV1 5.1 Is the Method Blank Summary (Form IV) present? 5.2 Frequency of Analysis: for the analysis of Pesticide TCL expounds, has a reagent/method blank been analyzed for each set of samples or every 20 samples of similar matrix (low water, med water, low soil, / medium soil) , whichever is more frequent? C ^ 1 __ __ 5.3 Qiromatography; review the blank raw data - chrccatograas, quant reports or data system printouts. Is the chrofflatographic performance ^baseline stability) s for each instrument acceptable for PEST/PCBs? f V/l __ __ ACTION: Use professional judgement to determine the effect on the data. 5.0 NOTE: "Water blanks" and "distilled water blanks" are validated like any other sample and are not used to qualify data. Do not confuse them with the other QC blanks dlsnreserl below. 6.1 Do any method/instrument/reagent blanks have positive results for PEST/PCBs? When applied as described below, the contaminant concentration in these blanks / are multiplied by the sample Dilution Factor. __ f Vi __ 6.2 Do any field/rinse blanks have positive PEST/PCS results? ACTION: Prepare a list of the samples associated with each of the contaminated blanks. (Attach a separate sheet.) TUT STANDARD OPERATING 31 of Data: March 1990 Revision 7 36 NOIZ: Only field/rinse blanks taken the same day as the samples are used to qualify data. Blanks nay not be qualified bemtffie of contamination in another blank. Blanks nay be qualified for surrogate, spectral, tuning or calibration QC problc ACHCN: YZS Follow the directions in the table below to qualify TCL results due to cm rumination. Use the largest value from all the associated blanks. NO N/A Sasple cone > CRQL but < 5x blank Flag sample result with a "U"? cross cut "B" flag Sample cone < CRQL & is < 5x blank value Reject sample result and report QS3L; cross cut "B" flag Sample cone > O3QL * > 5x blank value No qualification with every 6.3 Are there field/rinse/equipment blanks sacple? AdTCK: For low level samples, note in data asf*'Mr?"^Tt- that there is no associated field/rinse/equipment blank. Deception: samples taken from a drinking water tap do not have ftssnr-inted field blanks. .O ibratlon and GC 7.1 Are the following Gas Cnrcnatograms and Data System Printouts for both Prinary and Confirmation (conficaaticn standards not required if there - are no positive results above CRQL) column present: a. Evaluation Standard Mix A b. Evaluation Standard Mix B c. Evaluation Standard Mix C d. Individual Standard Mix A «. Individual Standard Mix B f. Multi-component Pesticides Ttxaph g. Aroclors 1016/1260 & Chlordane h. Aroclors 1221, 1232, 1242, 1248, and 1254 ACTICN: If no, take action specified in 3.2 above STANDARD OF5VJING FROCHL.7Z Page: 32 of 36 Date: March 1990 Revision 7 ~ ~ ~ " Y E S N O N / T 7.2 Is Fora VIU Pest-1 present and complete for each GC column (primary and oonf iraaticn) and each 72 hour of analyses? ACTION: If no, take action specified in 3.2 above. 7.3 Are there any t^> ^r*cg-»H~*"<(-i^/>raTr^^^'irj^ errors between raw data and Fora VIII? ACHCN: If large errors exist, "•"»?. lab for explanaticn / resubmit±al, make any necessary corrections and note errors under "Conclusions'*. 7.4 Has the total breakdown on quantitaticn or ccnfiraation / column rxnBerW 20% for IMT? __ Cv1 __ - for Endrin? __ r \/1 __ cor if Endrin aldehyde and 4,4'-EDO cc-elute and there is a peak at their retention tine, has the combined DOT and Endrin / breakdown exceeded 20*? __ [__] _\/ ACIICN: a. If EOT breakdown is greater than 20% en quantitaticn column beginning with the samples fallowing the last in uunitrol standard: 1. Flag all positive DOT results "J". 2. If DOT was not detected but OCO and/or DEE are positive, flag the DOT nan-detect "R". 3. Flag positive COD and DCE results "JN". 4. If DOT breakdown is > 20% en confinflation column and COT is identified on quantitaticn column but not on oonfiraaticn column, use professicnal judgement to determine whether COT should be reported on Form I (if reported, flag result "N"). b. If Brdrin breakdown is > 20% on quantitaticn column, beginning with, the sacples following the last in control standard: 1. Flag all positive Endrin results "J1*. 2. If Erdrin was not detected, but Endrin Aldehyde and/or Endrin Ketcne are positive, flag the Endrin ncn-detect "RM. 3. Flag Endrin Ketcne positive results "JIT. 4. If Endrin breakdown is > 20% en confirmation column and Endrin is identified on quantitaticn rnlvimn but not en confirmation column, use professicnal judgement to determine whether Endrin should be reported en Form I (if reported, flag result "N"). c. If the catbined breakdown is used (it can only be used if the conditions in 7.4 above are met) and is > 20% en quantitaticn column beginning with the last in miLml standard, take the actions specified in 7.4 a and b above. If the combined breakdown is >20% en confirmation column and Endrin or COT is identified on quantitaticn column but not en confirmation column, use professicnal judgement to determine whether Endrin or COT should be reported on Fora I (if reported, flag result "N"). OFEEAIDC ERDCEHJKE Page: 33 of 36 Date: March 1990 Revision 7 XES NO 7.5 Is the linearity check RSD of all four calibration factors / <10% for the quantitation column? f y~\ __ ACHCN: if no, flag positive hits for all pesticide and KB analytes "J" for an associated samples. Do not 1^*1 toxaphone or DOT if tbsy are quantified from a 3-point calibration curve. 7.6 Is the % difference between the EVAL A and each analysis (quantitation and conf iraaticn) DBC retention +-»™» within QC limits (2% for packed column, 0.3% for capillary [I.D. / < 0.32 am], 1% for aieqabaie [0.32 < I.D. < 2 mn]) ? f v 1 ACTION: DBC retention time cannot be evaluated if DBC is not detected. If it is present and has a retention time out of QC limits, then use professional judgement to determine the reliability of the analysis and flag results "R", if appropriate. 7.7 Was the proper analytical sequence followed for each / 72 hour period of analyses (page PEST D-36 in 8/87 SOW). r v i ACTION: If no, use professional judgement to determine the severity of the effect on the data and accept or reject it accordingly. Generally, the effect is negligible unless the sequence was grossly altered or the calibration was out of limits. 8.1 Is Form IX present and complete for each GC column and / 72 hr sequence of analyses? ^ ACTION: If no, take action specified in 3.2 above. 8.2 Are there any transcription/calculation errors between raw data and Form DC? ACITCN: If large errors exist, call lab for explanation / resubmittal, make any necessary corrections and note errors under "Conclusions". 8.3 Is COT retention *•?*•» for packed columns > 12 min / (except OV-1 and CV-101 columns)? r v \ __ __ ACHCN: If no, check that there is adequate resolution between individual components. If not, flag results for oorpounds that interfere with each other (co-elute) "R". 8.4 Do all standard retention times fall within the windows / established for the first DTO A and IND B analyses? f^ 1 __ __ TUT STANDARD OFE3ATDC FRDCEDL7L Page: 34 of 36 Date: March 1990 Revision 1 NO N/A" AdTCN: Beginning with the samples following the last in umtrol standard, check to see if the ehrrmntagrans contain peaks within an expanded window surrounding the retention times. If no peaks are found and, DBC is visible ncn-detects are valid. If peaks are present and cannot be i«j«nfr<*•*«** through "pattern recognition" or a consistent shift in standard retention tiaes, flag all affected compound results "R". 8.5 Are the continuing calibration standard calibration factors within 15* (for quantitaticn column) or 20% (for confirmation column) of the initial (at beginning of 72 hr sequence) calibration factors? f ^1 ACTION: If no, flag all nwiriaterl positive results "J". Use professional judgement to determine whether or not to flag nan-detects. ».0 Pesticide/PCB Identification 9.1 Is Form X complete for every sample in which a / pesticide or PCS was detected? [__] __ V ACTION: If no, take action specified in 3.2 above. — 9.2 Are there any transcription errors between raw / data and Fcra X? __ [__] v ACTION: If large errors exist, call lab for explanation / resubmittal, make any necessary corrections and note errors under "Conclusions11. 9.3 Are retention times of sample compounds within the calculated retention time windows for both quantitation and confirmation analyses? Was GC/JG confirmation provided when required (when oompound concentration is > 10 ug/ml in final ACTION: Reject ("R") an positive results (meeting quantitaticn column criteria, but missing confirmation by a second column or GC/HS (if appropriate). Also, reject ("R") an positive results not meeting retention time window criteria unless "tt*ff'i*t** standard compounds are similarly biased (i.e. base on RRT to DEC). 9.4 Check chrcnatograms for false negatives, especiany for the multiple peak components toxaphene and PCB's. Were there any false negatives? __ [_I_J —— ACTION: If appropriate PCS standards were not analyzed, or if the lab performed no confirmation analysis flag the appropriate data with an "RH. T1,,.. ,.,,„, ,_ STANDARD Or3*AT2C FBDdXJPZ Page: 35 of 36 Date: March 1990 Revision 7 YES 56 '0.0 ^'"B_ir*jj * 10.1 Are there any transcription / calculation errors in Form I results? Check at least two positive values. / Were any errors found? __ [__] v NOTE: Simple peak pesticide results can be checked for rough agreement between quantitative results obtained on the two GC columns. The reviewer should use professional judgement to decide whether a much larger concentration obtained on one column versus the other indicates the presence of an interfering compound. If an interfering compound is indicated, the lower of the two values should be reported and qualified as presumptively present at an estimated quantity ("JN"). This necessitates a determination of an estimated concentration on the confirmation column. The narrative should indicate that the presence- of interferences has obscured the attempt at a second ""l»w confirmation. 10.2 Are the CRQLs adjusted ta reflect sample dilutions / and, for soils, sample moisture? __ [__] v ACTION: If errors are large, mil lab for explanation / resuemittal, make any necessary corrections and note errors under "Conclusions". ACTION: When a sample is analyzed at more than one dilution, the lowest CHQLs are used (unless a QC exceedanoe dictates the use of the higher CHQL data from the diluted sample analysis). Replace concentrations that exceed the calibration range in the original analysis by crossing cut the *T" value on the original Fora I and substi- tuting it with data from the analysis of diluted sample. Specify which Fans I is to be used, then draw a red "X" across the entire page of all Fora I's that should not be used, including any in the summary package. 1.0 11.1 Were baselines stable? 11.2 Were any electropositive displacement (negative / peaks) or unusual peaks seen? __ f V 1 11.3 Were early eluting peaks (for early eluting / analytes) resolved to baseline? r V 1 __ ACTON: For 11.1 and 11.2, comment only. For 11.3, reject ("R") those analytes that are not T( iy sufficiently resolved. STANDARD OPERATING HQCSEG3E Page: 36 of 36 Data: Match 1990 Revision 7 YES NO JJ/A" .0 Field Dunli'^itg^ 12.1 Were any field duplicates suboittfld for KST/PCB / analysis? C VI __ __ XCXTCN: Ccopare the reported results for field duplicates and calculate the relative percent difference. ACHCN: Any gross variation between field dupl results oust be addressed in the reviewer narrative. However, if large differences exist, identification of field duplicates should be confirmed by contacting the sanpler. 1997 SDG # 900770 VIHA I Tutu Wells Site Contaminated Volatile Method Blanks and Their Associated Samples Method Blank Associated Samples VBLK01 VBLK02 VBLK03 VBLK04 Matthias Tillet, Hartman I (Gassett), Tillet(D), Trip Blank 10/03, Trip Blank 9/27, VIHA I Trip Blank 10/01, H2O Blk Tutu, Trip Blank 10/02, Dimitri, Diraitri MS Ramsey, Dimitri MSD, LaPlace, Bryan, Eglin I TUT OO2 199H GERAGHTY & MILLER, INC. SDG # 900770 VIHA I Tutu Wells Site Contaminated Trip Blanks and Their Associated Samples Trip Blank Associated Samples Trip Blank 10/01 (770-05) Trip Blank 10/02 (770-11) Trip Blank 10/03 (770-13) Trip Blank 9/27 (770-15) Bryan, Dimitri, Dimitri MS, Dimitri MSD, Matthias, Ramsey Eglin I, LaPlace, Tillet, TiUet(D) Hartman I (Gassett) VIHA I GERAGHTY 6? MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE I OFZI TOTAL REVIEW ~~ ~~ CLP DATA ASSESSMENT Functional Guidelines for Evaluating Organics Analysis Case No. ^OoniO SDG No. tX/H/frJlABORATORYfe/^c, SITE IZn; $(ll S'-fe. DATA ASSESSMENT: The current functional guidelines (1988) for evaluating organic data have been applied. All data are valid and acceptable except those analytes which have been qualified with a "Jn (estimated), "U" (non-detects) , "R" (unusable) , or "JN" (presumptive evidence for the presence of the raterial at an estimated value). All action is detailed on the attached sheets. Tvo facts should be noted by all data users. First, the "R" flag means that the associated value is unusable. In other words, due to significant QC problems the analysis is invalid and provides no information, as to whether the compound is present or not. "R" values should not appear on data tables because they cannot be relied upon, even as a last resort. The second fact to keep in irind is that no compound concentration, even if it has passed all QC tests, is guaranteed to be accurate. Strict QC serves to increase confidence in data but any value potentially contains error. Reviewer's S i gna t ur e : ^ /} /) W- tf%44U<L ______ Date : &} / oi 719 9; Verified By; ^£L^_ ^-P 5>~7^*- Date; // /V /19// "^^^~ "" "" " "^S^J^^"~xT *^———^-*l——^^——— •^^^••B i.^__^~ -^^^—— ATTACHMENT 1 SOP NO. HW-6 PAGE Z OF Zl DATA ASSESSMENT: 1. HOLDING TIME: The amount of an analyte in a sample can change with time due to chemical instability, degradation, volatilization, etc. If the specified holding time is exceeded, the data may not be valid. Those analytes detected in the samples whose holding time has been exceeded with be qualified as estimated, T. The non-detects (sample quantitation limits) will be flagged as estimated, "J", or unusable, "R", if the holding times are grossly exceeded. The following action was taken in the samples and analytes shown due to excessive holding time. All samples were analyzed within the holding time for volatile organic compounds except the trip blank dated 10/01/90. The chain of custody does not indicate whether or not this sample was preserved, therefore it is assumed that it wasn't. The trip blank 10/01 was analyzed 5 days over the 7 day aromatic volatile holding time; all aromatic volatile compound concentration values (hits and non-detects) are qualified with "J". All samples were analyzed within the holding time for semivolatile organic compounds except Tillet (RE) and Tillet(D)-RE (RE - re-extracted and reanalyzed). These samples are re-extractions which exceeded the 7 day holding time by 29 days and 31 days, respectively. All compound concentration values (hits and non-detects) are rejected for Tillet (RE) and Tillet(D)-RE. Note: The -RE suffix is used in this report to make a distinction between the first (original) extraction and second (re-extraction) extraction. All first extraction data are labelled "original" and the re- extraction data have the suffix -RE. The pesticides and PCBs were analyzed within holding times for all samples. TUT GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE 3 OF DATA ASSESSMENT: 2. BLANK CONTAMINATION Quality assurance (QA) blanks, i.e., method, trip, field, rinse, and water blanks are prepared to identify any contamination which may have been introduced into the samples during sample preparation or field activity. Method blanks measure laboratory contamination. Trip blanks measure cross-contamination of samples during shipment. Field blanks measure cross-contamination of samples during field operations. If the concentration of the analyte is less than 5 times the blank contaminant level (10 times for the common laboratory contaminants), the analytes are qualified as non-detects, "U". The following analytes in the samples shown were qualified with "U" for these reasons: A) Method blank contamination Volatile Organic Compounds Method blank VBLK01 is reported to contain methylene chloride at a concentration of 5 micrograms per liter (ug/L) and a tentatively identified compound (TIC) with a retention time (RT) of 3.83 minutes at a concentration of 7 ug/L. The sample Matthias is associated with this method blank and contains 9 ug/L of methylene chloride and 5 ug/L of the same TIC. The methylene chloride concentration value is qualified with "U" because it is less than 10 times the common contaminant concentration in the method blank. The TIC concentration value is qualified as a non-detect because it is less than 5 times the contamination in the method blank and therefore it is not reported. Method blank VBLK02 is reported to contain methylene chloride at a concentration of 5 ug/L, acetone at a concentration of 2 ug/L, and a TIC with a RT of 3.78 at a concentration of 5 ug/L The sample Tillet, which had a dilution factor of 5, is associated with this method blank and has a methylene chloride concentration of 40 ug/L and the same TIC at a concentration of 42 ug/L. The methylene chloride concentration value is qualified with "U" and the TIC concentration value is is not reported for the same reasons stated above. The samples Tillet(D) and VIHA I are also associated with this method blank and have methylene chloride and acetone concentrations at or above the contract required quantitation limits (CRQLs) as well as the same TIC contamination. The methylene chloride and acetone concentration values GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE H OF 2 DATA ASSESSMENT: are qualified with "U" and the TIC concentration values are not reported for reasons stated above. Method blank VBLK03 is reported to contain methylene chloride at a concentration of 2 ug/L and a TIC with a RT of 3.93 at a concentration of 6 ug/L. The sample Dimitri and the H2O Blk Tutu are associated with this method blank and have methylene chloride concentrations above the CRQL and the same TIC contamination. The methylene chloride concentration values are qualified with "U" and the TIC values are not reported for reasons stated above. Method blank VBLK04 is reported to contain methylene chloride at a concentration of 2 ug/L and a TIC with a RT of 3.97 at a concentration of 5 ug/L. The samples Bryan, Eglin I, Ramsey, and LaPlace are associated with this method blank and have methylene chloride concentrations at or above the CRQL and the same TIC contamination. The methylene chloride concentration values are qualified with "U" and the TIC concentration values are not reported for reasons stated above. Semivolatile Organic Compounds No contaminants are detected in the method blank. Pesticides/PCBs No contaminants are detected in the method blank. B) Field or rinse blank contamination ("water blanks" or "distilled water blanks" are validated like any other sample). All samples were taken directly from a drinking water tap into a collection bottle, therefore no field blanks were necessary. C) Trip blank contamination Only volatile organic compounds were analyzed for in trip blanks. GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE .f OF* I DATA ASSESSMENT: Trip blank 9/27 is reported to contain methylene chloride at a concentration of 16 ug/L. Sample VIHAI is associated with this trip blank and contains 3 ug/L of methylene chloride. This value is already qualified due to method blank contamination. Trip blank 10/01 is reported to contain methylene chloride at a concentration of 13 ug/L, acetone at a concentration of 6 ug/L, and a TIC with a RT of 3.95 at a concentration of 4 ug/L. The samples Bryan, Dimitri, Matthias, and Ramsey are associated with this trip blank. The methylene chloride and same TIC concentration values for these samples have already been qualified due to method blank contamination. Acetone is not detected in any of the associated samples. Trip blank 10/02 is reported to contain methylene chloride at a concentration of 14 ug/L, acetone at a concentration 7 ug/L, and a TIC with a RT of 3.95 at a concentration of 3 ug/L. The samples Eglin I and LaPlace are associated with this trip blank. The methylene chloride and same TIC concentration values for these samples have already been qualified due to method blank contamination. These samples also have acetone concentrations above the CRQL. These values are qualified with "U" because they are less than 10 times the common contaminant concentration in the trip blank. GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE 6 OF DATA ASSESSMENT: 3. MASS SPECTROMETER TUNING: Tuning and performance criteria are established to ensure adequate mass resolution, proper identification of compounds, and to some degree, sufficient instrument sensitivity. These criteria are not sample specific. Instrument performance is determined using standard materials. Therefore, these criteria should be met in all circumstances. The tuning standard for volatile organics is bromofluorobenzene (BFB) and for semi-volatiles is decafluorotriphenyl-phosphine (DFTPP). If the mass calibration is in error, all associated data will be classified as unusable, "R". All mass calibrations are acceptable for both the volatile and semivolatile analyses. TUT 002 GERAGHTY & MILLER. INC. ATTACHMENT 1 SOP NO. HW-6 PAGE 1 OF DATA ASSESSMENT: 4. CALIBRATION Satisfactory instrument calibration is established to ensure that the instrument is capable of producing acceptable quantitative data. An initial calibration demonstrates that the instrument is capable of giving acceptable performance at the beginning of an experimental sequence. The continuing calibration checks document that the instrument is giving satisfactory daily performance. A) RESPONSE FACTOR: The response factor measures the instrument's response to specific chemical compounds. The response factor for the Target Compound List (TCL) must be >. 0.05 (a ratio of areas) in both the initial and continuing calibrations. A value < 0.05 indicates a serious detection and quantitation problem (poor sensitivity). Analytes detected in the sample will be qualified as estimated, "J". All non-detects for that compound will be rejected ("R"). Volatile Organic Compounds The initial calibration performed on 9/28/90 has response factors < 0.05 for acetone, 2-butanone, and 2-hexanone. All samples are associated with this calibration and are qualified as stated above. The continuing calibration performed on 10/08 has response factors < 0.05 for 2-butanone and 2-hexanone. The continuing calibrations performed on 10/09, 10/13, and 10/14 have response factors <0.05 for acetone, 2-butanone,and 2- hexanone. These compounds are already qualified in the associated samples as a result of deficient initial calibration response factors. Semivolatile Organic Compounds All response factors are greater than or equal to 0.05 in both the initial and continuing calibrations. GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE i OF DATA ASSESSMENT: 5. CALIBRATION: A) PERCENT RELATIVE STANDARD DEVIATION (%RSD) AND PERCENT DIFFERENCE (%D): Percent RSD is calculated from the initial calibration and is used to indicate the stability of the specific compound response factor over increasing concentration. Percent D compares the response factor of the continuing calibration check to the mean response factor (RRF) from the initial calibration. Percent D is a measure of the instrument's daily performance. Percent RSD must be <30% and %D must be <25%. A value outside of these limits indicates potential detection and quantitation errors. For these reasons, all positive results are flagged as estimated, "J" and non-detects are flagged "UJ" (if %D or RSD > 50%). If there is a gross deviation of %RSD and %D, the non-detects may be rejected ("R"). For the PCB/PESTICIDE fraction, %RSD for aldrin, endrin, DDT, and dibutylchlorendate must not exceed 10%. Percent D must be within 15% on the quantitation column and 20% on the confirmation column. Volatile Organic Compounds The initial calibration performed on 9/28/90 has a %RSD greater than 30% for methylene chloride (66.948%) and acetone (71.280%). All samples are associated with this initial calibration. The methylene chloride concentration values will be qualified as stated above. The acetone concentration values are already qualified as a result of deficient response factors. The continuing calibration performed on 10/08 has a %D greater than 25% for 2-butanone (82.37%) and acetone (93.97%). The sample Matthias is associated with this calibration. These compounds are already qualified as a result of deficient response factors. The continuing calibration performed on 10/09 has a %D greater than 25% for the following compounds: TUT GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE 1 OF DATA ASSESSMENT: Compound %D Chloromethane 28.83 Bromomethane 27.18 Methylene Chloride 33.67 2-Butanone 75.79 Vinyl Acetate 46.25 4-Methyl-2-Pentanone 38.55 The samples Tillet, Tillet(D), Hartman I, Trip Blank 10/03, VIHA I, and Trip Blank 9/27 are associated with this calibration. The concentration values of the above compounds are qualified with "J" for positive hits. No action is taken for non-detects, except for 2-butanone, which are already qualified as a result of deficient response factors. The continuing calibration performed on 10/13 has a %D greater than 25% for the following compounds: Compound %D Bromomethane 39.46 1.1-Dichloroethane 28.41 trans-l,2,-Dichloroethene 30.42 Chloroform 40.08 1.2-Dichloroethane 48.71 1,1,1-Trichloroethane 37.61 Carbon Tetrachloride 34.44 Bromodichloromethane 40.12 1,2-Dichloropropane 31.95 trans-l,3-Dichloropropene 108.79 Trichloroethene 26.37 Dibromochloromethane 40.43 1,1,2-Trichloroethane 34.86 Benzene 33.19 Bromoform 27.06 4-Methyl-2-Pentanone 31.53 Chlorobenzene 27.12 ' •-•> ' 'J'-'2 2OO8 GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE «>OF DATA ASSESSMENT: The samples Dimitri, Trip Blank 10/01, H2O Blk Tutu and Trip Blank 10/02 are associated with this calibration. The concentration values of the above compounds are qualified with "J" for positive hits in the affected samples. No action is taken for non-detects, except for trans-l,3-dichloropropene, which will be qualified with "R" because the %D is greater than 90%. The continuing calibration performed on 10/14 has a %D greater than 25% for the following compounds: Compound %D Acetone 36.79 1,1,1-Trichloroethane 29.70 Vinyl Acetate 26.53 trans-l,3-Dichloropropene 38.95 cis-l,3-Dichloropropene 29.80 The samples Bryan, Ramsey, Eglin I, and La Place are associated with this calibration. The concentration values of the above compounds are qualified with "J" for positive hits. No action is taken for non-detects, except for acetone, which is already qualified as a result of deficient response factors. Semivolatile Organic Compounds No semivolatile organic compounds were detected in any of the samples. Therefore, the CRQLs will be qualified with "UJ" only when calibrations have %RSDs or %Ds greater than 50%. The continuing calibration performed on 10/27 has a %D greater than 50% for hexachlorocyclopentadiene (66.0%). Samples La Place, Tillet (original), and Tillet(D) (original) are associated with this calibration. The non-detect values will be qualified with "UJ". The continuing calibration performed on 11/08 has a %D greater than 50% forbenzoic acid (55.0%), 2,4-dinitrophenol (65.0%), and 2,4,6-tribromophenol (-55.0%). Sample Tillet(RE) is associated with this calibration. All semivolatile concentration values are already flagged with "R" due to holding time exceedence. GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE II OF 2-» DATA ASSESSMENT: Pesticides/PCBs The %RSD for aldrin, endrin, DOT, and dibutylchlorendate did not exceed 10%. The %D was within 15% on the quantitation column and within 20% on the confirmation column. GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGEIZOFZI DATA ASSESSMENT: 6. SURROGATES: All samples are spiked with surrogate compounds prior to sample preparation to evaluate overall laboratory performance and efficiency of the analytical technique. If the measured surrogate concentrations were outside contract specifications, qualifications were applied to the samples and analytes as shown below. Volatile Organic Compounds As specified in Method 524.2, only two surrogate compounds were used, bromofluorobenzene (BFB) and trans-l,2-dichlorobenzene-d4 (t-DCB). The recovery of BFB is outside the quality control (QC) limits (86-115%) in the following sample analyses: Sample %BFB Recovered Dimitri 82 H20 BLK Tutu 76 Trip Blank 10/03 82 Trip Blank 10/01 70 Trip Blank 10/02 74 VIHAI 82 DimitriMS 80 VBLK01 118 VBLK03 78 These samples were not re-analyzed. For each affected sample, the concentration values for compounds are qualified "J" for positive hits, and "UJ" for all non-detects. No QC limits are established for the recovery of t- DCB; however, when the BFB recovery is within QC limits, the t-DCB recovery is in the range of 80% to 120%. Semivolatile Organic Compounds The laboratory narrative states that in the original analyses of sample Tillet and Tillet(D) the recovery of the surrogates phenol-d5 (PHL) and 2- fluorophenol (2FP) were low, which lead to a re-extraction and re-analysis of TUT O02 20J..1 GERAGHTY & MILLER. INC. ATTACHMENT 1 SOP NO. HW-6 DATA ASSESSMENT: both samples. After the re-extraction, the Tillet (RE) surrogate recoveries were all within QC limits and the laboratory reported only this set of results. This re-extraction was performed out of holding time, therefore those results are qualified with "R" and are not reported. The original Tillet results were requested from the laboratory. The recoveries for PHL and 2FP were 8% and 11%, respectively, in the original Tillet analysis. Both PHL and 2FP are surrogates for the acid fraction, therefore only the acid fraction concentration values are qualified with "R" in the original Tillet sample as a result of one surrogate having less then a 10% recovery. After re-extraction, the Tillet (D)RE recoveries of the surrogates PHL and 2FP remained out of QC limits. The lab reported both sets of Tillet(D) results. The following are the recoveries for both Tillet(D) (original) and Tillet(D) RE analyses: Sample %PHL %2FP Tillet(D) - original 7 9 Tillet(D)RE 9 15 Only the acid fraction will be qualified "R" in each sample as a result of at least one acid fraction surrogate having less than a 10% recovery. Pesticides/PCBs The Dibutylchlorandate (DEC) recovery was high for sample VIHA I (191%, QC limits 24-154%). No pesticides or PCBs were found in this sample, therefore no qualifiers are necessary. GERAGHTY & MILLER. INC. ATTACHMENT 1 SOP NO. HW-6 PAGE/4OF2J DATA ASSESSMENT: 7. INTERNAL STANDARDS PERFORMANCE: Internal standard (IS) performance criteria ensure that the GC/MS sensitivity and response are stable during every experimental run. The internal standard area count must no vary by more than a factor of 2 (-50% to +100%) from the associated continuing calibration standard, the retention time of the internal standard must not vary more than +. 30 seconds from the associated continuing calibration standard. If the area count is outside the (-50% to +100%) range of the associated standard, all of the positive results for compounds quantitated using that IS are qualified as estimated, "J", and all non-detects as "UJ", or "R" if there is a severe loss of sensitivity. If an internal standard retention time varies by more than 30 seconds, the reviewer will use professional judgement to determine either partial or total rejection of the data for that sample fraction. All internal standard area counts and retention times are within QC limits for VOC analyses. The internal standard area count for Phenanthrene-dlO is extremely low for sample Tillet (original). All associated sample data quantitated using this internal standard are rejected. Sample Tillet (original) is reported to contain 20 ug/L of Di-n-Butylphthalate. This concentration was quantitated using the Phenanthrene-dlO internal standard area count. In the reviewer's professional judgement, this value is rejected because the quantitation is greatly altered by the low internal standard area count. If the area count were within QC limits, the reported value would be dramatically lower and would most likely be a non-detect. The internal standard area counts are within QC limits for the remaining volatile compound analyses. TUT O02 2013 GERAGHTY & MILLER. INC. ATTACHMENT 1 SOP NO. HW-6 PAGE 15C-F DATA ASSESSMENT: 8. COMPOUND IDENTIFICATION: A) VOLATILE AND SEMI-VOLATILE FRACTIONS: TCL compounds are identified on the GC/MS by using the anaiyte's relative retention time (RRT) and by comparison to the ion spectra obtained from known standards. For the results to be a positive hit, the sample peak must be within +_ 0.06 RRT units of the standard compound and have an ion spectra which has a ratio of the primary and secondary m/e intensities within 20% of that in the standard compound. For the tentatively identified compounds (TIC) the ion spectra must match accurately. In the cases where there is not an adequate ion spectrum match, the laboratory may have provided negative proofs. Volatile organic compounds are properly identified on the GC/MS and all TICs accurately match their ion spectra. No semivolatile target compounds were found in any sample. TICs accurately match their ion spectra. B) PESTICIDE/PCB FRACTION: The retention times of reported compounds must fall within the calculated retention time windows for the two chromatographic columns and a GC/MS confirmation is required if the concentration exceeds 10 nanograms per milliliter (ng/ml) in the final sample extract. No pesticides or PCBs were found in any sample^ GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE&OFZI DATA ASSESSMENT: 9. MATRIX SPIKE/SPIKE DUPLICATE, MS/MSD: The MS/MSD data are generated to determine the long-term precision and accuracy of the analytical method in various matrices. The MS/MSD may be used in conjunction with other QC criteria for some additional qualification of the data. All MS/MSD % recoveries are within QC limits for volatile, semivolatile organic compounds and pesticides/PCBs. TUT' OO2 20.L>j GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE II OF Z) DATA ASSESSMENT: 10. OTHER QC DATA OUT OF SPECIFICATION: A) Sample Receipt The chains of custody indicate that the lab received several vials which contained bubbles. As a result, all volatile organic data is assumed to be biased low and additional qualifiers are necessary. Bubbles were found in both vials for samples Tillet(D), LaPlace, and Eglin I. All positive hits for these samples are qualified with "J" and all non-detects are qualified with "R". These qualifiers supercede all others. Bubbles were found in only one vial for sample Tillet, but the lab was not able to distinguish which vial was used for the volatile organic analysis. Therefore, we must assume the vial with bubbles was used and additional qualifiers are necessary. All positive hits are qualified with "J" and all non detects are qualified with "R". B) Method Detection Limit Study Method 524.2 state that a method detection limit (MDL) study must be performed prior to sample analyses. The MDL study consists of seven repeat analyses of target compounds at concentrations of 1 ppb. The QC limits for mean accuracy (% recovery) and %RSD are 80-120% and 20%, respectively. The MDL study must be repeated if these standards are not met. The MDL study associated with SDG VTHAI results were performed in April 1990 and has the following deficiencies (*): Mean Compound Accuracv.% % RSD 1.1-Dichloroethene 72* 7.2 Methylene Chloride 148* 12.0 1.2-Dichloroethane 121* 7.9 Tetrachloroethene 76* 9.5 Bromoform 88 28.0 • 1,1,2,2-Tetrachloroethane 122* 7.3 GERAGHTY & MILLER. INC. ATTACHMENT 1 SOP NO. HW-6 PAGEl#OF2-l DATA ASSESSMENT: In addition, the following compounds were not included in the MDL study: acetone, carbon disulfide, 2-butanone, vinyl acetate, 4-methyl-2-pentanone and 2-hexanone. The above compounds are flagged "J" for all samples, except where compounds are qualified "R" for other deficiencies. C) Laboratory Fortified Blanks QC requirements established in Method 524.2 and the Sampling, Analysis, and Monitoring Plan (Appendix A) state that laboratory fortified blanks (LFBs) must be analyzed immediately following each continuing calibration and the accuracy must be between 80% to 120% recovery. The provided data indicate that the recoveries were out of QC limits for volatile compounds in each LFB. The LFBs were not always analyzed immediately after the calibrations. The affected samples and compounds are qualified "J" to reflect these deficiencies. GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 DATA ASSESSMENT: 11. SYSTEM PERFORMANCE AND OVERALL ASSESSMENT: The compounds of primary importance in this project are the volatile organics. SDG VIHA I has several volatile QC criteria out of specification. The MDL study had % recoveries out of QC limits as well as compounds which were not included in the study at all. The FLBs also had several compounds out of QC Limits and in two instances was not run immediately after the continuing calibrations. All target compounds were present in the FLBs. These MDL and FLB deficiencies indicate that the laboratory instrumentation has difficulties recovering certain compounds at low concentrations (1 ppb). As a result, the data is assumed to be biased low and the affected compounds are qualified with "J" in the associated samples. The volatile surrogate recoveries are out of QC limits in several samples as well as two (out of four) method blanks. For the affected samples, the identification of the compounds is acceptable, but for positive hits and non- detects the quantitation must be considered as estimated only. The concentration values and quantitation limits for the six affected samples have been qualified as such. The volatile calibrations are deficient for compounds which were either common lab contaminants or compounds not detected in any sample. The majority of the data is not seriously affected by these deficiencies. During the process of validation, the compound quantitation performed by the reviewer did not agree with the quantitation performed by the lab. The lab was notified and the laboratory personnel determined that the incorrect response factors were used to quantitate the compound concentrations for sample Matthias. The lab corrected the problem and sent a revised Form I(s) and quantitation report. These revisions are included with the data package. The bubbles in the vials have an impact on the quality of the volatile organic data for the affected samples. In samples Eglin I, LaPlace, Tillet, and Tillet(D), all non-detects in the affected samples are rejected "R" and all positive hits are qualified with "J". GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE20OF3H DATA ASSESSMENT: Overall, the volatile organic data is consistent although QC problems exist as discussed above. The semivolatile acid fraction surrogate recoveries for the samples Tillet and Tillet(D) were originally out of QC limits. Both samples were re-extracted and re-analyzed. Although the re-analysis presented some surrogate recoveries within QC limits, the re-extractions far exceeded the holding time, making the re-analysis data unusable (qualified "R"). The original Tillet sample results were received from the laboratory, and are reported in the table with the acid fraction concentration values rejected. In addition, several compounds are rejected because the associated internal standard area count was out of QC limits. The original Tillet(D) results are acceptable except for the acid fraction concentration values, which are rejected. All other semivolatile data is acceptable. The pesticide/PCB data is acceptable. The surrogate recovery was high for one sample, but no pesticides or PCBs were found, therefore it has no effect on the data. GERAGHTY & MILLER, INC. ATTACHMENT 1 SOP NO. HW-6 PAGE 21 OF DATA ASSESSMENT: 12. CONTRACT PROBLEMS: The MDL study failed to include six target compounds. Several results were out of QC limits established in Method 524.2 and the Sampling, Analysis, and Monitoring Plan. The laboratory fortified blanks were not analyzed immediately after the calibrations and many % recoveries are not within QC limits. The volatile organic analyses have several samples and two blanks with the surrogate BFB out of QC limits. The lab has failed to perform satisfactorily because there is no evidence of reanalysis for any sample or blank. 13. This package contains sample re-extraction, re-analysis or dilution. Upon reviewing the QA results, the following form I(s) are identified to be used. The Form I(s) for the original analyses of samples Tillet and Tillet(D) are to be used because they were performed within the holding time. GERAGHTY & MILLER. INC. ND. Evaluation of Metals Data for the Contract Laboratory Program <CL?) based on n SOU. 7/88 REV. 2/89 (SOP Revision X) 4~ / / * • F3EPWSD BY: ^/L^ ^c/ bvU-'/T/")_______ . . __ ERIE: ^jy- /A ~ ^ Hanif sieikh. Quality Assurance Chsroist 4 CaOCJPPZD BY; fTF+t^ /%l^4±s.>-i*f—-.. - ERIE:. Louis Bevilaqgua1, Sectio^J Chief Ttocic and " BY:r: ^ W^(^<F^ -£* (™> ^ Gerara F. McXpnna, Qiief ^B • Marnxorijij Managwient Branch 4 4 4^ "f'UI 002 2021 SCttGNQ OPSWT2C PROZDU?£ Title: Evaluation of inorganic Data for the Date: Feb. :«?:• Contract Laboratory Progran Number: H/:-2 Revision: 10 l.o Scope 1.1 This procedure is applicable to inorganic data obtained from contractor laboratories working for Hazardous Waste Site Contract Laboratory Program (CLP) . 1.2 Tfte data validation is based upon analytical and quality assurance requirements specified in Statement of Work (SOW) 7/88. 2.0 Responsibilities - Data reviewers vill corplete the following tasks as assigned by the Da Review Coordinator: 2.1. For a *ot-ai review: 2.1.1 The reviewer oust answer every question on the checklist. 2.1.2 The answer on the checklist trust match the action in the narrative (appendix A.2) and on Form I's. Do not use pencil to write the narrative. 2.1.3 This report is to be completed only when a serious contract violation is encountered, or upon the request of the Data Review Manager or Deputy Project Officer (DPQ). Forward 5 copies: one each for internal files, appropriate Regional DPO, Sanple Management Office (3-D) and last two addresses of Mailing List for Data Reviewers (Appendix A. 4). In other cases, all contract violations should be appended to end of Data Assessment Narrative (Sec. A. 2. 2). 2.1.4 Data 9urmarv 9ieet - amnarv of Inoreqrpr 'fHFJlitY Q**rol Data fAmmtix A.S). Enter in ink on Data Summary Sheet required QC values from Forms I through IX. Cin all values that require data qualification "Action". 2.1.5 CJf I^Tir* TSSStihMMlL SBBBrY 2.1.5.1 Appendix A. 6 Fill in the total number of analytes analyzed by different analyses and ^ the number of analytes rejected or flagged as estimated due to corresponding quality control criteria. Place an "X" in boxes where analyses were not performed, or criteria do not apply. 2.1.5.2 Anoerriix A. 7 Data reviewer is also required to fill out Inorganic Regional Data Assessment form (Appendix A. 7) provided by EPA Headquarters. Codes listed on the form will be used to describe the Data Assessment Summary. OPERATING WJL^JUHE Page 2 o: 35 Title: Evaluation of Inorganic Data for the Date: Feb. 19<?0 Contract Laboratory Program Number: K>;-2 Revision: 10 2.1-6 Data Review lag: It is reccmnended that each data reviewer should maintain a Ice cf reviews completed to include: a. date of start of case review b. date of completion of case review c. site d. case number e. contract laboratory f . number of samples g. matrix h. hours worked i. reviewer's initials 2.1.7 Telephone Record Loo - the data reviewer should enter the bare facts of inquiry, before initiating any phone conversation with CLP laboratory. After the case review has been completed, mail white copy of Telephone Record Log to the laboratory and pink copy to SMD. File yellow copy in the Telephone Record Log folder, and attach a xerox copy of the Telephone Record Log to the conpieted Data Assessment Narrative (Appendix A. 2) . 2.1.8 PYjruanjgrt Pfl ...1.8.1 Upon completion of review, the following are to be forwarded to the Regional Sarple Control Center (RSCC) located in the Surveillance and Monitoring Branch: a. data package b. completed data assessment checklist (Appendix A.I, original) c. S-O Contract Corpliance Screening (CCS) d. Data Summary Sheet (Appendix A. 5) along with completed Data Assessment Narrative (Appendix A. 2) e. Record of Communication (copy) f . CLP Reanalysis Request/Approval Record (original + 3 copies) g. Appendix A. 7 (original). ..1.8.2 Forward 4 copies of completed Data Assessment Narrative (Appendix A. 2) along with 2 copies of the Inorganic Data Assessment Form (Appendix A. 7) and Telephone Record Log , if any,: one each for appropriate Regional DFO, Sample Management Office (SMD) , and last two addressees of Mailing List for Data Reviewers (Appendix A. 4) (the Inorganic Data Assessment form does not go to the last two addressees) . OPERATING PRCCE3JRE Pace 3 c: 35 Title: Evaluation of Inorganic Data for the Date: Feb. 199-: Contract Laboratory Program Number: tt-:-2 Revision: 10 2.1.9 Filed Parfj-^rfr - upon completion of review, the following are to be filed within M-S files: a. Four copies of completed Data Assessment Narrative (Appendix A. 2) each carrying Appendix A. 7. b. Telephone Record Log (copy) c. S-D Report (copy Appendix A-3) d. CLP Data Assessment Summary Form (Appendix A.6). e. OP Reanalysis Request/Approval Record (copy) Indica-e incomplete data package on the computer tracking sheet located in M-2 office. Authorized contractor personnel may contact the laboratory after discovery of an inconpie: data package. If a laboratory will not return phone calls or does not respond to requests notify M-S coordinator of Region II for resolution. 4.0 Rejection of Data - All values determined to be unacceptable on the Inorganic Analysis Da- Sheet (Form I) must be lined over with a red pencil. As soon as any review criteria cause data to be rejected, that data can be eliminated from any further review or consideratio: 5.0 Acceptance Criteria - In order that reviews be consistent among reviewers, acceptance criteria as stated in Appendix A.I (pages 4-25) should be used. Additional guidance c be found in the National Inorganic Functional Guidelines of October 1, 1989. 6.0 fl^> QaTtract QniTPliflpce Screening (CCS) - This is intended to aid reviewer in locating a problems, both corrected and uncorrected. However, the validation should be carried o e/en if CCS is not present. Resutnu'ttals received from laboratory in response to CCS mu be used by the reviewer. 7.0 Poem****-, far fmnnlfnis ~ Data reviewers must note all items of contract non-compliance within Data Assessment Narrative. If holding times and sample storage tunes have not be exceeded, DPO may request reanalysis if items of non-compliance are critical to data asses srent- Requests are to be made on "CLP Re-Analysis Request/Approval Record". i I 8.0 Pflmrfl flf flrmtmjnicati°n ~ Provided by the Regional Sample Control Center (RSCC) to indicate which data packages have been received and are ready to be reviewed. I • o ftxiMJnq off yrirters - The data reviewer will follow the standard practice. TUT 002 QP2HAI21G o: 35 Title: Evaluation of Metals Data for the Contract Laboratory Program Appendix A.I: Data Assessment - Contract Compliance (Total Review - Inorganics) Date: Feb. 199: Number: ttv-2 Revision: 1C A. 1.1 (CCS) - Present? If no, contact RSCC. t_] A. 1.2 Pfft'i'Ji j p,f Cmuur''rrfTriari (film RSCC) - Present? ACTTCi:: if no, request from RSCC. A. 1.3 Trio Report - Present and complete? arnai: if no, contact RSCC for trip report. A. 1.4 I_1 Traffir P^rnFE - Present or on file? Legible? CTTa:: If no. request from Regional Sanple Control Center (RSCC). A. 1.5 Cover Paoe - Present? Is cover page properly filled in and signed by the lab manager or the manager's designee? Arrrcr:: if no, prepare Telephone Record Log, and contact laboratory. Do numbers of samples correspond to junbers on Record of Connunication? Do sample numbers on cover page agree with sample numbers on: (a) Traffic Report Sheet? (b) Fora I's? t if no for any of the above, contact RSCC for clarification. SIMEftPD OPERATING cm •. i rat- Pace 5 c: 25 Title: Evaluation of Metals Data for the Date: Feb. Contract Laboratory Program Number: Htc-2 Appendix A.I: Data Assessment - Contract Revision: 10 Compliance (Ibtal Review - Inorganics) NO r: ?, A.I.6 Form I (Final natal - Are all Form I's present and corplete? [\/_] _ _ __ ACTICN: if no, prepare telephone record log and contact laboratory for submittal. Are correct units (ug/1 for waters and mg/xg for soils) / indicated on Fora I's? [ V ] _ _ Are soil sarple results for each parameter corrected for / percent solids? [_] _ <X Are Z?A sanple # s and corresponding laboratory sanple ID * s the same as on the Cover Page, Form I's and / in the raw data? [ v ] __ _ Are computation/transcription errors less than 10* / of reported values? [ \X] _ _ Are all "less than IDL" values properly coded with "IT? [ \/\ __ _ was a brief physical description of sanples given on / Form I's? [ t/1 _ _ were the result qualifiers used correctly with final ./ data? [ V/l __ _ Acrid?; If no for any of the above, prepare Telephone Record Log, and contract laboratory for . corrected data. were any sanples diluted beyond requirements of contract? __ . C^X 1 _ If yes, were dilutions noted on Form I*s? [__] __ :£_ Acncu; If no, note under Contract-Problem/Non-Compliance of theTData Assessment Narrative". A.1.7 ffoiYtf in TJMBIS - (aqueous and soil samples ) (Examine sanple traffic reports and digestion/distillation logs.) Jtercury analysis (23 days). . . . . . . exceeded? ^ [_1, _ Cyanide distillation (14 days). . . . . exceeded? __ CF-3ATTC PROCEDURE C: 3s :le: Evaluation of Metals for the Contract Date: Feb. I9?o Laboratory Program Number: K-:-2~ Appendix A.l: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) Other Metals analysis (6 nonths). . . . exceeded? £2 D K __ [ y/l _ Prepare a list of all samples and analytes for which holding times have been exceeded. Specify the number of days from date of collection to the date of preparation (from raw data). Attach to checklist. If yes, reject (red-line) values less than Instrument. Detection Limit (IDL) and flag as estimated (J) the values above IDL even though sarrpie(s) was preserved properly. A.1.8 Raw Data A. 1.8.1 Digestion Log* for flame AVIC? (Form XIII) present? (V ] _ _ Digestion Log for furnace AA Fora XIII present? [ v ] _ . _ Distillation Log for mercury Form XIII present? [ v 1 _ _ _ Distillation Log for cyanides Form XIII present? [ i/l __ _ Are pH values (pH<2 for all metals, pH>12 for cyanide) s present in Digestion/Distillation Logs? [ v 1 _ __ •Weights, dilutions and volumes used to obtain values. Percent solids calculation present for soils/sediments? [_'J __ 5L. Are preparation dates present on Digestion Log? A.1.8.2 Measurement read out record present? ICP Flame AA [__] Furnace AA r i/l Marcury C v/1 Cyanides SDttCRSD GFE3&HXC TOGDCRZ Page 7 o: 35 Title: Evaluation of Metals Data for the Date: Feb. 19?-: Contract Laboratory Program Number: K\-i Appendix A.I: Data Assessment - Contract Revision: 10 Conpiiance (Total Review - Inorganics) - __ -~. A. 1.8.3 Are all rav data to support all sample analyses and / QC operations present? [ V/l _ Legible? • [ v/] __ Properly Labeled? [ N/l _ ACTTCNr if no for any of the above, write Telephone Record Log and contact laboratory. Flag metal data as estunated if pH of sample is greater tnan 2. Flag cyanide data as estimated if pH sanple is less than 12. A. 1.9 re»r* VaUrtation arri A. 1.9.1 rail Firm"* rn l. If less than 4 standards are measured in ab node, then the remaining standards in concentration mode must be run immediately after calibration and be within ±10% of true value. For all AA (except Hg) and Cyanide analyses, one calibration standard is at CRDL level. If not, write in the Q^tract-Problem/TJon-Campliance section of the "Data Assessment Narrative". A.l.9.1.1 Is record of at least 2 point calibration / present for 1C? analysis? [ v 1 __ _ Is record of 5 point calibration present for / Kg analysis? ... f V 1 __ _ Acnaj: if no for any of the above, write in the Contract Problem/Non-Con?liance section of the "Data Assessment Narrative". * 1.9.1.2 Is record of 4 point calibration present forr / Flame AA? [ _ ] _ _ V_ Furnace AA? f v 1 _ _ cyanides? 2 O2 8 OFESAI2C PPOdtSZ Page 8 o: 35 Title: Evaluation of Metals Data for the Date: Feb. 1990 Contract Laboratory Program Nursber: KX-2 Appendix A.l: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) 22 & EL*" ACTTJJ: Flag associated data as estiinated if standards are not within +10\ of true values (except CPDL calibration standard) . Do not flag the data as estiinated in linear range indicated by good recovery of standard. A. 1.9. 1.3 Is correlation "coefficient less than 0.995 for: Mercury Analysis? _ Cyanide Analysis? _ Atonic Absorption Analysis? V/ C: if yes. flag the associated data as estiinated. A. 1.9. 2 Form II A (Initial tft\ CHTffiSinn?3!? - The reviewer will calculate correlation coefficient. A. 1.9. 2.1 Present arv! conplete for every metal and cyanide? Present and conplete for AA and 1C? when both are / used for same analyte? [ __ 3 _ _ y arrrcNi if no for any. of the above, prepare Telephone Record Log and contact laboratory. A. 1.9. 2. 2 Circle all values on data suntary sheet that are outside contract windows. Are all calibration standards (initial and continuing) within "control limits? / Mstals 90-110\ [ \/ 1 __ __ Hg - 80-120* I VI __ __ Cyanides 85-115* QPESAI3G PHt'X rlTUPZ Page 9 ci 35 Title: Evaluation of Metals Data for the Date: Feb. 1990 Contract Laboratory Program Number: Kv-2 Appendix A.I: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) ILS Flag as estimated (J) all positive data (not flagged with a "IT*} analyzed between a calibration standard with %R between 75-89*. (65-79% for Hg; 70-84% for CN) or 111-125% (121-135% for Hg; 116-130% for CN) recovery and nearest good calibration standard. Qualify results <IDL as estimated (UJ). if the ICV or CCV %R is 75-89% (CN, 70-84% ; HG, 65-79%). Reject (red-line) as unacceptable data if recovery of the ICV or CCV is outside the range 75-125% (CN, 70-130%; Hg, 65-135%). Qualify five samples on either side of verification standard out of control limits. Was continuing calibration performed every 10 samples / or every 2 hours? [_J ^.. ACT7CK: If no, flag the excess samples (eleventh and up) data as estimated (J). was ICV for cyanides distilled? If no, write in the Contract-Problem/Nan-Compliance section of the "Data Assessment Narrative". A.1.9.3 Form II B fCRTTi fftfBT^yds for AA and A. 1.9.3.1 Was a CRDL standard (CRA) analyzed after initial calibration for all AA metals (except He)? *was a mid-range callb. verification standard distilled / and analyzed for cyanide analysis? f v 1 _ was a ZxCRDL ( or 2xIDL when IDLXKDL) analyzed (CRI) for each ICP run? (Note: CRI for AL,Ba,Ca,Fe,Mg,Na,or K is not required.) ACTTOM: if no for any of the above, flag as estimated all data falling within the affected ranges. The affected ranges are: __ AA Analysis - **True Value ± CRDL 1C? Analysis - **True Value ± 2CRDL CN Analysis - **True Value ± 0.5 x True Value. /ind the results of mid-range standard in the raw data. -True value of CHA, CRI or mid-range standard. 'Substitute IDL for CRDL when IDL > caoL. ru'i S3NSRD CE5RAI2G tWJQJLPZ Page 10 cf 35 Title: Evaluation of Metals Data for the Date: Feb. Contract Laboratory Program Number: KL-:-2 Appendix A.I: Data Assessment - Contract Revision: 10 Compliance (Ttotal Review - Inorganics) A. 1.9. 3. 2 Was CRI analysed after ICV/IC3 and before tne final / CCV/CC3, and for every four hours of 1C? run? [ y } _ _ Ad£LJ: If no, write in Contract Problem/Nan-Compliance Section of tne "Data Assessment Narrative". •..1.9.3.3 Circle all values on summary sheet that are outside acceptance windows. Are CRA and CRI standards within control limits: / Metals 80 - 120%R? ( _ ] v _ Is mid-ranae standard vithin control limits: / Cyanide 80 - 120%R? [ V 1 _ _ Flag as estimated all data within -the affected ranges if the recovery of the standard is between 50-79%; flag only positive data if the recovery is between 121-150*; reject (red line) all data if the recovery is less than 50\; reject only positive data if the recovery is greater than 150*. A.l.9.4 Form III flTU'fcial anrt A. 1.9.4.1 Present and ccctpiete? C v 1 _ __ For both AA and 1C? when both are used for same analyte? [__] __ v Was an initial calibration blank analyzed? [ v 1 __ _ Was a continuing calibration blank analyzed after every 10 samples or every 2 hours (whichever is more frequent)? If no, prepare Telephone Record Log, contact laboratory and write in the contract-problems/ rompliance section of the Data As Narrative. ;UT 002 2031 OPERATING PROCEDURE Pace 11 of 35 Title: Evaluation of Metals Data for the Date: Feb. Contract Laboratory Program Number: K-.--I Appendix A. l: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) YES NO r: V A. 1.9.4.2 Circle all calibration blank values on Data Surmiary Sheet that are above CRDL (or 2 x IDL when IDL > CRDL). Are all calibration blanks (when IDL<CRDL) less than or equal / to Contract Required Detection Limits (CRDL)? fv 1 _ _ Are all calibration blanks less than two times Instrument Detection Limit (when HL>CRDL)? [__3 __ If no for any of the above, flag as estimated (J) all positive data less than or equal to calibration blank values analyzed between calibration blank with value over CRDL (or 2xH3L) and nearest good calibration blank. Flag five samples on either side of the calibration blank. A. 1.9. 5 FCR*1 III (Note: Tne preparation blank for mercury is the same as the calibration blank.) A. 1.9.5.1 Was one prep, blank analyzed for: each 20 samples? [v 3 __ each batch? [>/l each matrix type? [__3 __ both AA and 1C? when both are used for same analyte? [__3 _ If no for any of the above, flag-as estimated (J) all associated positive data <10 x ULs for which prep, blank was not analyzed. M7TE: If only one blank was analyzed for more than 20 samples, then first 20 samples analyzed do not have to be flagged as estimated (J). A. 1.9.5.2 Is concentration of prep, blank greater than CRDL / when HTT. is less than or equal to CRDL? __ LkLJ —— If yes, is the concentration of the sample with the least concentrated analyte less than 10 times the prep, blank value? —— I——J SIWCP«RD GFSWITIG PRCGDURZ Title: Evaluation of Metals Data for the. Date: Feb. 199-:- Contract Laboratory Pimjiam Number: K-:-2 Appendix A. l: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) —————— ^ ^ ftCTiaj; If yes, reject^(red-line) all associated data greater than CRDL concentration but less than ten tines the prep, blank value found in the raw data. A.I.9.5.3 Do concentrarions of prep, blank fall belov two tunes / HL when ILL is greater than CRDL? [_] _ V If no, reject (red-line) all positive data that has a concentration less than 10 times the prep, blank value in the raw data. A.l.9.5.4 Is concentration of prep, blank below the negative CRDL? If yes, reject (red-line) all associateddata that has a concentration less than lOxCRDL. __ [}/.] _ A.1.9.6 Fonn IV (1CP Interference* 1.9.6.1 Present and complete? t v\ _. _ CNCTE: Not required for furnace AA, flame AA, mercury, cyanide and Ca, Mg, -K and Na.) Was ICS analyzed at beginning and end of run / (or at least twice every 8 hours)? [^ 1 __ _ ATTTCM-. if no, flag as estimated (J) all sanples for wnich AL, Ca, Fe, or Mq is higher than in ICS. A.l.8.6.2 Circle all values on Data Surcmary Sheet that are more than i- 20\ of true or established mean value. Are all Interference Cneclc Sanple results inside of control / limits (+ 20*)? C.y_J —— — ** •• If no. is concentration of Al, Ca. Fe. or Mg lower ' / than in ICS? I__1 —— ^^ ACTTOM; if no. flag as estimated (J) those positive results for which ICS recovery is between 121-150*; flag all sample results as estimated if ICS recovery falls within 50-79V reject (red-line) those sample results for which ICS recovery is less than 50*; if ICS recovery is above 150*, reject positive results only (not flagged with a "U"). TUT ur&r&ZZTJ PROCSHJrZ Pace 13 o: 35 Title: Evaluation of Metals Data for the Date: Feb. l?9v Contract Laboratory Program Nirtoer: K%-2 Appendix A. l: Data Assessment - Contract Revision: 10 Compliance (Total Review - inorganics) C t: A.l.9.7 FQrm V A (SpiVort JtonpT^ Pomuerv - Pre-Pio^StJ.Qn/Pre-Pigcillat'ifTT)- ( Note: Not required for Ca. MS, K, aod Na (both matrices), Al, and Fe (soil only.) '•..1.9.7.1 Present and complete for: each 20 samples? _ __ _ each matrix type? [__] __ _ %/ each cone, range (i.e. low, med., high)? [__] __ _ For both AA and 1C? when both are used for same analyte? If no for any of the above, flag as estimated (J) all positive data less than four times spiking level for which spiked sample was not analyzed. If one spiked sample was analyzed for more than 20 samples, then first 20 samples analyzed do not have to be flagged as estimated (J). A.l.9.7.2 was field blank used for spiked sample? Amg:: If yes, flag all positive data less than 4 x spike added as estimated (J) for which field blank was used as spiked sample. MOT-:.' Matrix spike analysis should be performed on a field blank when it is the only aqueous sample in SDG. A.l.9.7.3 Circle all values on Data Summary S^eet that are outside control limits (7S\ to 125\). Are all recoveries / within control limits? [_1 Y- — If no, is sample concentration greater than or equal / to four times spike concentration? [__1 ^£_ — If yes, disregard spike recoveries for analytes whose concentrations are greater than or equal to four tines spike added. If no, circle those analytes on Form V for which sample concentration is less than four times the spike concentration. TUT OO2 2O34 GFERAI2C PRQGDU?£ Page 14 o: 2s Title: Evaluation of Metals Data for the Date: Fes. 19?" Contract Laboratory Program Nisrtser: HI-;- 2 Appendix A.I: Data Assessnent - Contract Revision: 10 Conpiiance (Total Review - Inorganics) ffi Are results outside the control lifluts (75-125*.) / flagged with "N" on Form I's and Form VA? [>/ 1 _ _ aCHflL?: If no, write in the contract - Problem/Non - Conpliance section of "Data Assessment Narrative". A.I. 9. 7. 4 Aaugou^ Are any spike recoveries: / (a) less than 30%? £_ {_ J _ {b) between 30-74%? V [ _ ] _ (c) between 126-150%? __ [J/] _ (d) greater than 150%? _ If less than 30%, reject all associated aqueous data; if between 30-74%, flag all associated aqueous data as estimated ( J) ; if between 126-150%, flag as estimated (J) all associated aqueous data not flagged with a "IT ; if greater than 150%, reject (red-line) all associated aqueous data not flagged with a "IT. If pre-digestion spike result is rejectable due to coefficient of correlation of MSI, analytical spike recovery, or duplicate injections criteria, disregard spike recovery on Form V. Flag the associated data as estunated( J) . Are any spike recoveries: _ ^ / -..1.9.7.5 Soil/Sediment: recov (a) less than 10%? __ [_] (b) between 10-74%? __ [_1 (c) between 126-200%? __ [__1 X— (d) greater than 200%? __ I—1 . if less than 10%, reject all associated data; if between 10-74V flag all associated data as estimated; if between 126-200%, flag as estimated all associated data was not flagged with a TJ"; if greater than 200%, reject all associated data not flagged with a "U". iSATZC PSDCZ7.7£ Pass 15 c: 3: '.tie: Evaluation of Metals Data for the Date: Feb. is?; Contract Laboratory Projiam Number: Kw-2 Appendix A.I: Data Assessment - Contract Revision: 10 Compliance (Total Review - inorganics) _ _ _ „ _ — — -1.9.8 form VI wl.9.8.1 Present and ccrplete for: each 20 samples? each matrix type? [__] _ v each concentration range (i.e. low, med., high)? (__] both AA and 1C? when both are used for same analyte? [__] If no for any the above, flag as estimated (J) all data X3DL* for which duplicate sanple was not analyzed. 1. If one duplicate sanple was analyzed for more than 20 sanples, then first 20 sanples do not have to be flagged as estimated. 2. If percent solids for soil sample and its duplicate differ by more than 1\, prepare a Form VI for each duplicate pair, report concentrations in Hg/L on wet weight basis and calculate RPD or Difference for each analyte. A.l.9.8.2 Was field blank used for duplicate analysis? __ l.v/1 _ If yes, flag all data X3DL* as estimated (J) for which field blank was used as duplicate. Duplicate analysis should be performed on a field blank when it is the only aqueous sanple in SDG. A. 1.9.8.3 Are all values within control limits (RPD. 20\ or / difference < +CRDL)? t-fcLl .— — If no. are all results outside the control limits s flagged with an * on Form I's and VI? t_1 . _ ^L If no, write in the Contract - Problems/Non- Conpliance section of "Data Assessment Narrative". i. KPD is not calculable for an analyte of the sample - duplicate pair when both values are less than IDL. Substitute IDL for CSDL when IDL > CRDL. i . S1WCRSD Ufi^AlIfC PROCEDURE Page 16 c: 35 Title: Evaluation of Metals Data for the Date: Feb. l??j Contract Laboratory Program Nurnser: K-.-2 Appendix A.I: Data Assessment - Contract Revision: 10 Coipiiance ("Total Review - Inorganics) A. 1.9. 8. 6 Soil/Sediment Circle ail values on Data Sunroary Sheet that are: RH> > 100\, or Difference > 2 x CRDL* Is any RPD (where sanple and duplicate are both greater than or equal to 5 tines -CREL) : > ioo\? > 2X-CKDL? * Substitute IDL for CRDL when HL > CRDL. •« Use absolute values of sanple and duplicate to calculate the difference. TUT 2. If lab duplicate result is rejectable due to coefficient of correlation of MSA, analytical spike recovery, or duplicate injections criteria, do not apply precision criteria. 1.9.8.4 Is any value for sanple duplicate pair less thanCRDL* and other value greater than or equal to 10 x *CRDL? __ Acndh If yes, flag the associated data as estimated (J). A.l.9.8.5 Aeneous Circle all values or. Data Sjnnary Sheet that are: RPD > 50V or Difference > ± CRDL* Is any RPD greater than 50% where sanple and duplicate / YJ _. are both greater than or equal to 5 tines *CRDL? _ t Is arrjJ**difference between sanple and duplicate greater than *C3DL where sanple and/or duplicate is less than / 5 fjnes *CRDL? _ [j/J If yes. flag the associated data as estimated. Is any "difference between sarple and duplicate (where sanple and/or duplicate is less than 5x*CRDL) : __ I __ 1 2£- GF3JA73C PSCCZSUSi Page 17 01 35 Title: Evaluation of Metals Data for the Date: Fes. :«?: Contract Laboratory Program Number: K<-2 Appendix A.l: Data Assessment - Contract Revision: 10 . Compliance (Total Review - Inorganics) If yes, flag the associated data as estimated. A.I. 9. 9 Fi»"l«1 v/ A. 1.9. 9.1 were field duplicates analyzed? [v1 If yes, prepare a Form VI for each aqueous field duplicate pair. Prepare a Form VI for each soil duplicate pair, if percent solids for sanple and its duplicate differ by more than 1%; report concentrations of soils in ug/1 on wet weight basis and calculate RPDs or Difference for each analyte. 1. Do not calculate RFD when both values are less than IDL. 2. Flag all associated data only for field duplicate pair. A. 1.9. 9. 2 Is any value for sanple duplicate pair less than*CRDL / and other value greater than or equal to 10 x *CRDL? . _ l.jj . _ AcnaJ: if yes, flag the associated data as estimated. A.l.9.9.3 Circle all values on Form VI for field duplicates that are: RPD > SOVpr Difference > ± CRDL* Is any RPD greater than 50\ where sanple and duplicate / are both greater than or equal to 5 tijnes *CRDL? Y [__ J Is any "difference between sanple and duplicate greater than *CRDL where sanple and/or duplicate is less than / 5 times *CRDL? Z- I— J arncN; if yes, flag the associated data as estimated. * substitute IDL for CRDL when HZ. > CRDL. ** Use absolute values of sample and duplicate to calculate the difference. .• •,.-•, - .- O •_'.' *•••• TU'T QFSAT2C PRCC^?£ Page IS o: 35 Title: Evaluation of Metals Data for the Date: Feb. 19?:= Contract Laboratory Program Nuttjer: HX-Z Appendix A.I: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) A.I. 9. 9.4 Circle all values on Fora VI for field duplicates that are: RPD >100\, or Difference > 2 x CSDL* Is any RPD (where sanple and duplicate are both greater than 5 tines *CRDL) : / >100V _ [_ ] V Is any **difference between sanple and duplicate __ (vnere sanple and/or duplicate is less than 5x *ODL ): >2x *CRDL? _ [_ J V ACncr:: If yes, flag the associated data as. estimated. A.I. 9. 10 Form YTT flfti r>f Ht^TY ^^TltTPl ^»»^>T^) (Note: LCS - not repaired for aqueous Hg and cyanide analyses.) A. 1.9. 10.1 Was one LCS prepared and analyzed for: / every 20 water sanples? [ V ] _ , _ . every 20* solid sanples? t _ ] _ . \/_ both AA and 1C? when both are used for same analyte? [ __ ] _ _ \X Arngj; if no for any of the above, prepare Telephone Record Log and contact laboratory for sutmttal of results of LCS. Flag as estunated (J) all data for which LCS was not analyzed. NOTE: if only one LCS was analyzed for more than 20 sanples, then first 20 samples close to LCS do not have to be flagged as estimated. * Substitute 3£L for CRDL when HL > CRDL. **Use absolute values of sanple and duplicate to calculate the difference. "fu r 002 20:'',•-? QFERA23C PROCSUSE Page 19 QJ 35 Title: Evaluation of Metals Data for the Contract Laboratory Program Appendix X.I: Data Assessment - Contract Ccnpiiance (Total Review - Inorganics) Date: Feb. I9?c Number: H*-2 Revision: 10 A.l.9.10.2 A.l.9.10.3 Circle all LCS values outside control limits (80 - 120%- except aqueous Ag and Sb). Is any LCS recovery: less than 50%? _ between 50% and 79%? __ between 121% and 150%? _ greater than 150%? _ Less than 50%, reject (red-line) all data; between 50% and 79%, flag all associated data as estijnated (J); between 121% and 150%, flag all positive (not flagged with a "U") results as estimated; greater than 150%, reject all .positive results. 1. If Toind" value of LCS is rejectable due to duplicate injections or analytical spixe recovery criteria, regardless of LCS recovery, flag the associated data as estimated (J). 2. If IDL of ah analyte is equal to or greater than true value of LCS, disregard the "Action" below even though LCS is out of control limits. Is LCS Tound" value higher than the control limits on Form VII? __ If yes, qualify all associated positive data as estimated. Is LCS Tound" value lower than the Control limits on Form VII? if yes, qualify all associated data as estimated. __ [_ J 2040 SIWCftRD OP5WTZC FRQGiIX/B£ Page 20 01 35 Title: Evaluation of Metals Data for the Date: Feb. 199! Contract Latoratory Program Number: W<-Z Appendix A.I: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) A.I.9.11 Form IX f|rp serial Dilution) - Serial dilution analysis is required only for initial concentrations equal to or greater than 10 x EL. A. 1.9.11.1 Was Serial Dilution analysis performed for: / each 20 samples? [v 1 __ each matrix type? [__] __ each concentration range (i.e. low, med.)? t_] __ Arrrcr:: if no for any of the above, flag all positive data greater than or equal to lOxIDLs as estimated (J) for which Serial Dilution Analysis was not performed, and summarize the deficiency on the DPO report. * A. 1.9.11.2 was field blank(s) used for Serial Dilution Analysis? [V ] If yes, flag all associated data 2 10 x HZ. as estimated (J). Serial dilution analysis should be performed on a field blank when it is the only aqueous sanple in SDG. A.I.9.11.3 Are results outside control limit flagged with an T" on Form I »s and Form DC when initial concentration on Form IX is equal to 50 times HZ. or greater. If no. write in the contract-problenv/non- compliance section of the "Data Assessment Narrative11. A.l.9.11.4 Circle all values on Data Sumnary Sheet that are outside control limit for initial concentrations equal to or greater than 10 x TTT.e only. Are any % difference values: > 10\? ,_,'_ J. 100\? __ [>/J — "!"UT (JO 2 2O 4.1 OFEPA72C FWJLLJURZ Page 21 cf 35 Title: Evaluation of Metals Data for the Date: ret. 19?:- Contract Laboratory Program Number: K-.-2 Appendix A.I: Data Assessment - Contract Revision: 10 Corpiiance (Total Review - Inorganics) Flag as estimated (J) all associated equal to or greater than lOxULs for which percent difference is greater tnan 10% but less than 100V Reject (red-line) all associated sanple results equal to or greater tnan IQxTTT.s for which PD is greater than or equal to 100%. A. 1.9. 12 TVmu*'** ^^'TflJC' AfKOrhfiJan (AA) QC A. 1.9. 12.1 Are duplicate injections present in furnace raw data (except during full Method of Standard Addition) for / each sarple analyzed by GFAA? t^Lj if no, reject the data on Form I's for which duplicate injections were not performed. A.l.9.12.2 Do the duplicate injection readings agree within 20% Relative Standard Deviation (RSD) or Coefficient of Variation (CV) for concentration greater than CRDL? Was a dilution analyzed for sanple with post digestion / spike recovery less than 40\? [_] _ _ 2L. AcncrJ: If no for any of the above, flag all the associated data as estimated (J). A. 1.9.12.3 Is *post digestion spike recovery less than 10% or greater than 150% for any result? AcncM: if yes. reject (red-line) the affected data if recovery is <10\; reject data not flagged with "IT if spike recovery is >150\. NOTE: Reject the data only if the affected sanple was. not subsequently analyzed by Method of Standard Addition. * Post digestion spike is not required on the pre-digestion spiked sanple when predigest ssike recovery is within control limits of 75-125% or when SR>4xSA. Tln 002 2042 PROCIDUSi Page 22 o: 3 Title: Evaluation of Metals Data for the Date: Feb. l?9 Contract Laboratory Program Naaoer: K.-:-2 Appendix A.l: Data Assessment - Contract Revision: 10 Gonpiiance (Total Review - Inorganics) -9 -13 Ftonn VTTT (Metfrnrt pf fiftarrtarrt IV^ficri Spa » A.I. 9. 13.1 Present? [V } __ _ If no, is any Fora I result coded with "S" or a "«•"? _ [__ J \/ ACTia;:: if yes, write request on Telephone Record Log and con tact laboratory for submittal of Form VIII. A. 1.9. 13. 2 Is coefficient of correlation for MS>i less than 0.990 for / any sarple? _ [_ J ^/ ACTTO;-:: if yes, reject (red-line) affected data. A.I. 9. 13. 3 Was *KSA required for any sanple but not performed? _ [_yf } _ Is coefficient of correlation for MSA less than 0.995? _ [_ J \{_ Are KS^ calculations outside the linear range of the calibration curve generated at the beginning of the , analytical run? _ t_ J v Ama:: If yes for any of the above, flag all the associated data as estimated (J). A. 1.9. 13. 4 Was proper quantitation procedure followed correctly / as. outlined in the SOW on page E-16 through E-17? [ _ ] __ ^_ ATTTQ:: if no, note exception under contract problenv/ non-corrpliance of data assessment narrative, or prepare a separate list. A 1 9.14 T?1S!SO A.l.9.14.1 Were any analyses performed for dissolved as well as total analytes on the same sample(s). __ were any analyses performed for inorganic as well as total / (organic * inorganic) analytes on the same sample(s)? __ ljj/1 —— * MSA is not required on LCS and prep, blank. oO*V3 OP3BC3C FROCSjfJrZ Title: Evaluation of Metals Data for the Date: Feb. l?5v Contract Laboratory Program Nunber: K-:-2 Appendix A.I: Data Assessnent - contract Revision: 10 Compliance (Total Review - Inorganics) If more than 10%. flag both dissolved (or inorganic) and total values as estunated (J) ; if more than 50\, reject (red-line) the data for both values. A.l.9.15 Form 7 to IX A.I. 9. 15.1 Are all the Form I through Form DC labeled with: Laboratory name? [ v*- v// Cas«/»S number? Ufc sample No.? SOS NO.? Contract No.? [ Correct units? [ */] Matrix? t y^l 1. If yes, prepare a list comparing differences between all dissolved (or inorganic) and total analytes. Compute the differences as a percent of the total analyte only when dissolved concentration is greater than C3DL as well as total concentration. 2. Apply the following questions only if in- organic (or dissolved ) results are (i) above CRDL, and (ii) greater than total constituents. 3. At least one preparation blank, ICS, and LCS should be analyzed in each analytical run. A.l.9.14.2 Is the concentration of any dissolved (or inorganic) analyte greater than its total concentration by / more than 10%? _. (_ _] .V. A. 1.9.14.3 Is the concentration of any dissolved (or inorganic) . analyte greater than its total concentration by / more than 50\? _ [. _] v ^ I" i If no for any of the above, note under contract problem/non-compliance section of the "Data Assessment Narrative". O02 2O44 GFESnlEC PROCEDURE Page 24 c: 35 Title: Evaluation of Metals Data for the Date: Feb. 19?C- Contract Laboratory Program Nunber: H-J-2 Appendix A.. 1: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) A. 1.9.15.2 Do any corputation/transcription errors exceed 10\ of reported values on Forms I-DC for: (NCflZ: Check all forms against raw data.) (a) all analytes analyzed by ICP? __ [ V] _ (b) all analytes analyzed by GFAA? __ t^O _ (c) all analytes analyzed by AA Flame? __ [__] \/ (d) Mercury? __ [j/] _ (e) Cyanide? __ [_\/l _. Amct': If yes, prepare Telephone Log, contact laboratory for corrected data and correct errors with red pencil and initial. A.l.9.16 Form I (Field Rlarflrl - Circle all field blank values on Data Summary Sheet that are greater than CRDL, 2 x IDL when IDL > CRDL. Do concentrations of field blank(s) fall below CRDL (or 2 x IDL when IDL > CRDL) for all parameters of associated aqueous and soil samples? _ [__1 If no, was field blank value already rejected due to other QC criteria? t__1 _ if no, reject (except field blank results) all associated positive sample data less than or equal to five times the field blank value. TUT 2045 OPERATING PWJLiJjR£ Pace 25 Cf 35 Title: E'.'aluation of Metals Data for the Date: Feb. i99: Contract Laboratory Program Number: K-:-2 Appendix A.I: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) ——— yyg jjj A. 1 . 9 . 17 Ftann X. "XL . 3CTT (Verification of Instrmmna-l Pai A. 1.9. 17.1 Is verification report present for: Instrument Detection Limits (quarterly)? tJL_] ICP Interelement Correction Factors (annually)? l^_J ICP Linear Ranges (quarterly)? [\/ ] if no, contact DPO of the lab. A. 1.9. 17. 2 Form X (Instjrumeng Dgtecrion Limi^s) - (Note: ITL is not required for Cyanide. ) Are IDLs present for: all the analytes? all the instruments used? For both AA and 1C? when both are used for same analyte? Amcrj: if no for any of the above, prepare Telephone Record Log and contact laboratory. Is IDL greater than CRDL for any analyte? _ Ij^T ] — If yes, is the concentration on Form I of the sample . analyzed on the instrument whose IDL exceeds CRDL, / greater than 5 x IDL? t —— 1 — ^-~ if no, flag as estimated all values less than five tiines IDL of the instrument whose IDL exceeds CRDL. OO2 2O46 SDMEPJO (JfirlAiHC PPCGZXPZ Page 26 of 3: Title: Evaluation of Metals Data for tne Date: Feb. 1990 Contract Laboratory Pi LSI am Niatoer: B->2 Appendix A.l: Data Assessment - Contract Revision: 10 Conpiiance (Total Review - Inorganics) 225 tjj K V A.I.9.17.3 Form XI fT i if yes. qualify as estimated all data not previously rejected or flagged due to other QC criteria. Was any sanple result higher than high linear range of ICP. __ [ was any sanple result higher than the highest / caliJoration standard for non-ICP parameters? __ [.V ] If yes for any of the above, was the sanple diluted to obtain the result on Form I? [_.] _ . ftCTTJ-i: if no, flag the result reported on Form I as estimated (J). A. 1.9.18 Percent J^iiirtc nf Is soil eonLe-it in sediment(s) less than 50%? _ [ _ ] .V U.S. EPA - CLP DUPLICATES Lab Name: MIC. Lab Code: C-CtMic. Case No.: Matrix (soil/water): _ * Solids for Sample: £> Contract: EPA SAMPLE NO. 0073 / T,I (-LET SAS No.: SDG No. : Level (low/med) : \ Solids for Duplicate: O > 0 Concentration Units (ug/L or mg/kg dry weight): IIAnalyte |Aluminum^ I Antimony_ IArsenic ~ I Barium^_ j Beryllium ICadmium_ ICalcium_ j Chromium I Cobalt_; I Copper_ IIron___ I Lead IMagnesium j Manganese IMercury INicJcel^_ I Potassium j S«lenium_ I Silver__ j Sodium j Thallium_ IVanadium I Zinc___~ I Cyanide_ Control Limit Sample Q M FORM VI - IN 7/88 STANDARD OPERATING PROCEDURE MERCURY HOLDING TIMES EXCEEDED DATE DATE # DAYS SAMPLE LABI.D. SAMPLE COLLECTED SAMPLE ANALYZED EXCEEDED VfflAI 770-14 9-27-90 11-5-90 11 LaPlace 770-07 10-2-90 10-31-90 EglinI 770-06 10-2-90 10-31-90 Tillet 770-08 10-2-90 10-31-90 Tillet D 770-08 10-2-90 10-31-90 Dimitri 770-01 10-1-90 10-31-90 Bryan 770-09 10-1-90 10-31-90 Matthias 770-03 10-1-90 10-31-90 Ramsey 770-04 10-1-90 10-31-90 GERAGHTY & MILLER. INC. STANDARD OPERATING PROCEDURE Page / of f Title: Evaluation of Metals Data for the Date: Feb. 1990 Contract Laboratory Program Number: HW-2 Appendix A. 1: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) Case# 900770 Site Tutu Well Site Matrix: Soil SDG# VfflAI Lab Ceimic Water Contractor Geraghty & Miller Reviewer Donna Lesch Other A.2.1 The case description and exceptions, if any, are noted below with reason(s) for rejection or qualification as estimated values(s) J. This data package includes the analysis of the samples for SDG VTHA I. These_____ samples originated from St. Thomas on the 27th of September and the 1, 2, and 3_______ of October 1990.______________________________________ Samples VIHA I. LaPlace, Eglin I, Tillet. Tillet(D), Dimitri, Bryan, Matthias, and Ramsey were analyzed beyond the holding time for Mercury. All non-detects_____ (values less than the Instrument Detection Limit) are rejected and a red line is________ drawn through the data. The Mercury concentration value for LaPlace, the only_____ positive hit, is qualified with a "J".________________________________ The metal logbook indicates that samples Dimitri and Tillet were_____________ preserved at a pH of 5. Samples correctly preserved for metals and Mercury analyses should have a pH of 2 or less. All data for these two samples are qualified with________ "J" (except Mercury and Cyanide). The Mercury values in the affected samples____ remain qualified with "R". GERAGHTY & MILLER, INC. STANDARD OPERATING PROCEDURE Page Z of 5" Title: Evaluation of Metals Data for the Date: Feb. 1990 Contract Laboratory Program Number: HW-2 Appendix A. 1: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) A. 2.1 (continuation) The calibration correlation coefficient is less than 0.995 for the atomic______ absorption analysis of Arsenic (0.99219). The affected samples are Bryan,_______ Dimitri, Matthais, and Ramsey. The Arsenic concentration values for these_____ samples are qualified with "J".____________________________ The correlation coefficient is less than 0.995 for the atomic absorption_______ analysis of Thallium (0.98954). The affected samples are Matthias, Ramsey, LaPlace, Tillet, Tillet(D), and H2O blk Tutu. The Thallium concentration______ values for these samples are qualified with "UJ"._____________________ The Selenium analysis run on 10/29/90 at 16:48 contained 11 samples between the ICV and the CCV. The allowable number is 10 samples. The eleventh sample is not included in SDG VIHA I therefore no qualifiers are necessary._________ The CRDL standards are out of control limits (80-120% Recovery) for several metals and in several analyses. The CRI run on 10/17/90 has the following_____ deficiencies:_____________________________________ _______Metals__________%R____________________ _______Cadmium_________150____________________ _______Copper__________136____________________ _______Nickel__________121____________________________ Zinc 128 GERAGHTY & MILLER, INC. STANDARD OPERATING PROCEDURE Page 3 of 5" Title: Evaluation of Metals Data for the Contract Laboratory Program Appendix A. 1 : Data Assessment - Contract Compliance (Total Review - Inorganics) Date: Number: Revision: Feb. 1990 HW-2 10 A.2.1 (continuation) The CRA run on 10/31/90 has a 45% recovery for Mercury. The samples Bryan, Dimitri, Matthias, Ramsey. Eglin I, LaPlace, Tillet, Tillet(D), H20________ blk Tutu, and Hartman I are associated with the above deficiencies.____________ Positive hits for the listed metals are qualified "J" in the affected samples._______ The mercury concentration values are qualified "R" for all affected samples______ because the recovery is below 50%.________________________________ The CRI run on 11/01 has the following deficiencies:________________ _______Metal__________%R____________________ ________Antimony_________71.7_____________________ _______Cadmium________130.0____________________ _________Silver____________140.0____________________________________ The CRA run on 11/05 has a 50% recovery for Mercury. VIHA I is the only sample associated with the above deficiencies. The positive hits for the______ listed metals are qualified "J". The Mercury value has previously been_________ qualified "R"._________________________________________________________ The CRA run on 10/20 has a 133% recovery for Selenium. Samples Bryan,___ Dimitri. DimitriD, DimitriS, Matthias, and Ramsey are associated with this CRA analysis. The positive hits for Selenium are qualified with "J" for the samples. GERAGHTY & MILLER, INC. STANDARD OPERATING PROCEDURE Page V of S Tide: Evaluation of Metals Data for the Date: Feb. 1990 Contract Laboratory Program Number: HW-2 Appendix A. 1: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) A. 2.1 (continuation) The CRA run on 10/25 has a 125% recovery for Thallium. The samples Matthias. Ramsey. Eglin I. LaPlace. Tillet, Tillet(D), and the H2O blk Tutu are_______ associated with this deficiency. There are no positive hits, therefore no________ qualifiers are necessary. However. Thallium has previously been qualified________ "UJ" for these samples.________________________________ The Iron concentration value in the field duplicate has a RPD that________________ is greater than 50% where sample and duplicate are both greater than 5___________ times the CRDL. As a result, Iron values are qualified as estimated ("J")__________ in all samples. The Lead concentration values are less than 5 times the______ CRDL in both the sample and duplicate and the difference is greater than the___ CRDL, therefore all Lead values are qualified as estimated ("J") in all samples. Sample Dimitri was used for the matrix spike analysis. Selenium (36%) and_____ Thallium (25%) have % recoveries out of QC limits (75-125%). All Selenium results are qualified "UJ" for non-detects and "J" for positive hits. All___________ Thallium results are qualified "R", which supercedes previous qualifiers._________ In the ICP Serial Dilution, the initial concentration of Vanadium is greater______ than 10 times the IDL and the % difference is out of QC units. As a result._____ all Vanadium concentration values are qaulified with "J".______________ GERAGHTY & MILLER, INC. TUT 002 2053 STANDARD OPERATING PROCEDURE Page >5"bf 5" Title: Evaluation of Metals Data for the Date: Feb. 1990 Contract Laboratory Program Number: HW-2 Appendix A. 1: Data Assessment - Contract Revision: 10 Compliance (Total Review - Inorganics) A.2.2 Contract Problems/Non Compliance The holding time for Mercury analysis was exceeded for nine samples.______ Samples Dimitri and Tillet were not correctly preserved._____________ The correlation coefficients were out of QC limits for Arsenic and Thallium analyses._______________________________________ The Selenium analysis had eleven samples betwen the ICV and CCV, one sample over the QC limit. MMB Reviewer: ______________________ Date: Signature Contractor Reviewer: //^n^ /fa- <L* ____ Date: <y/>7/9/ Signature Verified by: f^tL/^a ^.AjtA*di^^*ruZLuj) Date: ^ ^ ^ - — n m m r r r y in ^ TUT OO2 2054 GERAGHTY & MILLER, INC. OP5WCTN3 PROCSXSE Page 30 o: 35 Title: Evaluation of Metals Data for the Date: Feb. ir-: Contract Laboratory Program Number: K.-.'-Z Appendix A.2: Data Assessnent Narrative Revision: 10 A. 2.2 Cantract-Problens/Non-Ccrrpliance Reviewer:____________________________ Bat* Signature /"I A A .Contractor Reviewer; l/^tn^A^u^/M-/^/^^^____________. Date:. 0/, Signature ro Verified b v : ^ _ V J ' 'UT 002 20513 Page/of 9 Table 1. Tutu Residential Wells Sampling Results, September 1990, Sample Delivery Group 900770 Sample Identification: •tile Organic Compounds (VOCs) Chlororaethane Bromomethane Vmyl Chloride Chloroethane Methylene Chloride Acetone Carbon Disulfide 1 , 1 -Dichloroethene 1 , J-Dichlorocthane 1 ,2-Dichlorocthenc (total) Chloroform 1,2-Dichloroethane 2-Butanone 1,1,1 -Trichloroetbane Carbon Tetrachloride Vinyl Acetate Bromodichloromethane 1 ,2-Dichloropropane cis-1 ,3-Dichloropropene Trichloroethene Dibromochloromethane ' 1 ,2-Trichloroethane _^ozene trans-1 ,3-Dichloropropene Bromoforra 4-Methyl-2-Pentanone 2-Hexanone Tetrachloroethene 1 , 1 ,2,2-Tetrachloroethane Toluene Chlorobenzene Ethylbenzene Styrene Total Xylenes Tentatively Identified VOCs Ethane, 1 , 1 ,2-Trichloro-l ,2,2 trifluoro Unknown Propane,2-Methoxy-2-methyl C5H12 isomer Aliphatic hydrocarbon C3-Benzene isomer C6H12 isomer C9H12 isomer 770-01 Bryan 2U 2U 2U 2U 2UJ R 1 UJ 1 UJ 1 U 1 U 1 U IUJ R 1 U 1 U 2UJ 1 U 1 U 1 U 1 U 1 U 1 U 1 U 1U 1 U 2UJ R 1 UJ 1 UJ 1 U 1 U 1 U 1 U 1 U 770-02 Diraitri 2UJ 2UJ 2UJ 2UJ 2UJ R IUJ IUJ IUJ 1 UJ IUJ IUJ R IUJ 1 UJ 2UJ 1 UJ IUJ IUJ IUJ IUJ 1 UJ 1 UJ R IUJ 2UJ R 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ IUJ 1 UJ 770-03 Matthias 2UJ 2UJ 2UJ 2UJ 9UJ R IUJ IUJ 1U 22 I U J IUJ R 1 UJ 1 U 2UJ 1 U 1 U 1 UJ 11 1 U 1 U 1 U I UJ 1 U 2UJ R 120 J 1 UJ 1 U 1 U 1 U 1 UJ 1 UJ 16 JN 770-04 Rarasey 4UJ 4UJ 4UJ 4UJ 17 UJ R 2UJ 2UJ 2UJ 2UJ 2UJ 2UJ R 2UJ 2UJ 2UJ 2UJ 2UJ 2UJ 2UJ 2UJ 2UJ 2UJ 2UJ 2UJ 4UJ R 3J 2UJ 2UJ 2UJ 2UJ 2UJ 2UJ 2JN 770-05 10/01 Trip Blank 2UJ 2UJ 2UJ 2UJ 13 J 6J IUJ 1 UJ 1 UJ 1 UJ 1 UJ IUJ R 1 UJ 1 UJ 2UJ 1 UJ I U J 1 UJ 1 UJ IUJ IUJ IUJ R 1 UJ 2UJ R 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ IUJ 1 UJ 1 JN 770-06 EglinI R R R R R R R R R 68 J R R R R R R R R R 10 J R R R R R R R 32 J R R R R R R 3JN 6JN All concentrations are reported in micrograms per liter (ug/L). Value is estimated. •w^ U - Compound is not detected. R - Value is rejected. N - Compound is a tentatively identified compound. GERAGHTY & MILLER. INC. Page2of*| Table 1. Tutu Residential Wells Sampling Results, September 1990, Sample Delivery Group 900770 Sample Identification: latile Organic Compounds (VOCs) Chloromethane Bromometbane Vinyl Chloride Chloroetbane Methylene Chloride Acetone Carbon Disulfide 1 , f-Dichloroctheoe 1 , 1 -Dichloroethane 1 ,2-Dichloroethene (total) Chloroform 1 ,2-Dichloroethane 2-Butanone 1,1,1 -Trichloroethane Carbon Tetrachloridc Vinyl Acetate Bromodichloromethane 1 ,2-Dichloropropane cis- 1 ,3-Dichloropropcnc Trichloroethene ""'bromochloromethane ^__^i ,2-Trichloroethane Benzene trans- 1 ,3-Dichloropropene Broraoform 4-Methyl-2-Pentanone 2-Hexanone Tetrachloroethene 1 , 1 ,2,2-Tetrachloroethane Toluene Chlorobenzene Ethylbenzene Styrenc Total Xylenes Tentatively Identified VOCs Ethane, 1 , 1 ,2-Trichloro- 1 ,2,2-trifluoro Unknown Propane,2-Methoxy-2-methyl C5H12 isomer Aliphatic hydrocarbon C3-Benzene isomer C6H12 isomer C9H12 isomer 770-07 LaPlace R R R R R R R R R 140 J R R R R R R R R R 24 J R R R R R R R 98 J R R R R R R 130 JN 770-08 Tillet R R 17 J R R R R R R 280 J R R R R R R R R R 56 J R R 32 J R R R R 120 J R R R R R R 21 JN 240 JN 121 JN 6JN 6JN 35 JN 6JN 770-09 Tillet-D (Replicate) R R 12 J R R R R R R 270 J R R R R R R R R R 47 J R R 26 J R R R R 98 J R R R R R R 39 JN 270 JN 230 JN 770-10 H20 Blank Tutu 2UJ 2UJ 2UJ 2UJ 2UJ R 1 UJ 1 UJ 1 UJ 1 UJ 1UJ 1UJ R 1UJ 1 UJ 2UJ 1UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ R 1 UJ 2UJ R 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 770-11 10/02 Trip Blank 2UJ 2UJ 2UJ 2UJ 14 J 7J 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ R 1 UJ 1 UJ 2UJ 1 UJ 1 UJ 1 UJ 1UJ 1 UJ 1 UJ 1 UJ R 1 UJ 2UJ R 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1UJ 1 UJ 3JN 770-12 Gassett (Hartmanl) 2UJ 2UJ 2UJ 2UJ 1UJ R 1UJ 1 UJ 1 U 1U 1 U 1 UJ R 1 UJ 1U 2UJ 1U 1 U 1 U 1 U 1 U 1 UJ 1U 1UJ 1UJ 1 UJ R 1 UJ 1 UJ 1 U 1U 1 U 1UJ 1 UJ 2JN concentrations are reported in micrograms per liter (ug/L). J - Value is estimated. U - Compound is not detected. R - Value is rejected. N - Compound is a tentatively identified compound. GERAGHTY & MILLER, INC. fUT Page3of9 Table 1. Tutu Residential Wells Sampling Results, September 1990, Sample Delivery Group 900770 Sample Identification: 'atile Organic Compounds (VOCs) Chloromethane Bromoraethane Vinyl Chloride Chloroethanc Methylene Chloride Acetone Carbon Disulftde 1 , 1-Dkhloroethene 1,1-Dichloroethane 1,2-Dichloroedicnc (total) Chloroform 1,2-Dichloroethane 2-Butanone 1,1,1 -Trichloroethane Carbon Tetrachloride Vinyl Acetate Bromodichloromethane 1 ,2-Dichloropropanc cis- 1 ,3-Dichloropropene Trichloroethene Dibromochlororaethane 1 1,2-Trichloroethane ^nzene trans-1 ,3-Dichloropropene Bromoform 4-Methyl-2-Pentanone 2-Hexanone Tetrachloroethene 1 , 1 ,2,2-Tetrachloroethane Toluene Chlorobenzene Ethylbenzene Styrene Total Xylenes Tentatively Identified VOCs 770-13 10/03 Trip Blank 2UJ 2UJ 2UJ 2UJ 1 UJ R 1 UJ 1 UJ 1 UJ 1 UJ 1UJ 1 UJ R 1 UJ 1 UJ 2UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 1 UJ 2UJ R 1 UJ 1 UJ 1 UJ 1 UJ 1UJ 1UJ 1 UJ 770-14 V1HAI 2UJ 2UJ 2UJ 2UJ 2UJ R 1UJ 1 UJ 1 UJ 6J 1UJ 1UJ R 1 UJ 1 UJ 2UJ 1 UJ 1 UJ 1 UJ 1 UJ I UJ 1 UJ 1 UJ 1 UJ 1 UJ 2UJ R 5J 1 UJ 1 UJ 1 UJ 1UJ 1 UJ 1 UJ 770-15 9/27 Trip Blank 2UJ 2UJ 2UJ 2UJ 16J R 1UJ 1 UJ 1U 1 U 1 U 1UJ R 1 UJ 1U 2UJ 1 U 1 U 1U 1 U I U I UJ 1 U 1 UJ 1 UJ 2UJ R 1 UJ 1 UJ 1 U 1 U 1 U 1UJ 1UJ Ethane, 1,1,2-Trichloro-1,2,2-trifluoro Unknown Propane,2-Methoxy-2-methyl C5H12 isomer Aliphatic hydrocarbon C3-Benzene isomer C6H12 isomer C9H12 isomer 1.5JN All concentrations are reported in micrograms per liter (ug/L). Value is estimated. •w^ U - Compound is not detected. R - Value is rejected. N - Compound is a tentatively identified compound. •TUT GERAGHTY & MILLER, INC. Table 1. Tutu Residential Wells Sampling Results, September 1990, Sample Delivery Group 900770 Sample Identification: Semivolatile Organic ipounds (SVOCs) Phenol bis(2-Chloroethyl)Ether 2-Chlorophenol 1 ,3-Dichlorobenzene 1 ,4-Dichlorobenzene Benzyl Alcohol 1 ,2-Dichlorobenzene 2-Methylphenol N-Nitro»o-Di-n-Propylamine Hexachloroethane Nitrobenzene Isophorone 2-Nitrophenol 2,4-Dimethylphenoi Benzoic Acid bis(2-Chloroethoxy)Methane 2 ,4-Dichlorophenol 1 ,2,4-Trichlorobenzene Naphthalene 4-Chloroaniline Hexnchlorobutadiene ' "Moro-3-Methylphenol , _ >iethylnaphthalene Hexachlorocyclopentadiene 2,4,6-Trichlorophenol 2,4,5-Trichlorophenol 2-Chloronaphthalene 2-Nitroaniline Dimethyl Phthalate Acenaphthylene 2,6-Dinitrotoluene 3-Nitroaniline Acenaphthene 2,4-Dinitrophcnol 4-Nitrophenol Dibenzofuran 2 ,4-Dinitrotoluene Diethylphthalate 4-Chloropheny!-phenylether Fluorene 4-Nitroaniline 4,6-Dinitro-2-Methylphenol N-Nitrosodiphenylamine 4-Bromophenyl-phenylether "-xachlorobenzene 770-01 Bryan 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U SOU 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 10 U 770-02 Dimitri 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 10 U 770-03 Matthias 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10V 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 10 U 770-04 Rarasey 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 10 U 770-06 EglinI 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 10 U PageMof 9 770-07 LaPlacc 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 UJ 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 10 U ^tfl concentrations are reported in micrograms per liter (ug/L). J - Value is estimated. U - Compound is not detected. N - Compound is a tentatively identified compound. GERAGHTY & MILLER, INC. Tir K>59 Table 1. Tutu Residential Wells Sampling Results, September 1990, Sample Delivery Group 900770 Sample Identification: Semivolatile Organic opounds (SVOCs) Pentachlorophenol Phenanthrene Anthracene Di-n-Burylphthalate Fluorantbene Pyrene Butylbenzylphthalate 3,3-Dichlorobcnzidine Benzo(a)Anthracene Chryiene bis(2-Ethylhexyl)Phthalate Di-n-Octyl Phthalate Benzo(b)Fluoranthene Benzo(k)Fluorantbene Benzo(a)Pyrene lndrao( 1 ,2,3-cd)Pyrene Dibenz(a,h)Anthr scene Benzo(g,h ,i)Perylene Tentarively Identified SVOCs Unknown Benzene, pentachlorofluoro- 770-01 Bryan SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 770-02 Dimitri SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 770-03 Matthias SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 4JN 770-04 Ramsey SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 770-06 EglinI SOU 10 U 10 U 10 U 10 U 10 U 10 U 20U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 12 JN PagoTofC) 770-07 LaPlace SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 42 JN ^.-i concentrations are reported in micrograms per liter (ug/L). J - Value is estimated. U - Compound is not detected. N - Compound is a tentatively identified compound. GERAGHTY & MILLER, INC. TUT Table 1. Tutu Residential Wells Sampling Results, September 1990, Sample Delivery Group 900770 Sample Identification: Semivolatile Organic jrapounds (SVOCs) Phenol bi*(2-Chloroethyl)Ether 2-CUorophenol 1 ,3-Dichlorobenzene 1 ,4-Dichlorobenzcne Benzyl Alcohol 1 ,2-Dichlorobenzene 2-Methylphenol N-Nitroso-Di-n-PropylemLne Hexachloroethane Nitrobenzene Isophorone 2-Nitrophenol 2,4-Dimethylphenol Benzoic Acid bis{2-Chloroethoxy)Methane 2 ,4-Dichlorophenol 1 ,2,4-Trichlorobenzene Naphthalene 4-Chloroaniline Hexachlorobutadiene ' -Chloro-3-Methylphenol ~A-Methylnaphthalene Hexachlorocyclopentadiene 2,4,6-Trichlorophenol 2 ,4 ,5-Trichlorophenol 2-Chloronaphthalene 2-Nitroanilinc Dimethyl Phthalate Acenaphthylene 2,6-Dinitrotoluene 3-Nitroaniline Acenaphthene 2 ,4-Dinitrophcnol 4-Nitrophcnol Dibenzofuran 2 ,4-Dinitiotoluene Diethylphthalate 4-Chlorophenyl-phenylether Fluorene 4-Nitroaniline 4,6-Dinitro-2-Methylphenol N-Nitrosodiphenylamine 4-Bromophenyl-phenylether * The first extraction results. 770-08 Tfflet* R 10 U R 10 U 10 U R 10 U R 10 U 10 U 10 U 10 U R R R 10 U R 10 U 10 U 10 U 10 U R 10 U 10 UJ R R 10 U sou 10 U 10 U 10 U sou 10 U R R 10 U 10 U 10 U 10 U 10 U sou R R R 770-09 Tillet-D (Replicate) 10 U 10 U R 10 U 10 U R 10 U R 10 U 10 U 10 U 10 U R R R 10 U R 10 U 10 U 10 U 10 U R 10 U 10 UJ R R 10 U sou 10 U 10 U 10 U sou 10 U R R 10 U 10 U 10 U 10 U 10 U sou R 10 U 10 U 770-10 H2O Blank 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10AJ 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U 770-12 Gassett (Hartman I) 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U tou 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U Page^of^ 770-14 VIHAI 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U sou 10 U sou 10 U 10 U 10 U sou 10 U sou sou 10 U 10 U 10 U 10 U 10 U sou sou 10 U 10 U v_-Jl concentrations are reported in raicrograms per liter (ug/L). J - Value is estimated. U - Compound is not detected. R - Value it rejected. N - Compound is a tentatively identified compound. GERAGHTY & MILLER. INC. TUT 002 2061 Table 1 . Tutu Residential Wells Sampling Results. September 1990, Sample Delivery Group 900770 Sample Identification: Semivolatile Organic jpounds (SVOCs) Hexachlorobenzene PentachlorophcncJ Phenanthreoe Anthracene Di-a-Butylphthalate Fluoranthenc Pyrcne Butylbenzylpbthalate 3,3-Dichlorobenzidine Benzo(a)Anthracene Chrysene bis(2-Ethylhexyl)Phthalate Di-n-Octyl Phthalate Benzo(b)Fluoranthene Benzo(k)Fluoranthene Benzo(a)Pyrene IndemX 1 ,2,3-cd)Pyrene Dibenz(a,h)Anthracene Benzo(g,h,i)Perylene Tentatively Identified SVOCs Unknown izene, pentachlorofluoro- 770-08 Tillet R R R R R R 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 770-09 Tillet-D (Replicate) 10 U R 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 82 JN 4JN 770-10 H2O Blank 10 U SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 770-12 Gassett (Hartman I) 10 U SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U Page lot *? 770-14 VIHAI 10 U SOU 10 U 10 U 10 U 10 U 10 U 10 U 20 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U 10 U All concentrations are reported in micrograms per liter (ug/L). J - Value is estimated. U - Compound is not detected. R - Value is rejected. N - Compound is a tentatively identified compound. 2061 GERAGHTY & MILLER. INC. Table 1. Tutu Residential Wells Sampling Results, September 1990, Sample Delivery Group 900770 Sample Identification: Pesticide/PCBs vna-BHC beta-BHC delta-BHC garama-BHC Heptachlor Aldrin Heptachlor epoxide Endowlfanl Dieldrin 4,4-DDE Endrin Endosulfan II 4,4-DDD Endosulfan sulfate 4,4-DDT Methoxychlor Endrin ketone alpha-Chlordane garama-Chlordane Toxaphcne Aroclor-1016 Aroclor-1221 •roclor-1232 _^oclor-1242 Aroclor-1248 Aroclor-1254 Aroclor-1260 770-01 Bryan 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU 0.50 U O.IOU 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U 770-02 Dimitri 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU 0.50 U O . I O U 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U 770-03 Matthias 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU 0.50 U O.IOU 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U 770-04 Ramsey 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU 0.50 U O.IOU 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U 770-06 EglinI 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU 0.50 U O.IOU 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U PageTofCf 70-07 LaPlace 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU 0.50 U O.IOU 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U All concentrations are reported in micrograms per liter (ug/L). U - Compound is not detected. GERAGHTY & MILLER. INC. TUT 002 2063 Table 1 . Tutu Residential Wells Sampling Results, September 1990, Sample Delivery Group 900770 Sample Identification: Pesticides/PCBs -pha-BHC beta-BHC delta-BHC gamma-BHC Heptachlor AMrin Heptachlor epoxide Endomlfan I Dieldrin 4,4-DDE Endrin Endosulfan II 4,4-DDD Endosulfan sulfate 4,4-DDT Methoxychlor Endrin ketone alpha -Chlordane gamma -Chlordane Toxaphene ArocIor-1016 Aioclor-1221 •oclor-1232 — rtfoclor-1242 Aroclor-1248 Aroclor-1254 Aroclor-1260 770-08 Tillet 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU 0.50 U O.IOU 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50U 1.0 U 1.0 U 770-09 TilletD 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU 0.50 U O.IOU 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U 770-10 H2OBlk 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU 0.50 U O.IOU 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U 770-12 HartmanI 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU 0.50 U O.IOU 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U 770-14 VIHAI 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU O.IOU 0.50 U O.IOU 0.50 U 0.50 U 1.0 U 0.50 U 0.50 U 0.50 U 0.50 U 0.50 U 1.0 U 1.0 U All concentrations are reported in micrograms per liter (ug/L). U - Compound is not detected. GERAGHTY & MILLER. INC. 2064 Table 1. Tutu Residential Sample Identification: Inorganics Analysis ^minum Antimony Arsenic Barium Beryllium Cadmium Calcium Chromium Cobalt Copper Iron Lead Magnesium Manganese Mercury Nickel Potassium Selenium Silver Sodium Thallium Vanadium ~nc _/anide Wells Sampling Results, September 770-01 Bryan 149 B 52 U 3 UJ 3 U 3 B 4 BJ 54300 7 B 18 U 17 BJ 63 BJ 4.6J 49100 2 B R 11 U 1000 B 2 UJ 7 U 83000 R 37 B 30 5 U 1990, Sample 770-02 Dimitri 163 BJ 52 UJ 3 UJ 3 UJ 4 BJ 3 BJ 37500 J 4 BJ 18 UJ 17 BJ 115 J 2.6BJ 27800 J 7 BJ R 14 BJ 2000 BJ 10 UJ 7 UJ 328000 J R 92 J 4 UJ 5 UJ Delivery Group 900770 770-03 Matthias 227 52 U 3 UJ 6 B 3 B 3 U 36300 5 B 18 U 18 BJ 20 UJ I.8BJ 34900 2 U R 20 BJ 1410 B 2 UJ 7 U 379000 R 21 B 4 BJ 5 U 770-04 Ramsey 187 B 52 U 3 UJ 3 U 3 B 3 BJ 43100 11 18 U 15 BJ 20 BJ 2.6BJ 34400 2 U R 21 BJ 1140 B 10 UJ 7 U 209000 R 43 B 7 BJ 5 U 770-06 EglinI 149 B 52 U 3 U 3 U 4 B 3 U 35300 12 18 U 14 BJ 20 UJ 2 BJ 28700 56 R 26 BJ 920 B 10 UJ 7 U 190000 R 34 B 13 BJ 5 U Page / of 2, 770-07 LaPlace 146 B 57 B 3 U 3 U 4 B 4 BJ 41000 8 B 18 U 49 J 55 BJ 2.3BJ 32600 2 B R 18 BJ 1140 B 10 UJ 7 U 250000 R 39 B 13 BJ 5 U All concentrations are reported in micrograms per liter (ug/L). J - Value is estimated. U - Analyte is not detected. R - Value is rejected. B - Value is between instrument detection limit and contact required detection limit. GERAGHTY & MILLER. INC. Table 1 . Tutu Residential Wells Sampling Results. September 1990, Sample Delivery Group 900770 Sample Identification: Inorganic Analysis Aluminum Antimony Arsenic Barium Beryllium Cadmium Calcium Chromium Cotalt Copper Iron Lead Magnesium Manganese Mercury Nickel Potassium Selenium Silver Sodium Thallium "»nadium _-*fl» Cyanide 770-08 Tillet 153 BJ 52 UJ 3 UJ 43 BJ 4 BJ 4 BJ 54800 J 8 BJ 18 UJ 48 J 953 J 1.5BJ 38300 J 1260 J R 33 BJ 760 BJ 10 UJ 7 UJ 192000 J R 25 BJ 162 J 5 UJ 770-09 Tillet-D (Replicate) 159 B 52 U 4.4B 40 B 4 B 3 BJ 48600 7 B 18 U 32 J 2660 J 8.5J 34500 1100 R 15 BJ 1190 B 10 UJ 7 U 169000 R 50J 124 J 5 U 770-10 H20 Blank Tutu 85 B 52 U 3 U 3 U 4 B 3 U 74 U 5 B 18 U 12 BJ 27 BJ 1 UJ 95 U 2 U R 11 UJ 300 B 2 UJ 7 U 158 B R 10 BJ 4-UJ 5 U 770-12 Gassett (Hartman I) 526 52 U 3 U 7 B 4 B 3 U 31200 4 B 18 U 10 BJ 418 J 1.4BJ 26300 853 R 11 U 880 B 10 UJ 7 B 236000 R 26 BJ 5 BJ 5 U PageZofZ- 770-14 VIHAI 154 B 54 BJ 3 U 5 B 3 B 4 BJ 49400 10 18 U 10 B 29 BJ 9 J 33900 2 U R 15 B 2000 B 1.4BJ 16 J 252000 R 67 J 16 B 9.7B All concentrations are reported in micrograms per liter (ug/L). J - Value is estimated. U - Analyte is not detected. R - Value is rejected. B - Value is between instrument detection limit and contract required detection limit. GERAGHTY & MILLER. INC. TUT