Document yrLg472L7gGBNkERzve1N4eQE

3M GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 GLP10-01-02: Interim Report 11 - Analysis o f PFBS. PFHS. and PFOS in Ground Water Samples Collected at the Former Sludge Incorporation Area (FSIA) located in Decatur. AL in November 2010 Study Title Analysis of Perfluorooctane Sulfonate (PFOS), Perfluorohexane Sulfonate (PFHS) and Perfluorobutane Sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M Decatur Phase 3 Site-Related Monitoring Program Data Requirement EPA TSCA Good Laboratory Practice Standards 40 CFR Part 792 Study Director Jaisimha Kesari P.E., DEE W eston Solutions, Inc. 1400 W eston Way W est Chester, PA 19380 Phone: 610-701-3761 Author Susan W olf 3M Environmental Laboratory Interim Report Completion Date Date of signing Performing Laboratory 3M Environmental Health and Safety Operations Environmental Laboratory 3M Center, Bldg 260-05-N-17 Maplewood, MN 55144 Project Identification G LP 10-01-02-11 Total Number of Pages 104 The testing reported herein meet the requirements of ISO/IEC 17025-2005 "General Requirements for the Competence of Testing and Calibration Laboratories", in accordance with the A2LA Certificate #2052.01. Testing that complies with this International Standard also operate in accordance with ISO 9001:2000. Testing Cert #2052.01 Page 1 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 This page has been reserved for specific country requirements. Page 2 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 GLP C o m p l ia n c e S ta te m e n t Report Title: Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Ground W ater Samples Collected at the Former Sludge Incorporation Area (FSIA) at Decatur, AL in November 2010 Study: Analysis of Perfluorooctane Sulfonate (PFOS), Perfluorohexane Sulfonate (PFHS) and Perfluorobutane Sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M Decatur Phase 3 Site-Related Monitoring Program. This analytical phase was conducted in compliance with Toxic Substances Control Act (TSCA) Good Laboratory Practice (GLP) Standards, 40 CFR 792, with the exceptions listed below: These are environmental samples where there is no specific test substance, no specific test system and no dosing of a test system. The reference substances have not been characterized under the GLPs and the stability under storage conditions at the test site have not been determined under GLPs. Page 3 of 104 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Q uality A ssurance Statement Report Title: Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Ground W ater Samples Collected at the Former Sludge Incorporation Area (FSIA) at Decatur, AL in November 2010 Study: Analysis of Perfluorooctane Sulfonate (PFOS), Perfluorohexane Sulfonate (PFHS) and Perfluorobutane Sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M Decatur Phase 3 Site-Related Monitoring Program. This analytical phase was audited by the 3M Environmental Laboratory Quality Assurance Unit (QAU), as indicated in the following table. The findings were reported to the principal investigator (P.I.), laboratory management and study director. Inspection Dates 3/24/11 -3/25/11 Phase Data / Report Date Reported to Testing Facility Management Study Director 4/25/11 4/25/11 Date Page 4 of 104 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Ta b le of C o n ten ts GLP Compliance Statem ent................................................................................................................. 3 Quality Assurance Statement................................................................................................................ 4 Table of Contents.................................................................................................................................. 5 List of Tables.......................................................................................................................................... 6 1 Study Information............................................................................................................................ 8 2 Summary......................................................................................................................................... 9 3 Introduction................................................................................................................................... 11 4 Test & Control Substances.......................................................................................................... 11 5 Reference Substances................................................................................................................. 12 6 Test System.................................................................................................................................. 13 7 Method Summary......................................................................................................................... 13 7.1 M ethods........................................................................................................................ 13 7.2 Sample Collection......................................................................................................... 13 7.3 Sample Preparation.......................................................................................................13 7.4 Analysis......................................................................................................................... 14 8 Analytical R esults......................................................................................................................... 15 8.1 Calibration..................................................................................................................... 15 8.2 System Suitability......................................................................................................... 15 8.3 Limit of Quantitation (LO Q )........................................................................................... 15 8.4 Continuing Calibration...................................................................................................16 8.5 Blanks............................................................................................................................ 16 8.6 Lab Control Spikes (LC Ss)........................................................................................... 16 8.7 Analytical Method Uncertainty...................................................................................... 21 8.9 Field Matrix Spikes (FMS)..............................................................................................22 Page 5 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 9 Data Summary andDiscussion..................................................................................................... 23 10 Conclusion.................................................................................................................................... 43 11 Data/Sample Retention............................................................................................................... 43 12 Attachm ents.................................................................................................................................. 43 13 Signatures..................................................................................................................................... 44 List of Tables Table 1. Summarized PFBS, PFHS, and PFOS Results (FSIA Groundwater, November 2010). .10 Table 2. Sample Description Key Code...........................................................................................13 Table 3. Instrument Parameters.......................................................................................................14 Table 4. Liquid Chromatography Conditions................................................................................... 14 Table 5. Mass Transitions................................................................................................................ 15 Table 6. Limit of Quantitation (LOQ)................................................................................................ 16 Table 7. Laboratory Control Spike Recovery................................................................................... 18 Table 8. Analytical Uncertainty........................................................................................................ 22 Table 9. Field Matrix Spike Levels................................................................................................... 22 Table 10. DAL GW 130R 101105....................................................................................................24 Table 11. DAL GW 130L 101105....................................................................................................24 Table 12. DAL GW 130S 101105....................................................................................................25 Table 13. DAL GW 131R 101103....................................................................................................25 Table 14. DAL GW 131L 101103................................................................................................... 26 Table 15. DALGW 131S 101103...................................................................................................26 Table 16. DAL GW 132R 101102................................................................................................... 27 Table 17. DAL GW 132L101103.................................................................................................... 27 Table 18. DAL GW 132S 101102....................................................................................................28 Table 19. DAL GW 133R 101102....................................................................................................28 Table 20. DAL GW 133L 101103....................................................................................................29 Page 6 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Table 21. DAL GW 133S 101103................................................................................................... 29 Table 22. DAL GW 134R 101105....................................................................................................30 Table 23. DALGW 134L 101105.................................................................................................... 30 Table 24. DAL GW 134S 101105....................................................................................................31 Table 25. DAL GW 135R 101105....................................................................................................31 Table 26. DAL GW 135L 101105....................................................................................................32 T able27. DALGW 135S 101105...................................................................................................33 Table 28. DAL GW 136L 101103....................................................................................................33 Table 29. DAL GW 136S 101103....................................................................................................34 Table 30. DAL GW 137L 101109....................................................................................................34 Table 31. DAL GW 137S 101109....................................................................................................35 Table 32. DAL GW 138S 101110....................................................................................................36 Table 33. DAL GW 138L 101110....................................................................................................36 Table 33. DAL GW CW26R 101110................................................................................................37 Table 34. DAL GW CW26L 101110.................................................................................................37 Table 35. DAL GW 140R 101104.................................................................................................... 38 Table 36. DALGW 141R 101110.................................................................................................... 38 Table 37. DAL GW 142R 101110.................................................................................................... 39 Table 38. DAL GW 144R 101110.....................................................................................................39 Table 39. Trip Blank.........................................................................................................................40 Table 40. Trip Blank 2......................................................................................................................40 Table 41. Trip Blank 3......................................................................................................................41 Table 42. Trip Blank 4 ......................................................................................................................41 Table 43. Rlnseate Blanks.............................................................................................................. 42 Table 44. GLP10-01-02-12 Soil Equipment Rinseate Blank...........................................................42 Page 7 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 1 Study Information Sponsor 3M Company Sponsor Representative Gary Hohenstein 3M EHS Operations 3M Building 224-5W-03 Saint Paul, MN 55144-1000 Phone: (651) 737-3570 Study Director Jaisimha Kesari, P.E., DEE Weston Solutions, Inc. West Chester, PA 19380 Phone: (610) 701-3761 Fax: (610) 701-7401 j.kesari@ westonsolutions.com Study Location Testing Facility 3M EHS Operations 3M Environmental Laboratory Building 260-5N-17 Maplewood, MN 55106 Study Personnel W illiam K. Reagen, Ph.D., 3M Laboratory Manager Cleston Lange, Ph.D., Principal Analytical Investigator, (clanqe@mmm.com): phone (651)-733-9860 Susan Wolf, 3M Analyst Chelsie Grochow, Analyst Study Dates Study Initiation: March 8,2010 Interim 11 Experimental Termination: February 11,2011 Interim Report Completion: Date of Interim Report Signing Location of Archives All original raw data and the analytical report have been archived at the 3M Environmental Laboratory according to 40 CFR Part 792. The test substance and analytical reference standard reserve samples are archived at the 3M Environmental Laboratory according to 40 CFR Part 792 Page 8 of 104 GLP10-01-02: Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 2 Summary - ' The 3M Environmental Laboratory received ground water samples from wells located at the Former Sludge Incorporation Area (FSIA) in Decatur, AL, representing thirty different sampling locations. A total of one hundred sixty-nine sample bottles were received at the 3M Environmental Laboratory for perfluorooctane sulfonate (PFOS), perfluorohexane sulfonate (PFHS) and perfluorobutane sulfonate (PFBS), and included duplicate ground water samples from each sampling location. Samples also included at least two field matrix spike (FMS) samples for each location, four trip blank sets containing M illi-QTM water and appropriate trip blank spikes, and two equipment rinseate blanks. In addition, one soil equipment rinseate blank from GLP10-01-02-12 was analyzed. The equipment rinseate blanks did not have FMS samples prepared for determination of PFBS, PFHS, and PFOS recovery. The ground water samples, trip blanks and two equipment rinseate blanks associated with GLP10-0102-11 were received from Weston personnel on November 18, 2010. The soil equipment rinseate blank associated with GLP10-01-02-12 was received from Weston personnel on October 15,2010. All of the samples were prepared and analyzed for PFBS, PFHS, and PFOS following 3M Environmental Laboratory Method ETS-8-044.0 and conducted under 3M project GLP-10-01-02-011. Many of the ground water samples required dilution to attain PFBS, PFHS, and/or POFS concentrations within the range of the curve, in some instances up to 100-fold dilution were required. The average measured PFBS, PFHS, and PFOS concentrations are summarized in Table 1. The equipment rinseate and the trip blank samples were below the lower limit of quantitation (LLOQ), indicating adequate control of sample contamination during shipping and sample collections. The PFBS concentration results for all ground water samples ranged from 0.0431 ng/mL to 81.2 ng/mL. The PFHS concentration results for all ground water samples ranged from 0.0914 ng/mL to 839 ng/mL. The PFOS concentration results for all ground water samples ranged from 0.315 ng/mL to 1510 ng/mL. The analytical method uncertainties associated with the reported results are: PFBS + 20%, PFHS + 22% and PFOS + 33%. For some samples, the method uncertainty was expanded for PFHS or PFOS. Page 9 of 104 GLP10-01-02: Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Table 1. Summarized PFBS, PFHS, and PFOS Results (FSIA Groundwater, November 2010). PFBS PFHS PFOS Sampling Location Avg. Cone. (nq/mL) RPD Avg. Cone. (ng/mL) RPD Avg. Cone. (ng/mL) RPD DAL GW 130R 101105 DAL GW 130S 10 1105 DAL GW 130L 101105 16.6 6 .6 % 3.50 11% 1.77 4.0% 128 0 .0 % 31.3 0.32% 14.4 3.5% 583 2.4% 117 3.4% 82.7 5.9% DAL GW131R 101103 81.2 4.2% 413 0.73% 1510 2.6% DAL GW 131S 101103 DAL GW 131L 101103 DALGW 132R 101102 0.785 3.2% 3.35 4.5% 8.03 3.5% 4.63 6.3% 20.7 4.8% 52.8 5.9% 5.55 5.6% 34.3 5.0% 295 1.7% DAL GW 132S 101102 25.9 2.3% 205 1.5% 633 12% DAL GW 132L 101103 DALGW 133R 101102 DAL GW 133S 101103 DAL GW 133L 101103 DALGW 134R 101105 8.89 3.8% 4.61 7.6% 14.0 0.0% 7.65 1.7% 56.2 13% 77.2 1.2% 31.1 6.4% 91.5 1.1% 53.4 2.4% 503 9.4% 293 5.5% 60.8 6 .1 % 224 3.6% 204 1.5% 1420 15% DALGW 134S 10 1105 DALG W 134L 101105 DALGW 135R 101105 DAL GW 135S 101105 DAL GW 135L 101105 DALGW 136S 101103 DAL GW 136L 101103 DALGW 137S 101109 0.143 4.2% 11.9 3.4% 81.0 2.7% 0.799 1.1% 5.73 3.8% 2.55 2.0% 2.53 7.9% 0.102 4.9% 1.71 6 .5 % (1) 1 1 2 0 .0 % 839 1.9% 6.25 3.2% 35.9 2.5% 16.5 5.5% 16.2 8 .0 % 0.0914 6.1% 11.4 1.8% 579 2.6% 892 2.6% 4.88 5.3% 2 2 .6 1 2 % 87.1 3.7% 79.2 8 .8 % 0.315 33% (2'3) DAL GW 137L 101109 DAL GW 138S 101110 DAL GW 138L 10 1110 DAL GWCW26R 101110 DAL GWCW26L 101110 0.0823 2.6% 4.69 2.3% 0.0473 5.3% 8.27 3.1% 12.9 5.4% 0.199 3.4% 23.5 4.7% 0.144 0.70% 63.1 4.3% 92.9 5.8% 0.893 3.6% 245 5.7% 0.581 0.17% 451 2.0% 848 9.4% DAL GW 140R 101104 DAL GW 141R 101110 1.63 2.5% 0.0431 6.0% 17.2 0.0% 0.258 12% 136 6 .6 % 4.23 12% DAL GW 142R 101110 1 . 6 8 1 .2 % 9.98 0.40% 108 6.5% DAL GW 144R 101110 1.95 3.6% 8.57 5.1% n r <4) Trip Blanks (Milli-QTM Water) <0.0250 <0.0250 <0.250 GLP10-01-02-11 Equipment rinseate blanks <0.0250 <0.0250 <0.250 GLP10-01-02-12 Soil Equipment rinseate blank <0.0250 <0.0250 <0.250 The analytical method uncertainties associated with the reported results are: PFBS 20%, PFHS 22%, and PFOS 33%. (1) The analytical uncertainty has been adjusted for PFHS based on FMS recovery for: DAL GW 134S to 35%. (2) The analytical uncertainty has been adjusted for PFOS based on FMS recovery for DAL GW 137S to 41 %. See discussion in section 9 of the report. (3) The RPD did not m eet method acceptance criteria of 20%. (4) NR = Not Reported; M atrix spike recovery was <50%. See section 9 of the report for additional information. Page 10 o f 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 3 Introduction This analytical study was conducted as part of the Phase 3 Environmental Monitoring and Assessment Program for the 3M facility located in Decatur, Alabama. The objective of the overall program is to gain information regarding concentrations of perfluorooctane sulfonate (PFOS), perfluorohexane sulfonate (PFHS) and perfluorobutane sulfonate (PFBS), in various environmental media such as ground water, soils and sediments that are associated with and near the Decatur facility. This analytical study was conducted to analyze ground water samples collected from various wells located at the Former Sludge Incorporation Area (FSAI) in Decatur, AL for PFBS, PFHS, and PFOS in an effort to characterize on site groundwater conditions. The 3M Environmental Laboratory prepared sample containers (250 mL high-density polyethylene bottles) which were shipped to Decatur, AL Weston personnel prior to field sampling. Sample containers for each sampling location included a field sample, field sample duplicate, and a minimum of two field matrix spike samples. Each empty container was marked with a "fill to here" line to produce a final sample volume of 200 mL. Containers designated for field matrix samples were fortified with an appropriate matrix spike solution containing PFBS (linear), PFHS (linear), and PFOS (linear) prior to being sent to the field for sample collection. See section 8.8 of the report for field matrix spike levels. The aqueous equipment rinseate samples were collected in plain bottles without markings or fortifications. Samples were prepared and analyzed according to the procedure defined in 3M Environmental Laboratory method ETS-8-044.0 "Determination of Perfluorinated Compounds In Water by High Performance Liquid Chromatography/Mass Spectrometry Direct Injection Analysis". Table 1 summarizes the average PFBS, PFHS, and PFOS concentrations for the duplicate samples collected, the trip blanks, aqueous equipment rinseate blanks, and aqueous soil-equipment rinseate blank samples. Tables 10-44 summarize the individual sample results and the associated field matrix spike recoveries. All results for the quality control samples prepared and analyzed with the samples are reported and discussed elsewhere in this report 4 Test & Control Substances There was not a test substance or control substances in the classic sense of a GLP study. This study was purely analytical in nature. Page 11 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 5 Reference Substances R eference Substance Chemical Name Chemical Formula Identifier Source Expiration Date Storage Conditions Chemical Lot Number TCR Number Physical Description Purity PFBS (predom inantly lin ear) Perfluorobutane sulfonate C 4 F 9SO 3 Potassium Salt 3M 1/10/2017 Frozen 41-2600-8442-5 TCR-121 White Powder 96.7% R eference Substance Chemical Name Chemical Formula Identifier Source Expiration Date Storage Conditions Chemical Lot Number TCR Number Physical Description Purity PFOS (lin ear) Perfluorooctane sulfonate C8 F17SO 3 Potassium Salt CAS # 2795-39-3 Wellington 10/18/2013 Frozen LPFOSKBM06 TCR08-0001 Crystalline 98% PFHS (lin ear) Perfluorohexane sulfonate C6F13SO 3 Sodium Salt Wellington 4/2/2013 Frozen LPFHXSAM08 TCR08-0018 Crystalline 98% PFOS (lin ea r + branched) Perfluorooctane sulfonate C8 F 17SO 3 Potassium Salt CAS # 2795-39-3 3M 12/14/2016 Frozen 171 TCR-696 White Powder 86.4% Page 12 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 6 Test System The test system for this study are ground water samples collected from wells located in Decatur, AL by Weston Solutions, Inc. personnel. Samples for this study are "real world" samples, not dosed with a specific lot of test substance. Table 2. Sample Description Key Code. String Number Example 1 2 3 4 5 String Descriptor Example DAL GW135L DB 101105 Sampling Location DAL = Decatur, AL Sample Type Sampling Point Well Level G W = Groundwater Example: 135 R = Residum shallow water-bearing zone L = Bedrock water-bearing zone Sampling Date Sample Type S = Eplkarst middle water-bearing zone 101105 = Novembers, 2011 0=primary sample DB=duplicate sample LS = low spike MS = m id spike HS = high spike 7 Method Summary 7.1 Methods Analysis for all analytes was completed following 3M Environmental Laboratory method ETS-8-044.0 "Determination of Perfluorinated Compounds In Water by High Performance Liquid Chromatography/Mass Spectrometry Direct Injection Analysis". 7.2 Sample Collection Samples were collected in 250 mL NalgeneTM (hlgh-density polyethylene) bottles prepared at the 3M Environmental Laboratory. Sample bottles associated with GLP10-01-02-11 were returned to the laboratory at ambient conditions on November 18, 2010. The equipment rinseate blank associated with GLP10-01 -02-12 was returned to the laboratory at ambient conditions on October 15,2010. Samples were stored refrigerated at the laboratory after receipt. A set of laboratory prepared Trip Blank and Trip Blank field matrix spikes were sent with each cooler of sample collection bottles. 7.3 Sample Preparation Samples were prepared by removing an aliquot of the well mixed sample and placing it in an autovial for analysis. Samples that required dilution were prepared by dilutions of 1mL sample with 9 mLs of Milli Q water (dilution 1:10). Most sampling locations were diluted 1:100 by further diluting the 1:10 dilution with additional Milli Q water. Page 13 of 104 GLP10-01-02: Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 7.4 Analysis All study samples and quality control samples were analyzed for PFBS, PFHS, and PFOS using high performance liquid chromatography/ tandem mass spectrometry (HPLC/MS/MS). Detailed instrument parameters, the liquid chromatography gradient program, and the specific mass transitions analyzed are described in the raw data hard copies placed in the final data packet, and are briefly described below. All samples were initially prepared on 12/30/10. Due to the large number of samples requiring analysis, along with network communication errors that were experienced during the analysis, the samples were broken up into three analytical runs. The LCS samples prepared with the samples on 12/30/10 were re analyzed with each analytical batch analyzed on ETS Buster from 1/7/11 -1 /4 /1 1 . Table 3. Instrument Parameters. Instrument Name Analytical Method Followed Analysis Date Liquid Chromatograph Guard column Analytical column Injection Volume Mass Spectrometer Ion Source Electrode Polarity Software ETS Buster ETS-8-044.0 1/7/11,1/10/11, and 1/14/11 -P F B S , PFHS, and PFOS Agilent 1100 Prism RP (2.1 mm X 50 mm), 5 n Betasil C18 (2.1 mm X 100 mm), 5u 2 o r10uL Applied Biosystems API 4000 Turbo Spray Turbo ion electrode Negative Analyst 1.4.2 ETS Ginger ETS-8-044.0 2/11/11 - PFBS and PFOS Agilent 1100 Prism RP (2.1 mm X 50 mm), 5 u Betasil C18 (2.1 mm X 100 mm), 5u 5or10w L Applied Biosystems API 5000 Turbo Spray Turbo ion electrode Negative Analyst 1.4.2 Table 4. Liquid Chromatography Conditions. Step Number 0 1 2 3 4 5 0 1 2 3 4 5 Total Time (min) 0 2.0 14.5 15.5 16.5 20.0 0 2.0 11.0 14.5 14.5 17.0 Flow Rate (fiL/min) Percent A (2 mM ammonium acetate) ETS-8-044.0 Analyzed on ETS Buster 300 97.0 300 97.0 300 5.0 300 5.0 300 97.0 300 97.0 ETS-8-044.0 Analyzed on ETS Ginger 300 97.0 300 97.0 300 5.0 300 5.0 300 97.0 300 97.0 Percent B (Methanol) 3.0 3.0 95.0 95.0 3.0 3.0 3.0 3.0 95.0 95.0 3.0 3.0 Page 14 o f 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Table 5. Mass Transitions. Analyte PFBS PFHS PFOS Mass Transition Q1/Q3 299/80 299/99 399m 399/99 499/80 499/99 499/130 Reference Material Structure Linear Linear Linear Dwell tim e was 50 msec for each transition. The individual transitions were summed to produce a "total ion chromatogram" (TIC), which was used for quantitation. 8 Analytical Results ? 8.1 Calibration Samples were analyzed against an external standard calibration curve. Calibration standards were prepared by spiking known amounts of the stock solution containing the target analytes into prepared in Milli Q water. A total of fifteen spiked standards ranging from 0.025 ng/mL to 100 ng/mL (nominal) were analyzed. Low or high curve points may have been disabled to meet method criteria. A quadratic, 1/x weighted, calibration curve of the peak area counts was used to fit the data for each analyse. The data were not forced through zero during the fitting process. Calculating the standard concentrations using the peak area confirmed accuracy of each curve point. Each curve point was quantitated using the overall calibration curve and reviewed for accuracy. Method calibration accuracy requirements of 10025% (10030% for the lowest curve point) were met for all analytes. The correlation coefficient (r) was greater than 0.995 for PFBS, PFHS, and PFOS. 8.2 System Suitability A calibration standard was analyzed four times at the beginning of each analytical sequence to demonstrate overall system suitability. The acceptance criteria of less than or equal to 5% relative standard deviation (RSD) for peak area and retention time criteria of less than or equal to 2% RSD was met for PFBS, PFHS, and PFOS. 8.3 Limit of Quantitation (LOQ) The LOQ for this analysis is the lowest non-zero calibration standard in the curve that meets linearity and accuracy requirements and for which the area counts are at least twice those of the appropriate blanks. The LOQ for all analytes can be found in Table 6. Page 15 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Table 6. Limit of Quantitation (LOQ). Analysis Date 1/7/11 and 1/10/11 Analysis 1/14/11 Analysis 2/11/11 Analysis 2/28/11 Analysis NA = Not Applicable Dilution 1 5 10 100 50 100 1 10 100 10 PFBS LOQ, nq/mL 0.0250 0.125 0.250 2.50 1.25 2.50 0.0250 0.250 2.50 NA PFHS LOQ, nq/mL 0.0250 0.125 0.250 2.50 1.25 2.50 0.0250 0.250 2.50 NA PFOS LOQ, nq/mL 0.250 1.25 2.50 25.0 12.5 25.0 0.0300 0.300 3.00 0.250 8.4 Continuing Calibration During the course of each analytical sequence, continuing calibration verification samples (CCVs) were analyzed to confirm that the instrument response and the initial calibration curve were still in control. All CCVs met method criteria of 100% 25% for PFBS, PFHS, and PFOS. 8.5 Blanks Two types of blanks were prepared and analyzed with the samples: method blanks and field/trip blanks. Method blank results were reviewed and used to evaluate method performance and to determine the LOQ for each analyte 8.6 Lab Control Spikes (LCSs) Low, mid, and high-level lab control spikes were prepared and analyzed in triplicate with each preparation set. LCSs were prepared by spiking known amounts of the analyte into Milli Q water to produce the desired concentration. The spiked water samples were then prepared and analyzed in the same manner as the samples. The method acceptance criteria, average of LCS at each level should be within 100% 20% with an RSD <20%AII samples were initially prepared on 12/30/10. Due to the large number of samples requiring analysis, along with network communication errors that were experienced during the analysis, the samples were broken up into three analytical runs. The LCS samples prepared with the samples on 12/30/10 were re-analyzed with each analytical batch analyzed on ETS Buster from 1/7/11 -1/4/11. 1/7/11 Analysis: Due to an autosampler error, the third replicate of the low set of LCS samples did not inject. The average recovery for the low set of LCS for PFBS was 122% and for PFHS 123%. All other LCS analyzed in this run met method acceptance criteria. 1/10/11 Analysis: The low set of LCS samples for PFHS had an average recovery of 122%. All other LCS analyzed in this run met method acceptacne criteria. 1/14/11 Analysis: All three sets of LCS method acceptance criteria for PFBS, PFHS, and PFOS. 2/11/11 Analysis: All three sets of LCS method acceptance criteria for PFBS, PFHS, and PFOS. As the reference material used for quantitation of PFOS is predominantly linear, and the PFOS present in the water samples are comprised of both linear and branched isomers, additional LCS samples of Page 16 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 PFOS (linear and branched) were prepared at three concentrations in triplicate to evaluate the potential for analytical bias. 1/7/11 Analysis: The low and mid sets of linear and branched PFOS LCS met method acceptance criteria, while the average recovery of the high set of LCS samples was 123%. 1/10/11 Analysis: The low and mid sets of linear and branched PFOS LCS met method acceptance criteria while the high set had an average recovery of 121%. 1/14/11 Analysis: All three sets of linear and branched PFOS LCS met method acceptance criteria. 2/11/11 Analysis: The low and mid sets of linear and branched PFOS LCS met method acceptance criteria while the high set had an average recovery of 133%. The recovery of the high sets of linear and branched PFOS suggest possible analytical bias when samples containing both linear and branched isomers of PFOS are quantitated against a calibration curve constructed of primarily linear PFOS. Therefore, the analytical method uncertainty for this study has been adjusted based on the highest average recovery of the linear and branched PFOS LCS samples to 33%. The following calculations were used to generate data in Table 7 for laboratory control spikes. LCS Percent Recovery = -C--a--l-c-u--l-a-t-e--d--C---o--n-c--e--n-t-r-a--t-io--n- ,, .100% Spike Concentration LCS% RSD = standard deviation L C S replicates . m % average LCS recovery Page 17 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Table 7. Laboratory Control Spike Recovery. ETS-8-044.0 Analyzed 1/7/11 Lab ID Spiked Concentration (ng/mL) PFBS Calculated Concentration (ng/mL) Spiked Concentration XoRecovery (ng/mL) PFHS Calculated Concentration (ng/mL) LCS-101230-1 LCS-101230-2 LCS-101230-3 0.497 0.497 NA(2) 0.631 0.580 NA(2) 127 117 NA<2) 0.498 0.498 NA(2) 0.631 0.595 n a (2) Average %RSD 122 5.8%<1) 123% 4.6%(1) LCS-101230-4 LCS-101230-5 LCS-101230-6 4.97 4.97 4.97 6 . 0 1 1 2 1 4.98 5.86 118 4.98 5.87 118 4.98 5.94 5.83 5.86 Average %RSD 119% 1.5% 118% 0.85% LCS-101230-7 LCS-101230-8 LCS-101230-9 Average %RSD 29.9 29.9 29.9 30.6 29.8 29.9 101% 1.3% 102 99.6 100 29.9 29.9 29.9 30.7 29.6 30.5 101% 2.1% %Recovery 127 119 NA(2) 119 117 118 103 99.0 102 ETS-8-044.0 Analyzed 1/7/11 PFOS (linear) PFOS (linear + branched) Lab ID Spiked Calculated Concentration Concentration (ng/mL) (ng/mL) XoRecovery Lab ID Spiked Calculated Concentration Concentration (ng/mL) (ng/mL) XoRecovery LCS-101230-1 LCS-101230-2 LCS-101230-3 Average %RSD 0.497 0.497 n a (2) 0.524 0.507 NA<2) 104% 2.0% 105 102 n a (2) LCS-101230-10 LCS-101230-11 LCS-101230-12 Average %RSD 0.492 0.492 NA(2) 0.539 0.498 n a <2) 106% 6.0% 110 101 n a (2) LCS-101230-4 LCS-101230-5 LCS-101230-6 4.97 4.97 4.97 5.81 5.78 5.81 117 LCS-101230-13 116 LCS-101230-14 117 LCS-101230-15 4.93 4.93 4.93 6 .1 0 5.87 5.77 124 119 117 Average %RSD 117% 0.49% Average %RSD 120% 3.0% LCS-101230-7 LCS-101230-8 LCS-101230-9 29.9 29.9 29.9 31.2 31.7 31.3 104 LCS-101230-16 106 LCS-101230-17 105 LCS-101230-18 29.6 29.6 29.6 36.4 35.7 37.3 123 121 126 Average %RSD 105% 1.0% Average %RSD 123% 2.0%(1) (1) The average recovery did not meet method acceptance criteria of 100% 20%. (2) NA = Not applicable; LCS was not injected due to an autosampler error. Page 18 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Table 7 continued. Laboratory Control Spike Recovery. ETS-8-044.0 Analyzed 1/10/11 PFBS PFHS Lab ID Spiked Calculated Spiked Concentration Concentration Concentration (ng/mL) (ng/mL) XoRecovery (ng/mL) Calculated Concentration (ng/mL) LCS-101230-1 LCS-101230-2 LCS-101230-3 Average %RSD 0.497 0.497 0.497 0.620 0.578 0.578 119 4.4% 125 116 116 0.498 0.498 0.498 0.627 0.586 0.602 122% 3.3%(1) LCS-101230-4 LCS-101230-5 LCS-101230-6 4.97 4.97 4.97 5.93 119 4.98 5.77 116 4.98 5.72 115 4.98 6.15 5.97 5.86 Average %RSD 117% 1.8% 120% 2.1% LCS-101230-7 LCS-101230-8 LCS-101230-9 Average %RSD 29.9 29.9 29.9 30.4 29.3 29.2 99.3% 2.4% 102 98.0 97.8 29.9 29.9 29.9 30.8 30.1 29.8 101% 1.7% YoRecovery 126 118 121 123 120 118 103 101 99.6 ETS-8-044.0 Analyzed 1/10/11 PFOS (linear) PFOS (linear + branched) Lab ID Spiked Calculated Concentration Concentration (ng/mL) (ng/mL) YoRecovery Lab ID Spiked Calculated Concentration Concentration (ng/mL) (ng/mL) YoRecovery LCS-101230-1 LCS-101230-2 LCS-101230-3 0.497 0.497 0.497 0.536 0.532 0.512 108 LCS-101230-10 107 LCS-101230-11 103 LCS-101230-12 0.492 0.492 0.492 0.559 0.509 0.551 114 103 112 Average %RSD 106% 2.5% Average %RSD 110% 5.3% LCS-101230-4 LCS-101230-5 LCS-101230-6 Average %RSD 4.97 4.97 4.97 5.92 5.84 5.87 118% 0.49% 119 LCS-101230-13 118 LCS-101230-14 118 LCS-101230-15 Average %RSD 4.93 4.93 4.93 5.97 5.69 5.65 117% 3.0% 121 115 115 LCS-101230-7 LCS-101230-8 LCS-101230-9 Average %RSD 29.9 29.9 29.9 30.6 30.7 30.3 102% 0.98% 1 0 2 LCS-101230-16 103 LCS-101230-17 1 0 1 LCS-101230-18 Average %RSD 29.6 29.6 29.6 35.2 36.0 35.9 121% 1.3%<1) 119 122 121 (1) The average recovery did not meet method acceptance criteria of 100% 20%. (2) NA = Not applicable; LCS was not injected due to an autosampler error. Page 19 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Table 7 continued. Laboratory Control Spike Recovery. ETS-8-044.0 Analyzed 1/14/11 Lab ID PFBS Spiked Calculated Spiked Concentration Concentration Concentration (ng/mL) (ng/mL) YoRecovery (ng/mL) LCS-101230-1 LCS-101230-2 LCS-101230-3 0.497 0.497 0.497 0.612 123 0.498 0.589 119 0.498 0.590 119 0.498 Average %RSD 120 1.9% LCS-101230-4 LCS-101230-5 LCS-101230-6 Average %RSD 4.97 4.97 4.97 5.99 5.73 5.78 117% 2.7% 121 115 116 4.98 4.98 4.98 LCS-101230-7 LCS-101230-8 LCS-101230-9 Average %RSD 29.9 29.9 29.9 30.4 30.1 29.9 101% 1.0% 102 101 99.9 29.9 29.9 29.9 PFHS Calculated Concentration (ng/mL) 0.602 0.589 0.589 119% 1.5% 6.03 5.82 5.81 118% 2.0% 31.0 30.5 30.5 103% 1.1% YoRecovery 121 118 118 121 117 117 104 102 102 ETS-8-044.0 Analyzed 1/14/11 PFOS (linear) PFOS (linear + branched) Lab ID Spiked Calculated Concentration Concentration (ng/mL) (ng/mL) YoRecovery Lab ID Spiked Calculated Concentration Concentration (ng/mL) (ng/mL) YoRecovery LCS-101230-1 LCS-101230-2 LCS-101230-3 Average %RSD 0.497 0.497 0.497 0.523 0.517 0.504 103% 2.0% 105 LCS-101230-10 104 LCS-101230-11 1 0 1 LCS-101230-12 Average %RSD 0.492 0.492 0.492 0.522 0.472 0.527 103% 5.9% 106 96.0 107 LCS-101230-4 LCS-101230-5 LCS-101230-6 Average %RSD 4.97 4.97 4.97 5.87 5.66 5.72 116% 1.8% 118 LCS-101230-13 114 LCS-101230-14 115 LCS-101230-15 Average %RSD 4.93 4.93 4.93 6.03 5.69 5.65 117% 3.4% 122 115 115 LCS-101230-7 LCS-101230-8 LCS-101230-9 Average %RSD 29.9 29.9 29.9 31.2 31.6 30.7 104% 1.5% 104 LCS-101230-16 106 LCS-101230-17 103 LCS-101230-18 Average %RSD 29.6 29.6 29.6 34.6 36.0 36.1 120% 2.4% 117 122 122 (1) The average recovery did not meet method acceptance criteria of 100% 20%. (2) NA = Not applicable; LCS was not injected due to an autosampler error. Page 20 of 104 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Table 7 continued. Laboratory Control Spike Recovery. ETS-8-044.0 Analyzed 2/11/11 Lab ID L C S -1 10210-1 LCS-110210-2 LCS-110210-3 Average %RSD LCS-110210-4 LCS-110210-5 LCS-110210-6 Average %RSD LCS-110210-7 LCS-110210-8 LCS-110210-9 Average %RSD PFBS Spiked Calculated Concentration Concentration (ng/mL) (ng/mL) 0.498 0.563 0.498 0.542 0.498 0.581 113 3.5% 4.98 5.37 4.98 5.52 4.98 5.58 110% 1.9% 29.9 29.8 29.9 31.1 29.9 32.0 104% 3.6% Spiked Concentration VoRecovery (ng/mL) 113 0.498 109 0.498 117 0.498 108 4.98 1 1 1 4.98 1 1 2 4.98 1 0 0 29.9 104 29.9 107 29.9 PFHS Calculated Concentration (ng/mL) 0.603 0.594 0.599 120% 0.83% 5.61 5.36 5.96 114% 5.3% 30.7 30.8 32.7 105% 3.3% VoRecovery 121 119 120 113 108 120 103 103 109 ETS-8-044.0 Analyzed 2/11/11 PFOS (lineai) PFOS (linear + branched) Lab ID Spiked Calculated Concentration Concentration (ng/mL) (ng/mL) VoRecovery Lab ID Spiked Calculated Concentration Concentration (ng/mL) (ng/mL) VoRecovery LCS-110210-1 LCS-110210-2 LCS-110210-3 0.498 0.498 0.498 0.650 0.587 0.540 130 LCS-110210-10 118 LCS-110210-11 108 LCS-110210-12 0.502 0.502 0.502 0.539 0.585 0.541 107 117 108 Average %RSD 119% 9.3% Average %RSD 111% 5.0% L C S -1 10210-4 LCS-110210-5 LCS-110210-6 4.98 4.98 4.98 5.43 4.93 5.86 109 LCS-110210-13 99.1 LCS-110210-14 118 LCS-110210-15 5.04 5.04 5.04 6.15 5.38 5.44 122 107 108 Average %RSD 109% 8.7% Average %RSD 112% 7.5% LCS-110210-7 LCS-110210-8 LCS-110210-9 29.9 29.9 29.9 30.8 30.7 32.4 103 LCS-110210-16 103 LCS-110210-17 108 LCS-110210-18 30.2 30.2 30.2 40.7 40.4 39.6 135 134 131 Average %RSD 105% 2.8% Average %RSD 133% 1.6%<1) (1) The average recovery did not meet method acceptance criteria of 100% 20%. (2) NA = Not applicable; LCS was not Injected due to an autosampler error. Page 21 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 8.7 Analytical Method Uncertainty Analytical uncertainty is based on historical QC data that is control charted and used to evaluate method accuracy and precision. The method uncertainty is calculated following ETS-12-012.2. The standard deviation is calculated for the set of accuracy results (in %) obtained for the QC samples. The expanded uncertainty is calculated by multiplying the standard deviation by a factor of 2, which corresponds to a confidence level of 95%. The most recent 50 data points were used to generate the method uncertainty values listed in Table 8. The analytical method uncertainty for PFOS when calculated following the above described procedure was found to be 18%. However, due to potential analytical bias that was observed when quantitating LCS samples containing linear and branched isomers of PFOS, the analytical for PFOS has been expanded to 33%. Table 8. Analytical Uncertainty. Analyte PFBS PFHS PFOS Standard Deviation 10.9 1 1 .0 9.07 Method Uncertainty 2 0 % 2 2 % 33% (1) (1) See section 8.6 o f the report for a discussion of the assigning of the analytical method uncertainty for PFOS. 8.8 Field Matrix Spikes (FMS) Low, mid and high field matrix spikes (FMS) were collected at each sampling point (low and high FMS only at 131R, 134R, and 135R) to verify that the analytical method is applicable to the collected matrix. Field matrix spikes were generated by adding a measured volume of field sample to a container spiked by the laboratory with PFBS (linear), PFHS (linear), and PFOS (linear) prior to shipping sample containers for sample collection. Field matrix spike recoveries within method acceptance criteria of 10030% confirm that "unknown" components in the sample matrix do not significantly interfere with the extraction and analysis of the analytes of interest. Field matrix spike concentrations must be 50% of the sample concentration to be considered an appropriate field spike. Field matrix spikes are presented in section 9 of this report. Table 9. Field Matrix Spike Levels. Sampling Location 136R, 137R, 137s, 137L, 138L 130L, 131L, 132L, 133R, 134S, 134L, 136S 130R, 130S, 131S, 132R, 132S, 133S, 133L, 135S, 135L , 136L, 138S , 138R 131R, 134R, 135R Trip Blank Spike Level Low Mid High Low Mid High Low Mid High Low High Low Mid M id -H ig h High PFBS, ng/mL 0.0972 0.972 9.72 0.972 9.72 97.2 9.72 97.2 972 97.2 972 0.972 9.72 97.2 972 PFHS, ng/mL 0.0961 0.961 9.61 0.961 9.61 96.1 9.61 96.1 961 96.1 961 0.961 9.61 96.1 961 PFOS, ng/mL 0.0978 0.978 9.78 0.978 9.78 97.8 9.78 97.8 978 97.8 978 0.978 9.78 97.8 978 Page 22 of 104 GLP10-01-02: Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 FMSR - Sam ple Concentration f FMS-Avcrage Concentration :Field Sample & Field Sample Dup.) t Spike Concentraton 8.9 Laboratory Matrix Spikes (LMS) The mid FMS sample for DAL GW 144R analyzed on 1/10/11 did not meet method acceptance criteria for PFOS with a recovery of 28.7%. The high FMS sample analyzed on 1/10/11 exceeded the instrument calibration range. Further dilution of the high FMS sample was not performed since the high FMS sample (spike level 978 ng/mL) was not appropriate as compared to the observed sample concentration. The sample set was reanalyzed on 2/28/11 along with a 50 ng/mL laboratory matrix spike. Laboratory matrix spike recoveries within method acceptance criteria of 10030% confirm that "unknown" components in the sample matrix do not significantly interfere with the extraction and analysis of the analytes of interest. See section 9 for a discussion of the PFOS results. 9 Data Summary and Discussion The tables below summarize the sample results and field matrix spike recoveries for the sampling locations as well as the Trip Blanks and rinseate blanks. Results and average values are rounded to three significant figures according to EPA rounding rules. Because of rounding, values may vary slightly from those listed in the raw data. Field matrix spike recoveries meeting the method acceptance criteria of 30%, demonstrate that the method was appropriate for the given matrix and their respective quantitative ranges. DAL GW 134S - The recovery of the low FMS sample for PFHS was 135%. The mid and high FMS samples met method acceptance criteria. Since the low spike was the most appropriate spike level as compared to the sample concentration, the analytical uncertainty has been adjusted for PFHS to 100% 35%. DAL GW 137S - The recovery of the mid FMS sample for PFOS was 58.8%, while the recovery of the high FMS was 59.4%. Since the mid spike was the most appropriate spike level as compared to the sample concentration, the analytical uncertainty has been adjusted for PFOS to 100% 41%. DAL GW 1 4 4 R -The sample set was diluted 1:10 and analyzed on 1/10/11. The recovery of the mid FMS sample for PFOS was 28.7%. The high FMS sample exceeded the instrument calibration range. Further dilution of the high FMS sample was not performed since the high FMS sample (spike level 978 ng/mL) was not appropriate as compared to the sample concentration. The sample set was re-diluted and analyzed on 2/28/11 along with a 49.8 ng/mL laboratory matrix spike. The recovery of the mid FMS sample was 33.4%, and the recovery of the LMS sample was 29.4%. Since the recovery of both matrix spike samples was <50%, no PFOS results will be reported for DAL GW 144R. Page 23 of 104 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Table 10. DAL GW 130R 101105 PFBS PFHS PFOS 3M UM SID Description Concentration (ng/mL) %Recovery GLP10-01-02-11-001 DAL GW 130R0 101105 16.0 NA GLP10-01-02-11-002 DAL GW 130R DB 101105 17.1 NA GLP10-01-02-11-003 DAL GW 130R LS 101105 28.0 118 GLP10-01-02-11-004 DAL G W 130R M S 101105 122 108 GLP10-01-02-11-005 DAL G W 130R H S 101105 998 101 Average Concentration (ng/mL) %RPD 16.6 ng/mL 6.6% Concentration (ng/mL) %Recovery 128 NA 128 NA 140 NC 232 108 1120 103 128 ng/mL 0.0% Concentration (ng/mL) %Recovery 590 NA 576 NA 606 NC 626 NC 1490 92.7 583 ng/mL 2.4% NA = Not Applicable NC = Not Calculated; the endogenous sample concentration Is greater than 2x the spike level. PFBS, PFHS, and PFOS were analyzed on 1/10/11 with a 1:10 dilution. Table 11. DAL GW 130L 101105 PFBS PFHS PFOS 3M UM SID Description GLP10-01-02-11-011 DAL GW 130L0 101105 GLP10-01-02-11-012 D A LG W 130L DB 101105 GLP10-01-02-11-013 D A LG W 130L LS 101105 GLP10-01-02-11-014 DAL GW 130L MS 101105 GLP10-01-02-11-015 DAL GW 130L HS 101105 Average Concentration (ng/mL) %RPD Concentration (ng/mL) %Recovery 1.80 1.73 2.91 13.0 107 NA NA 118 116 108 1.77 ng/mL 4.0% Concentration (ng/mL) %Recovery 14.1 NA 14.6 NA 15.9 25.3 NC 114 119 109 14.4 ng/mL 3.5% Concentration (ng/mL) %Recovery 85.1 NA 80.2 NA 82.1 NC 84.5 182 NC 102 82.7 ng/mL 5.9% NA = Not Applicable NC = Not Calculated; the endogenous sample concentration is greater than 2x the spike level. PFBS, PFHS, and PFOS were analyzed on 1/7/11 with a 1:10 dilution. Page 24 of 104 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Table 12. DAL GW 130S 101105 PFBS PFHS PFOS 3MUM SID Description GLP10-01-02-11-006 DAL GW 130S0 101105 GLP10-01-02-11-007 DAL GW 130S DB 101105 GLP10-01-02-11-008 GLP10-01-02-11-009 GLP10-01-02-11-010 D A LG W 130S LS 101105 DALG W 130S MS 101105 D ALG W 130S HS 101105 Average Concentration (ng/mL) %RPD Concentration (ng/mL) %Recovery 3.30 NA 3.70 13.9 NA 107 109 109 1020 105 3.50 ng/mL 11% Concentration (ng/mL) %Recovery 31.3 31.2 41.8 134 1060 NA NA NC 107 107 31.3 ng/mL 0.32% Concentration (ng/mL) %Recovery 119 NA 115 NA 127 NC 203 87.9 1070 97.4 117 ng/mL 3.4% NA = Not Applicable NC = Not Calculated; the endogenous sample concentration is greater than 2x the spike level. PFBS, PFHS, and PFOS were analyzed on 1/10/11 with a 1:100 dilution. Table 13. DAL GW 131R 101103 PFBS PFHS PFOS 3MUM SID Description GLP10-01-02-11-017 DAL GW 131R 0 101103 GLP10-01-02-11-018 GLP10-01-02-11-019 GLP10-01-02-11-020 DAL GW 131R DB 101103 D A LG W 131R LS 101103 DAL GW 131R HS 101103 Average Concentration (ng/mL) %RPD Concentration (ng/mL) %Recovery 82.9 NA 79.5 184 NA NC 1120 107 81.2 ng/mL 4.2% Concentration (ng/mL) %Recovery 411 NA 414 NA 512 NC 1440 107 413 ng/mL 0.73% Concentration (ng/mL) %Recovery 1490 NA 1530 NA 1610 NC 2700 122 1510 ng/mL 26% NA = Not Applicable NC = Not Calculated; the endogenous sample concentration is greater than 2x the spike level. PFBS, PFHS, and PFOS were analyzed on 1/14/11 with a 1:100 dilution. Page 25 o f 104 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Table 14. DAL GW 131L 101103 PFBS PFHS PFOS 3M L IM S ID Description GLP10-01-02-11-026 GLP10-01-02-11-027 GLP10-01-02-11-028 DAL GW 131L0 101103 D ALG W 131LD B 101103 D A LG W 131LLS 101103 GLP10-01-02-11-029 DAL GW 131L MS 101103 GLP10-01-02-11-030 D A L G W 1 3 1 L H S 101103 Average Concentration (ng/mL) %RPD Concentration (ng/mL) %Recovery 3.42 NA 3.27 NA 4.57 14.7 NC 117 109 109 3.35 ng/mL 4.5% Concentration (ng/mL) %Recovery 2 0 .2 2 1 .2 2 1 .6 32.8 NA NA NC NC 127 111 20.7 ng/mL 4.8% Concentration (ng/mL) %Recovery 33.4 NA 35.1 33.7 43.0 128 NA NC NC 95.9 34.3 ng/mL 5.0% NA = Not Applicable NC = Not Calculated; the endogenous sample concentration is greater than 2x the spike level. PFBS, PFHS, and PFOS were analyzed on 1/7/11 with a 1:10 dilution. Table 15. DALGW 131S 101103 PFBS PFHS PFOS 3MUM SID Description GLP10-01-02-11-021 DAL GW 131S 0 101103 GLP10-01-02-11-022 D A LG W 131S DB 101103 GLP10-01-02-11-023 D A LG W 131S LS 101103 GLP10-01-02-11-024 DAL GW 131S MS 101103 GLP10-01-02-11-025 DAL GW 131S HS 101103 Average Concentration (ng/mL) %RPD Concentration (ng/mL) %Recovery 0.772 0.797 1.98 NA NA 123 1 2 .6 122 1 1 2 114 0.785 ng/mL 3.2% Concentration (ng/mL) %Recovery 4.77 4.48 6.06 16.3 NA NA NC 121 112 112 4.63 ng/mL 6.3% Concentration (ng/mL) YoRecovery 5.39 NA 5.70 NA 5.73 NC 14.5 91.6 1 0 1 97.6 5.55 ng/mL 5.6% NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS, PFHS, and PFOS were analyzed on 1/7/11 with a 1:10 dilution. Page 26 of 104 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Table 16. DAL GW 132R 101102 PFBS PFHS PFOS 3MUM SID Description Concentration (ng/mL) %Recovery GLP10-01-02-11-031 DAL GW 132R 0 101102 8.17 NA GLP10-01-02-11-032 DAL G W 132R DB 101102 GLP10-01-02-11-033 DAL G W 132R LS 101102 7.89 19.3 NA 116 GLP10-01-02-11-034 DAL G W 132R MS 101102 GLP10-01-02-11-035 DAL G W 132R HS 101102 116 1060 111 108 Average Concentration (ng/mL) %RPD 8.03 ng/mL 3.5% Concentration (ng/mL) %Recovery 54.3 NA 51.2 65.4 NA NC 161 113 1130 112 52.8 ng/mL 5.9% Concentration (ng/mL) %Recovery 297 NA 292 NA 306 NC 397 NC 1270 99.7 295 ng/mL 1.7% NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS, PFHS, and PFOS were analyzed on 1/14/11 with a 1:100 dilution. Table 17. DAL GW 132L101103 3MUM SID Description GLP10-01-02-11-041 GLP10-01-02-11-042 GLP10-01-02-11-043 DAL GW 132L 0101103 DALGW 132L DB 101103 DALGW 132L LS 101103 GLP10-01-02-11-044 DAL GW 132L MS 101103 GLP10-01-02-11-045 DAL GW 132L HS 101103 Average Concentration (ng/mL) %RPD PFBS PFHS PFOS Concentration (ng/mL) %Recovery 9.06 8.72 19.5 114 1060 NA NA 109 108 108 8.89 ng/mL 3.8% Concentration (ng/mL) %Recovery 76.7 NA 77.6 NA 85.4 NC 177 104 1140 111 77.2 ng/mL 1.2% Concentration (ng/mL) %Recovery 285 NA 301 NA 367 NC 489 NC 1400 113 293 ng/mL 5.5% N A = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS, PFHS, and PFOS were analyzed on 1/7/11 with a 1:10 dilution. Page 27 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Table 18. DAL GW 132S 101102 3MUM SID Description GLP10-01-02-11-036 DAL GW 132S 0101102 GLP10-01-O2-11-037 DALGW 132S DB 101102 GLP10-01-02-11-038 DALG W 132SLS 101102 GLP10-01-02-11-039 DALGW 132S MS 101102 GLP10-01-02-11-040 DALGW 132S HS 101102 Average Concentration {ng/mL) %RPD PFBS PFHS PFOS Concentration (ng/mL) %Recovery 26.2 NA 25.6 NA 37.3 129 1040 NC 106 104 25.9 ng/mL 2.3% Concentration (ng/mL) %Recovery 203 206 209 300 1220 NA NA NC NC 106 205 ng/mL 1.5% Concentration (ng/mL) %Recovery 593 NA 672 584 612 1570 NA NC NC 95.9 633 ng/mL 12% NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS, PFHS, and PFOS were analyzed on 1/14/11 with a 1:100 dilution. Table 19. DAL GW 133R 101102 3MUM SID Description GLP10-01-02-11-046 DAL GW 133R 0101102 GLP10-01-02-11-047 DALGW 133R DB 101102 GLP10-01-02-11-048 DAL GW 133RLS 101102 GLP10-01-02-11-049 DAL GW 133R MS 101102 GLP10-01-02-11-050 DALGW 133R HS 101102 Average Concentration (ng/mL) %RPD PFBS PFHS PFOS Concentration (ng/mL) %>Recovery 4.78 NA 4.43 NA 5.35 NC 15.3 106 110 104 4.61 ng/mL 7.6% Concentration (ng/mL) %Recovery 32.1 NA 30.1 NA 30.4 NC 41.3 NC 132 105 31.1 ng/mL 6.4% Concentration (ng/mL) %Recovery 62.6 58.9 60.5 68.5 161 NA NA NC NC 103 60.8 ng/mL 6.1% NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS, PFHS, and PFOS were analyzed on 1/10/11 with a 1:10 dilution. Page 28 of 104 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Table 20. DAL GW 133L 101103 3M UM SID Description GLP10-01-02-11-056 GLP10-01-02-11-057 GLP10-01-02-11-058 DAL GW 133L 0101103 DALGW 133L DB 101103 DAL GW 133L LS 101103 GLP10-01-02-11-059 DALGW 133L MS 101103 GLP10-01-02-11-060 DALGW 133L HS 101103 Average Concentration (ng/mL) %RPD PFBS PFHS PFOS Concentration Concentration Concentration (ng/mL) %Recovery (ng/mL) %Recovery (ng/mL) %Recovery 7.71 NA 7.58 NA 18.3 110 114 109 984 100 7.65 ng/mL 1.7% 54.0 NA 52.7 NA 63.7 NC 154 105 1060 105 53.4 ng/mL 2.4% 205 NA 2 0 2 NA 198 NC 283 NC 1210 103 204 ng/mL 1.5% N A= Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS, PFHS, and PFOS were analyzed on 1/10/11 with a 1:10 dilution. Table 21. DAL GW 133S 101103 3M UM SID Description GLP10-01-02-11-051 GLP10-01-02-11-052 GLP10-01-02-11-053 GLP10-01-02-11-054 GLP10-01-02-11-055 DAL GW 133S 0101103 DALGW 133S DB 101103 DAL GW 133S LS 101103 DAL GW 133S MS 101103 DALGW 133S HS 101103 Average Concentration (ng/mL) %RPD PFBS PFHS PFOS Concentration (ng/mL) %Recovery 14.0 14.0 25.1 117 966 NA NA 114 106 97.9 14.0 ng/mL 0.0% Concentration (ng/mL) %Recovery 92.0 NA 91.0 NA 104 NC 192 1050 105 99.7 91.5 ng/mL 1.1% Concentration (ng/mL) %Recovery 228 NA 2 2 0 NA 235 NC 330 NC 1200 99.8 224 ng/mL 3.6% NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS, PFHS, and PFOS were analyzed on 1/10/11 with a 1:10 dilution. Page 29 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Table 22. DAL GW 134R 101105 3M UNIS ID Description GLP10-01-02-11-061 GLP10-01-02-11-062 GLP10-01-02-11-063 GLP10-01-02-11-064 DAL GW 134R 0101105 DAL GW 134RDB 101105 DALGW 134R LS 101105 DALGW 134R HS 101105 Average Concentration (ng/mL) %RPD PFBS PFHS PFOS Concentration (ng/mL) VoRecovery 59.9 52.5 162 1050 NA NA 109 102 56.2 ng/mL 13% Concentration (ng/mL) %Recovery 526 479 590 1450 NA NA NC 98.6 503 ng/mL 9.4% Concentration (ng/mL) %Recovery 1530 1310 1430 NA NA NC 2310 91.0 1420 ng/mL 15% NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS, PFHS, and PFOS were analyzed on 1/14/11 with a 1:100 dilution. Table 23. DALGW 134L 101105 3NILINIS ID Description GLP10-01-02-11-070 GLP10-01-02-11-071 GLP10-01-02-11-072 DAL GW 134L 0101105 DALGW 134L DB 101105 DAL GW 134L LS 101105 GLP10-01-02-11-073 GLP10-01-02-11-074 DALGW 134L MS 101105 DALGW 134L HS 101105 Average Concentration (ng/mL) 1 %RPD PFBS PFHS PFOS Concentration (ng/mL) %Recovery 11.7 1 2 .1 22.3 NA NA 107 110 101 N A (1> N A <1> 11.9 ng/mL 3.4% Concentration (ng/mL) %Recovery 112 112 120 203 N A <1) NA NA NC 94.7 N A (1) 112 ng/mL 0.0%, Concentration (ng/mL) %Recovery 571 586 617 646 1640 NA NA NC NC 109 579 ng/mL 2.6% NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS and PFHS were analyzed on 1/10/11 with a 1;10 dilution. PFOS was analyzed on 1/14/11 with a 1:50 dilution. (1) A dilution of the sample was not prepared as the spike level was not appropriate as compared to the sample concentrations. Page 30 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Table 24. DAL GW 134S 101105 3M LIMS ID Description GLP10-01-02-11-065 DAL GW 134S 0101105 GLP10-01-02-11-066 DALGW 134S DB 101105 GLP10-01-02-11-067 DALG W 134SLS 101105 GLP10-01-02-11-068 DALGW 134S MS 101105 GLP10-01-02-11-069 DALGW 134S HS 101105 Average Concentration (ng/mL) %RPD PFBS PFHS PFOS Concentration (ng/mL) %Recovery 0.146 NA 0.140 NA 1.27 116 1 1 .6 102 118 105 0.143 ng/mL 4.2% Concentration (ng/mL) %Recovery 1.76 NA 1.65 NA 3.00 135(1) 13.2 120 104 106 1.71 ng/mL 6.5% w Concentration (ng/mL) %Recovery 11.3 NA 11.5 NA 1 0 .2 NC 22.4 112 119 110 11.4 ng/mL 1.8% N A = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS, PFHS and PFOS were analyzed on 1/7/11 with a 1:5 dilution. (1) The field matrix spike did not meet method acceptance criteria of 100 30%. (2) The analytical uncertainty has been adjusted to 35%. Table 25. DAL GW 135R 101105 3 M L IM S ID Description GLP10-01-02-11-075 GLP10-01-02-11-076 GLP10-01-02-11-077 GLP10-01-02-11-078 DAL GW 135R 0101105 DALGW 135R DB 101105 DAL GW 135RLS 101105 DALGW 135R HS 101105 Average Concentration (ng/mL) %RPD PFBS PFHS PFOS Concentration (ng/mL) %Recovery 82.1 NA 79.9 195 1150 NA 117 110 81.0 ng/mL 2.7% Concentration (ng/mL) %Recovery 847 NA 831 NA 914 NC 1900 110 839 ng/mL 1.9% Concentration (ng/mL) %Recovery 903 NA 880 NA 955 NC 1890 102 892 ng/mL 2.6% N A= Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS, PFHS, and PFOS were analyzed on 1/14/11 with a 1:100 dilution. Page 31 of 104 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Table 26. DAL GW 135L 101105 3M UNIS ID Description GLP10-01-02-11-084 DAL GW 135L 0101105 GLP10-01-02-11-085 DALGW 135L DB 101105 GLP10-01-02-11-086 GLP10-01-02-11-087 GLP10-01-02-11-088 D ALG W 135LLS 101105 DALGW 135L MS101105 DALGW 135L HS 101105 Average Concentration (ng/mL) %RPD PFBS PFHS PFOS Concentration (ng/mL) VoRecovery 5.84 5.62 16.5 120 1060 NA NA 111 118 108 5.73 ng/mL 3.8% Concentration (ng/mL) %Recovery 35.4 36.3 48.0 150 NA NA NC 119 1090 110 35.9 ng/mL 2.5% Concentration (ng/mL) 23.9 21.3 39.8 134 1030 %Recovery NA NA NC 114 103 22.6 ng/mL 12% N A = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS and PFHS were analyzed on 1/14/11 with a 1:100 dilution. PFOS was analyzed on 2/11/11 with a 1:10 dilution. Page 32 of 104 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Table 27. DAL GW 135S 101105 3M UNIS ID Description GLP10-01-02-11-079 GLP10-01-02-11-080 GLP10-01-02-11-081 GLP10-01-02-11-082 GLP10-01-02-11-083 DAL GW 135S 0101105 DALGW 135S DB 101105 DALG W 135SLS 101105 DALGW 135S MS 101105 DALGW 135S HS 101105 Average Concentration (ng/mL) %RPD PFBS PFHS PFOS Concentration (ng/mL) %Recovery 0.794 NA 0.803 1.94 11.4 NA 117 109 N A <1) N A (1) 0.799 ng/mL 1.1% Concentration (ng/mL) %Recovery 6.35 NA 6.15 NA 7.26 105 16.8 N A (1) 110 N A (1) 6.25 ng/mL 3.2% Concentration (ng/mL) %Recovery 5.01 NA 4.75 NA 5.59 NC 14.8 N A (1) 101 N A <1) 4.88 ng/mL 5.3% NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS, PFHS and PFOS were analyzed on 1/7/11 without dilution. (1) A dilution of the sample was not prepared as the spike level was not appropriate as compared to the sample concentrations. Table 28. DAL GW 136L 101103 3NILINIS ID Description GLP10-01-02-11-094 DAL GW 136L 0101103 GLP10-01-02-11-095 DALGW 136L DB 101103 GLP10-01-02-11-096 GLP10-01-02-11-097 DALG W 136LLS 101103 DALGW 136L MS 101103 GLP10-01-02-11-098 DALGW 136L HS 101103 Average Concentration (ng/mL) %RPD PFBS PFHS PFOS Concentration (ng/mL) %Recovery 2.43 NA 2.63 NA 13.5 113 103 103 976 100 2.53 ng/mL 7.9% Concentration (ng/mL) %Recovery 15.5 NA 16.8 NA 27.2 115 117 1020 105 104 16.2 ng/mL 8.0% Concentration (ng/mL) YoRecovery 75.7 NA 82.7 NA 91.9 NC 171 93.9 1110 105 79.2 ng/mL 8.8% NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS, PFHS and PFOS were analyzed on 1/10/11 w itha 1:10 dilution. Page 33 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Table 29. DAL GW 136S 101103 3NI LINIS ID Description GLP10-01-02-11-089 GLP10-01-02-11-090 GLP10-01-02-11-091 GLP10-01-02-11-092 GLP10-01-02-11-093 DAL GW 136S 0101103 DAL GW 136SDB 101103 D ALG W 136SLS 101103 DALGW 136S MS 101103 DAL GW136S HS101103 Average Concentration (ng/mL) %RPD PFBS PFHS PFOS Concentration (ng/mL) %Recovery 2.52 NA 2.57 NA 3.66 NC 13.5 113 101 101 2.55 ng/mL 2.0% Concentration (ng/mL) %Recovery 16.0 NA 16.9 NA 17.7 NC 27.1 111 114 102 16.5 ng/mL 5.5% Concentration (ng/mL) %Recovery 85.5 NA 88.7 NA 87.2 NC 94.6 NC 180 95.0 87.1 ng/mL 3.7% NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS, PFHS and PFOS were analyzed on 1/10/11 with a 1:10 dilution. Table 30. DAL GW 137L 101109 3M LINIS ID Description GLP10-01-02-11-104 GLP10-01-02-11-105 DAL GW 137L 0101109 DALGW 137L DB 101109 GLP10-01-02-11-106 GLP10-01-02-11-107 GLP 10-01-02-11-108 DALG W 137LLS 101109 DALGW 137L MS 101109 DALGW 137L HS 101109 Average Concentration (ng/mL) %RPD PFBS PFHS PFOS Concentration (ng/mL) %Recovery 0.0812 0.0833 0.190 1 .2 2 10.7 NA NA 111 117 109 0.0823 ng/mL 2.6% Concentration (ng/mL) %Recovery 0.117 0 .1 2 1 0.240 1.25 NA NA 126 118 1 0 .8 111 0.199 ng/mL 3.4% Concentration (ng/mL) %Recovery 0.877 0.909 0.948 1.79 NA NA NC 91.7 1 0 .0 93.1 0.893 ng/mL 3.6% N A= Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS, PFHS and PFOS were analyzed on 1/7/11 without dilution. Page 34 o f 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Table 31. DAL GW 137S 101109 3M UM SID Description GLP10-01-02-11-099 GLP10-01-02-11-100 GLP10-01-02-11-101 GLP10-01-02-11-102 GLP10-01-02-11-103 DAL GW 137S 0101109 DALGW 137S DB 101109 DAL GW 137SLS 101109 DALGW 137S MS 101109 DALGW 137S HS 101109 Average Concentration (ng/mL) YoRPD PFBS PFHS PFOS Concentration (ng/mL) %Recovery 0.0990 0.104 0.206 1 .2 1 1 0 .6 NA NA 108 114 108 0.102ng/mL 4.9% Concentration (ng/mL) %Recovery 0.0886 NA 0.0942 NA 0 .2 0 1 1.15 10.4 114 110 107 0.0914 ng/mL 6.1% Concentration (ng/mL) %Recovery 0.367 NA 0.263 NA 0.328 NC 0.890 6 .1 2 5 8 .8 <1) 5 9 .4 <1) 0.315 ng/mL 33% 3> NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS, PFHS and PFOS were analyzed on 1/7/11 without dilution. (1) The field matrix spike did not meet method acceptance criteria of 100 30%. (2) The analytical uncertainty for PFOS has been adjusted for FMS recovery to 41 %. (3) The RPD did not meet method acceptance criteria of 20%. Page 35 of 104 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Table 32. DAL GW 138S 101110 3M LIMS ID Description GLP10-01-02-11-109 GLP10-01-02-11-110 GLP10-01-02-11-111 GLP10-01-02-11-112 GLP10-01-02-11-113 DAL GW 138S 0101110 DALGW 138S DB 101110 DAL GW 138SLS 101110 DALGW 138S MS 101110 DAL GW 138SHS 101110 Average Concentration (ng/mL) %RPD PFBS PFHS PFOS Concentration (ng/mL) %Recovery 4.74 NA 4.63 NA 16.2 118 99.8 97.9 949 97.2 4.69 ng/mL 2.3% Concentration (ng/mL) %Recovery 24.0 22.9 NA NA 35.4 NC 119 99.4 991 101 23.5 ng/mL 4.7% Concentration (ng/mL) %Recovery 252 NA 238 NA 256 NC 307 NC 1210 98.7 245 ng/mL 5.7% NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS, PFHS and PFOS were analyzed on 1/10/11 with a 1:50 dilution. Table 33. DAL GW 138L 101110 3M LIMS ID Description GLP10-01-02-11-114 GLP10-01-02-11-115 GLP10-01-02-11-116 GLP10-01-02-11-117 GLP10-01-02-11-118 DAL GW 138L 0101110 DALGW 138L DB 101110 D ALG W 138LLS 101110 DALGW 138L MS 101110 DALGW 138L HS 101110 Average Concentration (ng/mL) %RPD PFBS PFHS PFOS Concentration (ng/mL) %Recovery 0.0460 0.0485 0.157 1.16 NA NA 113 114 1 0 .8 111 0.0473 ng/mL 5.3% Concentration (ng/mL) %Recovery 0.143 NA 0.144 NA 0.259 1.28 120 118 10.9 112 0.144 ng/mL 0.70% Concentration (ng/mL) %Recovery 0.581 NA 0.580 0.684 1.29 NA NC 72.5 8.42 80.2 0.581 ng/mL 0.17% NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS, PFHS and PFOS were analyzed on 1/7/11 without dilution. Page 36 of 104 GLP10-01 -02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Table 33. DAL GW CW26R 101110 PFBS PFHS PFOS 3MLINISID Description GLP10-01-02-11-119 GLP10-01-02-11-120 GLP10-01-02-11-121 GLP10-01-02-11-122 GLP10-01-02-11-123 DAL GW CW 26R0 101110 DAL GW CW26R DB 101110 DAL GW CW26R LS 101110 DAL GW CW26R MS 101110 DAL GW CW26R HS 101110 Average Concentration (ng/mL) %RPD Concentration (ng/mL) %Recovery 8.14 NA 8.40 NA 19.2 112 105 N A (1) 100 N A (1) 8.27 ng/mL 3.1% Concentration (ng/mL) XRecovery 61.7 64.4 73.9 155 N A <1) NA NA NC 95.7 N A (1) 63.1 ng/mL 4.3% Concentration (ng/mL) %Recovery 455 NA 446 NA 439 NC 526 NC 1470 104 451 ng/mL 2.0% NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS and PFHS were analyzed on 1/10/11 with a 1:10 dilution. PFOS were analyzed on 1/14/11 with a 1:50 dilution. (1) A dilution of the sample was not prepared as the spike level was not appropriate as compared to the sample concentration. Table 34. DAL GW CW26L 101110 PFBS PFHS PFOS 3NIUNISID Description GLP10-01-02-11-124 DAL GW CW26L 0101110 GLP10-01-02-11-125 GLP10-01-02-11-126 GLP10-01-02-11-127 DAL GW CW26L DB 101110 DAL GW CW 26LLS 101110 DAL GW CW26L MS 101110 GLP10-01-02-11-128 DAL GW CW26L HS 101110 Average Concentration (ng/mL) %RPD Concentration (ng/mL) %Recovery 13.2 12.5 23.3 107 N A (1) NA NA 108 96.9 N A <1> 12.9 ng/mL 5.4% Concentration (ng/mL) %Recovery 95.6 90.2 102 183 N A (1) NA NA NC 93.8 N A (1) 92.9 ng/m Li 5.8% Concentration (ng/mL) %Recovery 8 8 8 NA 808 NA 896 NC 855 NC 1840 101 848 ng/mL 9.4% NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS and PFHS were analyzed on 1/10/11 with a 1:10 dilution. PFOS were analyzed on 1/14/11 with a 1:50 dilution. (1) A dilution of the sample was not prepared as the spike level was not appropriate as compared to the sample concentration. Page 37 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Table 35. DAL GW 140R101104 3 M U M S ID Description GLP10-01-02-11-129 GLP10-01-02-11-130 GLP10-01-02-11-131 GLP10-01-02-11-132 GLP10-01-02-11-133 DAL GW 140R 0101104 DALGW 140R DB 101104 DAL GW 140R LS 101104 DAL GW 140R MS 101104 DALGW 140R HS 101104 Average Concentration (ng/mL) %RPD PFBS PFHS PFOS Concentration (ng/mL) %Recovery 1.65 NA 1.61 NA 11.9 106 96.4 N A (1) 97.5 N A <1) 1.63 ng/mL 2.5% Concentration (ng/mL) %Recovery 17.2 NA 17.2 NA 27.2 104 115 N A (1) 102 N A (1) 17.2 ng/mL 0.0% Concentration (ng/mL) %Recovery 140 131 139 229 N A <1) NA NA NC 95.6 N A (1) 136 ng/mL 6.6% NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. (1) A dilution of the sample was not prepared as the spike level was not appropriate as compared to the sample concentration. Table 36. DAL GW 141R 101110 3MLIMS ID Description GLP10-01-02-11-134 GLP10-01-02-11-135 GLP10-01-02-11-136 DAL GW 141R0 101110 DAL GW 141R DB 101110 DAL GW 141R LS 101110 GLP10-01-02-11-137 DAL GW 141R MS 101110 GLP10-01-02-11-138 DAL GW 141RHS 101110 Average Concentration (ng/mL) %RPD PFBS PFHS PFOS Concentration (ng/mL) %Recovery 0.0444 NA 0.0418 1 0 .1 96.7 NA 103 99.4 977 101 0.0431 ng/mL 6.0% Concentration (ng/mL) %Recovery 0.273 NA 0.243 10.4 96.2 N A <1) NA 106 99.8 N A <1) 0.258 ng/mL 12% Concentration (ng/mL) %Recovery 4.48 3.97 11.4 81.2 N A (1) NA NA 73.4 78.7 N A (1) 4.23 ng/mL 12% NA = Not Applicable PFHS and PFOS were analyzed on 1/10/11 with a 1:10 dilution. PFBS was analyzed on 2/11/11. The sample, sample duplicate and LS were analyzed without a dilution, the MS with a 1:10 dilution, and the HS with a 1:50 dilution. (1) A dilution of the sample was not prepared as the spike level was not appropriate as compared to the sample concentrations. Page 38 of 104 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Table 37. DAL GW 142R 101110 PFBS PFHS PFOS 3MLIMS ID Description Concentration Concentration (ng/mL) %Recovery (ng/mL) XRecovery GLP10-01-02-11-139 DAL GW 142R 0101110 1.69 NA 1 0 .0 NA GLP10-01-02-11-140 DALGW 142R DB 101110 1.67 NA 9.96 NA GLP10-01-02-11-141 DALGW 142R LS 101110 11.9 105 19.8 102 GLP10-01-02-11-142 DAL GW 142R MS 101110 98.0 99.1 108 102 GLP10-01-02-11-143 DALG W 142RHS 101110 N A (1) N A <1) N A (1) N A (1) Average Concentration (ng/mL) 1 %RPD 1.68 ng/mL 1.2% 9.98 ng/mL 0.40% NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS, PFHS and PFOS were analyzed on 1/10/11 with a 1:10 dilution. (1) A dilution of the sample was not prepared as the spike level was not appropriate as compared to the sample concentrations. Concentration (ng/mL) %Recovery 1 1 1 NA 104 NA 118 200 N A (1) NC 94.6 N A <1) 108 ng/mL 6.5% Table 38. DAL GW 144R 101110 3MLIMS ID Description GLP10-01-02-11-144 GLP10-01-02-11-145 GLP10-01-02-11-146 GLP10-01-02-11-147 GLP10-01-02-11-148 DAL GW 144R 0101110 DALGW 144R DB 101110 DALG W 144RLS 101110 DAL GW 144R MS 101110 DALGW 144R HS 101110 Average Concentration (ng/mL) %RPD PFBS PFHS PFOS Concentration (ng/mL) %Recovery 1.98 1.91 1 1 .6 98.5 N A (1) NA NA 99.3 99.3 N A (1) 1.95 ng/mL 3.6% Concentration (ng/mL) %Recovery 8.79 8.35 17.9 103 N A (1) NA NA 97.1 98.3 N A (1) 8.57 ng/mL 5.1% Concentration (ng/mL) %Recovery Not Reported Not Reported * NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. PFBS, PFHS and PFOS were analyzed on 1/10/11 with a 1;10 dilution. (1) A dilution of the sample was not prepared as the spike level was not appropriate as compared to the sample concentrations. (2) Not Reported; The matrix spike samples prepared and analyzed for this sampling location for PFOS had recoveries <50%. Page 39 of 104 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Table 39. Trip Blank 3M UNIS ID GLP10-01-02-11-150 GLP10-01-02-11-151 GLP10-01-O2-11-152 GLP10-01-02-11-153 GLP10-01-02-11-154 Description TRIP BLANK 1 0 TRIP BLANK 1 LS TRIP BLANK 1 MS TRIP BLANK 1 MHS TRIP BLANK 1 HS NA = Not Applicable Table 40. Trip Blank 2 3NILIMSID GLP10-01-02-11-155 GLP10-01-02-11-156 GLP10-01-02-11-157 GLP10-01-02-11-158 GLP10-01-02-11-159 Description TRIP BLANK 2 0 TRIP BLANK 2 LS TRIP BLANK 2 MS TRIP BLANK 2 MHS TRIP BLANK 2 HS NA = Not Applicable PFBS PFHS PFOS Concentration (ng/mL) <0.0250 1 .1 2 1 0 .6 98.6 1050 %Recovery NA 115 109 101 108 Concentration (ng/mL) <0.0250 1 .1 0 10.5 101 1050 %Recove/y NA 114 109 105 109 Concentration (ng/mL) <0.250 1.04 10.3 104 930 %Recovery NA 106 105 106 95.1 PFBS PFHS PFOS Concentration (ng/mL) <0.0250 1 .1 2 1 0 .8 97.1 1040 %Recovery NA 115 111 100 107 Concentration (ng/mL) <0.0250 1.09 1 0 .8 99.3 1040 %Recovery NA 113 112 103 108 Concentration (ng/mL) <0.250 1 .0 1 10.7 105 952 %Recovery NA 103 109 107 97.3 Page 40 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Table 41. Trip Blank 3 3 M L IM S ID GLP10-01-02-11-160 GLP10-01-02-11-161 GLP10-01-02-11-162 GLP10-01-02-11-163 GLP10-01-02-11-164 Description TRIP BLANK 3 0 TRIP BLANK 3 LS TRIP BLANK 3 MS TRIP BLANK 3 MHS TRIP BLANK 3 HS NA = Not Applicable Table 42. Trip Blank 4 3MLIMS ID GLP10-01-02-11-165 GLP10-01-02-11-166 GLP10-01-02-11-167 GLP10-01-02-11-168 GLP10-01-02-11-169 Description TRIP BLANK 4 0 TRIP BLANK 4 LS TRIP BLANK 4 MS TRIP BLANK 4 MHS TRIP BLANK 4 HS NA = Not Applicable PFBS PFHS PFOS Concentration (ng/mL) <0.0250 1 .1 1 10.3 99.2 1030 %Recovery NA 114 106 102 106 Concentration (ng/mL) <0.0250 1.08 10.4 101 1040 %Recovery NA 112 108 105 108 Concentration (ng/mL) <0.250 1.03 9.96 105 925 %Recovery NA 105 102 107 94.6 PFBS PFHS PFOS Concentration (ng/mL) <0.0250 1 .1 0 10.7 99.5 1020 %Recovery NA 113 110 102 105 Concentration (ng/mL) <0.0250 1.09 1 0 .6 101 1020 VoRecovery NA 113 110 105 106 Concentration (ng/mL) <0.250 0.983 1 0 .2 103 909 %Recovery NA 101 104 105 92.9 Page 41 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Table 43. Rinseate Blanks 3 M L IM S ID GLP10-01-02-11-016 GLP10-01-02-11-149 Description DALGW 130L RB 101105 DALGW 144R RB 101110 PFBS PFHS PFOS Concentration (ng/mL) <0.0250 <0.0250 %Recovery NA NA Concentration (ng/mL) <0.0250 <0.0250 %Recovery NA NA Concentration (ng/mL) <0.250 <0.250 %Recovery NA NA N A= Not Applicable Table 44. GLP10-01-02-12 Soil Equipment Rinseate Blank 3 M L IM S ID GLP10-01 -02-12-009 Description DAL SS 607R RB 0040 NA = Not Applicable PFBS PFHS PFOS Concentration (ng/mL) <0.0250 %Recovery NA Concentration (ng/mL) <0.0250 %Recovery NA Concentration (ng/mL) <0.250 %Recovery NA Page 42 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 ; afgfps 10 Conclusion J jjj Laboratory control spikes and field matrix spikes were used to determine the analytical method accuracy and precision for PFBS, PFHS, and PFOS. Analysis was successfully completed following 3M Environmental Laboratory method ETS-8-044.0 described herein. 11 Data/Sample Retention All remaining samples and associated project data (hardcopy and electronic) will be archived according to 3M Environmental Laboratory standard operating procedures. 1 2 , Attachments Attachment A: Protocol Amendment 11 (General Project Outline) Attachment B: Representative Chromatograms and Calibration Curves Attachment C: Analytical Method Attachment D: Method Deviation Page 43 of 104 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 13 Signatures Cleston Lange, Ph.D., 3M Principal Analytical Investigator $ 7 /0 2 6 0 Date William K. Reagen, Ph.D., 3M Environmental Laboratory Department Manager Date Page 44 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Attachment A: Protocol A mendment GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Analytical Protocol: GLP10-01-02 Amendment 11 Study Title Analysis of Perfluorooctane Sulfonate (PFOS), Perfluorohexane Sulfonate (PFHS) and Perfluorobutane sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M Decatur Phase 3 Site-Related Monitoring Program PROTOCOL AMENDMENT NO. 11 Amendment Date: October 20, 2010 Performing Laboratory 3M Environmental, Health, and Safety Operations 3M Environmental Laboratory Building 260-5N-17 Maplewood, MN 55144-1000 Laboratory Project Identification GLP10-01-02 Sampling Event Former Sludge Incorporation Area (FSIA) Groundwater Page 1 of 7 Page 46 of 104 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Analytical Protocol: GLP10-01-02 Amendment 11 This amendment modifies the following portion of protocol: "Analysis of PFOS, PFHS and PFBS in Groundwater, Soil and Sediment for the 3M Decatur Phase 3 Site-Related Monitoring Program" Protocol reads: No changes to the wording of the protocol are required. A mend to read: No changes to the wording of the protocol are required. This amendment only addresses and documents the addition of the General Project Outline (GPO) for the collection and analysis of groundwater samples from Decatur, AL, and conducted as part of the 3M Decatur Phase 3 Program for PFOS, PFHS and PFBS (GLP10-01-02). The anticipated sample collection will occur around the timeframe of October 25, 2010. The groundwater samples for this sampling event will be entered into the 3M Environmental Laboratory LIMS as project GLP10-01-02-11 and reported as interim report GLP10-01-02-11, (reflecting study GLP10-01-02 and amendment -11). Reason: The reason for this amendment is to document the General Project Outline (GPO) which describes the anticipate groundwater sample collection event to be conducted for the 3M Decatur, AL facility. The GPO is four pages in length and included as attached to this amendment form. Page 2 of 7 Page 47 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Analytical Protocol: GLP10-01-02 Amendment 11 Amendment Approval Page 3 of 7 Page 48 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Analytical Protocol: GLP10-01-02 Amendment 11 Environmental Health & Safety Operations, Environmental Laboratory General Project Outline To: From: cc: Date: Subject: Gary Hohenstein, 3M EHS&Opns Susan Wolf, 3M EHS&Opns; Environmental Lab William Reagen, 3M EHS&Opns; Environmental Lab Cliffton Jacoby, 3M EHS&Opns; Environmental Lab Jai Kesarl, Weston Solutions Charles Young, Weston Solutions Tim Frinak, Weston Solutions October 20,2010 Analysis of Perfluorooctane Sulfonate (PFOS), Perfluorohexane Sulfonate (PFHS) and Perfluorobutane sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M Decatur Phase 3 Site-Related Monitoring Program; GLP Interim Report 11 - Former Sludge Incorporation Area (FSIA) Groundwater 1 General Project Information C o n ta c ts Lab Request Number Six D igit Departm ent Num ber Project Schedule/Test Dates 3M S ponsor Representative Gary Flohenstein 3M EHS Operations 3M Building 224-5W-03 Saint Paul, MN 55144-1000 Phone: (651)737-3570 aahohenstein@ m m m .com 3M Environm ental Laboratory M anagem ent William K. Reagen 3M EFIS Opns, Environmental Laboratory 260-5N-17 651 733-9739 wkreaaen@ m m m .com Principal A nalytical Investigator Cleston Lange 3M EHS Opns, Environmental Laboratory 260-5N-17 651 733-9860 cclanae@ m m m .com Sampling C oordinator Timothy Frinak Weston Solutions T im o th v .frin a k @ w e s to n s o lu tio n s .c o m Phone: (334)-332-9123 GLP10-01 -02-11 Dept #530711, Project #0022674449 Sampling scheduled for the week of October 25, 2010 All verbal and written correspondence will be directed to Gary Hohenstein. Page 4 of 7 Page 49 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Analytical Protocol: GLP10-01-02 Amendment 11 2 Background Information and Project Objective(s) The 3M EHS Operations Laboratory (3M Environmental Lab) will receive and analyze groundwater samples collected from twenty-seven groundwater wells for Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) from the Former Sludge Incorporation Area (FSIA). Analyses will be conducted under the GLP requirements of EPA TSCA Good Laboratory Practice Standards 40 CFR 792. Groundwater samples from Decatur, AL will be collected by Weston Solutions personnel the week of October 25, 2010. The 3M Environmental Laboratory will prepare the sample bottles with all required spikes to ensure that results for PFBS, PFHS, and PFOS are of a known precision and accuracy. The final report will be submitted to Gary Hohenstein and Jai Kesari upon completion under interim report GLP1001-02-11. 3 Project Schedule Sample collection bottles will be prepared by 3M Environmental Laboratory for sampling the week of June 21, 2010. Sample bottles will be shipped in coolers overnight to 3M Decatur for arrival on Friday, June 18,2010. Sample bottles should be stored refrigerated on-site until sample collection. Martin Smith \ Weston Trailer 3M Decatur Plant 1400 State Docks Road Decatur, Alabama 35601 4 Test Parameters The targeted limit of quantitation will be 0.025 ng/mL (ppb) for PFBS, PFHS, and PFOS. A total of thirty-four sampling locations have been specified. For each sampling location, a sample, sample duplicate and a minimum of two field matrix spikes will be collected. Table 1 indicates the well ID and corresponding field spike levels. The "fill to here" line on each 250 mL Nalgene bottle will be 200 mL. Four sets of trip blanks consisting of reagent-grade water, a low-level trip blank spike, mid-level field spike, mid-high field spike, and a high-level trip blank spike will be prepared at the 3M Environmental Laboratory and sent to the sampling location with the other bottles. Two additional bottles will be prepared to be used for the preparation of the equipment rinseate blanks. A total of 189 sample bottles will be prepared. Page 5 of 7 Page 50 o f 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Analytical Protocol: G LP10-01-02 Amendment 11 Table 1. Sampling Locations and Field Matrix Spike levels. Well No. Sample Level Spike Cone. (ng/mL) 136R, 137R,137S,137L, 138L 130L, 131L, 131S, 133R, 134S, 135S,136S 130R,130S,132R, 132L, 132S, 133S, 133L, 134L, 135L, 136L, 138S, 138R, CW26R, CW26L, 140R, 141R, 142R, 143, and 144R 131R, 134R, 135R Trip Blank Set 1,2, 3, and 4 Low Mid High Low Mid High Low Mid High Low High Low Mid Mid-High High 0 .1 1 .0 10 1 10 100 10 100 1000 100 1000 1 10 100 1000 5 Test Methods Samples will be prepared and analyzed by LC/MS/MS following ETS-8-044.0 "Determination of Perfluorinated Compounds In Water by High Performance Liquid Chromatography/Mass Spectrometry Direct Injection Analysis". The data quality objectives for these studies are quantitative results for the target analytes with an analytical accuracy of 10030%. Field matrix spikes not yielding recoveries within 10030% will be addressed in the report and the final accuracy statement may be adjusted accordingly. Based on the results from previously collected samples from the FSIA (GLP10-01 -02-07), most sampling locations will require dilution with laboratory reagent water prior to sample analysis by ETS-8-044.0. Alternately, samples may be analyzed by ETS 8-154.3 "Determination of Perfluorinated Acids, Alcohols, Amides, and Sulfonates In Water By Solid Phase Extraction and High Performance Liquid Chromatography/Mass Spectrometry". 6 Reporting Requirements For each sampling location, the report will contain the results for the sample, sample duplicate, and field matrix spikes. Trip blank and trip blank spikes will be reported for the sampling event as will any equipment/rinseate blanks prepared in the field. Laboratory control spikes of reagent water prepared at the time of sample preparation will also be reported and used to evaluate the overall method accuracy and precision. Method blanks of reagent water prepared at the time of sample preparation will be used to determine the method detection limit. For those sampling locations where the field matrix spike level was not appropriate, due to higher than expected analyte concentrations, a laboratory matrix spike may be prepared and will be included in the final report. 7 Email Correspondence Attachment A: Sampling Bottle Request Page 6 of 7 Page 51 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Analytical Protocol: GLP10-01-02 . Amendment 11 Attachment A Bottle Request DecatuO0r2nG1-8sr1iot.ue1n2F9dS.w1IA4a5teW.0r0eS0lal4smpling DATE REQUESTED: 18 October 2010 DATE REQUIRED: 25 October 2010 This request addresses the bottle requirements for the following wells: 130R 111133330101LRSS 132L 133R 111333433RLS 135S 135L 111333666RLS CC11W1W33388822LRS66LR 143R 144R 131L 132R 132S 113344LS 135R 137R 137S 137L 111444201RRR Total Wells: 34 Sample Summary No. of S432a4mples TGSRrairinompsuepBnaldletaewnTSakytasepmreple Comment WAniltlicnipeeadteH1PpLeCr cwooatleerr Note: Some of the wells have limited volume so the smaller the volume requirements the better. SHIPPING INFORMATION Please ship to the following address: D32M1M54ea60cr0-aD5ttiS5uent2craa-S,t6tmAeu18LrDit9hoP3cl5\ak6Wns0t1Resotaodn Field Office Page 7 of 7 Page 52 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Attachm ent B: R epresentative Sam ple C hrom atogram s and Calibration C urve Page 53 of 104 *** Buster J2930203 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Batch Name: bll0107a.dab b110107a.rdb (PFBS): "Quadratic" Regression ("1 / x" weighting): y = -7.8e+003 xA2 + 1.03e+006 x + 5.1e+003 (r = 0.9997) 4.8e7 4.6e7 4.4e7 4.2e7 4.0e73.8e7 3.6e7 3.4e7 3.2e7 3.0e7 2.8e7 2.6e7 2.4e7 2.2e7 2.0e7 1.8e7 1.6e7 1.4e7 1.2e7 1.0e7 8.0e6 6.0e6 4.0e6 2.0e6- 0.0 / / 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 Concentration, ng/mL Printing Time: 3:12:03 PM Page 1 of 1 Printing Date: Tuesday, February 01, 2011 Page 54 of 104 * * * Buster J2930203 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Batch Name: bl10107a.dab b110107a.rdb (PFHS): "Quadratic" Regression ("1 / x" weighting): y = -7.09e+003 xA2 + 9.06e+005 x + 4.64e+003 (r = 0.9997) 4.1e7 4.0e7 3.8e7 - 3.6e7 - 3.4e7 3.2e7 3.0e7 2.8e7 j 2.6e7 2.4e7 J <3 2.2e7 c 3 2.0e7 - CO . CD < 1,8e7 - 1.6e7- V / 1.4e7 1.2e7 1.0e7 / 8.0e6 6.0e6 4.0e6 - 2.0e6 0.0 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 Concentration, ng/mL Printing Time: 3:12:25 PM Printing Date: Tuesday, February 01, 2011 Page 1 of 1 Page 55 o f 104 *** Buster J29J0203 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Batch Name: bll01Q7a.cab b110107a.rdb (PFOS): "Quadratic" Regression ("1 / x" weighting): y = -6.1e+003 xA2 + 8.64e+005 x + 2.98e+004 (r = 0.9999) 4.2e7 4.0e7 - 3.8e7 3.6e7 3.4e7- O 3.2e7 3.0e7 2.8e7 2.6e7 2.4e7 2.2e7 t0o) 2.0e7 < 1.8e7 1.6e71.4e7 / / 1.2e7- 1.0e7 8.0e6 6.0e6 4.0e6 2.0e6- 0.0 / 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 Concentration, ng/mL Printing Time: 3:12:51 ?M Printing Date: Tuesday, February 01, 2011 Page 1 of 1 Page 56 of 104 *** Buster J293G2G3 Sample Name: "bl10l07a0l6' 1 .U rp le index: 16 Sample ID: "08008-194-4* File'*b110U)?a1.wifr emu* Concent .-at i -r-n: 0.99 ng/nl. Acq. D ite : l/S /2 5 1 1 ' 2.4*5 Fide. A lg cd tn n : InteliiO uan - M yll Basse Pertenrage: 90 "PtA*"k-i^Sluibt-. '----f<e1'"e- r- : b- c e . .. M l M ,i" 0.CC m Smoothing Width: 0 p oints Sxpeotea RT : 17.5 In l i l t . 7vpe : fc3.->n To Base ? 2J*s U *S 2.2*5 2.1eS 2.ie5 S tir: T iie : ....1 """" i:.3 in l''" 1.9eS 1.9*5 1.8e5 1.8*5 1.7#S 1.7o$ 1.6*5 i.fieS 1-5e5 1.5*5 1.4*5 14 1.3S 13eS | U *S 1.1*5 1.1S 1.0e5 9.5*4 9,0e4 8.5*4 8.0*4 7.5*4 7.0*4 6.5*4 6.0*4 S.S*4 5.0*4 4.5*4 4.0*4 3.5*4 3.0*4 2.5*4 2.0*4 1.5*4 1.0*4 5000.0 0.0..... ...........r ....' .... -i................. i ------- " i Printing Time: 2:56:41 PM Printing Date: Tuesday, March 29, 2011 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 12 51 B ' s ^ ' ^ T r i o i b ^ - ... S ^ t e IP: -savert Blank (MJ:Q Ek 1 Ssrtsie r i : M 0I> Acq. Pave: A i,,. 1'"* ' 1/8/701! .ol.i M F ro r. A ic s rith n : In s e lliu u a n - H91! Xr.is F*rcttU-*ge: 90 F ca k-Jp iU . Factor: 4 K in. *' Height.: 0.CC cps Smoot h: r.q Width: 0 p oints Expected P.T: 12.5 mtn In t . Type: Base To Bars Retention rime: 12.5 min S tart Tine: End 12.5 min l - . F min 1060 1M0 1020 ^ 900 ^ 860 0 620 800 780 Fie: *bll0107ai.Mr .......A -- a Tim*, min______________________________________________ 680 560 640 620 600 % 66 t 540 I 520 480 460. 440 420 400 380 360 : 280 260 240 220 200 180 ,60 ! 4 : 140 Of 4 Page 57 of 104 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Printing Time: 2:56:41 PM Printing Date: Tuesday, March 29, 2011 Page 2 of 4 Page 58 of 104 *** Buster J2930203 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Page 59 of 104 *** Buster J2930203 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Printing Tine: 2:56:41 PM Printing Date: Tuesday, March 29, 2011 Page 4 of 4 Page 60 of 104 Buster J29302C3 Printing Date: Tuesday, March 29, 2011 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Page 61 of 104 Buster J2930203 Printing Time: 2:58:15 PM Printing Date: Tuesday, March 29, 2011 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 IPCSaeomamkpmNteeanNmt:ae*m:5'pP:pF'bbOI'1CS0'S10EM7CaaF0s*4a7fe*As)n:nS*oa4tma9t9ipo.lne.I9~D.:0*aLrCmS>-,1409*S-.2a3f800-"-.03*amFud.4e9.9t.>(V1110310.007aaml.wu*ifr ype: .9 r.q/lH. f.lO r.g/r.L lJ : ijn 7.4e5 Kodiiiec: Yt* Pros. Aicorlthn: Intel,livuan - KOI ?_2e5 B ase. S ub. W indow: i.O C s in 7.0eS P eporc. L a r g e s t P eek : tio Kin. Peak Haight: O.CC t..pa 6A t* Smoothing Width: PT Window: Expected FI: Use Relative R7: 33.0 IS.; No 6.6eS 6.4*5 ri< 51e +30: 14.3 6.2*5 6.0eft- S.6e5 S.6e5 S.4e5 52eS 5.0*5 15.19 4.4*5 4.2*5 4.0e5 | 3.8*5 3.6eS 3.2*5 3De5 2.8*5 15.04-. 2.4*5 2.2*5 2.0e5 1.8*5 l.6eS 1.4*5 I2e5 1.0*5 8.0M 4.0e4 2AM 2 4 6 e 10 12 14 is 1S Page 2 of 3 Page 62 of 104 Buster J2930203 Printing Date: Tuesday, March 29, 2011 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Page of 3 Page 63 of 104 *** Buster J2930203 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Batch Name: bllOHOa.cab b110110a.rdb (PFHS): "Quadratic" Regression ("1 / x" weighting): y = -7.03e+003 xA2 + 9.02e+005 x + 6e+003 (r = 0.9995) 4.2e7 4.0e7 W 3.8e7- 3.6e7 3.4e7- O 3.2e7- 3.0e7- 2.8e72.6e7 ----- 2.4e7 c 2.2e7 - oo 2.0e7- s < 1.8e7 /// 1.6e7 1.4e7- / 1.2e71.0e7 8.0e6 - 6.0e6 4.0e6 2.0e6 - /0.0- / / / 0 / / / // /0 0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 Concentration, ng/mL Printing Time: 3:32:17 PM Page 1 of 1 Printing Date: Tuesday, February 01, 2011 // // \ \ \\ Page 64 o f 104 *** Buster J2930203 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Batch Name: bllOUQa.dab Page 65 of 104 *** Buster J2930203 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Batch Name: bllQUOa.dab b110110a.rdb (PFOS): "Quadratic" Regression ("1 / x" weighting): y = -6.12e+003 xA2 + 8.81e+005 x + 1.98e+004 (r = 0.9999) 4.3e7 4.2e7- 4.0e7 3.8e7 3.6e7- 3.4e7 - 3.2e7 3.0e7 2.8e7- 2.6e7 - 2.4e7 2.2e7- 2.0e7 1.8e7 1.6e7- / 1.4e7 1.2e7- 1,0e7 - 8.0e6 6.0e6- / 4.0e6 2.0e6 0.0- / 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 Concentration. ng/mL Printing Time: 3:32:45 ?M Printing Date: Tuesday, February 01, 2011 Page 1 of 1 Page 66 of 104 *** Buster J293C203 Sample Name: *J>110110a0l6* Sample 10- "08008-194-8' File: "6110110a.wtfr unu,299.0/80.0 amu' Annotation' " 2.2e5 2.2e5 'l'SOTpieN^:,yi101lba^'"^ I Saisple Type: C i l i a l i t e a C: Aeq. Sate: GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Fie: *b11011Qa.ir i Tlx: 12.5 2C4? coi ?.5ie*i?2 Printing Time: 3:03:21 PM Printing Da t e : Tuesday, March 29, 2011 Page 1 of A Page 67 of 104 *** Buster J29302G3 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Page 68 o f 104 Buster J2930203 Printing Date: Tuesday, March 29, 2011 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Page 69 of 104 *** Buster J29302C3 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Printing Tine: 3:03:21 PM Printing Pate: Tuesday, March 29, 2011 Page 4 of 4 Page 70 of 104 *** Buster J2930203 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Printing Tine: 3:04:17 PM Print ing Date: Tuesday, March 29, 2011 Page 1 of 3 Page 71 o f 104 *** Buster J293C203 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Page 72 o f 104 3uster J2930203 Printing Date: Tuesday, March 29, 2011 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Page 3 of 3 Page 73 of 104 * * * Buster J2930203 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Batch Name: bllOll^a.dab b110114a.rdb (PFHS): "Quadratic" Regression (" 1 / x" weighting): y = -6.64e+003 xA2 + 8.6e+005 x + 3.29e+003 (r = 0.9997) 4.0e73.8e73.6e7- 3.4e7 3.2e73.0e72.8e72.6e72.4e7 2.2e7 2.0e7 1.8e7 1,6e7 1.4e71.2e71.0e7 8.0e66.0e64.0e62.0e6- 0.0- / 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 Concentration, ng/mL ?ri.n :i.ng Time: 9:05:13 AM Page 1 of 1 ?rin :ing Date: Wednesday, February 02, 2011 Page 74 o f 104 *** Buster J2930203 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Batch Name: bllOll^a.cab b110114a.rdb (PFBS): "Quadratic" Regression (" 1 / x" weighting): y = -7.54e+003 xA2 + 9.96e+005 x + 5.76e+003 (r = 0.9996) 4.7e7 . 4.6e7 4.4e74.2e74.0e73.8e73.6e7 3.4e7 3.2e7 3.0e72.8e72.6e7 2.4e7 2.2e72.0e71.8e7 1.6e71.4e7 1.2e7 1.0e78.0e6 6.0e6 4.0e6 2.0e6 - 0.0- / / / O 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 Concentration, ng/mL i . - n n :i.nq Time: 9:05:51 AM ?rin .ing Date: Wednesday, February 02, 20L1 Page 1 of 1 Page 75 of 104 *** Buster J2930203 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Batch Name: bllOl1<a.dab B b110114a.rdb (PFOS): "Quadratic" Regression ("1 / x" weighting): y = -5.57e+003 xA2 + 8.19e+005 x + 5.51e+004 (r = 1.0000) 4.1e7 4.0e7- 3.8e7 - 3.6e7 3.4e7- 3.2e7 3.0e7- 2.8e7 2.6e7- 2.4e7 - 2 2.2e7 C B 2.0e7 CO 1.6e7 1.4e7- 1.2e7- 1.0e78.0e6 6.0e6 4.0e62.0e6 - / / / / / m / * 0.0- i / y / / / / / // s' s Ari oo Ct> *vj 0 5 10 15 20 25 30 35 Printing Time: 9:05:33 AM Printing Date: Wednesday, February 02, 2011 o _____________ ,s^'r 40 45 50 55 60 Concentration. ng/mL 65 70 75 Page 1 of 1 O _______ ........ 80 85 90 95 100 Page 76 of 104 *** Buster J2930203 I Sample Name: t.1 10114a01fi' Sample ID: "08008-194-e- File: *b1101i4a.wifT Peak Name: T f BS' assies); '2S9.0/99.0 amu,299.Q/80.0 amo* SaiCroplmemeinrAt:e*.1r..-0. ng/mL FICSstd in Mfi Q Water" Annotation- " Sarple Type: Standard Lve a?: 2.1eS 2.leS 1.7S 1.7eS i 1*s- GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 |&arnpteNNaamme: 'b110114a008" Sample ID. 'SolventSlann{MdliQ Eleir-en e: 'PFBS" Massi): "299..`99.0 amu^99.<V80.0 amu" 'MB: Q Water TN11-0008* Annotation: " aitale Zr.&".> ansie Type: simulated C: Fie: `b110114a.Mr Pres. Aierlthn: Irteli Start Tir.e: 12.3 $C?$ < i.P 'e*i i . 2^4 2.0e4 I3e4 1J>4 0.0 - TT T . A ______ ,. _ __ IZ21S02.....1.2........1.4..... ..1.6........16- 20 Printing Tine: 3:06:03 PM Printing Date: Tuesday, March 23, 2011 Page of 4 Page 77 o f 104 *** Buster J29302G3 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 m m m m m m m m m m m m m im m m im m m ' Printing Time: 3:06:03 PM Printing Date: Tuesday, March 29, 2011 Page 2 of 4 Page 78 of 104 Buster J2930203 Printing Date: Tuesday, March 29, 2011 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Page 79 of 104 *** Buster J2930203 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Printing Tine: 3:06:03 PM Printing Date: Tuesday, March 23, 2011 Page 4 o f 4 Page 80 of 104 Buster J2930203 Printing Date: Tuesday, March 29, 2011 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Page 81 o f 104 Buster J293G2C3 I Sample Name: *bi 10114034* Sample ID: ICS-101230-* Fie: `bl 10114a.wiT Peak Name: T>FOS* Masses). *499.0/99.0 amu.499.0/80.0 amu,499.0/130.0 amu* Comment: "Sppb LCS* Annotation- ** Sarpie Index: 3 Co>ic<-r.-.:aticn: .S>- n^.'ral. 1.12*6- 8.40*56.20*5S.OOcS- 7.60e57.40eS 7.20eS ?.00e5 G.COeS 6.60*5 5.0eS 6.205 6.00e5 5.80e5 S'S 5,60*5 2 5.4005 5.20e5 5.00e6 4.60*5 4.B0*54.40e$4,20*54.00*53.60e53.60eS3.40S 3.00*5- 2.60*5 2.40*52.20eS2.00eS 1.80*51.60*51.40e61.20*51.00*58.00e46.00*4 4.00 2.00O4 0.0 0 - Printing Time: 3:06:58 PM Printing Date: Tuesday, March 29, 20 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 15.20 I Sample Name: "bl 10114a047* Sample ID: TXS-101230-iy FUe:'t>110H4a.wr Peak Name: 'PFOS* Mas*(*sj: 99.0.99.0 amu,499.0/80.0 amu,499.0/130.0 amu* Comment: *5ppb LCS FCF* Annotation: ~ San: Cal: A:-q. P.T Wird;*: Expected (U: 33 .J : 1 5 .3 nil IS.2 mil 782?J c u m : 7.4 c *001- cp- 7.Ce5 6.6e5 6.6e5 6.4*5 6.2eS 6.0e5- 5.6*5 5.4*55.2e5S.Ce54.8*54.Se5 4.4e5 4Je5 t 3.8e5 | 3.6eS 3.4e5 3.2e5 3.0e5 2.6e5 2.8eS 2.2e5 2.0e5 1.8*5 1.4*5 1JeS 1S.19 15.05 15.0S^ Page 2 of 3 Page 82 of 104 Buster J29302C3 Printing Date: Tuesday, March 29, 2011 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Page 3 of 3 Page 83 of 104 *** Ginger AGQI330509 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Results Name: gll0211a .rcib g1 1021 la.rdb (PFBS): "Quadratic" Regression ("1 / x" weighting): y = -3.35e+003 xA2 + 6.88e+005 x + 3.41e+003 (r = 0.9997) 2.7e7- 2.6e7 2.5e7 2.4e7 2.3e7 2.2e7 2.1e7- 2.0e7 1.9e7 1.8e7 - 1.7e7- 1,6e7 1.5e7- </) 3 1.4e7 sO 1.3e7 < 1.2e7 1.1e7 1.0e7- 9.0e6 - 8.0e6- 7.0e6- 6.0e6 - 5.0e6 - 4.0e6 - 3.0e6 2.0e6 1.0e6 - / / 0. 0 - \ \ s' /s / / S' ./ / / / / S / S ' s s' s s '' S ''' 024 68 Printing Time: 3:16:33 PM Printing Date: Tuesday, March 29, 2011 10 12 14 16 18 20 22 24 26 28 30 32 34 36 38 40 42 44 46 48 50 Concentration, ng/mL Page 1 of 1 Page 84 of 104 Ginger AG0I330509 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Results Name: gll0211a.rdb g110211a.rdb (PFOS): "Quadratic" Regression ("1 / x " weighting): y = -1.24e+004 xA2 + 1.76e+006 x + 8.61e+003 (r = 0.9998) 5.9e7 . 5.8e7 5.6e7 5.4e7 5.2e7 5.0e7 4.8e7 4.6e7 4.4e7 4.2e7 4.0e73.8e7 3.6e7 3.4e7 3.2e73.0e7 2.8e7 2.6e7 2.4e7 2.2e7 2.0e7 1.8e7 j 1.6e71.4e71.2e71.0e7 -| 8.0e6 6.0e6-| 4.0e6 2.0e6 0.0- / / X / / :16:58 PM uesday, March 29, 2 Page 85 of 104 *** Ginger AG01330509 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Results Name: gll0211a.rdb Printing Date: Tuesday, March 29, 2011 Page 86 of 104 *** Ginger AG01330509 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Results Name: gll0211a.rdb Printing Tine: 3:14:55 PM Printing Date: Tuesday, March 29, 2011 Page 2 of 2 Page 87 of 104 *** Ginger AG0I330509 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Results Name: g l 1 0 2 1 1 a .rdb Page 88 o f 104 *** Ginger AG01330509 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Results Name: gll0211a.rdb Printing Time: 3:15:57 PM Printing Date: Tuesday, March 29, 2011 Page 89 of 104 Ginger AG01330509 Printing Pate: Tuesday, March 29, 2011 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Results Name: gll0211a.rdb Page 3 of 3 Page 90 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Attachm ent C: A nalytical M ethod Page 91 of 104 GLP10-01-02; Jnterim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 3M Environm ental Laboratory Method Method o f Analysis for the Determination o f Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis Method Number: ETS-8-044.0 Adoption Date: Upon Signing Effective Date: Q L f ^ /o "7 Approved By: William K. Reagen, Laboratory Manager >/ z j / o Date ETS-8-044.0 Page 1 of 11 Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis Page 92 of 104 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 1 Scope and Application This method is to be used to quantify Perfiuorobutanoic Acid (PFBA), Perfluoropentanoic Acid (PFPeA), Perfluorohexanoic Acid (PFHA), Perfluoroheptanoic Acid (PFHpA), Perfluorooctanoic Acid (PFOA), Perfluorononanoic Acid (PFNA), Perfluorodecanoic Acid (PFDA), Perfluoroundecanoic Acid (PFUnA), Perfluorododecanoic Acid (PFDoA), Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) by High Performance Liquid Chromatography coupled to a tandem Mass Spectrometric Detector (LC/MS/MS) in clean water samples. Water samples containing heavy particulate may require preparation by an alternate method such as ETS-8-154 "Determination of Perfluorinated Acids, Alcohols, Amides, and Sulfonates In Water By Solid Phase Extraction and High Performance Liquid Chromatography/Mass Spectrometry". This method is considered a performance-based method. Data is considered acceptable as long as the defined QC elements are satisfied. Sample collection is not covered under this analytical procedure. 2 Method Summary Clean aqueous samples are analyzed by direct injection using LC/MS/MS. Samples containing heavy particulate may not be suitable for analysis by this method. Samples containing suspended particulate should be centrifuge prior to removing a sample aliquot, or filtered. This is a performance-based method. Method accuracy is determined for each sample set using multiple laboratory control spikes at multiple concentrations. This method also requires that the precision and accuracy for each sample be determined using field matrix spikes to verify that the method is applicable to each sample matrix. Sample results for spikes outside of 70% to 130%, may be flagged as such (with expanded accuracy statements), or will not be reported due to non-compliant quality control samples. Fortification levels for field matrix spikes and for laboratory matrix spikes should be at least 50% of the endogenous level and less than 10 times the endogenous level to be used to determine the statement of accuracy for analytical results. 3 Definitions 3.1 Calibration Standard A solution prepared by spiking a known volume of the Working Standard (WS) into a predetermined amount of ASTM Type I, HPLC grade water, or other suitable water, and analyzed according to this method. Calibration standards are used to calibrate the instrument response with respect to analyte concentration. 3.2 Laboratory Duplicate Sample (LDS, or Lab Dup) A laboratory duplicate sample is a separate aliquot of a sample taken in the analytical laboratory that is analyzed separately with identical procedures. Analysis of LDSs compared to that of the first aliquot give a measure of the precision associated with laboratory procedures, but not with sample collection, preservation, or storage procedures. 3.3 Field Blank (FB)/Trip Blank ASTM Type I, HPLC grade water, or other suitable water, placed in a sample container in the laboratory and treated as a sample in all respects, including exposure to sampling site conditions, storage, preservation and all analytical procedures. The purpose of the FB is to determine if test substances or other interferences are present in the field environment. This sample is also referred to as a Trip Blank. ETS-8-044.0 Page 2 of 11 Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis Page 93 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 3.4 Field Duplicate Sample (FDS, Field Dup) A sample collected in duplicate at the same time from the same location as the sample. The FDS is handled under identical circumstances and treated exactly the same throughout field and laboratory procedures. Analysis of the FDS compared to that of the first sample gives a measure of the precision associated with sample collection, preservation and storage, as well as with laboratory procedures. 3.5 Field Matrix Spike (FMS) A sample to which known quantities of the target analytes are added to the sample bottle in the laboratory before the bottles are sent to the field for collection of aqueous samples. A known, specific volume of sample must be added to the sample container without rinsing. This may be accomplished by making a "fill to this level" line on the outside of the sample container. The FMS should be spiked between approximately 50% and 10 times the expected analyte concentration in the sample. If the expected range of analyte concentrations is unknown, multiple spikes at varying levels may be prepared to increase the likelihood that a spike at an appropriate level is made. The FMS is analyzed to ascertain if any matrix effects, interferences, or stability issues may complicate the interpretation of the sample analysis. 3.6 Trip Blank Spike (Field Spike Control Sample, FSCS) An aliquot of ASTM Type I, HPLC grade water, or other suitable water, to which known quantities of the target analytes are added in the laboratory prior to the shipment of the collection bottles. The FSCS is extracted and analyzed exactly like a study sample to help determine if the method is in control and whether a loss of analyte could be attributed to holding time, sample storage and/or shipment issues. A low and high FSCS are appropriate when expected sample concentrations are not known or may vary. At least one separate, un-spiked sample must be taken at the same time and place as each FMS. 3.7 Laboratory Control Sample (LCS) An aliquot of control matrix to which known quantities of the target analytes are added in the laboratory at the time of sample extraction. At least two levels are included, one generally at the low end of the calibration curve and one near the mid to upper range of the curve. The LCSs are extracted and analyzed exactly like a laboratory sample to determine whether the method is in control. LCSs should be prepared each day samples are extracted. 3.8 Laboratory Matrix Spike (LMS) A laboratory matrix spike is an aliquot of a sample to which known quantities of target analytes are added in the laboratory. The LMS is analyzed exactly like a laboratory sample to determine whether the sample matrix contributes bias to the analytical results. The endogenous concentrations of the analytes In the sample matrix must be determined in a separate aliquot and the measured values in the LMS corrected for these concentrations. LMSs are optional for analysis of aqueous samples. 3.9 Laboratory Sample A portion or aliquot of a sample received from the field for testing. 3.10 Limit of Quantitation (LOQ) The lower limit of quantitation (LLOQ) for a dataset is the lowest concentration that can be reliably quantitated within the specified limits of precision and accuracy during routine operating conditions. To simplify data reporting, the LLOQ is generally selected as the lowest non-zero standard in the calibration curve that meets method criteria. Sample LLOQs are matrix-dependent. The upper limit of quantitation (ULOQ) for a dataset is the highest concentration that can be reliably quantitated within the specified limits of precision and accuracy during routine operating conditions. The highest standard in the calibration curve that meets method criteria is defined as the ULOQ. ETS-8-044.0 Page 3 of 11 Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis Page 94 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 3.11 Method Blank An aliquot of control matrix that is treated exactly like a laboratory sample including exposure to all glassware, equipment, solvents, and reagents that are used with other laboratory samples. The method blank is used to determine if test substances or other interferences are present in the laboratory environment, the reagents, or the apparatus. 3.12 Sample A sample is an aliquot removed from a larger quantity of material intended to represent the original source material. 3.13 Stock Standard Solution (SSS) A concentrated solution of a single-analyte prepared in the laboratory with an assayed reference compound. 3.14 Surrogate A compound similar in chemical composition and behavior to the target analyte(s), but is not normally found in the sample(s). A surrogate compound is typically a target analyte with at least one atom containing an isotopically-labeled substitution. If used, surrogate(s) are added to all samples and quality control samples. Surrogate(s) are added to quantitatively evaluate the entire analytical procedure including sample collection, preparation, and analysis. Inclusion of a surrogate analyte is an optional quality control measure and is NOT required. 3.15 Working Standard (WS) A solution of several analytes prepared in the laboratory from SSSs and diluted as needed to prepare calibration standards and other required analyte solutions. 4 Warnings and Cautions 4.1 Health and Safety The acute and chronic toxicity of the standards for this method have not been precisely determined; however, each should be treated as a potential health hazard. The analyst should wear gloves, a lab coat, and safety glasses to prevent exposure to chemicals that might be present. The laboratory is responsible for maintaining a safe work environment and a current awareness of local regulations regarding the handling of the chemicals used in this method. A reference file of material safety data sheets (MSDS) should be available to all personnel involved in these analyses. 4.2 Cautions The analyst must be familiar with the laboratory equipment and potential hazards including, but not limited to, the use of solvents, pressurized gas and solvent lines, high voltage, and vacuum systems. Refer to the appropriate equipment procedure or operator manual for additional information and cautions. 5 Interferences During sample preparation and analysis, major potential contaminant sources are reagents and glassware. All materials used in the analyses shall be demonstrated to be free from interferences under conditions of analysis by running method blanks. ETS-8-044.0 Page 4 of 11 Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis Page 95 of 104 GLP10-01-02; Interim Report 11 Analysis o f PFBS, PFHS, and PFOS In Groundwater Former Sludge Incorporation Area - November 2010 Parts and supplies that contain Teflon should be avoided or minimized due to the possibility of interference and/or contamination. These may include, but are not limited to: wash bottles, Teflon lined caps, autovial caps, HPLC parts, etc. The use of disposable micropipettes or pipettes to aliquot standard solutions is recommended to make calibration standards and matrix spikes. 6 Instrumentation, Supplies, and Equipment 6.1 Instrumentation and Equipment A high performance liquid chromatograph capable of pumping up to two solvents and equipped with a variable volume injector capable of injecting 5-100 pL connected to a tandem Mass Spectrometer (LC/MS/MS). I Analytical balance capable of reading to 0.0001 g A device to collect raw data for peak integration and quantitation 15-mL and 50-mL disposable polypropylene centrifuge tubes. Gas tight syringes, 25pL, 50pL, 100pL, 250pL, 500pL, 1000pL. 1 mL plastic HPLC autovial. Disposable pipettes, polypropylene or glass as appropriate Centrifuge capable of spinning 15-mL and 50-mL polypropylene tubes at 3000 rpm. 6.2 Chromatographic System Guard Column: Prism RP, 4.6 mm x 50 mm, 5 pm Analytical Column: Betasil C18, 4.6 mm x 100 mm, 5 pm Temperature: 10C Mobile Phase (A): 2 mM Ammonium Acetate in Water Mobile Phase (B): Methanol Gradient Program: Time (min) 0.0 0.5 11.0 13.5 13.6 17.0 %A 97 97 5 5 97 97 %B 3 3 95 95 3 3 Flow Rate (mL/min) 1.0 1.0 1.0 1.0 1.0 1.0 Injection Volume: 100 pL. Quantitation: Peak Area - quadratic curve fit, 1/x weighted. Run Time: ~ 17 minutes. The previous information is intended as a guide; alternate conditions and equipment may be used provided that data quality objectives are met. ETS-8-044.0 Page 5 of 11 Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis Page 96 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 6.3 MS/MS System 6.3.1 Mode: Electrospray Negative ion, MRM mode, monitoring the following transitions: Analyte Transition Monitored PFBA 213 --> 169 PFPeA 263 ->219 PFHA 3 1 3 -> 2 6 9 and 313 -> 119 PFHpA 363 -> 319, 363 -> 169 and 363 -> 119 PFOA 413 369, 413 -> 219 and 413 -> 169 PFNA 463 419, 463 -> 169 and 463 -> 2 1 9 PFDA 513 469, 513 --> 219 and 513 -> 269 PFUnA 563 -> 519, 563 -> 269 and 563 -> 2 1 9 PFDoA 613 -> 569, 613 -> 169 and 613 -> 319 PFBS 299 -> 80 and 299 -> 99 PFHS 399 --> 80 and 399 --^ 99 PFOS 499 -> 80, 499 -> 99 and 499 -> 130 Multiple transitions for monitoring the analytes is an option, as summing multiple transitions may provide quantitation of isomers that more closely matches NMR data and may have the added benefit of increased sensitivity. The use of one daughter ion is acceptable if method sensitivity is achieved, provided that retention time criteria are met to assure adequate specificity. The previous information is intended as a guide, alternate instruments and equipment may be used. 7 Reagents and Standards 7.1 Chemicals Water - Milli-Q, HPLC grade, or other suitably appropriate sources Methanol - HPLC grade Ammonium Acetate -A .C .S . Reagent Grade 7.2 Standards Perfluorobutanoic Acid (PFBA - C4 acid); Oakwood Products, Inc Perfluoropentanoic Acid (PFPeA - C5 acid, also known as NFPA, nonafluoropentanoic acid); Alfa Aesar Perfluorohexanoic Acid (P F H A - C6 acid); Oakwood Products, Inc Perfluoroheptanoic Acid (PFHpA - C7 acid, also known as TDHA, tridecafluoroheptanoic acid); Oakwood Products, Inc Perfluorooctanoic Acid (PFOA - C8 acid); 3M Perfluorononanoic Acid (P F N A - C9 acid); Oakwood Products, Inc Perfluorodecanoic Acid (PFDA - C10 acid); Oakwood Products, Inc Perfluoroundecanoic Acid (PFUnA - C11 acid); Oakwood Products, Inc Perfluorododecanoic Acid (P FD oA -C 12 acid); Oakwood Products, Inc Perfluorobutanesulfonate (PFBS - C4 sulfonate); 3M Perfluorohexanesulfonate (PFHS - C6 sulfonate); 3M Perfluorooctanesulfonate (PFOS - C8 sulfonate); 3M ETS-8-044.0 Page 6 of 11 Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis Page 97 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 The previous information is intended as a guide. Reagents and standards from alternate sources may be used. 7.3 Reagent Preparation 2 mM Ammonium acetate solution (Analysis)-- Weigh 0.3 g of Ammonium acetate and dissolve in 2.0 L of reagent water. Note: Alternative volumes may be prepared as long as the ratios of the solvent to solute ratios are maintained. 7.4 Stock Standard Solution (SSS) and Working Standard Solution Preparation The following standard preparation procedure serves as an example. Weighed amounts and final volumes may be changed to suit the needs of a particular study. For example, pL volumes may be spiked into volumetric flasks when diluting stock solutions to appropriate levels. 100 pg/mL target analyte SSSs-- Weigh out 10 mg of analytical standard (corrected for percent salt and purity) and dilute to 10OmL with methanol or other suitable solvent, in a 10OmL volumetric flask. Transfer to a 125mL LDPE bottle or other suitable container. Prepare a separate solution for each analyte. Expiration dates and storage conditions of stock solutions should be assigned in accordance with laboratory standard operating procedure. An example of purity and salt correction is given below for PFOS. molecular weight of anion salt correction factor moclecular weight of salt PFOS (K +)salt correction factor = ------= 0.9275 538 10 mg C8F17S03`K+with purity 90% = 8.35mg C8F17S03~ (10 mg*0.90*0.9275=8.35 mg) 5 pg/mL (5000 ng/mL) mixed working standard-- Add 0.5mL each of the 10Opg/mL SSSs to a 10mL volumetric flask and bring up to volume with solvent. 250 ng/mL mixed working standard-- Add 1.25mL of the 5 pg/mL -mixed working standard solution to a 25mL volumetric flask and bring up to volume with solvent. 125 ng/mL mixed standard-- Add 625pL of the 5 pg/mL-mixed working standard solution to a 25mL volumetric flask and bring up to volume with solvent. Storage Conditions-- Store all SSSs and working standards in accordance with laboratory standard operating procedure or in a refrigerator at 42C for a maximum period of 6 months from the date of preparation. ETS-8-044.0 Page 7 of 11 Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis Page 98 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 7.5 Calibration Standards Using the working standards described above, prepare calibration solutions in ASTM Type I water, HPLC water, or other suitable water, using the following table as a guideline. Note: Volumes of water and working standards may be adjusted to meet the data quality objectives addressed in the general project outline. Calibration levels other than those listed below can be prepared as needed. Concentration o f WS, ng/mL 125 125 125 125 250 250 250 250 5000 5000 5000 Volume o f WS, ftL 10 15 20 30 20 50 100 200 25 50 100 Final Volume of Calibration Standard (m l o f ASTM Type 1 Water, or other suitable water) 50 50 50 50 50 50 50 50 50 50 50 Final Concentration of Calibration Standard, ng/mL (ppb) in ASTM Type 1 Water, or other suitable water 0.025 0.0375 0.050 0.075 0.100 0.250 0.500 1.00 2.50 5.00 10.0 8 Sample Handling 8.1 Water Sample Preparation This method is applicable to clean water samples. Samples containing heavy particulate may not be suitable for analysis by this method. Samples containing suspended particulate should be centrifuge prior to removing a sample aliquot, or filtered. Thoroughly mix sample before removing an aliquot and placing in a labeled plastic autovial. Plastic is preferred over the use of glass autovials, to prevent the possibly of fluorochemical sticking to the glass. Dilute sample, if necessary, with ASTM Type I, HPLC water, or other suitable water. Prepare method QC samples and multiple method blanks and aliquot into labeled plastic autovials. Prepare at least five method blanks. 9 Sample Analysis - LC/MS/MS Analyze the standard curve prior to each set of samples. The standard curve may be plotted using a linear fit, weighted 1/x or unweighted, or by quadratic fil (y = ax2+ bx + c), weighted 1/x or unweighted, using suitable software. The calibration curves may include but should not be forced through zero. The mathematical method used to calculate the calibration curve should be applied consistently throughout a study. Any change should be thoroughly documented in the raw data. High and/or low points may be excluded from the calibration curves to provide a better fit over the range appropriate to the data or because they did not meet the pre-determined acceptance criteria. Low-level curve points should also be excluded if their area counts are not at least twice that of the method and/or solvent blanks. The coefficient of determination (r2) value for the calibration curve must be greater than or equal to 0.990. Each point in the curve must be within 25% of the theoretical concentration with the exception of the LLOQ, which may ETS-8-044.0 Page 8 of 11 Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis Page 99 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 be within 30%. Justification for exclusion of calibration curve points will be noted in the raw data. A minimum of 6 points will be used to construct the calibration curve. If the calibration curve does not meet acceptance criteria, perform routine maintenance or prepare a new standard curve (if necessary) and reanalyze. Continuing calibration verifications (CCV) are analyzed to verify the accuracy of the calibration curve. Analyze a mid-range calibration standard, one of the same standards used to construct the calibration curve, at a minimum after every tenth sample, not including solvent blanks, with a minimum of one per sample set. Calibration verification injections must be within 25% to be considered acceptable. The calibration curve and the last passing CCV will then bracket acceptable samples. Multiple CCV levels may be used. Samples containing analytes that are quantitated above the concentration of the highest standard in the curve should be further diluted and reanalyzed. 10 Quality Control 10.1 Data Quality Objectives This method and required quality control samples is designed to generate data accurate to 30% with a targeted LOQ of 0.025 ng/mL. Any deviations from the quality control measures spelled out below will be documented in the raw data and footnoted in the final report. 10.2 Method Blanks Method blanks must be prepared with each analysis batch. At least five method blanks must be prepared. Method blanks may be injected multiple times, but no more than 3 injections should be removed from a single method blank. At a minimum, method blanks are analyzed prior to instrument calibration, prior to the analysis of CCV samples, and at the end of the analytical run. The mean area count for each analyte in the method blanks must be less than 50% of the area count of the LOQ standard. The standard deviation of the area counts of these method blanks should be calculated and reported. If the mean area counts of the method blanks exceed 50% of the LOQ standard, then the LOQ must be raised to the first standard level in the curve that meets criteria, or alternatively, the method blanks must be evaluated statistically to determine outliers, or technical justification to eliminate one or more results should be made. 10.3 Sample Replicates Samples duplicates are collected in the field. The relative percent difference, RPD, should be reported. RPD results greater than 20% will be flagged in the report, but will not be excluded from reporting. The requirement for replicates excludes field blanks. 10.4 Surrogate Spikes Surrogate spikes are not required but may be used on project specific requirements. 10.5 Lab Control Sample Triplicate lab control spikes at a minimum of two different concentrations are to be prepared with each preparation batch. Low lab control spikes should be prepared at concentrations in the range of five to ten times higher than the targeted LOQ and high lab control spikes should be prepared at concentrations near the mid-point of the curve. The relative standard deviation of the control spikes evaluated independently at each concentration level must be less than or equal to 20% and the average recovery must be 80-120%. If the above criteria are not met, the entire set of samples should be re-injected or re-prepared as appropriate. ETS-8-044.0 Page 9 of 11 Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis Page 100 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 10.6 Field Matrix Spikes / Lab Matrix Spikes Recoveries of field matrix spikes and laboratory matrix spikes are anticipated to be between 70% and 130% of the fortified levels. Sample results for spikes outside of 70% to 130%, may be flagged as such (with expanded accuracy statements), or will not be reported due to non-compliant quality control samples. The targeted fortification levels should be at least 50% of the endogenous level and less than 10 times the endogenous level to be used without justification to determine the statement of accuracy for analytical results. The average of the sample and the field duplicate should be used to calculate the recovery. 11 Data Analysis and Calculations Use the following equation to calculate the amount of analyte found (in ng/mL, based on peak area) using the standard curve (linear regression parameters) generated by an appropriate software program: . .. , . . . (Peak Area-Intercept) nr. Analyte found (ng/mL) = --------------------------- -- x DF DF = factor by which the final volume was diluted, if necessary. For samples fortified with known amounts of analyte prior to extraction, use the following equation to calculate the percent recovery. Total analyte found (ng/mL) - Average analyte found in sample (ng/mL) Recovery = x100 Analyte added (ng/mL) 12 Method Performance Any method performance parameters that are not achieved must be considered in the evaluation of the data. Nonconformance to any specified parameters must be described and discussed if the Technical Manager (nonGLP study) or Study Director (GLP study) chooses to report the data. If criteria listed in this method performance section are not met, maintenance may be performed on the system and samples reanalyzed, or other actions taken as appropriate. Document all actions in the raw data. If data are to be reported when performance criteria have not been met, the data must be footnoted on tables and discussed in the text of the report. 12.1 System Suitability System Suitability standards are not a required component of this method. If required by protocol or by the technical manager, a minimum of three system suitability samples are injected at the beginning of each analytical run prior to the calibration curve. Typically these samples are at a concentration near the mid level of the calibration curve and are repeated injections from one autosampler vial. The system suitability injections must have area counts with an RSD of 5% and a retention time RSD of 2% to be compliant. 12.2 Quantitation Calibration Curve: The coefficient of determination (r2) value for the calibration curve must be greater than or equal to 0.990. Each point in the curve must be within 25% of the theoretical concentration with the exception of the LLOQ, which may be within 30%. CCV Performance: The calibration standards that are interspersed throughout the analytical sequence are evaluated as continuing calibration verifications in addition to being part of the calibration curve. The accuracy of each curve point must be within 25% of the theoretical value (within 30% for lowest curve point). Samples that are bracketed by CCVs not meeting these criteria must be reanalyzed. ETS-8-044.0 Page 10 of 11 Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis Page 101 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Demonstration o f Specificity: Specificity is demonstrated by chromatographic retention time (within 4% of standard) and the mass spectral response of unique ions. 12.3 Sensitivity The targeted limit of quantitation for all analytes is 0.025 ng/mL. The LOQ for any specific analyte may vary depending on the evaluation of appropriate blanks and the accuracy of the low-level calibration curve points. Refer to Section 10 for additional details. 12.4 Accuracy This method and required quality control samples are designed to generate data that are accurate to +/-30%. Section 10 contains additional information regarding the required accuracy of laboratory control spikes, field matrix spikes and laboratory matrix spikes. 12.5 Precision Samples should be collected in duplicate in the field. The relative percent difference, RPD, should be reported. RPD results greater than 20% will be flagged in the report, but will not be excluded from reporting. The requirement for replicates excludes field blanks or rinse blanks. Section 10 contains additional information regarding the required precision of laboratory control spikes. 13 Pollution Prevention and Waste Management Waste generated when performing this method will be disposed of appropriately. The original samples will be archived at the 3M Environmental Laboratory in accordance with internal procedures. 14 Records Each data package generated fo ra study must include all supporting information for reconstruction of the data. Information for the data package must include, but is not limited to the following items: study or project number, sample and standard prep sheets/records, instrument run log (instrument batch records, instrument acquisition method, summary pages), instrument results files, chromatograms, calibration curves, and data calculations. 15 Affected Documents None. 16 Revisions Revision Number Summary of Changes ETS-8-044.0 Page 11 of 11 Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis Page 102 of 104 Attachm ent D: D eviation GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 Page 103 of 104 GLP10-01-02; Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Groundwater Former Sludge Incorporation Area - November 2010 R ecord of D eviation/N o nco nfo rm ance I. Identification Study / Project No. Date(s) of Occurrence: GLP10-01-02-11 1/7/11 -2/11/11 Deviation type 0 SOP Equipment Procedure 0 Method (Check one) Protocol_______ GPO________________ Other: II. Description (attach extra pages as needed) M ethod R equirem en ts:..................................... (1 j LCS average recovery of 100% 20%. Document Number: ETS-8-044.0 (2) Sample/Sample Duplicate RPD <20%. (3) Field matrix spike recovery of 100% 30%. Actual procedure/process: (1) 1/7/11; the average recovery for the low set of LCS for PFBS was 123% and for PFHS 123%. The average recovery of the high set of ECF LCS samples for PFOS was 123%. 1/10/11 ; the low set of LCS samples for PFHS had an average recovery of 122%. The average recovery of the high set of ECF LCS samples for PFOS was 121%. 2/11/11; the high set of ECF LCS for PFOS had an average recovery of 133%. (2) PFOS RPD value for DAL GW 137S was 33%. (3) PFOS FMS recovery; DAL GW 137S (59.4%) and DAL GW 144R (28.7%). PFHS FMS recovery; DAL GW 134S (135%).__________________________________________________________________________ III. Actions Taken (such as amendment issued, SOP revision, etc.) Corrective Action ( Yes 0 No) Reference: Acceptability of the nonconform ing work: 1) In general, the ECF LCSs for PFOS have been running 15-20% higher when quantitated using linear PFOS. All LCS were used in the determination of method uncertainty. The determination of the method uncertainty by ETS-12-012.2 was 18%. However, due to potential analytical bias that was observed when quantitating LCS samples containing linear and branched isomers of PFOS, the analytical for PFOS for this study has been expanded to 33%. 2) Sampling locations with RPD values 220% will be footnoted in the data tables. 3) Analytical uncertainties for DAL GW 137S and DAL GW 134S will be adjusted accordingly. Sampling location DAL GW 144R - PFOS results will not be reported. Samples were re-diluted and a LMS samples was prepared. Recoveries for the LMS sample for PFOS were still ~30% for the re-analysis. Actions: Halting of Work Client Notification Work Recall 0 Other: Deviations will be noted in finapreport. Project Lead/PAI Approval: Susa Withholding of Report Study Director (if GLP): S ponsor Approval (for G LP protocol deviations): NA Technical Reviewer (optional): NA Date: NA Laboratory Departm ent M anager Approval: Date: IV. Authorization to Resume Work Where halting o f work occurred, resumption o f work must first be approved by Laboratory Management Laboratory Departm ent M anager Approval: NA Date: NA Deviation No. (assigned by Study Director or Team Leader at the end of study or project) ETS-4-008.7 Page 1 of 1 Documentation of Deviations and Control of Nonconforming Testing Page 104 of 104