Document gb3nodEJOpR8obJ6XpGYvZKxq

INTERIM REPORT #22 - Analvsis of Soil Samples STUDY TITLE Analysis of PerfluorooctanoicAcid (PFOA) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LCMSMS for the 3M Decatur Monitoring Program DATA REQUIREMENTS EPA TSCA Good Laboratory Practice Standards 40 CFR 792 STUDY DIRECTOR Jaisimha Kesari P.E., DEE Weston Solutions, Inc. 1400 Weston Way West Chester, PA 19380 Phone: 610-701-3761 INTERIM REPORT COMPLETION DATE September 22,2006 PERFORMING LABORATORY Exygen Research 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 STUDY SPONSOR 3M Company 3M Building 0236-01-B-10 St. Paul, MN 55144 Phone: 651-733-6374 PROJECT Protocol Number: PO000760 Exygen Study Number: PO000760 Total Pages: 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT Exygen Study Number P0000760, entitled "Analysis of Perfluorooctanoic Acid (PFOA) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Program," conducted for 3M Company, is being performed in compliance with EPA TSCA Good Laboratory Practice Standards 40 CFR 792 by Exygen Research. //o h Flaherty / Principal Investigator Exygen Research Study Director Weston Solutions, Inc. Michael A. "To Sponsor Repr sentative 3M Company ?A%/' Date Exygen Research Page 2 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 QUALITY ASSURANCE STATEMENT Exygen Research's Quality Assurance Unit reviewed Exygen Study Number P0000760, entitled, "Analysis of Perfluorooctanoic Acid (PFOA) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LCMSMS for the 3M Decatur Monitoring Program". All reviewed phases' were inspected for conduct according to Exygen Research's Standard Operating Procedures, the Study Protocol, and all applicable Good Laboratory Practice Standards. All findings were reported to the Exygen Principal Investigator and Management and to the Study Director. Phase Date Insvected Date Reported to Date Reported to Principal Exygen Date Reported to Investigator Management Study Director 32. Raw Data Review and Interim Analytical Report Review 06106-09/06 06/29/06 06/30/06 07/07/06 33. Interim Analytical Report Review 34. Raw Data Review and Interim Analpcal Report Review 06/14/06 09120-21/06 06/29/06 09/22/06 0613 0106 09/22/06 07/07/06 09/22/06 `Note: All in-lab inspections will be documented in the QA statement for the final analytical report at the conclusion of the study. This QA statement involves only the review of the interim report and associated raw data. Exygen Research Page 3 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 CERTIFICATION OF AUTHENTICITY This interim report, for Exygen Study Number P0000760, is a true and complete representation of the raw data. Submitted by: Exygen Research 3058 Research Drive State College, PA 16801 (814) 272-1039 Principal Investigator, Exygen: Jdhn I Flaherty - I Date /Vice President Exygen Research Exygen Research Facility Management: Date Exygen Research Study Director,,jWeston Solutions, Inc. Weston Solutions, Inc. Sponsor Representative, 3M Company: Michael A. S a f m Director of R gulatory Affairs Exygen Research Page 4 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 STUDY IDENTIFICATION Analysis of Perfluorooctanoic Acid (PFOA) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Program PROTOCOL NUMBER: PO000760 EXYGEN STUDY NUMBER: PO000760 TYPE OF STUDY: Residue SAMPLE MATRIX: Soil and Water TEST SUBSTANCE: Perfluorooctanoic acid (PFOA) SPONSOR: 3M Company 3M Building 0236-01-B-10 St. Paul, MN 55144 STUDY DIRECTOR: Jaisimha Kesari P.E., DEE Weston Solutions, Inc. 1400 Weston Way West Chester, PA 19380 STUDY MONITOR: Michael A. Santoro 3M Company 3M Building 0236-01-B-10 St. Paul, MN 55144 PERFORMING LABORATORY: Exygen Research 3058 Research Drive State College, PA 16801 ANALYTICAL PHASE TIMETABLE: Study Initiation Date: 11/05/04 Interim Analytical Start Date: 04/15/06 Interim Analytical Termination Date:07/24/06 Interim Report Completion Date: 09/22/06 Exygen Research Page 5 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 PROJECT PERSONNEL The Study Director for this project is Jaisimha Kesari at Weston Solutions, Inc. The following personnel from Exygen Research were associated with various phases of this interim portion of the study: Name John Flaherty Karen Risha Eric Edwards Christine Edwards Mark Ammerman Amy Sheehan Mindy Cressley Brittany Kravets Krista Gallant Scott Crain Frances Crespi Sharareh Zolghadr Larissa Hoover Brian McAllister - Title Vice President Scientist Sample Custodian Technician Sample Custodian Associate Scientist Technician Technician Technician Technician Technician Technician Technician Sample Custodian Exygen Research Page 6 of 151 Interim Report #22 .Analysis of Soil Samples . Exygen StudyNo. PO000760 TABLE OF CONTENTS PaRe TITLE PAGE ....................................................................................................................... 1 GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT.............................. 2 QUALITY ASSURANCE STATEMENT .......................................................................... 3 CERTIFICATION OF AUTHENTICITY ........................................................................... 4 STUDY IDENTIFICATION................................................................................................ 5 PROJECT PERSONNEL..................................................................................................... 6 TABLE OF CONTENTS..................................................................................................... 7 LIST OF TABLES ............................................................................................................... 8 LIST OF FIGURES.............................................................................................................. 9 LIST OF APPENDICES.................................................................................................... 10 1.0 SUMMARY................................................................................................................ 11 2.0 OBJECTIVE ............................................................................................................... 12 3.0 INTRODUCTION....................................................................................................... 12 4.0 ANALYTICAL TEST SAMPLES.............................................................................. 12 5.0 REFERENCE MATERIAL ........................................................................................ 13 6.0 DESCRIPTION OF ANALYTICAL METHOD ........................................................ 15 6.1 Extraction Procedure For Soil .................................................................................. 15 6.2 Percent Solids Procedure For Soil ............................................................................ 15 6.3 Extraction Procedure for Water ................................................................................ 15 6.4 Preparation of Standards and Fortification Solutions............................................... 16 6.5 Chromatography ....................................................................................................... 17 6.6 Instrument Sensitivity............................................................................................... 17 6.7 Description of LC/MS/MS Instrument and Operating Conditions........................... 17 6.8 Quantitation and Example Calculation..................................................................... 18 7.0 EXPERIMENTAL DESIGN ...................................................................................... 20 8.0 RESULTS ................................................................................................................... 21 9.0 CONCLUSIONS......................................................................................................... 21 10.0 RETENTION OF DATA AND SAMPLES ............................................................. 22 Exygen Research Page 7 of 151 Interim Report #22 .Analysis of Soil Samples Exygen StudyNo .. PO000760 Table I. LIST OF TABLES Pane Summary of PFOA in Soil Samples ............................................................... 24 Table II. Summary of PFOA in Re-extracted Soil Samples.......................................... 32 Table III. Summary of PFOA in Associated Rinse Blanks and Trip Blanks.................33 Table IV. Matrix Spike Recovery of PFOA in Soil Samples ......................................... 34 Table V. Matrix Spike Recovery of PFOA in Re-extracted Soil Samples.................... 46 Table VI. Matrix Spike Recovery of PFOA in Associated Trip Blanks ......................... 48 Table VII. Surrogate Spike Recovery of 13CPFOA in Soil Samples .............................. 49 Table Vm. Surrogate Spike Recovery of 13CPFOA in Re-extracted Soil Samples........61 Table IX. Surrogate Spike Recovery of 13CPFOA in Associated Rinse Blanks and Trip Blanks ..................................................................................................... 63 Table X. Total Percent Solids in Soil Samples.............................................................. 64 Exygen Research Page 8 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Figure 1. Figure 2. Figure 3. Figure 4. Figure 5. Figure 6. Figure 7. Figure 8. LIST OF FIGURES Pane Typical Calibration Curve for PFOA in Methanol ...........,................,............70 Extracted Standards of PFOA in Methanol, 25 ng/mL and 50 ng/mL, Respectively........,...................,.....................,.....................,...............,...........71 PFOA in Methanol Reagent Blank, 50 ng/L Fortified Reagent Spk A, and 500 ng/L Fortified Reagent Spk B, Respectively..................................... 72 Chromatogram Representing a Soil Sample Analyzed for PFOA (Exygen ID: C0156344, Data Set: 041206AR) .............................................. 73 Typical Calibration Curve for 13CPFOA in Methanol................................... 74 Extracted Standards of I3CPFOA in Methanol, 25 ng/mL and 50 ng/mL, Respectively..............................,......................................,............................,.75 I3CPFOA in Methanol Reagent Blank, 50 ng/L Fortified Reagent Spk A, and 500 ng/L Fortified Reagent Spk B, Respectively..................................... 76 Chromatogram Representing a Soil Sample Analyzed for 13CPFOA (Exygen ID: C0156363, Data Set: 041306A) ................................................. 77 Exygen Research Page 9 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 LIST OF APPENDICES Pane Appendix A Study Protocol PO000760 (Exygen Study No. P0000760) with Analytical Methods and Protocol Amendments ........................................78 Exygen Research Page 10of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 1.0 SUMMARY Exygen Research extracted and analyzed soil samples for the determination of perfluorooctanoic acid (PFOA) according to Exygen Method VOOOl781 and water samples for the determination of perfluorooctanoic acid (PFOA) according to Exygen Method VOOOl780 (Appendix A). Thirty-three of the analyzed soil samples were not reported (NR) due to quality control failure. Eight of the thirty-three samples failed because the PFOA spikes were too low relative to the endogenous level in the sample to allow assessment of matrix interference. Twenty-five of the thirty-three samples failed for unknown reasons. Additional analytical work was performed in an attempt to provide quantitative results for these thirty-three samples. Quantitative PFOA results were obtained for all samples except for nine soil samples that are not reported due to quality control failures. The limit of quantitation for PFOA in soil was 0.2 ng/g. The LOQ provided is assuming wet weight values and the results for the actual samples are reported based on dry weight. The limit of quantitation for PFOA in water was 25 ng/L. Analytical results and assessed accuracies for the analysis of PFOA in soil samples based on dry weight are summarized in Table I. Analytical results and assessed accuracies for the analysis of PFOA in re-extracted soil samples based on dry weight are summarized in Table 11. Analytical results and assessed accuracies for the analysis of PFOA in water samples are summarized in Table 111. Field matrix spikes that were in the appropriate concentration range (primary concentration must be less than or equal to three times the spiking level) were used to calculate the assessed accuracies. When the field matrix spikes were not available or failed to meet recovery criteria, the laboratory spikes were used. Fortification recoveries for the analysis of PFOA in soil samples based on wet weight are summarized in Table IV. The overall average percent recovery & standard deviation for PFOA in soil samples based on wet weight was 80 f 19%. Fortification recoveries for the analysis of PFOA in re-extracted soil samples based on wet weight are summarized in Table V. The overall average percent recovery f standard deviation for PFOA in reextracted soil samples based on wet weight was 74 & 18%. Fortification recoveries for the analysis of PFOA in water samples are summarized in Table VI. The overall average percent recovery f standard deviation for PFOA in water samples was 92 f 7%. Fortification recoveries for I3C PFOA in soil samples based on wet weight are summarized in Table VII. The average percent recovery & standard deviation for I3C PFOA in soil samples based on wet weight was 91 f 32%. Fortification recoveries for 13C PFOA in re-extracted soil samples based on wet weight are summarized in Table VIII. The average percent recovery & standard deviation for I3C PFOA in re-extracted soil Exygen Research Page 11 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.:PO000760 samples based on wet weight was 48 k 30%. Fortification recoveries for 13CPFOA in water samples are summarized in Table IX. The average percent recovery rt standard deviation for 13CPFOA in water samples was 107 f 14%. The total percent solids for soil samples are detailed in Table X. 2.0 OBJECTIVE The objective of the analytical part of this study was to determine levels of perfluorooctanoic acid (PFOA) in soil and water according to Protocol PO000760 (Appendix A). 3.0 INTRODUCTION This report details the results of the analysis for the determination of PFOA in soil using the analytical method entitled, "V0001781:Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Soil by LC/MS/MS" and for the determination of PFOA in water using the analytical method entitled, "V0001780: Method of Analysis for the Determination of PerfluorooctanoicAcid (PFOA) in Water by LC/MS/MS." The study was initiated on November 5, 2004, when the study director signed protocol number P0000760. The analytical start date for this interim report was April 15, 2006 and the analytical termination date for this interim report was July 24,2006. 4.0 ANALYTICAL TEST SAMPLES Five water samples, representing one trip blank and its associated spikes and two rinse blanks (REI), and forty-seven soil samples (Exygen ID CO156344 - C0156395) were received on wet ice on March 2, 2006 from Tim Frinak at Weston Solutions, Inc. Six water samples, representing one trip blank and its associated spikes and three rinse blanks (RB), and twenty-three soil samples (Exygen ID C0159443 - C0159471) were received on wet ice on March 10, 2006 from Tim Frinak at Weston Solutions, Inc. Four water samples, representing one trip blank and its associated spikes and one rinse blank (RB), and thirty-four soil samples (Exygen ID C0160867 - C0160904) were received on wet ice on March 15, 2006 from Tim Frinak at Weston Solutions, Inc. Four water samples, representing one trip blank and its associated spikes and one rinse blank (RB), and thirteen soil samples (Exygen ID C0164222 - C0164260) were received on wet ice on March 24, 2006 from Tim Frinak at Weston Solutions, Inc. Please note that rinse blank (RB) samples do not have associated field spikes or laboratory spikes. The samples were logged in by Exygen personnel and placed in refrigerated storage. Exygen Research Page 12 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 The soil samples collected represent both soil boring samples and surface soil samples. Sample ID coding for the soil samples consisted of five sections or strings in the following format: DXXX-XX-XXXXXX-X(X)-XXXX. The first string of code, for the soil boring samples, contains DAL, which represents Decatur, Alabama. For the surface soil samples, the first string begins with D for Decatur, Alabama and the xxx defines the sampling location within the study area where: DF05 = Field 5 DF11 =Field 11 DF13 = Field 13 DFlO =Field 10 DF12 = Field 12 The second string defines the type of sample where: SB = soil boring sample SS = surface soil sample The third string for the soil boring samples defines the soil boring identification. For the surface soil sample, the third string defines the location within the sampling area. The fourth sting more specificallydefines the sample type where: 0 = primary field sample RB = equipment rinseate blank sample DB = field duplicate sample The fifth string defines the collection depth of the soil samples where: 0000 = 0 to 3 inches 0005 = 6 inches to 1 foot 0050 = 5 to 5.5 feet 0003 = 3 to 6 inches 0010 = 1 to 1.5 feet 0100 = 10 to 11 feet Sample login and chain of custody information is located in the raw data package associated With this interim report. Storage records will be kept at Exygen Research. 5.0 REFERENCE MATERIAL The analytical standard, PFOA (PFOA SP0005444), was purchased from Oakwood Products, Inc. and was received at Exygen on March 17, 2005. The analyhcal standard, PFOA (PFOA SP0007768), was received at Exygen on June 13, 2006 from the 3M Company. The surrogate spiking standard, 13Clabeled perfluorooctanoic acid (13CPFOA SP0004184), was received at Exygen on April 15, 2004 6om the 3M Company. The surrogate spiking standard, I3C labeled perfluorooctanoic acid (13CPFOA SP0006528), was received at Exygen on October 13, 2005 from the 3M Company. The surrogate Exygen Research Page 13 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 spiking standard, I3C labeled perfluorooctanoic acid (I3C PFOA SP0007767), was received at Exygen on June 13,2006 fiom the 3M Company. The available information for the reference materials is listed below. PFOA was stored ambient and I3C PFOA was stored frozen. Compound PFOA PFOA I3C PFOA I3C PFOA 13CPFOA Exvgen Inventory No. SP0005444 SP0007768 SP0006528 SP0004184 SP0007767 Lot # 203 HU14401DU 3507-195 3507-195 3507-277 Purity (%) 99 96.7 97 97 97.6 Expiration - Date 0313 1/07 12/15/06 03/29/09 03/29/09 07115/10 The molecular structure of PFOA is given below: PFOA Chemical Name: Perfluorooctanoic acid Molecular Weight: 414 Transitions Monitored: 413 + 369 (for quantification) and 413 + 219 (for confirmation) Structure: "C PFOA Chemical Name: 1,2-13C perfluorooctanoic acid Molecular Weight: 416 Transition Monitored: 415 + 370 Structure: F F F F,/\/\/\ F F I 13c I3C' O' H Exygen Research Page 14 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 6.0 DESCRIPTION OF ANALYTICAL METHOD The analytical methods "V0001781: Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Soil by L C N S N S " and "V0001780: Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Water by LC/MS/MS" were used for this study. 6.1 Extraction Procedure For Soil Before the samples were weighed for the extraction, they were placed into a new, clean Ziploc bag and mixed thoroughly. The samples were then transferred back to the sampling container. A 5-gram portion of soil was weighed into a fifty-milliliter centrifuge tube for the extraction. After fortification of appropriate samples, 5 mL of methanol was added to the samples. The samples were allowed to shake on a wrist action shaker for -15 minutes and were then sonicated in an ultrasonic bath for -15 minutes. The volume was taken to 40 mL with water and the samples were then centrifuged for -10 minutes at -3000 rpm. The supernatant was then loaded onto a C18 SPE cartridge conditioned with 10 mL of methanol and 5 mL of water. The eluate was discarded. Approximately five milliliters of methanol was added to the cartridge. Five milliliters of eluate was collected into a graduated 15 mL polypropylene centrifuge tube. Each sample was analyzed by LC/MS/MS electrospray. 6.2 Percent Solids Procedure For Soil Percent solids were determined using the procedure indicated in Exygen method V0000427. Approximately 20 grams of sample was weighed into a pan. The weight of the sample plus the pan was recorded. The samples were then dried in an oven overnight at 104f 2 "C.Then the samples were transferred to a dessicator and allowed to cool for -15 minutes. Each sample was then weighed again, including the weight of the pan. The percent solid for each sample was then calculated. See Table X for percent solids results. One soil sample, C00159446, was weighed at -8g for percent solid analysis, rather than at -2Og which is stated in the method. See deviation 6. The percent solid calculation was altered to reflect this change in mass. 6.3 Extraction Procedure for Water A 40 mL aliquot of the water sample was used for the extraction procedure. After fortification of appropriate samples, the samples were loaded onto a Cl8 SPE cartridge conditioned with 10 mL of methanol and 5 mL of water. The eluate was discarded. Approximately five milliliters of methanol was added to the cartridge. Five milliliters of Exygen Research Page 15 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 eluate was collected into a graduated 15 mL polypropylene centrihge tube. Each sample was analyzed by LC/MS/MS electrospray. 6.4 Preparation of Standards and Fortification Solutions A mixed stock standard solution of PFOA and I3CPFOA was prepared at a concentration of 1000 pg/mL by dissolving 100 mg of each of the standards (corrected for purity and salt content) in 100 mL of methanol. From this solution, the following fortification standards were prepared: Conc. of Fort Stock or Fort. Volume Solution (pg/mL)' 1000 10 100 10 10 10 1.o 10 0.1 10 of PFOA and I3CPFOA Final Volume 100 100 100 100 100 Final Conc. of Fortification Std. (Pg/mL) 100 10 1.o 0.1 0.01 A stock solution of only I3CPFOA was also prepared at a concentration of 100 pg/mL by dissolving 10 mg the standard (corrected for purity and salt content) in 100 mL of methanol. From this solution, the following fortification standards were prepared: Conc. of Stock or Fort. Solution (pg/mL)' 100 10 1.o 0.1 of I3CPFOA Fort Volume (mL) 10 10 10 10 Final Volume (mL) 100 100 100 100 Final Conc. of Fortification Std. tP&w 10 1.o 0.1 0.01 Exygen Research Page 16of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 A set of extracted calibration standards containing PFOA and "C PFOA were also made. The following concentrations were prepared before extraction: Conc. of Fort Fort Solution Volume (ng/mL)' (mL) - - 10 0.1 10 0.2 10 0.4 100 0.1 100 0.2 ' of 100 PFOA and 0.4 13CPFOA Volume of Fortified Sample (mL) 40 40 40 40 40 40 40 Final Conc. of Calibration Std. (ng/mL) 0 25 50 100 250 500 1000 The stock standard solution and all fortification and calibration standard solutions were stored in a refigerator (4' f 2C) when not in use. Documentation of standard preparation is located in the raw data package associated with this interim report. 6.5 Chromatography Quantification of PFOA was accomplished by LC/MS/MS electrospray. The retention time of PFOA was -1 1.2 min. Peaks above the LOQ were not detected in any of the reagent blank samples corresponding to the analyte retention time. 6.6 Instrument Sensitivity The smallest standard amount injected during the chromatographic run had a concentration of 0.2 ng/g of PFOA for sediment samples and a concentration of 25 ng/L for water samples. 6.7 Description of LC/MS/MS Instrument and Operating Conditions Instrument: Interface: Computer: Software: HPLC: API 4000 Biomolecular Mass Analyzer Turbo Ion Spray Liquid Introduction Interface DELL OptiPlex GX400 WindowsNT, Analyst 1.4.1 Hewlett Packard (HP) Series 1100 HP Quat Pump HP Vacuum Degasser HP Autosampler HP Column Oven Exygen Research Page 17 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 HPLC Column: Therm0 Fluophase RP,50 mm x 2.1 mm Column Temp.: -30" C Injection Vol.: 15 pL Mobile Phase (A): 2 mM Ammonium Acetate in water Mobile Phase (B): Methanol Time (min) %A - % B 0.0 65 35 1.o 65 35 8.0 25 75 10.0 25 75 11.0 65 35 18.0 65 35 Total run time: -18 min Flow Rate: 0.3 mL/min Ions monitored: Analvte PFOA PFOA Confirm Ion 13C PFOA Mode negative negative negative Transition Monitored 413 + 369 413 +219 415 + 370 Approximate Retention Time (min) -1 1.2 min. -1 1.2 min. -1 1.2 min. 6.8 Quantitation and Example Calculation PFOA concentrations are quantitated in nanogram of PFOA per liter of extract and then converted to nanogram per gram. Fifteen microliters of sample or calibration standard were injected into the LCMSMS. The peak area was measured and the standard curve was generated (using l/x fit weighted linear regression) by Analyst software using six concentrations of standards. The concentration was determined fiom the equations below. Equation 1 calculated the amount of analyte found (in ng/L, based on peak area) using the standard curve (linear regression parameters) generated by the Analyst software program. Equation 1: Analyte found (ng/L) = (Peak area - intercepax DF Slope Where: DF = Dilution Factor, factor by which the final volume was diluted, if necessary. Exygen Research Page 18 of 151 Interim Report #22 - Analysis of Soil Samples Exygen StudyNo.:PO000760 For samples fortified with known amounts of PFOA and 13CPFOA prior to extraction, Equation 2 was used to calculate the percent recovery. Equation 2: Recovery (%) = (analvte found (ndL) - analvte in control (ndL)J x 100% amount added (ng/L) Note: For the PFOA recovery calculation, the "control" is the unspiked aliquot of the primary field sample. Equation 3 was used to convert the amount of PFOA found in ng/L to ng/g (ppb) in the soil samples. Equation 3: PFOA found (ppb) =IPFOA found (ndL) x volume extracted (0.04L)I sample weight (5 g) Equation 4 was then used to calculate the amount of PFOA found in ppb based on dry weight. Equation 4: PFOA found (ppb) dry weight =PFOA found (ppb) x [100%/ total solids(%)] NOTE: Total solids (%) = [wet weight (g) / dry weight (g)] x 100% An example of a calculation using an actual sample follows: Soil sample Exygen ID C0160874 Spk C (Set: 041706B), fortified at 500 ng/L with PFOA where: peak area intercept slope dilution factor ng/L PFOA added (fort level) - 121349 - 18700 - 1060 - 10 - 500 n g L in corresponding sample (ng/L) = volume extracted (L) - sample weight (g) - - total solids (%) - 502 0.04 5 87.24 Exygen Research Page 19 of 151 ~ Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 From equation 1: Analyte found (ng/L) = 1121349- 187001x 10 1060 = 968ng/L From equation 2: % Recovery = (968 neJL - 502 nn/L) x 100% 500 ng/L = 93% From equation 3: PFOA found (ppb) = (968 ng/L x 0.04L) 5g = 7.74ppb From equation 4: PFOA found (ppb) dry weight = 7.74 ppb x (100% / 87.24%) = 8.87ppb Note: Numbers may vary slightly due to rounding. 7.0 EXPERIMENTAL DESIGN 13CPFOA was used as a surrogate for all of the samples. 13CPFOA was added to the soil samples in the laboratory after the samples were weighed for extraction. For soil samples designated as laboratory matrix spikes, PFOA was also added at a known concentration to the samples in the laboratory after the samples were weighed for extraction. For all of the water samples, I3CPFOA was added to the sample collection bottles in the laboratory before being shipped to the field for sampling. For water samples designated as field matrix spikes, PFOA was also added at a known concentration to the bottles in the laboratory before being shipped to the field. The samples were filled to a 200 mL volumetric fill line in the field. The soil samples were extracted in thirty-two sets. Each set included one reagent blank and two reagent blanks fortified at known concentrations. Twenty-two of the sets contained five samples sites and one set contained two sample sites. One sample was collected for each sample site. For each site, two laboratory matrix spikes and a laboratory duplicate were extracted. The last eight sets were re-extraction sets. Four sets contained eight samples, three sets contained seven samples, and one set contained six samples. Each re-extraction set consisted of one sample and variable laboratory matrix spikes. Exygen Research Page 20 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 The water samples were extracted in two sets. Each set included one reagent blank and two reagent blanks fortified at known concentrations. Set one contained three rinse blanks, two trip blanks with the associated spikes. Set two contained four rinse blanks and two trip blanks with the associated spikes. 8.0 RESULTS Analytical results and assessed accuracies for the analysis of PFOA in soil samples based on dry weight are summarized in Table I. Analytical results and assessed accuracies for the analysis of PFOA in re-extracted soil samples based on dry weight are summarized in Table 11. Analytical results and assessed accuracies for the analysis of PFOA in water samples are summarized in Table 111. Field matrix spikes that were in the appropriate concentration range (primary concentration must be less than or equal to three times the spiking level) were used to calculate the assessed accuracies. When the field matrix spikes were not available or failed to meet recovery criteria, the laboratory spikes were used. Quantitative PFOA results were obtained for all samples except for nine soil samples that are not reported due to quality control failures. Fortification recoveries for the analysis of PFOA in soil samples based on wet weight are summarized in Table IV. The overall average percent recovery & standard deviation for PFOA in soil samples based on wet weight was 80 f 19%. Fortification recoveries for the analysis of PFOA in re-extracted soil samples based on wet weight are summarized in Table V. The overall average percent recovery f standard deviation for PFOA in reextracted soil samples based on wet weight was 74 & 18%. Fortification recoveries for the analysis of PFOA in water samples are summarized in Table VI. The overall average percent recovery & standard deviation for PFOA in water samples was 92 f 7%. Fortification recoveries for 13C PFOA in soil samples based on wet weight are summarized in Table VII. The average percent recovery k standard deviation for 13C PFOA in soil samples based on wet weight was 91 f 32%. Fortification recoveries for 13C PFOA in re-extracted soil samples based on wet weight are summarized in Table VIII. The average percent recovery f standard deviation for 13C PFOA in re-extracted soil samples based on wet weight was 48 f 30%. Fortification recoveries for 13CPFOA in water samples are summarized in Table IX. The average percent recovery f standard deviation for 13CPFOA in water samples was 107f 14%. The total percent solids for soil samples are detailed in Table X. 9.0 CONCLUSIONS Except as noted above, the soil and water samples were successfully extracted and analyzed for PFOA according to analytical methods V0001781 and V0001780, Exygen Research Page 21 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 respectively. There were no circumstances that would have affected the quality or integrity of the data. 10.0 RETENTION OF DATA AND SAMPLES All original paper data generated by Exygen Research that pertains to this interim report will be shipped to the study director. This does not include facility-specific raw data such as instrument or temperature logs. Exact copies of all raw data, as well as a signed copy of the interim analytical report and all original facility-specific raw data, will be retained in the Exygen Research archives for the period of time specified in EPA TSCA Good Laboratory Practice Standards 40 CFR 792. Exygen Research Page 22 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.:PO000760 TABLES Exygen Research Page 23 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table I. Summary of PFOA in Soil Samples Client Analyte Found (ppb, nglg) Dry Weight C8 Acid PFOA Assessed ACCUTlCy co156344 DF13-SS-SSO3-0-0000 NR COl56344 Rep DFl3-SS-SSO3-0-0000' NR c0156345 DFl3-SS-SSO3-0-0003 NR C0156345 Rep DFI3-SS-SSO3-0-0003' NR C0156346 DFl3-SS-SSO4-0-0000 56.7 40 C0156346 Rep DF13-SSSSO4-0-0000' 58.6 40 C0156347 DFl3-SS-SSO4-0-0003 339 40 C0156347 Rep DF13-SSSSO4-0-0003* 288 40 C0156351 DF13-SSSS05-0-0000 NR C0156351 Rep DF13-SS-SSO5-0-0000* NR C0156352 DF13-SS-SS05-0-0003 NR C0156352 Rep DF13-SS-SSO5-WOO3' NR c0156353 DFI3-SSSS05-DB-0003 NR C0156353 Rep DF13-SS-SS05-DB-0003' NR C0156354 DF10-SS-SSOl-0-0000 NR C0156354 Rep DFl0-SS-SSOI-0-0000' NR c0156355 D F lO-SS-SSO1-0-0003 191 50 C0156355 Rep DF10-SSSSO1-0-0003' 220 50 C0156356 DFl O-SS-SSO2-0-0000 119 50 C0156356 Rep DF10-SS-SSO2-0-0000' 116 50 C0156357 DF10-SS-SS02-DB-0000 105 40 C0156357 Rep DF1O-SS-SSO2-DB-OOOO" 108 40 C0156358 DF10-SS-SSO2-0-0003 99.8 40 C0156358 Rep DF10-SS-3302-0-0003' 98.9 40 C0156360 DF10-SS-SS03-0-0000 16.9 50 C0156360 Rep DFl0-SS-SS03-0-0000* 15.2 50 C0156361 DF10-SS-SS03-0-0003 20.3 30 C0156361 Rep DF10-SS-SSO3-0-0003' 20.8 30 C0156362 DFl O-SS-SSO4-0-0000 339 30 C0156362 Rep DFlO-SS-SSO4-0-0000* 363 30 'Laboratory Duplicate ND = Not detected at or above the Limit of Quantitation (LOQ) of 0.2 ng/g (wet weight). NR = Not Reported due to Quality Control failures, see Table II for re-extract data. Exygen Research Page 24 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table I. Summary of PFOA in Soil Samples Continued Client Analyte Found (ppb, ndg) Dry Weight C8 Acid PFOA Assessed Accuracy C0156363 DFI0-SS-SSO4-0-0003 387 30 COI56363 Rep DF10-SS-SSO4-0-0003' 435 30 COI 56364 DFIO-SS-SS050-0000 338 50 CO156364 Rep DFI0-SSSSO50-0000' 313 50 C0156365 DFI0-SS-SSO50-0003 699 50 C0156365 Rep DF10-SS-SS050-0003' 560 50 C0156366 D F lI-SS-SSOl-0-0000 257 30 COI56366 Rep DF11-SSSSOI-0-0000' 250 30 C0156367 DF11-SS-SSO1-0-0003 NR C0156367 Rep DF11-SS-SSOI-0-0003' NR COI 56368 D F I 1-SS-SSO2-0-0000 NR COl56368 Rep DFI 1-SS-SSO2-0-0000' NR COI 56370 DFI I-SSSSO2-0-0003 NR C0156370 Rep DF11-SSSS02-0-0003* NR C0156371 DFI 1-SSSSO3-0-0000 NR C0156371 Rep DFI I-SS-SSO3-0-0000' NR COI 56372 DFI 1-SS-SS03-DB-0000 138 50 COI56372 Rep DFl I-SS-SS03-DB-O000' 170 50 COI 56373 DFI I-SS-SSO3-0-0003 NR C0156373 Rep DFI 1-SS-SSO3-0-0003' NR c0156374 D F I 1-SS-SSO4-0-0000 28.7 40 COI56374 Rep DFI I-SS-SSO4-0-0000* 32.2 40 COI 56375 D F I I-SSSSO4-0-0003 102 40 C0156375 Rep DFI I-SS-SSO4-0-0003' 97.6 40 C0156376 DFI 1-SS-SSO50-0000 48.9 30 C0156376 Rep D F I 1-SS-SSO50-0000' 47.4 30 COI 56377 DFI 1-SS-SSO50-0003 53.4 40 COI56377 Rep D F I I-SS-SSO50-0003* 58.5 40 C0156378 DF05SS-SSOl-0-0000 119 50 CO156378 Rep DFOSSS-SSOI-0-0000' 121 50 C0156379 DF05SS-SSOI-0-0003 51.6 40 C0156379 Rep DF05SS-SS01-O-OO03' 40.5 40 COI 56380 DF05SS-SS02-0-0000 346 30 COI56380 Rep DF05-SS-SS02-0-0000' 366 30 C0156381 DFO5SS-SSO2-0-0003 NR C0156381 Rep DF05SS-SS02-0-0003' NR 'Laboratoty Duplicate ND = Not detected at or above the Limit of Quantitation(LOQ) of 0.2 ng/g (wet weight). NR = Not Reporteddue to Quality Controlfailures, see Table II for re-extractdata. Exygen Research Page 25 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table I. Summary of PFOA in Soil Samples Continued Client Analyte Found (ppb, nglg) Dry Weight C8 Acid PFOA Assessed Accuracy C0156382 DFl2-SS-SSO1-0-0000 49.8 30 C0156382 Rep D F l2-SSSSO1-0-0000' 82.8 30 C0156383 DFl2-SSSSOl-0-0003 NR C0156383 Rep D F l2-SSSSO1-0-0003' NR C0156384 DFl2-SS-SS02-0-0000 NR C0156384 Rep DFl2-SS-SSO2-0-OOOO' NR C0156385 DFl2-SSSS02-0-0003 NR C0156385 Rep DFl2-SSSS02Q0003' NR C0156386 DF12-SS-SS03-0-0000 NR C0156386 Rep DFl2-SSSSO3-0-0000' NR C0156387 DFl2-SSSS03-0-0003 29.9 50 C0156387 Rep DFl2-SSSS03-0-0003' 40.7 50 C0156388 DFl2-SSSS04-0-0000 NR C0156388 Rep DFl2-SS-SS04-0-0000' NR C0156389 DF12-SS-SSO4-0-0003 NR C0156389 Rep DFl2-SS-SS04-0-0003' NR C0156390 DF 124s-SSO5-0-0000 42.1 30 CO156390 Rep DF12-SS-SSO5-0-0000' 48.8 30 C0156391 DF 12-SSSSO5-0-0003 176 40 C0156391 Rep DF12-SS-SS05-0-0003' 174 40 C0156392 DFl3-SS-SSOl-0-0000 310 50 C0156392 Rep DFl3-SS-SSOl-0-0000' 315 50 C0156393 DFl3-SS-SSOI-0-0003 NR C0156393 Rep DF13-SS-SS01-0-0003' NR C0156394 DFI3-SS-SSO2-0-0000 NR C0156394 Rep DFl3-SS-SS02-0-0000' NR C0156395 DFI3-SS-SSO2-0-0003 NR C0156395 Rep DFl3-SS-SS02-0-0003' NR C0159446 DAL-SB-603R-0-0000 NR C0159446 Rep DAL-SB-603R-0-0000' NR C0159447 D AL-SB-603R-0-0005 4.02 50 C0159447 Rep DAL-SB-603R-0-0005' 4.04 50 'Laboratory Duplicate N D = Not detected at or above the Limit of Quantitation (LOQ) of 0.2 ng/g (wet weight). NR = Not Reported due to Quality Control failures, see Table II for re-extract data. Exygen Research Page 26 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table I. Summary of PFOA in Soil Samples Continued Exyeen ID c COI 59448 COI59448 Rep COI 59449 COI59449 Rep C0159450 COI59450 Rep C0159451 COW9451 Rep C0159453 C0159453 Rep C0159451 COl59454 Rep COI 59455 C0159455 Rep COI 59456 C0159456 Rep COI 59457 COI 59457 Rep COI 59458 C0159458 Rep COI 59459 C0159459 Rep c0159460 COI59460 Rep C0159461 C0159461 Rep C0159462 CO159462 Rep COI 59463 COI59463 Rep C0159464 C0159464 Rep c0159466 C0159466 Rep COI 59467 COI59467 Rep COI 59468 C0159468 Rep Client Sample ID DAL-SB-603R-0-0010 DAL-SB-603R-0-0010' DAL-SB-603R-0-0050 DAL-SB-603R-0-0050' DAL-SB-603R-0-0100 DAL-SB-603R-0-0100' DAL-SB-603R-DB-OI OO DAL-SB-603R-DB-OI OO' DAL-SB-604R-0-0000 DAL-SB-604R-0-0000' DAL-SB-604R-0-0005 DAL-SB-604R-0-0005' DAL-SB-604R-0-0010 DAL-SB-604R-0401O* DAL-SB-604R-0-0050 DAL-SB-604R-0-0050' DAL-SB-604R-0-0100 DAL-SB-604R-0-0100' DAL-SB-605R-0-0000 DAL-SB-605R-0-0000* DAL-SB-605R-DB-0000 DALSB-605R-DB-0000' DAL-SB-605R-0-0005 DAL-SB-605R-O-0005' DAL-SB-605R-0-0010 DAL-SB-605R-O-0010' DAL-SB-605R-0-0050 DAL-SB-605R-0-0050' DAL-SB-605R-0-0 100 DALSB-605R-O-OIOO* D A L - S E I 38R-0-0000 DAL-SB-I38R-0-0000' DAL-SB-I 38R-0-0005 DAL-SB-138R-O-0005' DAL-SB-138R-0-0010 DAL-SB-I 38R-0-0010" DAL-SB-I 38R-0-0050 DALSB-I38R-0-0050' Analyte Found (ppb, nglQ)Dry Weight C8 Acid PFOA Perfluorooctanoic Acid 5.34 4.78 NR NR I.45 1.10 0.936 0.990 NR NR NR NR 1.46 I.62 5.71 5.52 ND 0.356 7.95 7.86 7.61 7.98 7.82 7.46 2.64 3.33 I. O l I.03 0.849 0.862 27.6 29.1 48.8 57.2 40.7 47.4 NR NR Assessed Accuracy (+I- %) 40 40 40 40 30 30 30 30 30 30 30 30 40 40 30 30 30 30 30 30 30 30 30 30 30 30 30 30 30 30 'Laboratory Duplicate ND = Not detected at or above the Limit of Quantitation (LOCI) of 0.2 nglg (wet weight). NR = Not Reporteddue to QualityControlfailures, see Table II for re-extractdata. Exygen Research Page 27 of 151 Interim Report #22 - Analysis of Soil Samples Exygen StudyNo.:PO000760 Table I. Summary of PFOA in Soil Samples Continued Client Analyte Found (ppb, n@/g)Dry Weight C8 Acid PFOA Asmessed Accuracy C0159470 DAL-SB-138R-0-0100 354 40 COl5947ORep DAL-SB-138R-0-0100' 269 40 C0159471 DAL-SB-138R-DB-0100 308 30 CO159471 Rep DAL-SB-138R-DB-0100' 309 30 COi 60871 DF05-SS-SS03-0-0000 NR C0160871 Rep DF05-SS-SS03-0-0000" NR C0160872 DF05SSSS03-0-0003 NR C0160872 Rep DFO5-SSSSO3-0-0003' NR C0160873 DF05-SS-SS04-0-0000 NR C0160873 Rep DF05-SS-SS04-0-0000' NR C0160874 DF05-SS-SS04-0-0003 4.60 30 CO160074 Rep DF05-SS-SS04-0-0003' 4.62 30 C0160875 DF05-SS-SS05-0-0000 5.79 40 C0160875 Rep DF05-SS-SS05-0-0000' 5.71 40 C0160876 DF05-SS-SS05-0-0003 7.23 30 C0160876 Rep DFO5-SS-SSO5-0-OOO3' 6.76 30 C0160877 DF05-SS-SS05-DE-0003 7.41 50 C0160877 Rep DF05-SSSS05-DB-0003' 7.12 50 C0160878 DF09-SS-0006-WOOO 14.8 30 C0160878 Rep DFOSSS0006-0-0000' 14.9 30 C0160879 DF09-SS-0006-0-0003 16.3 30 C0160879 Rep DF0SSS-0006-0-0003* 15.4 30 C0160880 DF09-SS0006-0-0010 8.91 40 C0160880 Rep DFWSS-0006-0-0010' 8.92 40 C0160881 DF09-SS-0007-0-0000 173 50 C0160881 Rep DF09-SS-0007-0-0000' 182 50 C0160882 DF09-SS-0007-0-0003 124 50 C0160882 Rep DFOSSS-0007-0-0003' 112 50 'Laboratory Duplicate ND = Not detected at or above the Limit of Quantitation(LOQ) of 0.2 ng/g (wet weight). NR = Not Reporteddue to Quality Control failures, see Table I1for re-extractdata. Exygen Research Page 28 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table I. Summary of PFOA in Soil Samples Continued Client Analyte Found (ppb, nglg) Dry Weight C8 Acid PFOA Assessed Accuracy C0160883 DF09-SS-0007-0-0010 46.7 50 C0160883 Rep DFOQ-SS-0007-0-0010' 51.4 50 C0160884 DF09-SS-0007-DB-0010 38.9 30 C0160884 Rep DF09-SS-0007-DB-0010' 47.9 30 C0160885 DF09-SS-0008-0-0000 176 30 C0160885 Rep DFOQ-SS-0008-0-0000' 149 30 COI 60886 DFO9-SS-0008-0-0003 149 40 C0160886 Rep DFOQ-SS-0008-0-0003' 135 40 C0160887 DF09-SS-00080-0010 122 30 C0160887 Rep DFOQ-SS-0008-0-0010" 108 30 C0160888 DF09-SS-0009-0-0000 10.1 40 C0160888 Rep DFOQ-SS-0009-0-0000' 11.1 40 C0160889 DFO9-SS-000900003 12.2 30 C0160889 Rep DFOQ-SS-0009-0-0003' 14.6 30 C0160890 DF09-SS-0009-DE-0003 12.3 30 C0160890 Rep DF09-SS-0009-DB-0003' 13.5 30 C0160891 DFO9-SS-0009-0-0010 19.0 30 C0160891 Rep DFOQ-SS-00080-0010' 23.1 30 C0160892 DF09-SS-0010-0-0000 886 30 C0160892 Rep DFOQ-SS-0010-0-0000' 934 30 C0160893 DF09-SS-0010-0-0003 51 1 30 C0160893 Rep DFOQ-SS-0010-0-0003" 498 30 C0160894 DFOQ-SS-0010-0-0010 461 30 C0160894 Rep DFOQ-SS-0010-0-0010' 357 30 C0160895 DF09-SS-0011-0-0000 253 30 C0160895 Rep DFOQ-SS-0011-0-0000' 297 30 C0160896 DF09-SS-0011-0-0003 284 30 C0160896 Rep DFOQ-SS-0011-0-0003' 360 30 'Laboratory Duplicate ND = Not detected at or above the Limit of Quantitation(LOQ)of 0.2 ng/g (wet weight). NR = Not Reported due to Quality Controlfailures, see Table II for re-extract data. Exygen Research Page 29 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table I. Summary of PFOA in Soil Samples Continued Exygen ID Client Sample ID Analyte Found (ppb, nglg) Dry Weight C8 Acid PFOA Perfluorooctanoic Acid Assessed Accuracy (+/- %) i COI 60897 DF04SS-0011-0-0010 NR COI60897 Rep DF04SS-0011-0-0010" NR COI 60898 DF04SS-0012-0-0000 NR C0160898 Rep DF04SS-0012-0-0000' NR CO160899 DF04SS-0012-DB-0000 535 30 CO160899 Rep DF0!3-SS-0012-DB-0000' 500 30 COI 60900 DF04SS-0012-0-0003 NR CO160900 Rep DF04SS-0012-0-0003' NR co160901 DFOSSS-0012-0-0010 481 40 C0160901 Rep DF04SS-0012-0-0010' 454 40 c0160902 DFO4SS-OO13Q0000 21 .I 30 C0160902 Rep DF04SS-0013-0-0000' 21 .o 30 c0160903 DF04SS-0013-0-0003 25.4 30 C0160903 Rep DF04SS-0013-0-0003' 29.3 30 COI 60904 DF04SS-0013-0-0010 50.5 40 COI 60904 Rep DF04SS-0013-0-001'0 42.7 40 C0164247 DAL-SB-602R-0-0000 6.1 I 30 C0164247 Rep DAL-SB-602R-0-0000' 6.58 30 COI 64248 DAL-SB-602R-0-0005 6.91 30 C0164248 Rep DAL-SB-602R-0-0005' 6.73 30 C0164249 DAL-SB-602R-0-0010 4.03 30 C0164249 Rep DAL-SB-602R-0-001 0' 3.24 30 c0164250 DAL-SB-602R-0-0050 0.766 30 C0164250 Rep DAL-SB-602R-0-0050' 0.674 30 C0164251 DAL-SB-602R-0-0100 0.665 40 C0164251 Rep DAL-SB-602R-0-01 00' 0.561 40 C0164252 DAL-SB-601R-0-0000 I.75 30 C0164252 Rep DAL-SB-601R-0-0000' 2.1 1 30 COI 64253 DAL-SB-601R-DB-0000 2.22 30 C0164253 Rep DAL-SB-601R-DB-0000 1.97 30 c0164254 DAL-SB-601R-0-0005 1.91 30 C0164254 Rep DAL-SB-601R-0-0005 I.87 30 'Laboratoty Duplicate ND = Not detected at or above the Limit of Quantitation (LOQ) of 0.2 ng/g (wet weight). NR = Not Reporteddue to QualityControlfailures, see Table II for re-extract data. Exygen Research Page 30 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table I. Summary of PFOA in Soil Samples Continued Client Analyte Found (ppb, ndg) Dry Weight C8 Acid PFOA Assessed Accuracy COI 64255 DAL-SB-601R-0-0010 NR C0164255 Rep DAL-SB-601R-0-0010 NR COI 64256 DAL-SB-601R-DB-0010 2.15 40 C0164256 Rep DAL-SB-601R-DB-0010 1.66 40 C0164257 DALSB-601R-0-0050 0.895 30 C0164257 Rep DAL-SB-601R-0-0050 1.42 30 COI 64259 DAL-SB-601R-0-0100 0.477 30 C0164259 Rep DAL-SB-601R-0-0100' 0.438 30 c0164260 DAL-SB-601R-DB-0100 0.485 30 C0164260 Rep DAL-SB-60IR-DB-0100' 0.399 30 'Laboratory Duplicate ND = Not detected at or above the Limit of Quantitation (LOQ) of 0.2 ng/g (wet weight). NR = Not Reported due to Quality Control failures, see Table II for re-extract data. Exygen Research Page 31 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table 11. Summary of PFOA in Re-extracted Soil Samples Client Analyte Found (ppb, nglg) Dry Weight C8 Acid PFOA Assessed Accuracy co156344 DF13-SS-SSO3-04000 525 40 C0156345 DF13-SS-SSO3-04003 551 30 C0156351 DF 13-SS-SSO50-0000 1130 40 C0156352 DFl3-SS-SSO50-0003 1020 30 c0156353 DFl3-SS-SS05-DB-0003 857 50 C0156354 DFl0-SS-SSOl-O-OOOO NR C0156367 DF11-SS-SSO1-0-0003 86.8 30 C0156368 D F I 1-SS-SSO2-0-0000 NR C0156370 D F I 1-SS-SS02-0-0003 818 30 C0156371 DFI1-SS-SSO3-0-0000 102 40 c0156373 DFl l-SS-SSO3-0-0003 NR C0156381 DFO5SS-SSO2-0-0003 335 50 C0156383 DF12-SS-SSOl-0-0003 197 30 c0156384 DF12-SS-SSO2-04000 2140 50 C0156385 DF12-SSSS02-0-0003 3910 40 c0156386 DFl2-SSSS03-04000 28.6 50 C0156388 ' DF12-SS-SSWOOO 4390 30 C0156389 DFl2-SS-SS04-0-0003 11900 30 c0156393 DF13-SS-SSO1-0-0003 561 30 C0156394 DF13-SS-SSO2-0-0000 3350 50 C0156395 DF13-SS-SSO2-0-0003 5930 30 c0159449 DAL-SB-603R-0-0050 3.71 30 C0159453 DAL-SB-604R-04000 2.29 50 c0159454 DAL-SB-604R-04005 3.75 30 C0159468 DAL-SB-138R-0-0050 104 30 C0160871 DF05SS-SS03-0-0000 227 40 C0160872 DF05SS-SS03-0-0003 NR C0160873 DF05SS-SS04-0-0000 NR C0160897 DF09-SS-0011-0-0010 238 40 C0160898 DFO9-SS-0012-0-0000 NR C0160900 DFO9-SS-0012-0-0003 NR C0164255 DAL-SB-601R-0-0010 NR ND = Not detectedat or above the Limit of Quantitation (LOQ) of 0.2nglg. NR = Not mported due to quality control failures. Exygen Research Page 32 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table 111. Summary of PFOA in Associated Rinse Blanks and Trip Blanks Client Analyte Found (ppt, ng/L) C0 Acid PFOA Assessad Accuracy co156348 DF13SS-TRIP14460221 ND 30 C0156359 DFlO-SS-SS03-RB4)000 ND 30 C0156369 DF11SS-SSO2-RB-0003 ND 30 C0159443 DALSB-TRIP14460302 ND 30 C0159452 DAL-SB-603R-RB-0100 ND 30 C0159465 DAL-SB-138R-RB-0000 ND 30 C0159469 DAL-SB-138R-RE4100 ND 30 C0160867 DF05SS-TRIP24460308 ND 30 C0160870 DFO5-SS-SS03-RB4000 ND 30 co164222 DAL-SB-TRIP-0460316 ND 30 co164258 DAL-SB-601R-RB4100 ND 30 ND = Not detectedat or above the Limitof Quantitatiom (LOQ) of 25 ng/L. Exygen Research Page 33 of 151 - ~~ ~~ Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 -- - - Table IV. Matrix Spike Recovery of PFOA in Soil Samples Amount Amt Found C8 Acid PFOA Amount Sample Spiked in Sample Recovered Recovery DF13SS-SSO3-0-0000 (CO154344 Spk C. 4 ppb Spike) 4 NR NR NR DFl3SSSS03-0-0000 (COlSI344Spk D. 400ppb Spike) 400 NR NR NR DFl3SSSSO3-0-0003 (COlSI345Spk E,4 ppb Splko) 4 NR NR NR DFl3SSSS03-0-0003 (COlSIW Spk F,400ppbSplko) 400 NR NR NR DF13SSSSO4-04000 (C01- Spk 0.4 ppb Spike) 4 47.3 52.7 DF13SS-SSO4-0-0000 (COlSIUr Spk H. 400 ppb Spike) 400 47.3 298 63 DF13SSSS04-0-0003 (C0158347 Spk I, 4 ppb Splke) 4 296 284 DF13SS-SS04-0-0003 (Cor56347 Spk J, 400 ppb Spike) 400 296 570 69 DF13SSSS050-0000 (COlSUSl Spk K, 4 ppb Spike) 4 NR NR NR DFl3SS-SS054-0000 (CMSI351 Spk L, 400 ppb Spike) 400 NR NR NR DF13SS-SSO5M)oO3 (COlSI3U Spk C. 4 ppb Spike) 4 NR NR NR DFl3SSSSO54-0003 (COlsrssZ Spk D, 400 ppb Splko) 400 NR NR NR DF13-SSSSO5-DB-0003 (COlSIU, Spk E, 4 ppb Spike) 4 NR NR NR DF13-SSSS05DB-0003 (CMSI3.53 Spk F. 400 ppb Spike) 400 NR NR NR DF1OSS-SSO1-0-0000 (COlSUSr Spk 0 . 4 ppbSpike) 4 NR NR NR DFlOSSSS01~ (COlst354 Spk H, 400 ppb Spike) 400 NR NR NR DFlOSS-SSOl-0-0003 (C01#3# spk I,4 ppbSPlL.) 4 166 161 DFlOSSSSOl-0-0003 (COl!X355 Spk J, 400 ppb Splko) 400 166 397 58 DFlOSSSSO2-0-0000 (COl5CM6 Spk K, 4 ppb Spike) 4 102 105 DFlOSS-SS02a0000 (CMSISSI Spk L, 400 ppb Spike) 400 102 330 57 'Sample residuaexceedsthe spiking level significantly(3xspiking level); therefore. an accurate recoveryvalue cannot be calculated. ND = Not detected at or above the Limit of QuanUtation (LOQ) of 0.2 ng/g (wet weight). NR = Not Reporteddue to Quality Contrdfailures. see Table V forre-extfactdata. Note: Since this summarytable shows rounded mults, recoveryvalues may vary slightly from the values In the raw data. Exygen Research Page 34 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table IV. - - - Matrix Spike Recovery of PFOA in Soil Samples Continued I Amount Amt Found C0 Acid PFOA Amount -= Sample Spiked in Sample Recovered Recovery DFlOSSSS02-DB-0000 (COlW357 Spk C. 4 ppb Spike) 4 91.2 102 DFlO-SSSS02-DB-0000 (COlW357Spk D. 400Dpb Spike) 400 91.2 364 88 DFlOSS-SSO2-0-0003 (C0150368 Spk E, 4 ppb Spike) 4 06.4 02.4 DFlOSSSS02-0-0003 (COlW350 Spk F, 400 ppb Spike) 400 06.4 330 61 DFlOSSSS03-0-0000 (COlWM Spk 0 . 4 ppbSpike) 4 13.0 14.8 DFlOSSSS03-0-0000 (COlWuO Spk H.400 ppb Spike) 400 13.0 246 58 DF10SS-SS03-0-0003 (COlWrl Spk 1.4 ppb Spike) 4 17.1 19.4 DF10SS-SS03-0-0003 (COl58361Spk J. 400 ppb S p h ) 400 17.1 304 72 . DF10SS-SS04-0-0000 (COlW382Spk K, 4 ppb Spike) 4 242 198 DFlOSSSS04-0-0000 (COlW362spk r,400ppb Splke) 400 242 530 72 DFlOSS-SS04-0-0003 ( C O l W Spk C, 4 ppbSpike) 4 293 310 DFlOSSSS04-0-0003 (CCOlW383Spk 0,400ppb Spike) 400 293 598 76 . DFlOSS-SSO50-0000 (COlWW Spk E,4 ppb Spike) 4 278 263 DFlOSS-SSO5oM)o ( C O l W Spk F. 400ppbSpike) 400 270 490 53 DFlOSS-SS050-0003 (COl50305Spk G. 4 ppbSpike) 4 577 598 DFlOSSSS050-0W3 (COIB365Spk H. 400 ppb Spike) 400 577 800 56 DFllSS-SSOl-MH)oo (COlsrSrcspk I,4 ppb spike) 4 209 228 DFllSSSSOl-0-0000 (Cor58366 Spk J, 400 ppb Spike) 400 209 498 72 DFll-SS-SS01-0-0003 (COlWSI7Spk K, 4 ppb Spike) 4 NR NR NR DFllSS-SS01-0-0003 (C0150307 Spk L. 400 ppb Spike) 400 NR NR NR 'Sample residueexceeds the spikinglevelsignificantly (3x spikinglevel);therefore. anaccuraterecweryvaluecannotbe calculated. ND = Not detectedat o( abovethe Limitof Quantitah (LW) of 0.2 nglg (wet WeiQht). NR= NotReporteddueto QualityControlfailures, see TableV for re-extractdata. Note: Since this summarytableshow roundedresults, recoveryvaluesmayvary slightlyfrom thevalues Inthe raw data. Exygen Research Page 35 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table IV. Matrix Spike Recovery of PFOA in Soil Samples Continued Sample Description DFl1SS-SS02-0-0000 (CO11W Spk C. 4 ppb Splke) - Amount Spiked 4 Amt Found in Sample miweight NR C8 Acid PFOA Amount Recovered (na/Q)wet weight - Recovery ( 1 % NR NR DFllSSSS02-0-0000 (CO11360 Spk D, 400 ppb Spike) 400 NR NR NR DFllSS-SSO2-0-0W3 (C011170 Spk E, 4 ppb Splke) 4 NR NR NR DFl1SSSS02-0-0003 (C011370 Spk F, 400 ppb Splke) 400 NR NR NR DF11SS-SSO3-0-0000 (C0156.371Spk 0 . 4 ppb Spike) 4 NR NR NR DFl1SS-SSO3-O-0000 (C01.56371 Spk H, 400 ppb Splke) 400 NR NR NR DFll-SSSS03-DB-OOOO (CO158372 Spk 1.4 ppb Spike) 4 110 113 DF1l-SSSS03-DB-0)000 (COlS372 Spk J, 400 ppb Spike) 400 110 316 52 DFllSS-SSO3-0-0003 (COl1373 Spk K, 4 ppb Spike) 4 NR NR NR DF11SSSS03-0-0003 (C011373 Spk L, 400 ppb Spike) 400 NR NR NR DFl1SSSSO4-o-DooO (CO156.374 Spk C. 4 ppb Splke) 4 24.9 29.4 DF11SSSS04-0-0000 (CO156374 Spk D. 400 ppb Spike) 400 24.9 298 68 . DFl1SS-SSOe0-0003 (C0158376 Spk E, 4 ppb Spike) 4 91.2 96.0 DFl1SSSS04-04003 (CM1376 Spk F, 400 ppb Splke) 400 91.2 342 63 . DF1lSSSSO5-0-0000 (C0156378 Spk G,4 ppb Spike) 4 40.9 34.6 DF1-sls-sS05-0-0000 (COlS376 Spk H, 400 ppb Spike) 400 40.9 322 70 DFl1SSSSOW-OW3 (COl1377 spk 1.4 ppb Spike) 4 45.5 44.9 DFl lSsSS050-0003 (COlS377 Spk J. 400 ppb Spfko) 400 45.5 317 68 DF05SSSSOl-0-0000 (C011378 Spk K, 4 ppb Splke) 4 96.8 128 DF05SS-SS01-0-0000 (C011378 Spk I.,400ppb Splke) 400 96.8 318 55 *Sample residueexceeds the spiking level signiffcantly (3x spiking level); therefore, anaccurate recoveryvalue cannot be calculated. ND = Not detected at or abovethe Limit of Quantitati (LW) of 0.2 na/g (wet weight). NR = Not Reported due to Quality Control failures. see Table V for re-extract data. Note: Since t h k summary table shows rounded recult., recoveryvalues mayvary slightly from the values in the raw data. Exygen Research Page 36 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table IV. Matrix Spike Recovery of PFOA in Soil Samples Continued Sample DFOISSSSOI-0-0003 ( C O 1 ~ 7%s k c. 4 ppb Spike) DFO5SS-SSOl-O-OOO3 (COlSO37S Spk D, 400 ppb Splko) DF05SS-SS02-0-0000 (COlSOW Spk E, 4 ppb Splke) DF05SS-SS02-O-OOW (COlSr3M Spk F, 400 ppb Splke) DF05SSSS02-0-0003 (COlsrSrl Spk G, 4 ppb Splke) DF05SS-SS024-0003 (COlW11 Spk ti, 400 ppb Splke) DF12SS-SS01-0-0000 (COlWW Spk I,4 ppbSplko) DF12SS-SSOl-0-OOOO (COlsrsU Spk J, 400ppbSpike) DF124s-SSO1-0-0003 (COlSO13 Spk K, 4 ppb Splke) DF12SS-SSOl-OM)O3 (COlSO383Spk L 400ppb Splke) DF12SS-SSO2-0-0000 (COlSO3MSpk C, 4 ppb Spllu) DF12SS-SS02-0-0000 (COlSO3M Spk D. 400 ppb Splke) DFlZSS-SSOZ-OMX)3 (COlsUrs spk E. 4 ppb Spllu) DF12SS-SS02-0-0003 (COlSOS6 Spk F, 400 ppb Splke) DF12SS-SS03-0-0000 (CO1603USpk G 4 ppbSplke) DF12-SS-SSo3oMxK, ( C O I I U O Spk H, 400ppbSpike) DFl2SS-SSO3-pooo3 (COlSO387Spk I.4 ppbSpik.) DFI2SS-SSO3-04003 (C0156367 Spk J. 400 ppb Spike) DFI2-SSSS04-0-0000 ~ ~ i wspulr r 4 ppb splke) DF12SS-SSO4-0-0000 (COl5UM Spr I.,400 ppbSplke) .p a E- Amount Amt Found Spiked in Sample A 4 43.4 400 43.4 4 285 400 285 4 NR 400 NR 4 41.2 400 41.2 4 NR 400 NR 4 NR 400 NR 4 NR 400 NR 4 NR 400 NR 4 28.2 400 26.2 4 NR 400 NR C8 MiPFOA Amount Recovered 45.0 303 410 08 1 NR NR 80.8 326 NR NR NR NR NR NR NR NR 22.3 254 NR NR Recovery . 65 99 NR NR 71 NR NR NR NR NR NR NR NR . 57 NR NR 'Sample residueexceeds the spiking levelsignificantly (3x spikinglevel); therefore.anaccuraterecoveryvaluecannotbe calculated. ND = Not detectedator abovethe Limitof Quantitation(LOQ) of 0.2 ng/g (wet weight). NR = N d Repotteddue to QuaMyConbd failures, see TableV for re-extractdata. Note: Slncethis summarytable shows roundedrerub, recoveryvalues mayvary sllghtlyfrom the values In the raw Uata. Exygen Research Page 37 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table IV. - Matrix Spike Recovery of PFOA in Soil Samples Continued P c - C8 Acid PFOA , - i Amount Amt Fwnd Amount Sample Spiked in Sample Recovered Recovery Description As9L (nglg) wet weight (nglg) wet weight DFl2SSSSoeO-0003 (COl#ue Spk C, 4 ppb Spike) 4 NR NR NR DFl2SSSSoeO-0003 (CO158389Spk D, 400ppbSpike) 400 NR NR NR DFl2SSSS05-0-0000 (COI58JlOSpr E, 4 ppb Spike) 4 33.0 37.3 DFl2SSSS054-0000 (COl58390Spk F. 400ppb Spike) 400 33.0 406 93 . DF12SSSS05-0-ooO3 (COlWUl Spk 0 4 ppb Spike) 4 143 148 DFI2SS-SS05-0-0003 (CO15w11 Spk H. 400 ppb Spike) 400 143 407 66 DF13SSSSOI40000 (C0158392 Spk I,4 ppb Spike) 4 240 251 DFl3SSSSOl-0-0000 (CO158312Spk J, 400ppb Spike) 400 240 438 50 DFI34s-SSOl-0-0003 (COlWUS Spk K, 4 ppb Spike) 4 NR NR NR DF13SSSSOl-0-0003 (COl56.393 Spk L 400 ppb Spike) 400 NR NR NR DFI~SSSSO~-O-OOOO (COl54394Spk C. 4 ppb Spike) 4 NR NR NR DFI3SSSS02-0-oooO (CO158SMSpk D, 400 ppb Spike) 400 NR NR NR DFI3SSSS02-0-0003 (COlSU96 Spk E. 4 ppb Spike) 4 NR NR NR DFI3SSSS02-0-0003 (C0158395 Spk F. 400 ppb Spike) 400 NR NR NR DAL-SB603R-0-0000 ( C O l W Spk E. 4 ppb Spike) 4 NR NR NR DAL-SB603R-04000 (CO159448Spk F. 100ppb Spike) 400 NR NR NR DAL-SB603R-0-0005 (C0159447 Spk 0.4 ppb Spike) 4 3.45 5.57 53 DALSB-803R-0-0005 (C0159447 Spk H, 400 ppb Spike) 400 3.45 268 66 DALSB-603R-0-0010 (COlsr*cr Spk I.4 ppbSpike) 4 4.36 6.81 61 - DALSBsO3R-M)OlO (COl59440Spk J. 100ppbSpike) - 400 4.36 282 69 'Sample residue exceeds the spiking l e d significantly (3xspikingl e d ) ; therefore, an accurate recoveryvalue cannot be calculated. ND = Not detected at Q above the Limitof Quantitation(LOQ) of 0.2 ng/g (wet weight). NR = Not Repotteddue to Q u a l i Contmlfailures. 888 Table V for redxtractdata. Note: Since thir summarytable shows mundedresults, recoveryvaluesmayvary slightlyfrom tha values In the n w d8ta. Exygen Research Page 38 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table IV. Matrix Spike Recovery of PFOA in Soil Samples Continued - Amount Amt Found Amount Sample Spiked in Sample 0(MJ/Q) wet weight Recovered (ng/g) wet weight 1 Recovery %) DAL-SB-603R-0-0050 (C015U48 Spk K. 4 ppb Spike) 4 NR NR NR DAL-SB-603R-0-0050 ( C M W Spk L, 400 ppb Spike) 400 NR NR NR DAL-SB-603R-0-0100 ( C O l M Spk C. 4 ppb Spike) 4 1.21 3.60 65 DAL-SB-603R-0-0100 (COlSWiO Spk D, 400 ppbSph) 400 1.21 303 75 DAL-SB5OIR-DB-0100 (CO15S451 Spk E, 4 ppb Spike) 4 0.733 3.72 75 DAL-SB-603R-DB-0100 (COlSs451 Spk F, 400 ppb Spike) 400 0.733 295 74 DAL-SB-604R-0-0000 (COlSM53Spk 0 . 4 ppbSpike) 4 NR NR NR DAL-SB-604R-0-0000 (COlSS463 Spk H. 400 ppb Spike) 400 NR NR NR DAL-SB-604R-0-0005 (CO158454 Spk 1.4 ppb Spike) 4 NR NR NR DAL-SB-604R4-0005 (Cor58454 Spk J. 400 ppb Splke) 400 NR NR NR DAL-SB-604R-0-0010 (CO158455 Spk K, 4 ppb Splb) 4 1.20 4.14 74 DAL-SB-604R-0-0010 (CO151455 spk L, 100 ppb Spike) 400 1.20 343 85 DAL-SB-604R-0-0050 (CO16UM Spk C. 4 ppb Splke) 4 5.04 9.20 104 DAL-SB604R-0-0050 (CO16UM Spk D. 400ppb Spike) 400 5.04 294 72 DAL-SB604R-M)100 (COlS8457 Spk E. 4 ppb Spike) 4 ND 3.93 98 DAL-SB-604R-O-0100 (COl50457 Spk F. 400 ppb Spike) 400 ND 328 a2 DAL-SB-605R-0-0000 (COlSeUr Spk Q 4 ppb Spike) 4 6.47 11.7 131 DAL-SB-605R-0-0000 ( C O l W Spk H. 400ppbSplko) 400 6.47 361 89 DAL-SB-605R-DB-0000 m1- Spk 1.4 ppb Syk.1 4 6.22 10.6 110 DAL-SB-605R-DB-0000 (COlsorSe Spk J. 400 ppb Spike) 400 6.22 387 95 'Sample residueexceedsthe spiking level signhicantly(3x spiking level);therefore. an accurate recoveryvalue cannot be calculated. ND = Not detected at or above the Limit of Quantbtlon (LOQ) of 0.2 nglg (wet weight). NR = Not Repcnted due to Quality Control failures, see Table V for re-extractdata. Note: Since this summary table shows rounded msulb, recoveryvalues mayvary slightly from the values in the raw data. Exygen Research Page 39 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.:PO000760 Table IV. Matrix Spike Recovery of PFOA in Soil Samples Continued Sample Description DAL-SB605R4-0005 (COlse4co spk K, 4 ppb Spike) DAL-SBsO5R-0-0005 (cor- spk L 400 Ppb Spike) DALSBsOIR-0-0010 (COlW481spk c, 4 ppbSpike) DAL-SBB05R-0-0010 (COlSWOl Spk D, 400 ppb Spike) DAL-SB-005R-0-0050 ( C O l M Spk E, 4 ppb Spike) DALSBsO5R-O-0050 (corm462 spk F, 400 ppb Spike) DAL-SBsO5R-0-0100 (COlSsrrS Spk 0.4 ppb Splko) DAL-SBSO5R-0-0100 (COlSWOS Spk H, 400 ppb Spike) DAL-SB138R-0-0000 (COlSWU Spk I,4 ppb Spike) DAL-SB-138R-0-0000 ( C M W Spk J, 400 ppb Spike) DALSB-138R-0-0005 (COlWcr spk K, 4 ppbSpike) DAL-SB-138R-O-OO05 (COlsS4u Spk L 400 ppb Spike) DAL-SB-138R-0-0010 (CO1-7 Spk C, 4 ppb Spike) DAL-SB-138R-O-0010 (W1-7 Spk D, 400 ppb Spike) DALSEl38R-O-0050 ( C 0 1 W Spk E. 4 Ppb Spike) DAL-SB-138R-0-0050 ( C O l M Jpk F.400ppb Spllrr) DAL-SB-138R-0-0100 (COlSS470 Spk G, 4 ppb Spike) DALSB-138R-0-0100 (COlSH70 Spk H, 400 ppb Splko) DAL-SB-138R-DB-0100 (COlW71 Spk 1.4 ppbSpike) DALSB-138R-DB-0100 (COlW71 Spk J, 4W ppbSyh) DFO5-SS-SSO3-0-0000 ( c a m 7 1 N k 0.4 ppbsyru) DF05SSSS03-0-0000 (COlrOnl Spk H, 400ppb Spike) Amount Spiked (nglg) 4 400 4 400 4 400 4 400 4 400 4 400 4 400 4 400 4 400 4 400 4 400 Amt Found in Sample (nglg) wet weight C8 Acid PFOA Amount RWXvered (nglg) wet weight 0.03 10.5 0.03 320 2.17 6.00 2.17 281 0.808 3.9g 0.808 309 0.027 3.07 0.027 280 23.8 29.0 23.8 388 42.9 48.7 42.9 407 35.0 46.7 35.0 337 NR NR NR NR 278 345 278 540 247 378 247 543 NR NR NR NR Recovery (%) 97 80 90 70 80 92 70 71 80 91 70 NR NR . 07 . 74 NR NR 'Sample residue exceeds the spiking level significantly(3x spikinglevel);therefore,an accurate recoveryvalue cannot be calculated. ND = Not detected at or above the Limitof Quanutation(LOQ) of 0.2 ng/g(wet weight). NR = Not Reported due to Quality Controlfailures. ow Table V forre-exbactdata. Note: Sincethis summarytable shows roundedresults, recoveryvalues may vary slightlyfrom the values In the raw data. Exygen Research Page 40 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table IV. - Matrix Spike Recovery of PFOA in Soil Samples Continued Amount Amt Found C8 Acid PFOA Amount Sample Spiked in Sample Recovered Recovery DF05SS-SS03-0-0003 (corw.72 3pk I, 4 ppb spurr) 4 NR NR NR DF05SS-SS03-0-0003 (COlW72 Spk J. 400ppb Splko) 400 NR NR NR DF05SS-SS04-0-0000 (COlW73 Spk K, 4 ppb Splko) 4 NR NR NR DF05SSSS04-0-0000 (COlW71Spk I.,400ppbSplL.) 400 NR NR NR DFOSSSS04-0-0003 (COlW74 Spk C. 4 ppbSpiko) 4 4.02 7.72 93 DF05SS-SS04-0-0003 (COlW74 Spk D, 400 ppbSpike) 400 4.02 333 82 DF05SSSS05-0-0000 (COlW875 Spk E. 4 ppb Splko) 4 5.01 7.89 67 DF05SSSS05-0-0000 (COlW75 Spk F, 400ppb Spike) 400 5.01 310 76 DF05SS-SSOW-0003 (COlW870Spk 0.4 ppb Spiko) 4 8.26 9.60 84 DF05SS-SS05M)003 (coiwan spr n. 400 ~ psbme) 400 8.26 314 77 DF05SSSS05-DB-0003 (COlW77 Spk I, 4 ppb Spike) 4 6.44 8.56 53 DF05SSSS05-DB-0003 (COlW877 Spk J. 400 ppb Spike) 400 6.44 298 73 DFO9-SS-00o80-0000 (COlW70 tpk K, 4 ppb Splko) 4 13.2 16.0 DFogSS-000604000 (COlW7. spr,.I 400 ppbSplko) 400 13.2 392 95 DFOgSS-0006-0-0003 ( C O l W n Spk C, 4 ppbSplko) 4 14.2 19.8 b n DF09-SS-0008-0-0003 (COlWls Spk D. 400ppbSplke) 400 14.2 332 DF09SS-00064-0010 (co1- Spr 5 4 ppb spliu) 4 7.68 13.0 133 DF09-SS-00064-0010 (COlcoerO Spk F, 400 ppb Splko) 400 7.68 335 82 DFWS-0007-0-0000 (COlWOOl Spk G, 4 ppb Splko) 4 150 138 DFOQ-SS-0007-0-0000 ( C O l I M I l Spk H. 400 ppb Splko) 400 150 357 52 *Sample residueexceeds the spiking level significantty(3x spiking level);therefom. an accurateracoveryvalue cannot be calculated. ND = Not detscted at ofabove the Umit of QuantltaUon (LW)of 0.2 ng/g (wetweight). NR = Not Repotted due to QualityControl failures. see Table V for re+- data. Note:Since thio summarytableshows rounded results, recoveryvalues may vary slightlyfrom the values In the n w data. Exygen Research Page 41 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table IV. Matrix Spike Recovery of PFOA in Soil Samples Continued A Sample DFOgSS-0007-04003 ( C 0 1sp~k I, 4 ppb Spike) DF09-SS-0007-04003 (COlrorU Spk J, 400 ppb Spike) DFOg-SS-0007-04010 ( W l W M 1Spk K,4 ppb Spike) DFOgSS-0007-0-0010 (COlW883 Spk & 400 ppb Spike) DF09-SS-0007-DB-0010 (Wl60884 Spk C, 4 ppb Spike) DFO9-SS-0007-DB-0010 (CO160884 Spk D, 400 ppb Spike) DF09-SS-0008-0-0000 (COlW885 Spk E, 4 ppb Spike) DFOBSS-0008-0-0)000 (COlcoUSSpk F, 400ppb Spike) DF09-SS4008-0-0003 ( C O l W MSpk 0 , 4 ppbSpike) DFO9-SS-0008-0-0003 ( W l W 8 MSpk H, 400 ppb Spike) DFOgSS-00O&0-0010 (COIMM7 Spk 1.4 ppb Spike) DFOgSS-0008-0-0010 (COlrols7 Spk J. 400 ppb Spike) DF09-SS-0009-0-0000 ( C O l m MSpk K,4 ppb Spike) DF09-SS-00080-0000 ( C M W Spk L 400 ppb spike) DFW-SS-0009-0-0003 (W1808U Spk C, 4 ppb Spike) DFOBSS-0009-0-0003 (Cal6OM#Spk D. 400 ppb Spike) DF09-SS-0009-DB-0003 (COlWEW Spk E. 4 ppb Spike) DF09-SS-0009-DB-0003 (COl60890Spk F. 400 ppb Spike) DF09-SS4009-0-0010 (C0160881 Spk G, 4 ppb Spike) DFOgSS-0009-0-0010 (COlWE#lSpk H,400 ppbSiylu) Amount Spiked Amt Found in Sample M g ) wet weight C8 Acid PFOA Amount Recovered (ndg) wet weight 4 ill 109 400 111 319 4 41.8 44.2 400 41.8 206 4 34.8 38.7 400 34.8 425 4 152 150 400 152 518 4 131 120 400 131 371 4 108 99.2 400 108 426 4 8.88 14.2 400 8.88 ~ 435 4 10.8 15.8 400 10.8 486 4 10.9 14.7 400 10.9 394 4 16.7 20.8 400 16.7 422 L%) Recovery * t 52 50 98 . 92 80 80 133 107 125 119 95 96 101 'Sample midue exceeds the spiking level&gniRcantiy (3x spiking level);therefore. an accurate recovery value cannotbe calculated. ND = Not detectedat w a h Me Limitof Quantitatim(LOa) of0.2 ng/g (wet weight). NR = Not Repoiteddue to Quality Conbd failures, sea TableV for re-exbact data. Note: Since thio summary table show roundedmultr, recoveryvalues mayvary rllgMlyfrom the values In the raw data. Exygen Research Page 42 of 151 ~ ~~~ Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table IV. Matrix Spike Recovery of PFOA in Soil Samples Continued Sample Description DFO9SS-0010-0-0000 (COlWo12 spk I. 4 ppb spik.) DFO9SS-0010-0-0000 (COlcoWZ Spk J, 400 ppb Splko) DFO9SS401O-O4003 (COlrOrOS Spk K,4 ppb Splk.) DFO9SS-001MJ-0003 (COl00803 Spk L, 400 ppb SplL.) DF09SS-0010-04010 (C016OSW Spk C, 4 ppb Splko) DF09SS-0010-0-0010 (COlWW4 Spk D, 400 ppb Splk.) DFO9SS-0011-O-OOOO (COl80685 Spk E, 4 ppb Spike) DFO9SS-0011-0-OOOO (COlcoWSSpk F, 400 ppbSplk.) DFO9SS-0011-0-0003 (COlrOm Spk 0 . 4 ppb Splk.) DFOOSS-OO11-0-0003 (coi6omspr n.400 ppb splb) DFOgSS-0011-0-0010 (COl80687 Spk I, 4 PDb S p b ) DFO9SS-0011-0-0010 (COlrOrO7 Spk J. 400 ppb Splb) DF09SS4012-00000 (COl80688 Spk K,4 ppb Splb) DF09SS-OO12-0-0000 (COl808M Spk L, 400 ppb Splb) DF09-SS-0012-DB-0000 (COlcOrsr spk c,4 ppb Splh) DF09-SS-0012-DB-0)000 (COl6OCiW Spk 0.400 ppb SplL.) DFOQSS4012-0-0003 (COlrocoOSpk E, 4 ppbS p b ) DF09SS4012-0M)03 (COlroMo Spk F, 400 ppb Splk.) DFO9SS-OOl2-0-0010 (COl6OWl Spk G,4 ppb spik.) DFO9SS-OO12-0-0010 (COl6OWl Spk H, 400 ppb Splk.) Amount Amt Found Spiked in Sample 0s g ) wet weight 4 638 400 638 Cs Add PFOA Amount Recovered (ndg) wet weight 706 1070 4 386 367 400 386 810 4 353 440 400 353 683 4 222 234 400 222 507 4 247 307 400 247 550 4 NR NR 400 NR NR 4 NR NR 400 NR NR 4 484 433 400 484 764 4 NR NR 400 NR NR 4 418 373 400 418 692 RecoVely %- ( 108 108 83 . 71 70 NR NR NR NR . 70 NR NR 69 'Sample residue exceeds the spiking levelsignlcantly (3x spiking level);therefore,an accurate recoveryvalue cannot be calculated. ND = Not detectedat or above the Umlt of QvanUtation (LOa) of 0.2 nglg (wet weight). NR = NotReporteddue to QuaMy COnW failures,see Table V far re%xtnct data. Note: Slnco this summary tableshows munded mult., recoveryvaluer mayvary sllghtly from the values In the raw data. Exygen Research Page 43 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table IV. Matrix Spike Recovery of PFOA in Soil Samples Continued Sample Amount Spiked P Amt Found in Sample C8 Acid PFOA Amount Recovered . DFOQSS-OO13P0000 ( C O l ~ O ZSpk 1.4 ppbSpike) 4 18.5 23.8 DFOQSS-OOI3-0-0000 (COlrOeoZ spk J. 400 ppb Spike) 400 18.5 342 81 DFOQSS-OO13-0-0003 (COlrOeo3 Spk K. 4 ppb Spiko) 4 22.2 23.7 DFOQSS-OO3I -0-0003 (COlloeW Spk L, 400 ppb Spike) 400 22.2 377 89 DFOQSS-0OI3-O-0010 (COlMW4 Spk C. 4 ppb Spiko) 4 43.3 46.7 DFOQSS-OO3I -0-0010 (COl60904 Spk 0.400 ppb Spike) 400 43.3 289 61 DAL-SB602R-0-0000 (COlUZ47 Spk K. 4 ppb Spike) 4 4.75 7.58 71 DAL-SB602R-0-0000 (C0104247 Spk L, 400 ppb Spike) 400 4.75 305 75 DALSB602R-0-0005 ( C O l u W Spk C. 4 ppb Spike) 4 5.69 8.80 70 DALSB602R-0-0005 (C0164248 spk 0,400 ppb Spiko) 400 5.69 327 80 DAL-SB602R-O-0010 (COluuO Spk E, 4 ppb Spiko) 4 3.39 6.38 75 DALSB602R-0-0010 (COlsluo Spk F,400 ppb Spiko) 400 3.39 415 103 DAL-SB602R-M)050 (COlU250 Spk Q. 4 ppb Spike) 4 0.630 3.41 70 DAL-SB602R-O-OO50 (CO1642SO Spk H,400ppb Spike) 400 0.630 304 76 DALSB602R-0-0100 (COW4261 Spk I. 4 ppb Splko) 4 0.555 3.00 61 DALSB602R-0-0100 (W104251 Spk J, 400 ppb Spike) 400 0.555 277 69 DALSBSOI R-0-0000 (CO104252 Spk K. 4 ppb Spike) 4 I.57 4.51 74 DAL-SB-601R-0-0000 (COlcCW Spk L, 400 ppb Spike) 400 I.57 383 95 DAL-SB-601R-DB-OOOO (COW4253 Spk C. 4 ppb Spike) 4 I.95 5.52 89 DAL-SB-601R-DB-OOOO (COlU253 Spk 0,400 ppb Spike) 400 I.95 494 123 'Sample ntddue exceeds the spiking levelrignilicantly(3x spiking level);therefore,an accuraterecoveryvalue cannot be calculated. ND = Not detectedat or above the Limit of QuantiWon(LOQ) of 0.2 ng/g (wetweight). NR = Not Reporteddue to Qualitycontrolfailures. see TableV for re-rudractdata. Note: Since thlr summary table shorn roundedmulb, recoveryvalues mayvary slightlyfrom the values In the raw data. Exygen Research Page 44 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table IV. Matrix Spike Recovery of PFOA in Soil Samples Continued C8 Acid PFOA Sample Description DALSB-801R-0-0005 (COlMZS4 Spk E, 4 ppb Splkr) 4 1.70 5.15 88 DAL-SB-801R-0-0005 (COlU254 Spk F. 400ppb Splko) 400 1.70 394 98 DAL-SB-601R-04010 (COl84255 Spk 0.4 ppb Splk.) 4 NR NR NR DAL-SB-801R-0-0010 (COl(4W Spk H. 400ppb Splkr) 400 NR NR NR DAL-SB-801R-DB-0010 (C01- Spk I.4 ppb Splke) 4 1.90 7.43 138 DALSB-801RDB-0010 (COlcUSCSpk J, 400ppb Splke) 400 1.90 490 122 DAL-SB-601R-0-0050 (CO104257 Spk IC, 4 ppb Splk.) 4 0.720 3.00 77 DAL-SB-801R-O-0050 (COlU257 spk L, 400 ppb Splkr) 400 0.728 270 87 DAL-SB-801R-0-0100 (C0164Sa Spk C, 4 ppb Splko) 4 0.414 3.78 84 DAL-SB-01 R-0-0100 (CO184259 Spk D, 440 ppb Splko) 400 0.414 308 91 DAL-SB-801RDB-0100 (COl642W Spk E, 4 ppb Splke) DALSB-801RDB-0100 (COl64ZW Spk F. 400 ppb Spike) 4 400 P 0.400 3.22 70 0.408 328 81 -c Average: 80 Standard DevlaUon: 19 `Sample residueexceeds the spikinglevel significantly(ax spiking level);therefore,an accuraterecoveryvalue cannot be calculated. ND = Notdetectedat QT above the Limit oFQuantitation(LOQ) of 0.2 ng/g (wet wight). NR = Not Reporteddue to QualityControlfailures,see Table V forre-extractdata. Note: Slma this summary tablerhows r0Und.dmultr.mcovwyvalues m y vary slightlyfrom the values in the raw data. Exygen Research Page 45 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table V. Matrix Spike Recovery of PFOA in Re-extracted Soil Samples Sample Description DF13-SSSS03-0-0000 (Cor56344 Spk E, 400 ppb Splke) DF13-SSSSOM-OOO3 (COl58345 Spk G, 400 ppb Spike) DF13-SSSS050-0000 (COlWul Spk M. zoo0ppb Splke) DFl3ssSS050-OOO3 (COl56352Spk E, Moo ppb Spike) DFl3-SSSS05DB-0003 (COlSrW Spk G, ZOQO ppb Spike) DF10-SS-SSOl-0-0000 (COl56354Spk I.400 ppb Splke) DF11-SS-SSOl-0-OOO3 (CO150367 Spk N, 400 ppb Spike) DFllSSSSO2-0-0000 (COlsrU, Spk E. 2OOO ppb Spike) DFl1-SS-SSO2-0-0003 (COlW70 Spk 0. EO0 ppbSpike) DF11-SS-SSO3-0-0000 (C0156371Spk I,400 ppb Spike) DF11-SS-SSO3-0-0003 (C0156373 SpL M, 400 ppb Spike) DFO5SS-SSO2-0-0003 (COl50361Spk I,400ppb Spike) DF12-SSSSOl-0-0003 (COlwsUSpk M. 400ppb Spike) DF12-SS-SS02-0-0000 ( C O l W W Spk E. 2000 ppb Spike) DF12-SSSSO2-0-0003 (C0156385Spk 0.4000 ppb Spike) DF12SS-SS030-0000 (COl56380SpL 1.40 ppbspike) DF12-SS-SS0400000 (COl56WSpk M. 8000 ppb Spike) DFl2-SSSSO4-0-0003 (COlW3SO Spk E,20,OOO ppb Spike) DFl3-SS-SSOl-0-0003 (C01563USpk M, 400ppbSplkO) DFl3-SS-SSO2-0-0000 (COlW3M Spk E, 4OOO ppb Spike) Amount Spiked A Amt Found in Sample (ng/g) wet weight 400 344 400 422 2Ooo 880 2Ooo 884 2Ooo 714 400 NR 400 72.7 2Ooo NR 800 579 400 81.8 400 NR 400 282 400 180 2000 1470 4000 2880 40 23.5 8Ooo 3280 2oooo 9280 400 450 4Ooo 2540 C8 Acid PFOA Amount Recovered (ndg) wet weight 585 824 2120 3180 1750 NR 402 NR 1140 357 NR 510 481 2520 5400 45.7 10800 29800 794 4780 Recovery (%) 80 101 82 116 52 NR 82 NR 70 69 NR 57 80 53 63 56 92 103 88 56 NR = ~ or t e mdue to Qualitycontroihilum. Not.: Since &is summaryhbleshows roundedresults, recovery values mayvary slightlyfrom the values In UN raw data. I Exygen Research Page 46 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table V. Matrix Spike Recovery of PFOA in Re-extracted Soil Samples Continued - Sample Description C8 Acid PFOA DFl3-SS-SSO2-04003 (COlseJosSpk 0,4000 ppb Splke) 4000 4760 7920 79 DAL-SB-603R-0-0000 (C0158440 Spk E. 4 ppb Spike) 4 NR NR NR DAL-SB-603RQOO50 (C0159449 Spk Y, 4 ppb Spika) 4 3.07 6.50 06 DAL-SB-604ROO000 (C0150453Spk 1.4 ppb Spike) 4 2.05 4.29 56 DALSB-604R-0-0005 (C0159454 Spk K, 4 ppb Spike) 4 3.00 6.26 80 DAL-SB-130R-O-0050 (C0158468Spk 0,400 ppb Spike) 400 05.6 490 103 DF05-SSSS03-0-0000 (Col60871 Spk I. 400 ppb Spike) 400 103 442 65 DFO5-SSSSO3-0-OOO3 (COlM872 Spk K, 400 ppb Spike) 400 NR NR NR DF05-SS-SS04-0-0000 (COl60873 Spk Y. 4 ppb Spike) 4 NR NR NR DFO9-SS-0011-0-0010 (Cole0807 Spk K, 400 ppb Spike) 400 205 455 63 DF09-SS-00124-0000 (COW0888Spk M, 400ppb Spika) 400 NR NR NR DFOgSS-0012-0-0003 (COlsoeoO Spk 0,400 ppb Spike) 400 NR NR NR DALSB-601ROOOlO ( C O l u 2 u Spk 1.4 ppb Wka) 4 NR NR NR Avenge: 74 StmdJrd Deviation: 18 NR = Not reported due to quality contml failures. Not.: Slnw this rummry table shows munded results, mcovelyvalue8 may v8lysllgMfy from the v8lurs In tha raw d8b. Exygen Research Page 47 of 151 ~~ Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table VI. Matrix Spike Recovery of PFOA in Associated Trip Blanks Sample Description - Amount Spiked (nglL) Amt Found in Sample (nglL) C8 Acid PFOA Amount Recovered (nglL) Recovery (%) DF13-SS-TRIP1-LS-060221 (CO156349,l.O ppb Field Spike) DF1SSS-TRIP1-HS-060221 (C0156350, I00 ppb Field Spike) 1000 ND 100000 ND 989 99 96700 97 DAL-SB-TRIP i-LS-060302 (C015S444,l.O ppb Field Splke) DAL-SB-TRIP1-HS-060302 (C0159445.100 ppb FIeid Splke) 1000 ND 100000 ND 862 86 81500 82 DFO5-SS-TRIP2-LS-060308 (COl60868,l.O ppb Field Spike) 1000 ND 985 99 DFOS-SS-TRIP2-HS-060308 (C0160860, I00 ppb Field Spike) 100000 ND 96900 97 DAL-SB-TRIP-LS-060316 (C0164223,l.O ppb Field Spike) DAL-SB-TRIP-HS-060316 (C0164224, I O ppb Fleld Spike) 1000 ND 10000 ND 907 91 8390 84 Average: 92 Standard Deviation: 7 ND = Not detected at or above the Limit of Quantitation ( L a ) of 25 ng/L. Note: Since thls summary table shows rounded results, recovery values may vary slightly from the values in the raw data. Exygen Research Page 48 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table VII. Surrogate Spike Recovery of 13CPFOA in Soil Samples Exygen ID Sample Description Amount Spiked (ng/)l Amount Recovered Wet Weight Recovery (%I COI 56344 DF13-SS-SSO3-0-oooO 4 NR NR CO156344 Rep DFl3-SS-SSO3-0-0000 4 NR NR CO156344 Spk C DFl3-SS-SSO3-0-0000 4 NR NR CO156344 Spk D DF13-SS-SSO3-0-0000 400 NR NR COI 56345 DF 13-SS-SSO3-0-0003 4 NR NR C0156345 Rep DFl3-SS-SSO3-0-0003 4 NR NR COI56345 Spk E DFl3-SS-SSO3-0-0003 4 NR NR C0156345 Spk F DF13-SS-SSO3-0-0003 400 NR NR C0156346 DF13-SS-SSO4-0-0000 4 4.87 122 C0156346 Rep D F I3-SS-SSO4-0-0000 4 4.78 120 CO156346 Spk G DF13-SS-SSO4-0-0000 4 2.28 57 C0156346 Spk H D F I3-SS-SSO4-0-0000 400 240 60 C0156347 D F I3-SS-SSO4-0-0003 4 4.18 105 C0156347 Rep DF13-SS-SSO4-0-0003 4 4.03 101 C0156347 Spk I DFI3-SS-SSO4-0-0003 4 2.69 67 C0156347 Spk J D F I3-SS-SSO4-0-0003 400 267 67 C0156351 DFI3-SS-SSO50-0000 4 NR NR C0156351 Rep DF13-SS-SS05-0-0000 4 NR NR C0156351 Spk K DFl3-SS-SSO50-0000 4 NR NR C0156351 Spk L DF13-SS-SS050-0000 400 NR NR C0156352 DFl3-SS-SS050-0003 4 NR NR C0156352 Rep DFl3-SS-SSO50-0003 4 NR NR C0156352 Spk C DF13-SS-SSO50-0003 4 NR NR C0156352 Spk D DFl3-SS-SSO5-0-0003 400 NR NR C0156353 DF13-SS-SS05DB-0003 4 NR NR C0156353 Rep D F I3-SS-SS05DB-0003 4 NR NR C0156353 Spk E DFl3-SS-SS05DB-0003 4 NR NR C0156353 Spk F DFl3-SS-SS05-DE0003 400 NR NR C0156354 DF10-SSSSOl-0-0000 4 NR NR C0156354 Rep DFl0-SS-SS01-0-0000 4 NR NR C0156354 Spk G DFl0-SS-SSO1-O-OOOO 4 NR NR COI56354 Spk H DFI0-SS-SSOI-0-0000 400 NR NR COI 56355 DFl0-SS-SSOI-0-0003 4 3.98 100 C0156355 Rep DF10-SS-SSOI-0-0003 4 3.91 98 C0156355 Spk I DFI0-SS-SSOI-0-0003 4 1.90 48 C0156355 Spk J DF10-SS-SSOI-0-0003 400 233 58 C0156356 D F I0-SS-SSO2-0-0000 4 4.49 112 COI56356 Rep DFIO-SS-SS02-0-0000 4 4.32 108 C0156356 Spk K DFl0-SS-SS02-0-0000 4 2.10 53 C0156356 Spk L D F I0-SS-SSO2-0-0000 400 246 62 Note: Since this summary table shows rounded results, recoveryvalues may vary slightlyfrom the values in the raw data. NR = Not Reporteddue to Quality Controlfailures, see Table Vlll for re-extract data. Exygen Research Page 49 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table VII. Surrogate Spike Recovery of I3CPFOA in Soil Samples Continued Exygen ID Sample Description Amount Spiked (rids) Amount Recovered Wet Weight Recovery (W C0156357 DF10-SS-SS02-DB-0000 4 4.90 123 C0156357 Rep DFl0-SSSS02-DB-0000 4 4.95 124 C0156357 Spk C DF10-SSSS02-DE0000 4 2.43 61 C0156357Spk D DFl0-SSSS02-DB-0000 400 250 63 COI 56358 DFi0-SS-SS02-0-0003 4 4.85 121 C0156358 Rep DFl0-SS-SSO2-0-0003 4 4.98 125 C0156358 Spk E DFl0-SS-SSO2-0-0003 4 2.74 69 C0156358 Spk F DFl0-SS-SSO2-0-0003 400 247 62 COI 56360 DFIO-SS-SS03-0-0000 4 5.31 133 C0156360 Rep DFl0-SS-SSO3-0-0000 4 5.25 131 COi 56360 Spk G DFl0-SS-SSO3-O-OOOO 4 2.64 66 COI56360 Spk H DFI0-SS-SSO3-0-0000 400 235 59 co156361 DFl0-SS-SS030-0003 4 5.62 141 C0156361 Rep DFl0-SS-SS03-0-0003 4 5.46 137 C0156361Spk I DFl0-SSSSO3-0-0003 4 2.90 73 COl56361 Spk J DF 10-SS-SSO3-0-0003 400 270 68 C0156362 DFl O-SS-SSO4-0-0000 4 5.41 135 C0156362 Rep DFl0-SS-SSO4-0-0000 4 5.17 129 C0156362 Spk K DF10-SS-SSO4-0-0000 4 3.15 79 C0156362 Spk L DF 10-SS-SSO4-0-0000 400 253 63 C0156363 DFl0-SSSSO4-0-0003 4 3.10 78 C0156363 Rep DFl0-SS-SSO4-0-0003 4 2.78 70 C0156363 Spk C DF10-SS-SSO4-0-0003 4 1.78 45 C0156363 Spk D DFl0-SS-SSO4-0-0003 400 258 65 C0156364 DFl0-SS-SSO50-0000 4 3.53 88 C0156364 Rep DF10-SS-SS050-0000 4 3.28 82 C0156364 Spk E DF10-SS-SS050-0000 4 1.78 45 C0156364 Spk F DFl0-SS-SS050-0000 400 243 61 C0156365 DF10-SS-SS050-0003 4 2.86 72 C0156365 Rep DFI0-SS-SSO50-0003 4 2.78 70 C0156365 Spk G DFl0-SS-SS050-0003 4 1.38 35 C0156365 Spk H DF10-SS-SSO50-0003 400 235 59 C0156366 D F l 1-SSSSOl-0-OOOO 4 2.24 56 C0156366 Rep DFI 1-SS-SSOl-0-0000 4 2.90 73 COi56366 Spk I D F l 1-SS-SSOl-0-OOOO 4 1.61 40 C0156366 Spk J D F l 1-SS-SSOI-0-0000 400 250 63 C0156367 DF11-SS-SSOl-0-0003 4 NR NR C0156367 Rep DFl l-SS-3301-0-0003 4 NR NR C0156367 Spk K DF1i-SSSSOl-O-OW3 4 NR NR C0156367 Spk L D F l 1-SSSSO1-0-0003 400 NR NR Note: Since this summary table shows rounded results, recovery values may vary slightly from the values in the raw data. NR = Not Reporteddue to Quality Controlfailures, see Table VI11 for re-extract data. Exygen Research Page 50 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table VII. Surrogate Spike Recovery of 13CPFOA in Soil Samples Continued I3C-PFOA C0156368 DFl l-SS-SSO2-0-0000 4 NR NR C0156368 Rep DFl l-SS-SSO2-0-0000 4 NR NR C0156368 Spk C DFI 1-SS-SSO2-0-0000 4 NR NR C0156368 Spk D DFl1-SS-SSO2-0-0000 400 NR NR C0156370 DFl l-SS-SSO2-0-0003 4 NR NR C0156370 Rep DFl l-SS-SSO2-0-0003 4 NR NR C0156370 Spk E DFl l-SS-SSO2-0-0003 4 NR NR C0156370 Spk F DF11-SS-SSO2-0-0003 400 NR NR C0156371 DF11-SS-SSO3- 0-0000 4 NR NR C0156371 Rep DFl l-SS-SSO3-0-0000 4 NR NR C0156371 Spk G DFl l-SS-SSO3-0-0000 4 NR NR C0156371 Spk H DFl l-SS-SSO3-0-OOOO 400 NR NR C0156372 DFl l-SS-SS03-DB-0000 4 3.74 94 C0156372 Rep DFI 1-SS-SS03-DB-0000 4 3.10 78 C0156372 Spk I DFl1-SS-SS03-DB-0000 4 1.65 41 C0156372 Spk J DFl l-SS-SS03-DB-0000 400 203 51 C0156373 DFl1-SS-SSO3-0-0003 4 NR NR C0156373 Rep DFl l-SS-SSO3-0-0003 4 NR NR C0156373 Spk K DFl l-SSSSO3-0-0003 4 NR NR C0156373 Spk L DFI 1-SS-SSO3-0-0003 400 NR NR C0156374 DFl l-SS-SSO4-0-0000 4 4.80 120 C0156374 Rep DFl1-SS-SS04-0-0000 4 4.52 113 CO156374 Spk C DFl l-SS-SS04-0-0000 4 2.29 57 CO156374 Spk D D F l l-SS-SSO4-O-OOOO 400 259 65 c0156375 DFl1-SS-SSO4-0-0003 4 4.15 104 C0156375 Rep D F l l-SS-SSO4-O-OOO3 4 4.15 104 C0156375 Spk E DFl1-SS-SSW0-0003 4 1.77 44 C0156375 Spk F DFI 1-SS-SS04-0-0003 400 267 67 C0156376 DF11-SS-SSO50-0000 4 4.66 117 CO156376 Rep DF11-SS-SSO50-0000 4 4.27 107 C0156376 Spk G DFl l-SS-SSO50-0000 4 2.55 64 C0156376 Spk H DFl l-SS-SSO50-0000 400 288 72 C0156377 DFl l-SS-SS050-0003 4 4.38 110 C0156377 Rep DF11-SS-SS050-0003 4 4.12 103 C0156377 Spk I D F l 1-SS-SSO50-0003 4 2.22 56 C0156377 Spk J DFl l-SS-SSO50-0003 400 270 68 C0156378 DF05SS-SSOl-0-0000 4 3.74 94 C0156378 Rep DFO5SS-SSOl-0-0000 4 3.42 86 C0156378 Spk K DF05SS-SSOI-0-0000 4 1.86 47 C0156378 Spk L DF05SS-SS01-0-0000 400 244 61 Note: Since this summary table shows rounded results, recovery values may vary slightly from the values in the raw data. NR = Not Reporteddue to Quality Controlfailures. see Table Vlll for re-extrad data. Exygen Research Page 5 1 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table VII. Surrogate Spike Recovery of 13CPFOA in Soil Samples Continued %-PFOA C0156379 DFO5SSSSOl-0-0003 4 4.70 118 C0156379 Rep DF05-SSSSOl-0-0003 4 4.59 115 C0156379 Spk C DF05SS-SSOl-0-0003 4 3.04 76 C0156379 Spk D DF05SS-SSOl-0-0003 400 278 70 C0156380 DFO5SS-SSO2-0-0000 4 1.37 34 C0156380 Rep DF05SS-SS02-0-0000 4 1.16 29 C0156380 Spk E DF05-SSSS02-0-0000 4 0.625 16 C0156380 Spk F DFO5-SS-SS02-0-0000 400 248 62 CO156381 DF05SS-SS02-0-0003 4 NR NR C0156381 Rep DF05SS-SS02-0-0003 4 NR NR C0156381 Spk G DF05SSSS02-0-0003 4 NR NR C0156381 Spk H DF05SSSS02-0-0003 400 NR NR C0156382 DFl2-SS-SSOl-0-0000 4 3.87 97 C0156382 Rep DFl2-SS-SSOl-0-0OOO 4 2.66 67 C0156382 Spk I DF12-SS-SSOI -0-0000 4 1.90 48 C0156382 Spk J DFl2-SS-SS01-0-0000 400 270 68 C0156383 DFl2-SS-SSOl-0-0003 4 NR NR C0156383 Rep DFl2-SS-SSOl-0-0003 4 NR NR C0156383 SpkK D F l2-SS-SSOl-0-0003 4 NR NR C0156383 SpkL DFl2-SS-SSOI-0-0003 400 NR NR C0156384 DF 12-SS-SSO2-0-0000 4 NR NR C0156384 Rep DF12-SSSS02-0-0000 4 NR NR C0156384 Spk C DFl2-SS-SS02-0-0000 4 NR NR C0156384 Spk D DFl2-SS-SSO2-0-0000 400 NR NR C0156385 DFl2-SS-SSO2-0-0003 4 NR NR C0156385 Rep DF 12-SS-SSO2-0-0003 4 NR NR C0156385 Spk E DF12-SS-SSO2-O-0003 4 NR NR C0156385 Spk F DFl2-SS-SSO2-0-0003 400 NR NR C0156386 DF 12-SS-SSO3-0-0000 4 NR NR C0156386 Rep DFl2-SS-SS03-0-0000 4 NR NR C0156386 SpkG DF l2-SSSSO3-O-OOOO 4 NR NR C0156386 Spk H DFl2-SS-SS03-0-0000 400 NR NR C0156387 DFl2-SS-SS03-0-0003 4 4.54 114 C0156387 Rep DFl2-SS-SSO3-0-0003 4 4.29 107 C0156387 Spk I DF12-SS-SSO3-0-0003 4 2.32 58 C0156387 Spk J DFl2-SS-SSO3-0-0003 400 2.14 1 C0156388 DF12-SS-SSO4-O-OOOO 4 NR NR C0156388 Rep DFl2-SS-SSO4-0-0000 4 NR NR C0156388 Spk K DF 12-SSSSO4-0-OOOO 4 NR NR C0156388 Spk L DF 12-SSSSO4-0-0000 400 NR NR Note: Since this summary table shows rounded results, recovery values may vary slightly from the values in the raw data. NR = Not Reporteddue to Quality Controlfailures, see Table Vlll for re-extractdata. Exygen Research Page 52 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table VII. Surrogate Spike Recovery of 13CPFOA in Soil Samples Continued Exygen ID Sample Description Spiked (WQ) %-PFOA Recovered Wet Weight ReCOveW (%I C0156389 DFl2-SS-SSO4-04003 4 NR NR C0156389 Rep DF 12-SS-SSO4-0-0003 4 NR NR C0156389 Spk C DF 12-SS-SSO4-04003 4 NR NR C0156389 Spk D DF12-SS-SSO4-0-0003 400 NR NR C0156390 DFl2-SS-SSO50-0000 4 2.34 59 C0156390 Rep DFl2-SSSS050-0000 4 2.30 58 C0156390 Spk E DFl2-SSSSO50-0000 4 1.57 39 C0156390 Spk F DFl2-SS-SS050-0000 400 335 84 C0156391 DF12-SS-SSO5-04003 4 1.71 43 C0156391 Rep DFl2-SS-SSO50-0003 4 1.70 43 C0156391 Spk G DFl2-SSSS050-0003 4 0.944 24 C0156391 Spk H DFI2-SS-SSO5-O-OOO3 400 281 70 C0156392 DF13-SS-SSOl-0-0000 4 0.880 22 C0156392 Rep DFl3-SS-SS01-M)OOO 4 1.37 34 C0156392 Spk I DFI3-SS-SSOl-0-0000 4 0.547 14 C0156392 Spk J DF13-SS-SSOl-0-0000 400 216 54 c0156393 DFl3-SS-SSOl-M)oo3 4 NR NR C0156393 Rep DFl3-SS-SSO1-0-0003 4 NR NR C0156393 Spk K DFl3-SS-SSO1-0-0003 4 NR NR C0156393 Spk L DF13-SS-SSO1-0-0003 400 NR NR C0156394 DFl3-SS-SSO2-O-OOOO 4 NR NR COW394 Rep DF 13-SS-SS02-0-OOOO 4 NR NR C0156394 Spk C DFl3-SS-SSO2-0-0000 4 NR NR C0156394 Spk D DF13-SS-SSO2-0-0000 400 NR NR C0156395 DFI3-SS-SSO2-0-0003 4 NR NR C0156395 Rep DFl3-SSSSO2-0-0003 4 NR NR C0156395 Spk E DF13SSSS02-M)003 4 NR NR C0156395 Spk F DFl3-SS-SSO2-O-OOO3 400 NR NR C0159446 DAL-SB-603R-0-0000 4 NR NR C0159446 Rep DAL-SB-603R-0-0000 4 NR NR C0159446 Spk E DAL-SB403R-0-0000 4 NR NR C0159446 Spk F DAL-SB-603R-0-0000 400 NR NR C0159447 DAL-SB-603R-0-0005 4 4.62 116 C0159447 Rep DAL-SB-603R-0-0005 4 4.32 108 C0159447 Spk G DAL-SB-603R-0-0005 4 2.53 63 C0159447 Spk H DAL-SB-603R-0-0005 400 265 66 C0159448 DAL-SB-603R-0-00 10 4 4.47 112 C0159448 Rep DAL-SB-603R-0-00 10 4 4.86 122 C0159448 Spk I DAL-SB-603R-0-00 10 4 2.82 71 COI59448 Spk J DAL-SB-603R-0-0010 400 285 71 Note: Since this summary table shows rounded results, recovery values may vary slightly from the values in the raw data. NR Not Reporteddue to Quality Controlfailures, see Table Vlll for re-extractdata. Exygen Research Page 53 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table VII. Surrogate Spike Recovery of 13CPFOA in Soil Samples Continued Exygen ID > C0159449 C0159449 Rep GO159449 Spk K C0159449 Spk L C0159450 C0159450 Rep C0159450 Spk C C0159450 Spk D C0159451 C0159451 Rep C0159451 Spk E C0159451 Spk F c0159453 C0159453 Rep C0159453 Spk G C0159453 Spk H c0159454 C0159454 Rep C0159454 Spk I C0159454 Spk J C0159455 C0159455 Rep C0159455 Spk K C0159455 Spk L C0159456 C0159456 Rep GO159456 Spk C C0159456 Spk D C0159457 C0159457 Rep C0159457 Spk E C0159457 Spk F C0159458 C0159458 Rep C0159458 Spk G C0159458 Spk H C0159459 GO159459 Rep C0159459 Spk I C0159459 Spk J Sample Description DAL-SB-603R-0-0050 DAL-SB-603R-0-0050 DAL-SB-603R-0-0050 DAL-SB-603R-0-0050 DAL-SB-603R-0-0100 DAL-SB-603R-0-0100 DAL-SB-603R-0-0100 DAL-SB603R-0-0100 DALSWOBR-DB-Ol OO DALSB-603R-DB-0100 DAL-SB-603R-DB-0100 DAL-SB-603R-DB-0100 DAL-SB-604R-0-0000 DAL-SB-604R-0-0000 DAL-SB-604R-0-0000 DAL-SB-604R-0-0000 DAL-SB-604R-0-0005 DAL-SB-604R-0-0005 DAL-SB-604R-0-0005 DAL-SB-604R-0-0005 DAL-SB-604R-0-0010 DAL-SB-604R-0-0010 DAL-SB-604R-0-00 10 DAL-SB-604R-0-0010 DAL-SB-604R-0-0050 DAL-SB-604R-0-0050 DAL-SB-604R-Q.0050 DAL-SB-604R-0-0050 DAL-SB-6MR-0-0100 DAL-SB-604R-0-0100 DAL-SB-604R-0-0100 DAL-SB-604R-0-0100 DAL-SB-605R-0-0000 DAL-SB-605R-O-0000 DAL-SB-605R-0-0000 DAL-SB-605R-0-0000 DAL-SB-605R-DE0000 DAL-SB-605R-DB-0000 DAL-SB-605R-DB-0000 DAL-SB-605R-DB-0000 Spiked (ng/g) 4 4 4 400 4 4 4 400 4 4 4 400 4 4 4 400 4 4 4 400 4 4 4 400 4 4 4 400 4 4 4 400 4 4 4 400 4 4 4 400 'k-PFOA Recovered Wet Weight (nglg) NR NR NR NR 5.24 5.04 2.56 296 4.79 4.85 2.94 287 NR NR NR NR NR NR NR NR 5.26 5.32 3.08 348 5.16 5.29 3.34 305 5.69 5.14 3.63 314 5.18 5.15 3.14 351 4.76 5.22 2.95 362 Recovery (%) NR NR NR NR 131 126 64 74 120 121 74 72 NR NR NR NR NR NR NR NR 132 133 77 87 129 132 84 76 142 129 91 79 130 129 79 88 119 131 74 91 Note: Since this summary table shows roundedresults, recoveryvalues may vary slightly from the values in the raw data. NR = Not Reporteddue to QualityControl failures, see Table Vlll for re-extract data. Exygen Research Page 54 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table VII. Surrogate Spike Recovery of 13CPFOA in Soil Samples Continued Exygen ID Sample Description Spiked (nda) "GPFOA Recovered Wet Weight Recovery (%I C0159460 DAL-SB-605R-0-0005 4 5.60 140 C0159460 Rep DAL-SB-605R-0-0005 4 5.37 134 C0159460SpkK DAL-SB-605R-0-0005 4 2.59 65 C0159460 Spk L DAL-SB-605R-0-0005 400 323 81 C0159461 DAL-SB-605R-0-0010 4 5.94 149 C0159461 Rep DAL-SB-605R-0-0010 4 5.89 147 C0159461 Spk C DAL-SB-605R-0-0010 4 2.71 68 C0159461 Spk D DAL-SB-605R-0-0010 400 278 70 C0159462 DAL-SB-605R-0-0050 4 5.54 139 CO159462 Rep DAL-SB-605R-0-0050 4 5.53 138 C0159462 Spk E DAL-SB-605R-0-0050 4 2.98 75 C0159462 Spk F DAL-SB-605R-0-0050 400 357 89 C0159463 DAL-SB-605R-0-0100 4 5.46 137 C0159463 Rep DAL-SB-605R-0-0100 4 5.06 127 C0159463 Spk G DAL-SB-605R-O-0100 4 2.98 75 C0159463 Spk H DAL-SB-605R-O-0100 400 276 69 C0159464 DAL-SEI 38R-O-0000 4 5.45 136 C0159464 Rep DAL-SB-138R-0-0000 4 5.52 138 C0159464 Spk I DAL-SB-138R-0-0000 4 2.93 73 C0159464 Spk J DAL-SB-138R-04000 400 329 82 C0159466 DAL-SB-138R-0-0005 4 4.82 121 C0159466 Rep DALSB-138R-WOO5 4 4.85 121 C0159466 Spk K DAL-SB-138R-0-0005 4 2.67 67 C0159466 Spk L DAL-SB-138R-0-0005 400 359 90 C0159467 DAL-SB-138R-0-0010 4 5.58 140 C0159467 Rep DAL-SB-138R-0-0010 4 5.35 134 C0159467 Spk C DAL-SB-138R-0-0010 4 3.03 76 C0159467 Spk D DAL-SB-138R-0-0010 400 291 73 C0159468 DAL-SB-138R-0-0050 4 NR NR C0159468 Rep DAL-SB-138R-0-0050 4 NR NR C0159468 Spk E DAL-SB-138R-0-0050 4 NR NR C0159468 Spk F DAL-SB-138R-0-0050 400 NR NR C0159470 DAL-SB-138R-0-0100 4 4.54 114 C0159470 Rep DAL-SE138R-O-0100 4 5.06 127 C0159470 Spk G DAL-SE138R-0-0100 4 2.78 70 C0159470 Spk H DAL-SEI38R-O-0100 400 274 69 C0159471 DAL-SB-138R-DE0100 4 4.40 110 C0159471 Rep DAL-SB-138R-DE0100 4 4.19 105 C0159471 Spk I DAL-SB-138R-DE0100 4 2.41 60 C0159471 Spk J DAL-SB-138R-DE0100 400 328 82 CO160871 DFO5-SSSSO3-0-0000 4 NR NR C0160871 Rep DF05SSSS03-0-0000 4 NR NR C0160871 Spk G DFO5-SSSSO3-O-0000 4 NR NR C0160871 Spk H DF05-SSSS03-0-0000 400 NR NR Note: Since this summary table shows rounded results. recovery values may vary slightly from the values In the raw data. NR = Not Reporteddue to Quality Control failures,see TaMe Vlll for re-extractdata. Exygen Research Page 55 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table VII. Surrogate Spike Recovery of 13CPFOA in Soil Samples Continued Exygen ID Sample Description Spiked ~ng/l) I3C-PFOA Recovered Wet Weight Recovery (%I C0160872 DFO5SS-SSO3-0-0003 4 NR NR C0160872 Rep DF05SS-SS03-0-0003 4 NR NR C0160872 Spk I DF05SSSS03-0-0003 4 NR NR C0160872 Spk J DF05SS-SS03-0-0003 400 NR NR C0160873 DF05SS-SSWO-0000 4 NR NR C0160873 Rep DF05SS-SSW0-0000 4 NR NR C0160873 Spk K DFO5SS-SSW0-0000 4 NR NR C0160873 Spk L DF05SSSS04-0-0000 400 NR NR C0160874 DF05SS-SS04-0-0003 4 5.19 130 C0160874 Rep DFO5SSSSO4-0-0003 4 5.19 130 C0160874 Spk C DF05SS-SSW0-0003 4 3.00 75 C0160874 Spk D DF05SS-SS04-0-0003 400 306 77 C0160875 DF05-SS-SS050-0000 4 5.61 140 C0160875 Rep DF05SS-SS050-0000 4 5.34 134 C0160875 Spk E DF05SS-SS050-0000 4 2.85 71 C0160875 Spk F DF05SS-SS050-0000 400 294 74 C0160876 DF05SSSS050-0003 4 5.39 135 C0160876 Rep DFO5SS-SS050-0003 4 5.14 129 C0160876 Spk G DFO5SS-SSO50-0003 4 3.94 99 C0160876 Spk H DF05SS-SS050-0003 400 314 79 C0160877 DF05SS-SS05DB-0003 4 5.38 135 C0160877 Rep DF05SSSSOSDB-0003 4 4.94 124 C0160877 Spk I DF05-SS-SS05-DE0003 4 3.09 77 C0160877 Spk J DF05-SS-SS05DB-0003 400 291 73 C0160878 DF09-SS-0006-0-0000 4 5.23 131 C0160878 Rep DFO9-SS-0006-0-0000 4 5.21 130 C0160878 Spk K DF09-SS-000&0-0000 4 4.02 101 C0160878 Spk L DF09-SS-0006-0-0000 400 390 98 C0160879 DF09-SS-0006-0-0003 4 6.04 151 C0160879 Rep DF09-SS-0006-0-0003 4 5.62 141 CO160879 Spk I DF09SS-0006-0-0003 4 3.83 96 C0160879 Spk J DF09-SS-0006-0-0003 400 348 87 C0160880 DFOSSS-0006-0-00 10 4 5.81 145 C0160880 Rep DF09-SS-0006-0-00 10 4 5.58 140 C0160880 Spk K DF09-SS-0006-0-0010 4 3.00 75 C0160880 Spk L DF09-SS-0006-0-0010 400 348 87 C0160881 DFO9-SS-OOO7-0-OOOO 4 2.86 72 C0160881 Rep DF09SS-0007-0-0000 4 2.55 64 C0160881 Spk C DFO9-SS-0007-0-0000 4 1.74 44 C0160881 Spk D DF09-SS-0007-0-0000 400 261 65 Note: Since this summary table shows rounded results, recovery values may vary slightly from the values in the raw data. NR = Not Reporteddue to Quality Controlfailures,see Table Vlll for re-extract data. Exygen Research Page 56 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table VII. Surrogate Spike Recovery of 13CPFOA in Soil Samples Continued Sample Description Spiked I3C-PFOA Recovered Wet Weight Recovery (%I C0160882 DF09-SS-0007-0-0003 4 3.07 77 C0160882 Rep DFO9-SS-0007-0-0003 4 3.00 75 C0160882 Spk E DF09-SS-0007-0-0003 4 1.70 43 C0160882 Spk F DF09-SS-0007-0-0003 400 240 60 C0160883 DF09-SS-0007-0.0010 4 4.26 107 C0160883 Rep DF09-SS-0007-0-0010 4 4.05 101 C0160883 Spk G DF09-SS-0007-0-0010 4 2.24 56 C0160883 Spk H DF09-SS-0007-0-0010 400 251 63 C0160884 DFOSSS-0007-DB-0010 4 4.88 122 C0160884 Rep DF09-SS-0007-DB-0010 4 4.93 123 C0160884 Spk I DF09-SS-0007-DB-0010 4 3.50 88 C0160884 Spk J DF09-SS-0007-DE0010 400 395 99 C0160885 DF09-SS-0008-0-0000 4 2.68 67 C0160885 Rep DF09-SS-0008-0-0000 4 2.61 65 C0160885 Spk K DF09-SS-000&0-0000 4 2.03 51 C0160885 Spk L DF09-SS-0008-0-0000 400 369 92 C0160886 DF09-SS-0008-0-0003 4 2.10 53 C0160886 Rep DF09-SS-0008-0-0003 4 2.35 59 C0160886 Spk C DF09-SS-0008-0-0003 4 1.39 35 CO160886 Spk D DFOBSS-0008-0-0003 400 278 70 C0160887 DF09-SS-0008-0-0010 4 2.79 70 C0160887 Rep DFO9-SS-0008-0-0010 4 3.04 76 C0160887 Spk E DFO9-SS-0008-0-0010 4 1.84 46 C0160887 Spk F DFO9-SS-0008-0-00 10 400 330 83 C0160888 DF09-SS-0009-0-0000 4 5.10 128 C0160888 Rep DF09-SS-0009-0-0000 4 5.22 131 C0160888 Spk G DFO9-SS-OOO9-O-OOOO 4 3.70 93 C0160888 Spk H DFO9-SS-0009-0-0000 400 429 107 C0160889 DFO9-SSOOO9-0-OOO3 4 5.1 1 128 C0160889 Rep DFO9-SSOOO9-0-0003 4 5.1 1 128 C0160889 Spk C DFO9-SS-0009-0-0003 4 3.46 87 C0160889 Spk D DF09-SS-0009-0-0003 400 480 120 C0160890 DF09-SS-0009-DB-0003 4 4.94 124 C0160890 Rep DF09-SS-0009-DB-0003 4 5.00 125 C0160890 Spk E DF09-SS-0009-DB-0003 4 3.42 86 C0160890 Spk F DFO9-SS0009-DB-0003 400 391 98 CO160891 DF09-SS-0009-0-0010 4 5.10 128 C0160891 Rep DF09-SS-0009-0-0010 4 4.82 121 C0160891 Spk G DF09-SS-0009-0-0010 4 2.92 73 C0160891 Spk H DF09-SS-0009-0-00 10 400 413 103 Note: Since this summary table shows roundedresults, recoveryvalues may vary slightly from the values in the raw data. NR = Not Reporteddue to Quality Control failures, see Table Vlll for re-extract data. Exygen Research Page 57 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table VII. Surrogate Spike Recovery of 13CPFOA in Soil Samples Continued Sample Description Spiked (ng/g) I3C-PFOA Recovered Wet Weight Recovery (%I C0160892 DFO9-SS-0010-0-0000 4 3.26 82 C0160892 Rep DF09-SS-0010-0-0000 4 3.26 82 C0160892 Spk I DF09-SS-0010-0-0000 4 2.14 54 C0160892 Spk J DF09-SS-0010-0-OOOO 400 370 93 C0160893 DF09-SS-0010-0-0003 4 4.02 101 C0160893 Rep DF09-SS-0010-0-0003 4 3.34 84 C0160893 Spk K DF09-SS-0010-0-0003 4 2.40 60 C0160893 Spk L DFO9-SS-0010-0-0003 400 330 83 C0160894 DFO9-SS-0010-0-0010 4 3.10 78 C0160894 Rep DFO9-SS-0010-0-0010 4 4.30 108 C0160894 Spk I DF09-SS-0010-0-0010 4 2.44 61 C0160894 Spk J DF09-SS-0010-0-0010 400 349 87 C0160895 DF09-SS-0011-0-0000 4 3.73 93 C0160895 Rep DF09-SS-0011-0-0000 4 3.35 84 C0160895 Spk K DF09-SS-0011-0-0000 4 2.13 53 C0160895 Spk L DF09-SS-0011-0-0000 400 298 75 C0160896 DF09-SS-0011-0-0003 4 3.45 86 C0160896 Rep DF09-SS-0011-0-0003 4 3.29 82 C0160896 Spk C DF09-SS-0011-0-0003 4 1.64 41 C0160896 Spk D DF09-SS-0011-0-0003 400 275 69 C0160897 DF09-SS-0011-0-0010 4 NR NR C0160897 Rep DF09-SS-0011-0-0010 4 NR NR C0160897 Spk E DF09-SS-0011-0-0010 4 NR NR C0160897 Spk F DF09-SS-0011-0-0010 400 NR NR C0160898 DFO9-SS-0012-0-0000 4 NR NR C0160898 Rep DFO9-SS-0012-0-0000 4 NR NR C0160898 Spk G DF09-SS-0012-0-0000 4 NR NR C0160898 Spk H DF09-SS-0012-0-0000 400 NR NR C0160899 DFOSSS-0012-DB-0000 4 3.95 99 C0160899 Rep DF09-SS-0012-DB-0000 4 4.10 103 C0160899 Spk C DFOSSS-0012-DB-0000 4 2.49 62 C0160899 Spk D DFOQSS-00 12-DB-0000 400 365 91 C0160900 DF09-SS-0012-0-OOO3 4 NR NR C0160900 Rep DF09-SS-0012-0-OOO3 4 NR NR C0160900 Spk E DF09-SS-0012-0-OoO3 4 NR NR C0160900 Spk F DF09-SS-0012-0-0003 400 NR NR C0160901 DFO9-SS-0012-0-00 10 4 4.02 101 C0160901 Rep DF09-SS-0012-0-0010 4 4.22 106 C0160901 Spk G DFO9-SS-0012-0-0010 4 2.15 54 C0160901 Spk H DFO9-SS-0012-0-0010 400 326 82 Note: Since this summary table shows rounded results, recovery values may vary slightly from the values in the raw data NR = Not Reported due to Quality Control failures, see Table Vlll for re-extract data. Exygen Research Page 58 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table VII. Surrogate Spike Recovery of 13CPFOA in Soil Samples Continued Exygen ID C0160902 C0160902 Rep C0160902 Spk I C0160902 Spk J C0160903 C0160903 Rep C0160903 Spk K C0160903 Spk L C0160904 C0160904 Rep C0160904 Spk C C0160904 Spk D C0164247 C0164247 Rep C0164247 Spk K C0164247 Spk L C0164248 CO164248 Rep C0164248 Spk C C0164248 Spk D C0164249 C0164249 Rep C0164249 Spk E C0164249 Spk F C0164250 C0164250 Rep GO164250 Spk 0 C0164250 Spk H C0164251 C0164251 Rep C0164251 Spk I C0164251 Spk J C0164252 C0164252 Rep C0164252 Spk K C0164252 Spk L C0164253 C0164253 Rep C0164253 Spk C C0164253 Spk D Sample Description DF04SS-0013-0-0000 DF09-SS-0013-0-0000 DF04SS-0013-0-0000 DFO4SS-0013-0-0000 DF09-SS-0013-0-0003 DF04SS-0013-0-0003 DF04SS-0013-0-0003 DF09-SS-0013-0-0003 DFOSSS-0013-0-0010 DFO4SS-0013-0-0010 DFOSSS-0013-0-0010 DFO4SS-0013-0-0010 DAL-SB-602R-0-0000 DAL-SB-602R-0-0000 DAL-SB-602R-0-0000 DAL-SB-602R-0-0000 DAL-SB-602R-O-0005 DAL-SB-602R-0-0005 DAL-SB-602R-O-0005 DAL-SB-602R-0-0005 DAL-SB-602R-0-0010 DAL-SB-602R-0-0010 DAL-SB-602R-0-0010 DAL-SB-602R-0-0010 DAL-SB-602R-0-0050 DAL-SB-602R-0-0050 DAL-SB-602R-0-0050 DAL-SB-602R-0-0050 DAL-SB-602R-O-0100 DAL-SB-602R-0-0100 DAL-SB-602R-O-0100 DAL-SB-602R-0-0100 DAL-SB-601R-0-0000 DAL-SB-601R-0-0000 DAL-SB-601R-0-0000 DAL-SB-601R-0-0000 DAL-SB-601R-DB-0000 DAL-SB-601R-DB-0000 DAL-SB-601R-DB-0000 DAL-SB-601R-DB-0000 Spiked (ns/e) 4 4 4 400 4 4 4 400 4 4 4 400 4 4 4 400 4 4 4 400 4 4 4 400 4 4 4 400 4 4 4 400 4 4 4 400 4 4 4 400 %-PFOA Recovered Wet Weight (nglg) 4.50 4.82 2.89 326 5.14 5.32 2.37 357 4.43 4.38 2.22 245 5.40 5.17 2.90 299 5.34 5.22 2.86 309 5.89 5.78 4.30 408 5.40 4.87 2.69 295 3.97 4.68 2.58 276 5.36 5.26 2.72 390 7.01 5.75 4.02 473 Recovery (%I 113 121 72 82 I29 133 59 89 111 110 56 61 135 129 73 75 134 131 72 77 147 145 108 102 135 122 67 74 99 117 65 69 134 132 68 98 175 144 101 118 Note: Since this summary table shows rounded results, recovery values may vary slightly from the values in the raw data. NR = Not Reported due to QualityControl failures, see Table Vlll for rwxtract data. Exygen Research Page 59 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table VII. Surrogate Spike Recovery of 13CPFOA in Soil Samples Continued Exygen ID Sample Description Amount Spiked (Wg) l3C-PF0A Amount Recovered Wet Weight Recovery (%) c0164254 DAL-SB-601R-0-0005 4 5.88 147 C0164254 Rep DAL-SB-601R-0-0005 4 5.60 140 C0164254 Spk E DAL-SB-601R-0-0005 4 3.16 79 C0164254 Spk F DAL-SB-601R-0-0005 400 397 99 C0164255 DAL-SB-601R-0-0010 4 NR NR C0164255 Rep DAL-SB-601R-0-0010 4 NR NR C0164255 Spk G DAL-SB-601R-0-0010 4 NR NR COW4255 Spk H DAL-SB-601R-0-0010 400 NR NR C0164256 DAL-SB-601R-DB-0010 4 5.89 147 C0164256 Rep DALSB-601R-DB-0010 4 5.54 139 C0164256 Spk I DAL-SB-601R-DB-0010 4 3.70 93 C0164256 Spk J DAL-SB-601R-DB-0010 400 499 125 C0164257 DAL-SB-601R-0-0050 4 5.10 128 C0164257 Rep DAL-SB-601R-0-0050 4 4.93 123 C0164257 Spk K DAL-SB-601R-0-0050 4 2.79 70 C0164257 Spk L DAL-SB-601RQ0050 400 269 67 C0164259 DAL-SB-601R-0-0100 4 5.96 149 COI64259 Rep DAL-SBdOl R-0-0100 4 5.91 148 C0164259 Spk C DAL-SBdOl R-0-0100 4 3.29 82 C0164259 Spk D DAL-SB-601R-0-0100 400 352 88 C0164260 DAL-SB-601R-DB-0100 4 5.78 145 C0164260 Rep DAL-SB-601R-DB-0100 4 5.41 135 C0164260Spk E DAL-SB-601R-DB-0100 4 2.81 70 C0164260 Spk F DAL-SB-601R-DB-0100 400 322 81 Average: 91 Standard Devlatlon: 32 Note: Since this summary table shows rounded results, recovery values may vary slightly from the values in the raw data. NR = Not Reported due to Quality Control failures, see Table Vlll for re-extract data. Exygen Research Page 60 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table VIII. Surrogate Spike Recovery of 13CPFOA in Re-extracted Soil Samples - Amount %-PFOA Amount men Sample Spiked Recovered Recovery ID Description Wet Weight (%) co156344 DFl3-SS-SS03-0-0000 4 0.639 16 COl56344 Spk E DF13-SS-SS03-0-0000 400 113 28 c0156345 DF13-SS-SS03-0-0003 4 0.268 7 C0156345 Spk G DFl3-SS-SSO3-0-0003 400 87.2 22 C0156351 DFl3-SS-SS05-0-0000 4 0.468 12 C0156351 Spk M DF13-SS-SS05-0-0000 2000 832 42 C0156352 DFl3-SS-SS05-0-0003 4 0.550 14 C0156352 Spk E DF13-SS-SS05-0-0003 2000 2170 109 C0156353 DFl3-SS-SS05-DB-0003 4 0.438 11 C0156353 Spk G DFl3-SS-SS05-DB-0003 2000 792 40 C0156354 DFl0-SS-SS01-0-0000 4 NR NR C0156354 Spk I DF 10-SS-SSO1-0-0000 400 NR NR C0156367 DF11-SS-SSO1-0-0003 4 0.928 23 C0156367 Spk N DFll-SS-SSO1-0-0003 400 153 38 C0156368 DFl l-SS-SSO2-0-0000 4 NR NR coi56368 spk E DF11-SS-SSO2-0-0000 2000 NR NR C0156370 DFl l-SS-SSO2-0-0003 4 0.594 15 C0156370 Spk G DFl l-SS-SSO2-0-0003 aoo 425 53 C0156371 DFl l-SS-SSO3-0-0000 4 1.50 38 C0156371 Spk I DF11-SS-SSO3-0-0000 400 215 54 C0156373 DFlI-SS-SSO3-0-0003 4 NR NR C0156373 Spk M DF11-SS-SSO3-0-0003 400 NR NR ~0156381 DF05-SS-SS02-0-0003 4 1.80 45 ~0156381spk I DF05-SSSS02-0-0003 400 654 164 coi56383 DFl2-SS-SSOl -0-0003 4 1.34 34 ~0156383spk M DF12-SS-SSOl-0-0003 400 214 54 C0156384 DF12-SS-SS02-0-0000 4 1.04 26 C0156384SpkE DF12-SS-SS02-0-0000 2000 1010 51 ~0156385 DFl2-SS-SSO2-0-0003 4 0.928 23 C0156385 Spk G DFl2-SS-SS02-0-0003 4000 1810 45 C0156386 DFl2-SS-SS03-0-0000 4 4.05 101 C0156386 Spk I DF12-SS-SS03-0-0000 40 21.4 54 C0156388 DF12-SS-SSW0-0000 4 1.13 28 coi56388 spk M DF12-SS-SSWO-0000 8000 6380 ao coi 56389 DF12-SS-SSO4-0-0003 4 1.12 28 coi56389 spk E DF12-SS-SSO4-0-0003 20000 23000 115 C0156393 DF 13-SS-SSOl-0-0003 4 1.34 34 C0156393 Spk M DFl3-SS-SSO1-0-0003 400 263 66 NR = Not reported due to quality control failures Note: Since this summary table shows rounded results, recovery values may vary slightly from the values in the raw data. Exygen Research Page 61 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table VIII. Surrogate Spike Recovery of 13CPFOA in Re-extracted Soil Samples Continued Exygen ID Sample Description Amount Spiked (nab) %-PFOA Amount Recovered Wet Weight Recovery (%) c0156394 DFl3-SS-SSO2-0-0000 4 1.08 27 C0156394 Spk E DFl3-SS-SSO2-0-0000 4000 2160 54 C0156395 DFl3-SS-SSO2-0-0003 4 0.888 22 C0156395 Spk G DF 13-SS-SSO2-0-0003 4000 2680 67 C0159446 DAL-SB-603R-0-0000 4 NR NR C0159446 Spk E DAL-SB-603R-0-0000 4 NR NR C0159449 D AL-SB-603R-0-0050 4 3.42 86 C0159449 Spk M DAL-SB-603R-0-0050 4 1.79 45 c0159453 DAL-SB-604R-0-0000 4 3.06 77 C0159453 Spk I DAL-SB-604R-0-0000 4 1.54 39 C0159454 DAL-SB-604R-0-0005 4 3.18 80 C0159454 Spk K DAL-SB-604R-0-0005 4 2.46 62 C0159468 DAL-SB-138R-0-0050 4 2.40 60 C0159468 Spk G DAL-SB-138R-0-0050 400 218 55 C0160871 DF05SS-SS03-0-0000 4 1.33 33 C0160871 Spk I DF05SS-SS03-0-0000 400 162 41 C0160872 DF05SS-SS03-0-0003 4 NR NR C0160872 Spk K DF05SS-SS03-0-0003 400 NR NR C0160873 DF05SS-SS04-0-0000 4 NR NR C0160873 Spk M DF05SS-SS04-0-0000 4 NR NR C0160897 DFO4SS-0011-0-0010 4 2.10 53 C0160897 Spk K DFOSSS-0011-0-0010 400 154 39 C0160898 DF09-SS-0012-0-0000 4 NR NR C0160898 Spk M DF04SS-0012-0-0000 400 NR NR C0160900 DF04SS-0012-0-0003 4 NR NR C0160900 Spk G DFO4SS-0012-0-0003 400 NR NR C0164255 DAL-SB-601R-0-0010 4 NR NR C0164255 Spk I DAL-SB-60lR-0-0010 4 NR NR Average: 48 Standard Devlatlon: 30 NR = Not reported due to quality control failures Note: Since this summary table shows rounded results, recovery values may vary slightly from the values in the raw data. Exygen Research Page 62 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table IX. Surrogate Spike Recovery of I3CPFOA in Associated Rinse Blanks and Trip Blanks , %PFOA Amount Amount Sample Spiked Recovered Recovery C0156348 C0156349 C0156350 COI 56359 C0156369 COI 59443 COI 59444 C0159445 COI 59452 C0159465 C0159469 COI 60867 COI 60868 C0160869 C0160870 COI 64222 C0164223 COI 64224 COI 64258 DFI3-SS-TRiPl-0-060221 DFI3-SS-TRIP1-LS060221 DFI3-SS-TRIPI-HS-060221 DFl0-SS-SS03-RB-0000 DFII-SS-SS02-RB-0003 DAL-SB-TRIPI -0-060302 DAL-SB-TRIPI-LS-060302 DAL-SB-TRIPI-HS-060302 DAL-SBBOSR-RB-OI OO DAL-SB-138R-RB-0000 DAL-SB-138R-RB-0100 DF05-SS-TRIP2-0-06038 DF05SS-TRIP2-LS-060308 DF05-SS-TRIP2-HS-060308 DF05-SS-SS03-RB-0000 DAL-SB-TRIP-0-060316 DAL-SB-TRIP-LS-060316 DAL-SB-TRIP-HS-060316 DAL-SB-601R-RB-0100 500 541 108 1000 875 88 100000 87200 87 500 566 113 500 530 106 500 595 119 1000 I010 101 100000 99800 100 500 619 124 500 573 115 500 601 120 500 602 120 1000 883 88 100000 86500 87 500 555 111 500 666 133 lo00 998 100 I0000 9150 92 500 594 119 Avenge: 107 Standard Deviation: 14 Note: Since this summary table shows rounded results, recovery values may vary slightly from the values In the raw data. Exygen Research Page 63 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table X. Exygen ID C0156344 C0156345 C0156346 c0156347 C0156351 C0156352 C0156353 C0156354 C0156355 C0156356 C0156357 C0156358 C0156360 C0156361 C0156362 C0156363 C0156364 C0156365 C0156366 C0156367 C0156368 C0156370 C0156371 C0156372 c0156373 c0156374 C0156375 C0156376 C0156377 - Total Percent Solids in Soil Samples Sample Description Total Solids (K) DFl3-SSSSO3-0-oooO 65.54 DF13-SSSSO3-0-0003 76.73 DF13-SSSSO4-0-0000 DFl3-SSSSO4-0-0003 DFl3-SSSSO5-0-0000 DFl3-SSSSO5-0-0003 DF13-SS-SSO5-DB-0003 DFl0-SSSSOl -0-0000 83.41 87.27 78.17 84.70 83.33 84.27 DFl0-SSSSOl -0-0003 86.73 DFl0-SSSSO2-0-0000 86.29 DFl0-SS-SS02-DB-0000 DFl0-SSSSO2-0-0003 DF10-SSSSO3-0-0000 DF10-SS-SSO3-0-0003 DFl0-SS-SSO4-0-0000 86.48 86.56 81.74 84.16 71.57 DFl0-SSSSO4-0-0003 DF10-SSSSO50-0000 DFl0-SSSS050-0003 DFl1-SSSSOl-0-0000 DFl l-SSSSO1-0-0003 DFl1-SSSS02-0-0000 DFl1-SSSS02-0-0003 DFl1-SSSSO3-0-0000 DFl l-SS-SS03-DB-0000 DFl l-SSSSO3-0-0003 DFll-SSSSO4-0-oooO DFl l-SSSSO4-0-0003 75.62 82.18 82.54 81.11 83.77 67.83 70.80 79.72 79.82 85.23 86.67 89.38 DFl l-SSSSO5-0-0000 DFl1-SSSSO50-0003 83.65 85.17 Exygen Research Page 64 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table X. Exygen ID Total Percent Solids in Soil Samples Continued Sample Description Total Solids (%) C0156378 DFO5-SS-SSO1-0-0000 81.57 C0156379 DF05-SS-SSO1-0-0003 84.09 COI 56380 COl56381 C0156382 C0156383 C0156384 DF05SS-SS02-0-0000 DF05-SS-SS02-0-0003 DF12-SS-SSOl-0-0000 DFl2-SS-SSOl -0-0003 DFl2-SS-SSO2-0-0000 82.35 84.38 82.65 81.26 68.74 C0156385 COI 56386 C0156387 C0156388 C0156389 C0156390 C0156391 DF12-SS-SS02-0-0003 DFl2-SS-SSO3-0-0000 DFl2-SS-SS03-0-0003 DF12-SS-SSO4-0-0000 DF12-SS-SSO4-0-0003 DFl2-SS-SSO5-0-0000 DFl2-SS-SSO5-0-0003 73.68 82.19 87.57 74.29 78.13 78.20 81.22 CO156392 DF13-SS-SSOl-0-0000 77.44 COI 56393 C0156394 DFl3-SS-SSO1-0-0003 DFl3-SS-SSO2-0-0000 80.09 75.65 C0156395 C0159446 c0159447 DF13-SS-SSO2-0-0003 DAL-SB-603R-0-0000 DAL-SB-603R-0-0005 80.31 90.63 85.84 C0159448 c0159449 C0159450 C0159451 co159453 COI 59454 DAL-SB-603R-0-0010 DAL-SB-603R-0-0050 DAL-SB-603R-0-0100 DAL-SB-603R-DB-0100 DAL-SB-604R-0-0000 DAL-SB-604R-0-0005 81.62 82.85 83.40 78.33 89.54 82.I 3 C0159455 c0159456 DAL-SB-604R-0-0010 DAL-SB-604R-0-0050 81.93 88.21 Exygen Research Page 65 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table X. Exyaen ID Total Percent Solids in Soil Samples Continued Sample Description Total Solids (%) c0159457 DAL-SB-604R-0-0100 77.17 C0159458 DAL-SB-605R-0-0000 81.42 C0159459 C0159460 C0159461 DAL-SB-605R-DB-0000 DAL-SB-605R-0-0005 DAL-SB-605R-0-0010 81.76 84.78 82.01 C0159462 DAL-SB-605R-0-0050 79.83 C0159463 DAL-SB-605R-0-0100 73.86 C0159464 DAL-SB-138R-0-0000 86.23 C0159466 DAL-SB-138R-0-0005 87.94 CO159467 C0159468 C0159470 C0159471 DAL-SB-138R-0-0010 DAL-SB-138R-0-0050 DAL-SB-138R-0-0100 DAL-SB-138R-DB-0100 86.15 81.93 78.61 80.36 CO160871 DF05SS-SS03-0-0000 80.74 C0160872 DF05SS-SS03-0-0003 83.20 C0160873 DFO5-SS-SSO4-0-0000 84.22 C0160874 DF05-SS-SS04-0-0003 87.24 C0160875 C0160876 C0160877 DF05SS-SS05-0-0000 DFO5SS-SSO5-0-0003 DF05SS-SS05-DB-0003 86.54 86.68 86.89 C0160878 DF09-SS-0006-0-0000 89.09 C0160879 DF09-SS-0006-0-0003 87.28 C0160880 DF09-SS-0006-0-0010 86.20 CO160881 DF09-SS-0007-0-0000 86.39 C0160882 DF09-SS-0007-0-0003 89.57 CO160883 DF09-SS-0007-0-0010 89.36 C0160884 DF09-SS-0007-DB-0010 89.39 C0160885 DF09-SS-0008-0-0000 86.47 Exygen Research Page 66 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table X. Total Percent Solids in Soil Samples Continued Exygen Sample ID Description Total Solids (%) C0160886 C0160887 C0160888 COI 60889 C0160890 COI 60891 DF09-SS-0008-0-0003 DF09-SS-008-0-0010 DFO9-SS-0009-0-0000 DF09-SS-0009-0-0003 DF09-SS-0009-DB-0003 DF09-SS-0009-0-0010 88.27 88.54 87.96 88.35 88.75 87.79 COI 60892 DF09-SS-0010-0-0000 72.09 C0160893 DF09-SS-0010-0-0003 75.60 COI 60894 C0160895 C0160896 C0160897 COI 60898 COI 60899 COI 60900 DF09-SS-0010-0-0010 DF09-SS-0011-0-0000 DFO9-SS-0011-0-0003 DFO9-SS-0011-0-0010 DF09-SS-0012-0-0000 DF09-SS-0012-DB-0000 DFO9-SS-0012-0-0003 76.57 87.53 86.92 86.19 90.45 90.43 88.07 C0160901 DFO9-SS-0012-0-0010 87.02 COI 60902 C0160903 COI 60904 DF09-SS-0013-0-0000 DFO9-SS-0013-0-0003 DF09-SS-0013-0-0010 87.52 87.52 85.76 COI 64247 COI 64248 COI 64249 DAL-SB-602R-0-0000 DAL-SB-602R-0-0005 DAL-SB-602R-0-0010 77.82 82.30 84.24 C0164250 DAL-SB-602R-0-0050 82.18 C0164251 C0164252 COI 64253 COI 64254 DAL-SB-602R-0-0100 DAL-SB-601R-0-0000 DAL-SB-601R-DB-0000 DAL-SB-601R-0-0005 83.52 89.43 87.98 88.75 C0164255 DAL-SB-601R-0-0010 88.87 Exygen Research Page 67 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Table X. Exygen ID CO164256 C0164257 CO164259 C0164260 Total Percent Solids in Soil Samples Continued Sample Description Total Solids (X) DAL-SB-601 R-DB-0010 DAL-SB-601R-0-0050 DAL-SB-601R-0-0100 DAL-SB-601R-DB-0100 87.99 81.36 86.85 83.56 Exygen Research Page 68 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 FIGURES Exygen Research Page 69 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Figure 1. Typical Calibration Curve for PFOA in Methanol 0412M1AR P7w)-1131Sutfaoe Soil REV1,rdb (PFOq): 'Lineat" Regression("1 td' weighting): y- 003 x + 2.121+W4 (r= O.oOo1) Concentration. ng/L Exygen Research Page 70 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Figure 2. Extracted Standards of PF'OA in Methanol, 25 ng/mL and 50 ng/mL, Respectively 2500 J 1 1.23 2000 - vP) 1500: - c c al 1 0 0 0 c 600 -. 0.62 0-. I . . . . . . . . . . . . . . . . . . . . . I 2 4 5 7 10 11 3 6 8 0 I - - Time, min ~ ~ 0 4 1 3 0 6P2FOA (StJndJId)413.013bQ.O rmu rrmpir 3 of 4~ ftom W I M O A R . ~ ~ ~ I Area: 74142 countr Height4.40.+003 cpr RT: 1 1 2 min . . 12 . . 13 . . 14 . . 15 . . I6 . . 17 1121 Time. min Exygen Research Page 71 of 151 Interim Report #22 - Analysis of Soil Samples Exygen StudyNo.:PO000760 Figure 3. PFOA in Methanol Reagent Blank, 50 ng/L Fortified Reagent Spk A, and 500 ng/L Fortified Reagent Spk B, Respectively 0' 1 2 3 4 5 0 7 8 0 10 11 12 13 14 15 16 17 I - Time. min Reagent SpkA - PFOA(OC)413.0E+W.O rmu rampie 10 of 40 from W1206AR.wiff h e r : 71789 counk Height4.25e+003 cps RT: 11.2 rnin 1122 02 4300- 8 g 2000- mc d.. - 0 2.04 1 2 3 4 5 0 7 8 0 10 11 12 13 1 4 15 16 17 I . - Time. min Reagent Spk B PFOA(OC)413.0/384.0 amu sample 11 of 49 from W1206AR.wiff A 1 ~ ~ : 5 0 2 0 1o0ounk Height 3.70e+004 cps RT: 1 1 2 min 2v) 3.014- 2.014- - c %? 1.014c 11.20 Exygen Research Page 72 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Figure 4. Chromatogram Representing a Soil Sample Analyzed for PFOA (Exygen ID: C0156344, Data Set: 041206AR) - COl56344 PfOA (urkroWrJ 4l3cIJCLO amy -sample 240149 from Wl20CllRwdW Area: 538244counb tinight: 4 l 7 e + W c p r RT:11.2riu 43..08.4.41 1 0 38.4 3.414- 3.24- 3.014- 2.814- 2.6.4 - 2.4.4- 0 2.2.4- 2.0i al c C 1.8a4- ld.4- 1.4.4- 1.214- 1.0.4 - 8ooo.o - - moo.0 4 4ooo.o 1 1 2M)(l0.o.o 10.75, 1 2 3 4 5 6 7 8 0 10 1 12 13 14 15 16 17 lima, min Exygen Research Page 73 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Figure 5. Typical Calibration Curve for 13CPFOA in Methanol 041206E Soil.rdb (13C PFOA): " L i n e d Regression ("1 /x" weighting): y = 478 x + 0.00111 (r= 0.W78) Conoentration. n g R Exygen Research Page 74 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Figure 6. Extracted Standards of I3C PFOA in Methanol, 25 ng/mL and 50 ng/mL, Respectively 2 m- 1m - l o 0 0 m- 0-. . . I - I . I . I - . - I- I 1 - . Time. min XCW1306-2 lJC.PFOA(Standrrd)415.01370.0 rmu sample 3 of 38 from W1306A.Wlff A1*~:5634Jcounis Height: 4.99e+M13 cps RT: 11.2 min 11.20 4ooo (D a u 3m - % c -a, c 2000 10W 0 Time. min Exygen Research Page 75 of 151 Interim Report #22 - Analysis of Soil Samples Exygen StudyNo.:PO000760 Figure 7. 13CPFOA in Methanol Reagent Blank, 50 ng/L Fortified Reagent Spk A, and 500 ng/L Fortified Reagent Spk B, Respectively 11.20 8v) 15 g 10 c -a, 6 c - 0 1 2 3 4 5 6 7 8 0 10 11 12 13 14 15 I 6 17 I - Time. min Reagent Spk A- 13C-PFOA (QC)415.0/370.0 amu sample 10 of 38 from 041306A.wiff &ea: -1 counts Height: 6.42-3 cps RT: 11.2 min v) Q 0 400(3- a, m : -c c 1 . . Time. min ReJgent Splc B 13C-PFOA(QC)415.0/370.0amu sample 11 of 38 from 0413WAwiff Area: 553376 counts Height 4.86*+004 cps RT: 11.2 min 1123 Time. min Exygen Research Page 76 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Figure 8. Chromatogram Representing a Soil Sample Analyzed for 13CPFOA (Exygen ID: C0156363, Data Set: 041306A) 13.O14 2.8.4 - 2.2r4 2.0e4cn 1.8.4- Q 0 & 1.0~4- cn c - 1.4r4- 1.2e4-I l.Oe4- - 8ooo.o -,m . 0- 4Ooo.o - 2000.0 0.0 - Exygen Research Page 77 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 APPENDIX A Study Protocol PO000760 (Exygen Study No. P0000760) with Analytical Methods and Protocol Amendments Exygen Research Page 78 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen Pmtocol Number: PoooO760 STUDY PROTOCOL Study Title: Analysis of PerfluorooctanoicAcid (PFOA) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Program Exygen Protocol Number: PO000760 Performine Lab0ratorv: Exygcn Research 3058 Research Drive State College, PA 16801 Phone: (814) 272-1039 Sponsor Representative: Michael A. Santom Director of Regulatory Affairs 3M Building 0236-01-B- 10 St. Paul, MN 55 144 Phone: (651) 733-6374 Exygen Research Page 79 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.:PO000760 Exygen Protocol Number: PO000760 DISTRTBUTION: 1) JaisimhaKeSari, Study Director, Weston Solutions 2) JohnM. Flaheaty, PrincipalInvestigator,Exygen Research 3) Michael A. Santoro, SponsorRepresentative,3M Company 4) Exygm Research Quality Assurance Unit Page 2 of 6s _- - . .. __ Exygen Research Page 80 of 151 Interim Report #22 - Analysis of Soil Samples Exygen StudyNo.:PO000760 - PROTOCOL APPROVAL Exygm Protocol Number: PO000760 Study Title: Analysis of Pduorooctanoic Acid (PFOA) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Livers and Small Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Program Exygen ProtocolNumber:PoooO760 APPROVALS Weston Solutions w k / B Michael A. S d r o . SponsorRepresentative ' 3M Company / Exygen Research &=&/zAj ident, Facility Management f//fl/o+ 'Date Date %-bx-mq Date .. Exygen Research Page 3 of65 .. Page 81 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygcn Rotocol Numbcr: PoooO760 TABLE OF CONTENTS TlTLJ3PAGE.................................................................................................................................................... 1 DISTRIBUTION............................................................................................................................................... 2 PROTOCOLAPPROVAL................................................................................................................................ 3 TABLEOF CONTENTS.................................................................................................................................. 4 ........................ .............. .............................................................................................. SURROGATEFIEL.D SPIKE COMPO^............................................................................. OBJECTIVE .................................................................................................................................. TESTING FACILITY................................................................................................................. STUDYDIRECTOR......................................................................................................................................... 6 SPONSORREPRESENTATIVE...................................................................................................................... 7 PRINCIPAL.INVESTIGATOR........................................................................................................................ 7 PROPOSEDEwERIMEElTAL STARTAND TERMINATIONDATES ..................................................... 7 IDENTIFICATIONAND JUSTIFICATIONOF THETEST SYSTEM ......................................................... 7 SAMPLEPROCUREMENT,RECEIPTAND RETENTION................................................... ........... 8 SAMPLEIDENTIFICATION.......................................................................................................................... 8 ANALYTICAL PROCEDURESUMMARY ................................................................................................... 9 VERIFICATIONOF ANALYTICALPROCEDURE...................................................................................... 9 MEIlIoD FOR CONTROLOFBIAS............................................................................................ I1 STATISTICALMETHODS ................................................................................................. I1 GLP STATEMENT.......................................................................................................................................... I 1 REPORT ........................................................................................................................................................... I I SAFETY AND HEALTH.................................................................................................................... AMENDMENTSTOPROTOCOL.................................................................................................................. I3 DATA RECORDKEEPING ...................................................................................... QUALITY ASSURANCE ............................. ............................................... 14 RETFNTIONOF DATA AND ARCHMNG ........................................................... ........................... 14 APPENDIX I. ANALYllCAL METHODS................................... ......................... Exygen Research - . Page 82 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen Protocol Number: PoooO760 The purpose of this study is to perform analysis for perfluorooctanoic acid (PFOA) in water, soil. sediment, fish, clams, vegetation, small mammal livers and small mammal serum using LC/MS/MS for the 3M Decatur Monitoring program. The study will be audited for compliance with EPA TSCA Good Laboratory Practice Standards 40 CFR 792 by the Quality Assurance Unit of Exygen Research. TEST MATE= The test material is perfluorooctanoic acid (PFOA) and was purchased from Sigma-Aldrich. PFOA ChemicalName: Pertluorooctnnoicacid Molecular Weight: 414 Lot Number: 231 16HB Purity: 97.64% Transitions Monitored: 413 +369 (for quantification)and 413 +219 (for confirmation) structure: The surrogate field spiking compound is "C labeled pertluorooctanoic acid ("C PFOA) and was purchased by 3M from Perkin-Elmer Life and Analytical Sciences. "C PFOA ChemicalName: 1,2-13C perfluorooctanoicacid MolscularWeight: 416 Lot Number. 3507-195 Purity: 97% Transition Monitored: 415 + 370 Page S of 6s Exygen Research Page 83 of 151 Interim Report #22 - Analysis of Soil Samples Exygen StudyNo.:PO000760 Exygen Protocol Number: PO000760 The purpose of this study is to perform analysis for pduorooctanoic acid (PFOA) in water, soil, sediment, fish,clams, vegetation, small mammal livers and small mammal serum for the 3M Decatur Monitoring Program using the current versions of the followingExygen analytical methods: V0001780: V0001781: V0001782: VOOOl783: VOOOl784: V0001785: VOOO1786 "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Water by LCIMSIMS" "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Soil by LCIMSIMS" "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Sedimentby LCIMSIMS' "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Fish and Clams by LCIMSIMS" "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA)in Vegetationby LC/MS/MS' "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Small Mammal Liver by LC/MS/MS" "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Small Mammal Serum by LCIMSIMS" TESTING FACILITY Exygen Research 3058 Research Drive State College, PA 16801 Phone: (814) 272-1039 STUDY DIRECTOR Jaisimha Kesari P.E., DEE Weston Solutions, Inc. 1400Wcston W a y West Chester, PA 19380 Phone: (610) 701-3761 Fax: (610) 701-7401 j.kd@westonsolutions.com - Page 6of 6s Exygen Research Page 84 of 151 Interim Report #22 - Analysis of Soil Samples * SPONSOR REPRESENTATIVE Michael A. Santom 3M Company Director of Regulatory Afiairs 3M Building 0236-01-B-10 St. Paul, MN 55144 Phone: (651) 733-6374 PRINCIPAL INVESTIGATOR John M.Flahaty Exygcn Research 3058 Research Drive State College, PA 16801 Phone: (814) 272-1039 john.f l a h e c x y g c n . c o m Exygen Study No.: PO000760 Exygen pratocol Number: PO0O0760 It is proposed that the analytical portion of this study be conducted from October 01,2004 to December 31,2005. The actual experimental start and termination dates will be included in the final report. IDENTIFICATION AND JUSTIFICATION OF THE TEST SYSTEM The followingarc the test systems for this study: Water (groundwaterand surfacewater) Soil sediment Fish Clams Veptation SmallMammalLivcr SmallMammalScrum The samples will be collected by Weston Solutions. The control samples will be purchased and prepared by the testing facility. Purchase and processing Poge 7 of6S . Exygen Research Page 85 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.:PO000760 Exygen Rotocol Number: woo0760 details for the control samples will be included in the final report associated with this study. The test systems werc chosen to access the environmental impact of PFOA in the Decatur, Alabama area. SAMPLE PROCUREMENT, ReCEWf AM3 RETENTEON Water, soil, sediment, fish, clam, vegetation, small mammal liver and small mammal serum samples will be received at Exygen directly from Weston Solutions. The details of sample procurement for this study are outlined in the 3M work plan entitled "Phase 2 Work Plan for Sampling Environmental Media" The number and types of samples collected will vary depending availability in the field. The total number of samples received and analyzed for each matrix will be documented in the final report associated with this study. Water, soil. and sediment samples will be used as received without further processing at Exygen. Thcse samples will be stored refrigerated at 2OC-8"C. Fish, clam, vegetation and small mammal liver samples will be processed according to the appropriate analytical method (see Appendix I). These P- samples will be stored fiozen at S -10C. Small mammal whole blood sampleswill be centrifiged in the field at the time of collection and the serum fraction will be used for the study. Small mammal serum will be stored h z e n at 5 -10C. The receipt and processing of the samples will be documented in the final report and raw data apsociated with the study. SAMPLE fDENTIFICAITON Prior to analysis, each sample will be assigned a laboratory sample reference number. The reference number will be unique and will distinguish each laboratory sample that is processed throughout the analytical procedure.. Chromatographic data will be identified by the laboratory sample reference number. Sample storage conditions and locations will be documented throughout the study. .. - . Page 8 of 65 Exygen Research Page 86 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen Protocol Numkr: woo0760 ANALYTBCAL PROCEDURE SUMMARY References: V0001780: V0001781: V0001782: V0001783: V0001784: V0001785: V0001786 "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Water by LC/MS/MS" `Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA)in Soil by LC/MS/MS" "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) inSedimentby LCIMS/MS" `Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Fish and Clams by LC/MS/Ms" `Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA)in Vegetationby LC/MS/MS" "Methodof Analysis for the Dctamination of Perfluorooctanoic Acid (PFOA)inSmall Mammal Liver by LC/MS/MS" "Method of Analysis for the Determination of Perfluomctanoic Acid (PFOA) in Small Mammal Serum by LC/MS/Ms" The above methods use analytical conditions capable of separating the isomers of PFOA. The final report will include the isomers summed into total PFOA found. VERIFICATION OF ANALYTICAL PROCEDURE A laboratory control sample will be used for the preparation of fortified control samples. The test substance will be made into solutions as per the method, and added to the matrices via a micropipette. For water sampling, Exygen will supply one bottle per sample collected. The bottles will be 500 mL preclcaned Sci/Spec Premier wide mouth HDPE bottles. These bottles have bcen routinely used for PFOA sample collection at the testing facility and have been shown to be free of PFOA. All containers used for water sample collection will be shipped to the sample location containing 100 ng of "C PFOA (equivalent to 500 n g L in the final sample). Sampleswill be addedto each container to a volumetric fill line at 200 rnL. A field duplicate, a low field spikeand a high field spike of each sample will be collected. The low and high field spikes will contain PFOA as well as perfluorobutanesulfonate QFBS), pduorohexanesulfonate (PFHS), and pduomtanesulfonate (PFOS). These compounds arc included in the solutions used to spike the samples. The results for PFBS, PFHS and PFOS will not be rcported in this study. Exygen will supply one field blank (control water) and two field blank spikes (control water fortified with PFOA at a low Page 9 0165 . . Exygen Research Page 87 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygca Protocol Numbcr: PO000760 and high level) for every twenty samples collected. At the testing facility, each water sample (excluding field duplicates and field spikes) will be extracted in duplicate and will also be fortified at a low and high concentration with PFOA and processed through the described procedure to determine method accuracy and to check for bias. For soil, sediment, clams, and vegetation, Exygen will supply one 500 mL precleaned ScUSpec premier wide mouth HDPE bottle per sample collected or a zip-seal bag. All containerslbagsused for samplecollection will be shipped to the sample location. Samples will be added to each container or bag in the field. At the testing facility, each sample will be extracted in duplicate and will also be fortified at a known concentration with PFOA at both a low and high level and processed through the described procedure to determine method accuracy and to check for bias. "C-PFOA will also be added to each sample in the laboratoryprior to extractionat the level specified below. For small mammal liver. Exygen will supply a 50 mL polypropylene centrifuge tube. For small mammal scrum, Exygen will supply a collection kit for each sample containing serum separator tubes (red top), vacutainers. n d e holders and needles, transfer pipettes, and polypropylenetubes. At the testing facility, each liver and serum sample will be extracted in duplicate and will also be fortified at a known concentration with PFOA at both a low and high level and processed through the described procedure to determine method accuracy and to check for bias. "C-PFOA will also be added to each sample in the laboratoryprior to extractionat the level specified below. Low and high spiking levels for each matrix are defined below: I I LowPFOA I HiehPFOA I '' C-PFOA 1 R ~ v c r i c sarc anticipated to bo batween 70% and 1305/0 of the fortified levels; however, the exact precision and accuracy will be determined by the analysis of the quality control samples described above. A statement of accuracy will be included in the final report. Prior to sample analysis, a laboratory control spike study will be conducted in water to justify the use of "C PFOA results to establish precision and accuracyof PFOA samples. The followingsamplesarc to be prepared: Page IO of 63 Exygen Research Page 88 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen Protocol Number: P0000760 Two control water blanks Two control water samples fortified at 250n f l with `ICPFOA 0 Two control water samplesfortified at 250n f l with `kPFOA and at 250n f l with PFOA. 0 Two control water samples fortified at 5000 ng/L with `ICPFOA and at 5000n f l with PFOA. The above samples arc to be extracted and analyzed according to method V0001780 entitled "Method of Analysis for the Determination of PerfluorooctanoicAcid (PFOA)in Water by LC/MS/MS." METHOD FOR CONTROL OF BLAS Controlof bias will be addressedby taking representativesub-samplesfiom a homogeneousmixture of each matrix h m untreated control samples, and by analyzing at least two levels of fortifications. STATISTICAL METHODS Statistics will be limited to those specified in the subject methods and to the calculationof averagerecoveries, as applicable. GLP STATEMENT All aspects of this study shall be performed and rcported in compliance with EPA TSCA Good Laboratory Practice Standards 40 CFR 792. The final report or data package (supplied to the Sponsor)shall contain a statement that the study was conducted in compliance with cumnt and applicable GLP standards and will outline any deviations in the study fiom those standards. This statement will be signed by the Study Director and Sponsor Representative. REPORT A final report will be prepared by the principal investigator or their designee at the conclusion of the study. The repart will include, but will not be limited to, the following: Page I I of 65 Exygen Research Page 89 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen Protocol Number: woo0760 The name and address of the Study Director, Sponsor Representative. and of the testing facility. A statement of GLP compliance (any related documentation, such as chain-of-custodyrecords, must be in the study records). The signed and dated statement by the Exygen Research Quality Assurance Unit regarding dates of study inspections and dates findings were reported to the Study Director and Management. A description of the exact analytical conditions employed in the study. If the subject method was followed exactly, it is necessary to include only a copy of the analytical method. Any modifications to this method will be incorporated into the report. If the method is photo-reduced, the project number and page number must be included on each page. Descriptionof the instrumentationused and operatingconditions. All results from all sets analyzed. Control and fortified samples will be identified and the data table will include sample number and fortification level. R e p m t a t i v e chromatogramsfor each analyte in each matrix, including chromatogramsof a standardand a control sample, and a chromatogram at a fortification level. The location of the analyte peaks will be clearly identified in all chromatograms. All circumstances that may have affected the quality or integrity of the datawill be documentedin the report. Locations whcrc raw data and the final report arc to be archived. Additions or corrections to the final rcport shall be in the form of an amendment signed by the Study Director. The amendment shall clearly identify that part of the report that is being altered and the reasons for the alterations. The amendment will be signed and dated by the Study Director and the Sponsor Representative. SAFETYANDHEALTH Laborptory personnel will practice good sanitation and hcalth habits. Every reasonable precaution shall be taken to prevent inadvertent exposure of personnel and the environment to the test or reference substance(s). Page 12 of 6S Exygen Research Page 90 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygcn Protocol Number: woo0760 All significant changes to the analytical protocol outlined here will be expressed in writing, signed and dated by the Study Director and Sponsor Representative. Amendmentsusually will be issued prior to initiationof study plan change. However, when a change is required without sufficient time for the issue of a written amendment, that change may be effected verbally with supporting documentation signed and dated by the Study Director and followed with a written amendment as soon as possible. In this case, the effective date of the written amendment will be the date of the documented change. Copies of the signed amendmentswill be appended to all distributed study plan copies. The original amendment will be maintained with the original study plan. Any deviations from the study plan or from the analytical method as provided will be documented and reportedpromptly to the Sponsor Representative. Records to be maintained include the following (as appropriate): Sampletracking shcet(s) Samplereceipt records, storagehistory, and chains of custody History and preparation of standards(stock, fortification,calibration) Descriptionof any modificationsto the method Instrumentrun sheets, bench-sheetsor logs Analytical data tables All chromatographicand instrumentalconditions Sample extraction and analysis dates A complete listing of study personnel, signatures and initials Chronologicalpresentationof all studycorrespondence Any otherdocumentationnecessary for the reconstruction of the study Chromatograms-All chromatogramswill contain the following: 8 Sample identification, injection date, mow or other indication of the area ofinterest.and injectionnumber correspondingto the run. 8 Additionally, fortifications will include the amount of analyte added and the sample number of the sample that was fortified. 8 Analytical standard ~ h r o m a t ~ g r a mw~ill additionally include the concentration (e.g.. pgImL). Page I3 of 65 Exygen Research Page 91 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen Protocol Number: PoooO760 As part of the documentationthe followingsheets will be included in each analytical set: a run sheet listing the samples to be run in the set, and an instrument conditions sheet describing the instrument type and operating conditions. All applicable requirements for reporting of study results as per 40 CFR 792.185. QUALITY ASSURANCE The QA Unit of Exygen Restarch will inspect the study at intervals adequate to assure compliancewith GLP's,and will report the findings of audits to the Study Director, Exygen Management, and the Sponsor Representative. RETENTIONOF DATA AND ARCEWING All hard copy raw data, including, but not limited to, the original chromatograms, worksheets, correspondence, and rcsults shall be included with the data package submitted to the Study Director. These will be archived with the original study plan, amendments, final report, and all pertinent information from the Sponsor. The testing facility shall keep all electronic raw data and any instrument, equipment, and storage l o g for the period of time specified in 40 CFR 792.195. An exact copy of the materials submitted to the study director will also be kept at ExygenResearch. Exygen will obtain permission ftom the study director before discarding or returning samples. . Exygen Research Page I4 of6S - Page 92 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen Protocol Number: PoooO760 APPENDIX I ANALYTICAL METHODS V0001780 V0001781: V0001782: V0001783: V0001784: V0001785: V0001786 "Method of Analysis for the Determination of Pduorooctanoic Acid (PFOA) in Water by LC/MS/MS" "h4ethod of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Soil by Lc/MS/MS" "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Sedimentby LC/MS/MS" "Method of Analysis for the Determination of Pcrfluorooctanoic Acid (PFOA) in Fish and Clams by LC/MS/MS" "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Vegetationby LC/MS/MS" "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Small Mammal Liver by LC/MS/MS" "Method of Analysis for the Determination of Pduorooctanoic Acid (PFOA) in Small Mammal Serum by LC/MS/MS" Exygen Research Page IS of 65 Page 93 of 151 Interim Report #22 - Analysis of Soil Samples ExygenStudy No.:PO000760 Exygca protocol Number: woo0760 ANALYTICAL METHOD M a h o d N ~ ~ n bVeo~oO1780 c- Method d krbJ, lor the Detwmiaubmof PerfluemoctuokAdd (?MA) l m Water Exygen Research ToulPya: 7 Page I6 of 6s ~ Page 94 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen protocol Numbs: PoooO760 Exygen Research Page I7 of 65 __ Page 95 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygea Protocol Number: P0000760 xiadmuzu 0.0 65 1.o 65 8.0 25 20.0 25 22.5 65 6 6 FbWRuc ILBlmLhird 35 0.3 35 0.3 75 0.3 75 0.3 35 0.3 Exygen Research Page I8 of 65 Page 96 of 151 Interim Report #22 - Analysis of Soil Samples Exygen StudyNo.:PO000760 Exygen Protocol Numkr:PoooO760 9.0 S l d m d P r q m d o n 9.1 ~ S t o d J p a c i h u t i m S o h t i o l l 9.1.1 Prrprc I MOL sohdionof-lM p g h L of PFOA by w e i m g 10 rng m. of rulylicd (ramclodfor purity) .addilute IO 100 mL with nlehmll in I 12FmL LDPe 9.13 A l O p @ L f o d d m solution of PFOA u prrpped by bringing IU m L o f t b 100pg/mLsolutiontaiL d volume of 100 with rnihnol in I 125 mL LDPB boalo. 9.1.3 Al.OpJmLfbollif*ltioasolutimofPFOAiipnp.Rdbybringing Ill lllL of m0 10 rJIDLlolutionOI I lad volume of 100 with msthrn~in~ I125 mL LDPE bocuc. 9.1.4 A 0.1 pJIDL fbnifludon solutionof PFOA is pop.rodby brinylnp I o mLoftbo 1.0 r@Lsolutionto I MI volume of I 0 0 with anh.n01in I I25 mL LDPEboab. 9.1.5 A 0.01 p#mL lb1U5ratimsohciooo f PPOA L prrppedby brinJn# IO mL of tk 0.1 pJmL solvtiOn IO I8nrl volunw of 100 with achrplin. 125 mL LDPE bottle. 9.1.6 T&S?ck d fod&rtion soldmam 10be stored in imtrigeruor11 4 ~ m m m I d y 4 . Cd am arbla for i&urn p a i d of6 monlh Ihnum~ofpOpatiOn. 9.1 S c l n d r d C d i i S o l u t i o n ~ 9.2.1 U l i b n t i o n ~ u s p n P n d i n H p L C w u e r .The idalhltoumpk 9 3 3 T& b l mia I rrpiul uqb:dditiaul amcamtiom may be poprod=- PW Cawouuiolr F a I U l l d a ~ Vobmmof C b c ~ h U i a n o f Calihtion ofFaIUtlcuim Volvnv Pmil*dcolmol Wibntia StpdvdlD sdu(ioa(eDb) (UL) 0 0 10 loo s a dr ( d ) 40 40 991d.rdm. 0 25 kxanw le) -n-O xcmmddyy.1 10 loo 40 50 XChddyy.2 10 4m 40 I00 xcmmddyy-I 100 io0 40 loo 100 40 250 XCmmddyy-t 500 XCaunddYyJ -io0 4m 40 loo0 xcaunddYY4 Ibo ox^^ ofth.+ibdonnmndd u oqurl IO I x i u initid concQld~buIOtbcoc#a(nhollof (lultlldrdl- tbr nbwion (SPE). XC cntnddd b d m ct.ldud. Pops 19 of 61 Exygen Research Page 97 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen Protocol Number: PoooO760 10.0 w s a u p 12.0 hom*ogrphy 12.1 121 12.3 12.4 Pa#. 5 of 7 . .- Page 20 of 65 Exygen Research Page 98 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygcn Protocol Number PoooO760 13.0 lrcoopUnsr QiIh 13.1 13.1 133 11.4 133 13.6 D F - haDlbywhichaV finrl volumewu dllucod,If mw8amy. Exygen Research Page 21 of 65 Page 99 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.:PO000760 Exygen Protocol Number: PoooO760 Exygen Research Poge 22 of 65 ..- - Page 100 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen Protocol Number: PoooO760 ANALYTICAL METHOD LdolhQdNIIIpbQ:VMW)I781 Exygen Research Page 23 of 6s ____ _- Page 101 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen RotocolNumber: PoooO760 1.o 2.0 3.0 4.0 5.0 Exygen Research Poge 24 of6S . Page 102 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.:PO000760 Exygen Rotowl Number: P0000760 7.1 Modo: Ekchwpny Nop(ivc MRMmode.monitoring413 -b 369 W r foi PFOA Exygen Research Page 25 of 63 Page 103 of 151 ~ Interim Report #22 - Analysis of Soil Samples Exygen Study No.:PO000760 Exygen Rotocol Numbcc PoooO760 I -lrrJ ANALYTICALMrmOD kuhodofM y i s bor llwDarmhvtimofPiLuus/Ms L u b d N u m b VoM1781 I Acid (PFOA) in Soil by 9.0 StaddRp.nti00 9.1 St8ddSlo*IForciduciollSolu(ion 9.1.1 F+qmirtosL wlutionof-100 &nL ofPFOA by weighing IO my o f d ~ ~ ( c o n o s l o d f c ? p u r i t y ) m d d i l u t o1t0o0mLwilh 65 m W l in i1 2 5 4 LDPEboa*. 9.13 A 10 rJmt M c u i o n wluti00ofPWA i#PIOpudby bringingIO mL ofUm 100 u&nL wlution to ifLul v o h of 100 with mcchlnol m i 11s lllL bollla 9.1.3 A l . O ~ & L l a r i & u i m w l ~ n o f P P O A u p c p l r e d b y b r i ~ n gIO "9. mLofW 10 pJmL wlutioDtoiharlwhmc of 100 with mthvlol in L 115 mL LDPE 9.1.4 A0.1 p&Lforhhnm whdhof PFOA L m i by bringingIO mLof &a 1.0 pohnLwlutiocl to ih l v o l m of 100with nh.nolin i125 mL LDPEboalo. 9.13 A 0.01 p&L fonihutim lolutiam olPFOA is prepad by bringing 10 mL of tbc 0.1 pJmL wlu(ion to ihrvl volume of 100 with mdboolioi125 mL LDPE boalo. 9.1.6 Thottoft md forcificltioa wlutiolu110 u)k ltorodin irehigaitor iI Ippodmr(cty4.C ud uc &bk fc? imuimumpaidof6 monh Immlhodnoof~oa 9.2 shadmnlClh'bntionSolvtiolv 9.2.1 LCIMSMS CrlibUbD almdm& 110 prqmd in HPLC wuer. The ulintiorr amdrb 110 poocuad tbugh ths sxmction procedure. idmlidto~k 93.2 llu 13Uowh#u itypiul axmnple:dditiaulcollccamtimr may k prplrodUoocdod. Find C a m m l b n Fatif*.cia Voharof Cawnnoltionof 0fFdtbtiOn V h Qatillodcolllml Wibruion Chlibuion Sund.rdW IO 400 40 IM IM Exygen Research Page 26 of 65 Page 104 of 151 Interim Report #22 - Analysis of Soil Samples Exygen StudyNo.:PO000760 Exygcn Pmtocol Nuder: PoooO760 10.0 Burbsaup 12.0 Q o m * o g p b y Exygen Research Poge 27 of 65 .-- Page 105 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.:PO000760 Exygm htocol Number: Woo0760 1 ANALYTICAL METHOD M e t b o d o f ~ y s i s b r t ohf P~duaDauDoic Acid (PFOA) UI Soil by LUUSIMS 12.4 12.5 Exygen Research Page 28 of 63 - Page 106 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 E t y p I*rpcL ~~Voal1711 I I AYALYTlCALME"tl0D Mabodof kvlnLlorthe Ddamiwim ofP c r f l u o m o i c Acid (PFOA)in Soil by LCIMSIMS 14.0 f 3 h M o n s Exygen Research Page 29 of 65 Page 107 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.:PO000760 Exygen Protocol Number: Po000760 ANALYTICAL MJ3"HOD MdhodEhtmbr: VOW1782 Exygen Research Page 30 of 65 Page 108 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen Protocol Number: PoooO760 Exygen Research Page 31 of 65 . ._ Page 109 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.:PO000760 Exygcn Protocol Number: PoooO760 6.0 6.1 62 6.3 6.4 6.5 Iimdahlu 0.0 65 1.o 65 8.0 25 20.0 15 22.5 65 UfIuniRl 35 0.3 35 0.3 75 0.3 15 0.3 35 0.3 6.6 IqirtiDll V- 15 &(em kinorurodtou muchu 50 pL), 6.7 Qoariluioll: PakAra-extaulNadudc.likuioncwc. 6.1 R u n r i : 7.0 6.0 Exygen Research Page 32of 4S _.___. Page 110 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen Protocol Number: PoooO760 9.1 ~ s l o & F a l i 6 a l h S d u t i m e 9.1.1 R o p r r i ~ l o ~ o I - l W p a o f P F O A b y w u 3 u n10gmg of U m d d (cometadlotpnity)rad dilute to 100 mL with lIlc&mol in 1 12Sd.LDPa boclla 9.13 A I O p ~ f d 6 a h olonlutimof PFOA h pnp.ndby bringmy 10 mL of tb 100 &LI mhnionto 1 ihu)volume of 100 with mcthrnol in I I25 mL LDPE bott*. 9.1.3 A 1.0 r & L rOrtifiulioaduti0n of PPOA u Pepvodby bringing 10 mLoftbrlOpJlnLlolutioatoifiDlJvoI~of100withmslhllolin a 125 mLLDPE b o t h 9.1.4 A0.I ~&LrOrtiidutioomlotiollofPFOAuProPPDdbybrinDinIgO mLoftb 1.0 lolotiollto 1thul vok.noof 100with nwlnnol Ill IUmLLDPEWa 9.1.5 A 0.01 fodhtioa lolutimof PPOA is pmpual by bringing IO mL of tb 0.1 p a COMioa to 1 MI volumc of 100 with ar(winr I25 mL LDPEboata 9.1.6 Tbo mdfatidutbnalulioocIR tobe aorod h i m b i p w at w m x m u t d y 4 T md u.u b l a for imuimum paidof6 numb &antb dmmofpnpnlim. 93 100 2 100 2 1) 10 IO 100 I .o 5 10 100 0.1 2 10 I00 0.2 Pose 33 of 6s Exygen Research Page 111of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen Protocol Number: woo0760 I .- Mahod of AMI* WNwrbrrV0001712 i ANALYI'KCALMETBOD IOItb.Dawilutioll of Pdwrwdamic Acid(PFOA) in Sedimentby LCIMSIMS 11.1 11.2 11.3 11.4 11.5 11.6 11.7 11.8 11.9 11.10 11.11 11.12 Exygen Research Page 34 of 65 .- Page 112 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen Protocol Nwnber: P0000760 12.1 12.2 12.3 12.4 12.5 13.1 133 13.3 13.4 13.5 Exygen Research Page 35 of 65 .- Page 113 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.:PO000760 Exygen ProtDcol Number: PoooO760 P Exygen Research ?q*7 of I Page 36of 65 - Page 114 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.:PO000760 Exygen Protocol Number: PoooO760 ANALYTICAL METHOD MWN- VOW1783 fu4 Duo Duo Exygen Research TohlpyCr: 8 Page 37 of 65 .- Page 115 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.:PO000760 1.0 2.0 3.0 4.0 4.1 4.2 4.3 4.4 4.5 4.6 4.7 4.8 4.9 4.10 4.11 4.12 4.13 5.0 Exygen Research Page 38 of 65 Page 116of 151 Interim Report #22 - Analysis of Soil Samples ~~~ ~~ Exygen Study No.:PO000760 Exygen Protocol Number: PoooO760 6.0 ' Syl(0m 6.1 rWytiulc0hum Fbq4useRP(Kcynoocssiontiflc).2.1 nun x 50 nun, 5~ (P/N: azsos-osziw) 6.2 :-T 30% 6.3 MOW.F%aw(A): 2mHAnrmollilunAc&teinW.ta 6.4 MobilomuO(B): Metho1 6.5 OldlaCPmpm: -2flfja- 1.0 65 35 1.0 25 75 20.0 25 75 22.5 65 35 Plow Ruc 0.3 0.3 0.3 0.3 0.3 - 6.6 lr&d?nVobw 15 pL(ao k bwnwdto u muchu SO JIL). 6.7 Qlunnmaa: PeakA m CXMul *mdudulibdw curve. 6.1 RunTLms: -23minuta S b c h cmidiliomarointmddurplidomd amy bc b a e d in uder to opthniulbm x 8yMlU. -. . - ._ _ Exygen Research Puge 39 of 65 _- Page 117 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygcn Protocol Number: PoooO760 Exygen Research Page 40 of 6s Page 118 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygcn Protocol Number: PoooO760 10.0 11.0 Exygen Research Page 41 of 65 Page 119 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygea Protocol Number: PoooO760 12.1 12.2 12.3 12.4 Exygen Research Page 42 of 6s - .. Page 120 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen Rotocol Number: woo0760 14.0 Exygen Research Page 43 of 63 Page 121 of 151 Interim Report #22 - Analysis of Soil Samples Exygen StudyNo.:PO000760 Exygen Protocol Number: PoooO760 Exygen Research Page 44 of 65 Page 122 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen Rotocol Number: PO000760 ~ - - _ _ _ _ -. Exygen Research Page 45 of 65 Page 123 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen F'rotocol Numba: P0000760 - Exygen Research Page 46 of 65 Page 124 of 151 Interim Report #22 - Analysis of Soil Samples Exygen StudyNo.:PO000760 Exygcn htocol Number: PoooO760 5.4 5.5 5.6 5.1 5.8 5.9 5.10 5.ll 5.12 5.13 5.14 5.15 7.0 MSMSS m 7.1 Ldodr: akeocpnyNogdvoMRMmodo. moniPPoTr 413 -b 369 d z for Exygen Research Page 125 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygca hotocol Nuder: PoooO760 8.0 9.0 Exygen Research Poge 48 of 6s Page 126 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen Protocol Number: pooO0760 ofFoMc&m VoL.ru gdutimludml) (d) MUBdrO (mL) f3nca1Exlici1 DW) 1.0 5.0 100 0.05 1.0 2.5 100 0.021 1.0 1.0 loo 0.01 0.05 10 100 0.005 0.021 10 I00 0.0025 0. I 10 100 0.001 0.005 10 100 0.W5 9.2.3 StaD .II~rlibntimItrdrbin llknL LDPE MIIUW-~OU~~ bottla at2Tto6K!,uptodx~~ 9.2.4 AHmrc.volunsl udc#xnmmu of madvdr m y k pcpvcd IS needed. 11.0 SmpkExamim 11.1 113 11.3 11.4 113 11.6 11.7 .. Page 49 of 6s Exygen Research Page 127 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 ExygcnProtocolNumber: PoooO760 12.0 aumWo*y 12.1 123 12.3 F- 12.4 12.5 13.0 -czit.rL 13.1 ~ m v r t o h o rwpakof rduyMr ion u 369 ammu fmm r parent of 413 PLP Tb 413 OIU pnnc - m q m d I to tho PMA anion,while thc d&ta im(369 our)rcpum&@(bo h of oubondioxid.. Pap6011 Exygen Research Page 128 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen Protocol Number: PO000760 14.0 C&uUian 14.1 14.2 143 Exygen Research Page 51 of 65 -- Page 129 of 151 Interim Report #22 - Analysis of Soil Samples Exygen StudyNo.:PO000760 Exygen Protocol Numbn: woo0760 Exygen Research Page 52 of 65 Page 130 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.:PO000760 Exygen Protocol Number: POW0760 1.0 scop 2.0 s* Exygen Research .__. Page 33 of63 . Page 131 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen Protocol Number PO000760 6.0 Pbw Rata IilwmyykklL.30.w 3 0.0 1 a 65 35 0.3 8.0 25 75 0.3 20.0 2s 7s 0.3 22.5 6S 35 0.3 7.0 Exygen Research Page 54 of 65 -- Page 132 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 ExygenRotocolNuder: PoooO760 9.1.1 9.12 9.13 9.1.4 Repro r a o L ahahof -100 rJmL of PFOA by weilhinp IO my of # d u d (wmstod forpurity) Ud diluteto 100 mL with mDQuDolin r lU.4F P E M e . A l . O m f o r ( l & m a ,altuionof FTOA m prepadby bringing I mL of th 100 p a loMm to r Aall volumo of 100with nahool in. 125 mL LDPE b o t k 1s A 0.1 pg/mL rOrtieutiOnahrtionofPVOA is by bringing 10 mLofoW 1.0 pg/mLmlutiontor 6 ~wIlumoof 100with medun01in r mLLDPEboth Ibc d bnitlutioslm h u h IR toba s c d in Irefrigemtoru -4.C d a.&ta for r mnimum paid Of ti rnonlhs hmtlmdateofprrpmtirn Exygen Research Page SS of65 Page 133 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen F'rotocol Nuder: PoooO760 Exygen Research Page S6 oj6S ._ .- Page 134 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 ._ Exygen Research Pose SI of 65 Page 135 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.:PO000760 P Exygen Research Page 58 of 65 Page 136 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.:PO000760 Exygen Rotocol Number: PO000760 Exygen Research Page 59 of 65 _- .. Page 137 of 151 Jnterim Report #22 - Analysis of Soil Samples Exygen Study No.:PO000760 Exygen Protocol Number: PoooO760 Exygen Research Page 138 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen Protocol Number: PoooO760 6.0 ROW- 2LBfllumid 0.0 0.3 1..0. 65 35 0.3 8.0 25 7s 0.3 20.0 25 75 0.3 22.5 65 35 0.3 6.6 6.7 6.8 - - lnjcaimVolumo: 15 pL (cmbe inonwdto u muchu Qudution: prlc Am m dsnwhrdulibrmionw Run T h o : 23 minuW. 50 e pL). . mabowoordiaiolllam intadad II a gui& ad m y be dunged inorder 10 optimiptbpwLcsylum. 7.0 MslMsSySlQ 7.1 Modc: BlsccmcpnyNopivoMRM mod* monilch# 413 -+ 369 nVz for PPOA. m &ow cunditiona M iauadsd u iguida and m y k clunged in ordw IO opthnizetheMShtSsyUan. 8.0 Rwmlialof solutiopr Exygen Research Page 61 of 65 Page 139 of 151 Interim Report #22 - Analysis of Soil Samples ~~ Exygen Study No.: PO000760 Exygen Protocol Number: PoooO760 pya-- &Ibd W r VoOo118b 1 I ANALY"ICAL.MEIllOD Mahoaof~yahforth.D*amioltionofPcrfluomoGtlnoicAcid (PFOA)in Small M.mnulSCWllbyLCIMS/MS 9.0 S ~ ~ ~ ~ P R P U & X I 9.I S m d u dStooWpcdiEdm Solutim dm 9.1.1 PnpM IaocL mlvtion of-IW pJmL of PFOA by wcighiig IO mu of cmdud (omoaodbw purity) ud dilutoto 100 mL with n#chaolin IIU-mLLDPE bottle. 9.1.2 A 1.0 pJmL foccifiutionmlutim of PFOA u p m p d by bringing I mL of th.IM) p m wlutioll to I5nd volume of 100 with rmhanol in. 1 2 s m ~ ~ ~ ~ e b o t l * . 9.1.3 A 0.1 p@, f o r t i 6 c h wlntimof PPOA u PrpMdby bringiw I O mL of cb 1.0 pJmL lolutimto IRnrlvolumeof 100with meihrol in I125 mL LDPE bottle. 9.1.4 TbO aook dfocci6d0n colutiollr KO to be Icorrd ina refrigomor at approximatdy4*Cmd w cubk fw a muimUm psriod of6 monh bmaQ d.tcofprepation. 9 3 scodvdwbnrioDSohnionr -9.21 LCIMSIMSCrlibntiaD#dad8 EO poprodin nmlluool v u dilution of cb 0.1 @nL. bolcitlcuion lohciw. 9.2.2 Tho following L Itypic4 armplo: ddiliontl MDcQ1R(iolu m y k PrplndUWdOi. Find ofPdRotion Volun Diluudto Conemmion A- tm 1 .o 5.0 IO 2.0 10 1 .o 93.3 Stondl 100 I00 loa 100 in -1 I .o os 0.2 0. I m e -w-muth bMtin uZ*Cto6.C. ~ptodrmrrmhr. 9.24 A l t a a n c v o l u n l M d'W ~ I of I1.rdubmay be pnpucd M rladad. Exygen Research Poge 62of 65 Page 140 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygm Rotocol Number: PoooO760 12.0 c l m m o p @ y Exygen Research .. . -. Poge 63of 65 Page 141 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 Exygen Protocol Number: Po000760 Exygen Research Page 64of4S Page 142 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.:PO000760 Exygen Protocol Number: PoooO760 e Exygen Research Page 45 of 45 .- Page 143 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.: PO000760 .-y,.. - . . 3058 D& ' Phonc: 814-272-1039 State coucqC,PA M O l Fw: 814-231-1580 11AnaMiaJ ProcedureSummav V0001780:sedlon 0.1 .. *+iJ .J Exygen Research Page 144 of 151 Interim Report #22 - Analysis of Soil Samples Exygen StudyNo.:PO000760 -'. .: . , - ,.'-.f 3058 Research Drhre phont: 814-272-1030 RESEARCH . Amendment Number. Effective Date: PROTOCOL AMENDMENT 2 03107/05 Page 1 of1 Exygen Study Number WOO0760 Client Study Number: None DESCRIPTIONOF AMENDED SECTlOY Report, page11 of65 LlrmQmm Insteadof onefinal report, intodmreporta WOI khued. MwuunuX The client will kableto mdve and rsvkwthodata momquickly. Exygen Research ADMINISTRATI& FORM Page 145 of 151 Interim Report #22 - Analysis of Soil Samples -Wr-I-IO..l c - . I:ll,r.--F-,f C.l E l r n.M...I o # + Exygen StudyNo.:PO000760 T4n r.mmo2 HII f ._. -0 v L Exygen Research Page 146 of 151 Interim Report #22 - Analysis of Soil Samples ~ ~~ Exygen Study No.:PO000760 3058 Retcard,O M phone: 814-272-1039 State Cotkge, PA 16801 Fax 814231-1580 Amendment Number: EEfWhfe 0- ErygctnStudyNumber PROTOCOL AMENDMENT 4 07ii CUentstudyNUmber: CRlPrtONOF AMVerificsrtlon of AnatyUc4 F%o#rdum,p, age 10 of prdhco(. P a p i of1 NA J . LIBRARY ID:w X x ) l r n Exygen Research Exygen QAU Page 147 of 151 Interim Report #22 - Analysis of Soil Samples Exygen StudyNo.:PO000760 RESEARCH 3058 Research Drive Phone: 814-272-1039 State College, PA 16801 Fax: 814-231-1580 Amendment Number: Effective Date: Exygen Study Number PROTOCOLAMENDMENT 5 0911305 P760 Client Study Number: Page 1 of 1 NA ESCRlPTlONOF AMENDED SECTION Analvtlcal Proceduk Supmmarv: V0001780:'Method of Anahrsis for the Determination o PerflioroooctanoicAcid (PFOA) inWater by LCNSIMS." AMENDED TQ The reanalysis of two water samples, DF09-GW-13lR-0-040126 and DFB-GW-135L-0. 040121 will be performed using the following procedure: An aliquot of the water sample is spiked with the surrogate standard and/or other matri~ spike compounds as appropriate. Add methand to the fortifed aqueous sample. Mir and aliquot for LCIMSIMS analysis. The LC conditions include the use of a Betasil C18, 2.1 x 50 mm column, a gradient of 30% B to 100% B in 10 minutes, where A=2mM ammonium acetate in water and B=Methand(6 min equilibration). Use a 5 pL injectior volume and a 0.3 mUrnin flow rate. LC conditions may be further modified a5 appropriate for the system being used. An interim report will be issued that will include the exact details of the reanalysis. RATIONALC DFO9-GW-13lR-0-040126 and DF8b-GW-l35L-0-W0121 couM not be reported quantitatively in interim report #3 due to qualify control sample failures. The study director and sponsor have requested reanalysis using the above conditions. IMPACT ON STUDY No negative impact on the study. More usable data may be obtained. Study DLeclwsknahne Date -0 --__ Sponsor Signatum (if required) LIBRARY ID: VOOOI2264 Exygen Research Date ExygenQAU Review Oh.& q f i j / O r ADMINISTRATIVE FORM Page 148 of 151 Interim Report #22 - Analysis of Soil Samples - 3C-HSEHM E&%H.A,SR 236.1B ,I-..". -.-- -6.5.1-73-3.1.-95-8-.- Ep.13.885 l:%m em Exygen Study No.: PO000760 09/14 '05 09:27 N0.915 02/02 w.ur r.6 - PROTOCOL AMENDMENT .. RECEIMD T I M soD.14. 10:4Jm Exygen Research PfWT TIM sEp.14. 18:44Fy? Page 149 of 151 Interim Report #22 - Analysis of Soil Samples Exygen Study No.:PO000760 m:rlg8142311588 p(o.294 P . t P: 2'2 3056 Rerarch Drive Phrme: 814-272-1039 State College, PA 16801 Fax: 614-231-1580 . hymdrnertl Number: EffecWe Date: Exygen Study Number PROTOCOL AMENDMENT 5 OWladM P760 client Shxly Numbor: Pagaldl NA jlESCRlPTlON OF AMFNDED=TI0 N Analytical PrpaduroSummary: V000178oiMelhodof h i y s & fathe 08termlnation F P ~ r p o o d a n dAccid (PFOA) InWater by LCIMSIMS: AMENDED TO - The reanalvsis of hno vater 6amplar. DM9Gw-131RowoI26 and DF8-W-135L-C 04121 wnibe parformed uriwttk ~ O ~ W ~ IpI Qrocedum: An aliquot ofthewatersample is spiked with thesuncgatrstandad andior olkr mtrl spike compounds as appmprlets. Add methanol to the Wkd aqueous sample. Mc and aliquot fw LUMWS ane)yds, The LC d i t i i n s includethe use of a Betasil CIB 21 x 50 mm calumn, a gradknt bt 30% B to 100% 9 in 10 minutes, where Anlmh ammoniuamcetate h w k and B=Methanol(6min equiibratlon). Usea 5 pL I n j d h volume and a 0.3 rnUmin flow rara. LC cbndilons may be furuIer modW I appropriate for the system being used. An interim report Wm k b u d that will include the exacl detatls of me mrmlysis. RATTONALE DF~-131R-o-040128and D F 8 b G W ~ W L - ~ O l Zml u# not be rep- quantitstivldy in interkn #3 due to quaHy axW -le fipiLnes. The rdudl director and sponsor have ngutsted reenalysisusingthe above amdidom. JMPACTON STUDY No nsgatlw inpacton flw mrdy. Mom usabledata may beobtained. -- ----- ECEIKD T I M Exygen Research sEp.14. 10:37Rl PRINT TIME: SEP.14. la:= Page 150 of 151 Interim Report #22 - Analysis of Soil Samples 1 Exygen Study No.: PO000760 ETBenQ3058 ResearchDrive R E S E A R C H State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1'380 Amendment Number: Effective Date: Exygen Study Number PROTOCOLAMENDMENT 6 09/20105 P760 Client Study Number: Page 1 of 1 NA DESCRIPTION OF AMENDED SECTION The identification of the two water samples listed in protocol amendment No 5 an incorrect AMENDED TO The two water samples for reanalysis should be DFO!&GW-l31R-O440120 an( DF8b-GW-135R-0040121. RATIONALE The correct samplesare identifiedfor reanalysis. IMPACT ON STUDY No negative impad on the study. StudyDirectorSigna&re, , Date I 3fmsor Signature (ifrequired) u a w y ID: v000122&8 Exygen Research Date ExygenQAU Review h . W 9/zo/oT ADMlNlSTRAnVE FORM Page 151of 151