Document ZJ2v3BnNN1O5NKn16z5L1wpOO

226-3648 INTERIM REPORT #1 Analysis o f Oakdale W ater Samples STUDY TITLE Analysis o f Perfluorooctanoic Acid (PFOA), Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFS) in Water, Soil, Sediment, Fish, and Clams Using LC/MS/MS for the 3M Cottage Grove 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 May 19, 2005 PERFORMING LABORATORY Exygen Research 3058 Research Drive State College, PA 16801 , Phone:814-272-1039 STUDY SPONSOR 3M Company 3M Building 0236-1-B-10 St. Paul, MN 55144 Phone: 651-733-6374 PROJECT Protocol Number: P0001400 Exygen Study Number: P0001400 Total Pages: 110 000024 Interim Report #1 -Analysis o f Oakdale Water Samples Exygen Study No.: P000140 GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT Exygen Study Number P0001400, entitled "Analysis of Perfluorooctanoic Acid (PFOA), Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfbnate (PFOS) in Water, Soil, Sediment, Fish, and Clams Using LC/MS/MS for the 3M Cottage Grove Monitoring Program," conducted for 3M Company, is being performed in compliance with EPA TSCA Good Laboratory Practice Standards 40 CFR 792 by Exygen Research. Study Director Weston Solutions, Inc. Robert A. Paschke Sponsor Representative 3M Company Exygen Research lx - i *i ; ;: c //? M Date s f a j( K Date / 1Jg -s Date Page 2 o f 110 000025 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 QUALITY ASSURANCE STATEMENT Exygen Research's Quality Assurance Unit reviewed Exygen Study Number P0001400, entitled, "Analysis o f Perfluorooctanoic Acid (PFOA), Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and PerfluoTooctanesuIfonate (PFQS) in Water, Soil, Sediment, Fish, and Clams Using LC/MS/MS for the 3M Cottage Grove Monitoring Program." All reviewed phases1 were inspected for conduct according to Exygen Research's Standard Operating Procedures, the Study Protocol, and all applicable Good Laboratory Practice Standards. All findings ware reported to the Exygen Principal Investigator and Management and to the Study Director. Phase 1. Protocol Review Date Inspected 03/24/05 Date Reported to Date Reported to Principal Exygen Date Reported to Investigator M saasmept Studv Director 03/25/05 03/29/05 05/19/05 2, Extraction Review 03/24/05 03/25/05 03/29/05 05/19/05 3. Raw Data Review and Interim Analytical Report Review 05/16-17/05 05/18/05 05/19/05 05/19/05 'Note; All inspections will be documented in the QA statement for the final analytical report at the conclusion o f the study. Exygen Research Page 3 o f 110 000026 Interim Report #1-Analysis of Oakdale Water Samples Exygen Study N.: P0001400 CERTIFICATION OF AUTHENTICITY This interim report, for Exygen Study Number PO0OI4OO, is a true and complete representation o f the raw data. Submitted by: Exygen Research 3058 Research Drive State College, PA 16801 (814) 272-1039 Principal Investigator, Exygen: Exygen Research Date Study Director, W eston Solutions, Inc Jaisimha Kesari P.E., DEE Weston Solutions, Inc. Sponsor Representative, 3M Company: Robert A. Paschke Manager, 3M Corporate Environmental Programs Exygen Research i- f fc$ 6 / q ;/os~ Date Page 4 of 110 000027 Interim Report #1 -Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 STUDY IDENTIFICATION Analysis o f Perfluorooctanoic Acid (PFOA), Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) in Water, Soil, Sediment, Fish, and Clams Using LC/MS/MS for the 3M Cottage Grove Monitoring Program PROTOCOL NUMBER: POOO1400 EXYGEN STUDY NUMBER: POOO1400 TYPE OF STUDY: Residue SAMPLE MATRIX: Water TEST SUBSTANCE: Perfluorooctanoic acid (PFOA), Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) SPONSOR: 3M Company 3M Building 0236-01-B -10 S t Paul, MN 55144 STUDY DIRECTOR: Jaisimha Kesari P.E., DEE Weston Solutions, Inc. 1400 Weston Way West Chester, PA 19380 SPONSOR REPRESENTATIVE: Robert A. Paschke 3M Company 3M Building 42-2-E-27 St. Paul, MN 55144 PERFORMING LABORATORY : Exygen Research 3058 Research Drive State College, PA 16801 ANALYTICAL PHASE TIMETABLE: Study Initiation Date: 03/03/05 Interim Analytical Start Date: 03/21/05 Interim Analytical Termination Date:04/21/05 Interim Report Completion Date: 05/19/05 Exygen Research Page 5 of 110 000028 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P000I400 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 o f this interim portion o f the study: Name John Flaherty Karen Risha Paul Connolly Chrissy Edwards Mark Ammerman Amy Sheehan Eric Edwards James Miller Edward Kaiser Title Vice President Scientist Technical Lead-LC/MS Technician Sample Custodian Associate Scientist Sample Custodian Scientist Scientist Exygen Research Page 6 of 110 000029 Interim Report #1 -Analysis o f Oakdale Water Samples Exygcn Study No.: P0001400 TABLE OF CONTENTS Page TITLE PA G E............................................................................................................................ 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........................................................................................................ 11 1.0 SUMMARY....................................................................................................................12 2.0 OBJECTIVE..................................................................... 12 3.0 INTRODUCTION................................................................. 12 4.0 ANALYTICAL TEST SAMPLES....................................... 13 5.0 REFERENCE MATERIAL................................................. 13 6.0 DESCRIPTION OF ANALYTICAL METHOD......................................................... 15 6.1. Extraction Procedure......................................................... ........................................ 15 " 6.2. Preparation o f Standards and Fortification Solutions...... ......................................... 16 6.3. Chromatography............................................................... 17 6.4. Instrument Sensitivity..................................................................................................17 6.5. Description o f LC/MS/MS Instrument and Operating Conditions...........................17 6.6. Quantitation and Example Calculation....................................................................... 18 7.0 EXPERIMENTAL DESIGN........................................................................................ 19 8.0 RESULTS...................................................................................................................... 20 9.0 CONCLUSIONS........................ 20 10.0 RETENTION OF DATA AND SAMPLES.............................................................. 2 0 Exygen Research Page 7 o f 110 000030 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table I. LIST OF TABLES Page Summary of PFBS, PFHS, PFOS and PFOA in Water Samples..... ............................................................................ .......................... 22 Table EL Matrix Spike Recovery of PFBS and PFHS in Water Samples......................24 Table IH. Matrix Spike Recovery of PFOS and PFOA in Water Samples.....................30 Table IV. Surrogate Spike Recovery o f I3C PFOA in Water Samples...........................36 Exygen Research Page 8 of 110 000031 Interim Report # I-Analysis o f Oakdale Water Samples Exygen Study No. : P0001400 Figure 1. LIST OF FIGURES Page Typical Calibration Curve for PFOA in Reagent Water................................. 43 Figure 2. Extracted Standards of PFOA in Reagent Water, 25 ng/L and 50 ng/L, Respectively............................................................................ ...........................44 Figure 3. PFOA in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively............................................. 45 Figure 4. Chromatogram Representing an Oakdale Water Sample Analyzed for PFOA, DF=100 (Exygen ID: C0064522, Data Set: 032405CR)......................................................................................... 46 Figure 5. Typical Calibration Curve for l3C PFOA in Reagent W ater.......................... 47 Figure 6. Extracted Standards o f n C PFOA in Reagent Water, 25 ng/L and 50 ng/L, Respectively.................................... 48 Figure 7. !3C PFOA in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively......................................49 . Figure 8. Chromatogram Representing an Oakdale Water Sample Analyzed for 13C PFOA (Exygen ID: C0064522, Data Set: 032405C)......... 50 Figure 9. Typical Calibration Curve for PFBS in Reagent Water.................................. 51 Figure 10. Extracted Standards o f PFBS in Reagent Water, 25 ng/L and 50 ng/L, Respectively..................................................... 52 Figure 11. PFBS in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively..............................................53 Figure 12. Chromatogram Representing an Oakdale Water Sample Analyzed for PFBS, DF=100 (Exygen ID: C0064522, Data Set: 032405CR).................................................... 54 Figure 13. Typical Calibration Curve for PFHS in Reagent W ater................................. 55 Figure 14. Extracted Standards of PFHS in Reagent Water, 25 ng/L and 50 ng/L, Respectively....................................................................................................... 56 Figure 15. PFHS in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively............................................. 57 Figure 16. Chromatogram Representing an Oakdale Water Sample Analyzed for PFHS, DF=100 (Exygen ID: C0064522, Data Set: 032405CR)........................................................ 58 Figure 17. Typical Calibration Curve for PFOS in Reagent W ater.................................59 Exygen Research Page 9 o f 110 000032 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 LIST OF FIGURES Continued Figure 18. Extracted Standards o f PFOS in Reagent Water, 25 ng/L and 50 ng/L, Respectively....................................................................................................... 60 Figure 19. PFOS in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively............................................. 61 Figure 20. Chromatogram Representing an Oakdale Water Sample Analyzed for PFOS, DF=100 {Exygen ID: C0064522, Data Set: 032405CR)........................................ 62 Exygen Research Page 10 of 110 000033 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 LIST OF APPENDICES Appendix A Study Protocol P0001400 (Exygen Study No. P0001400) with Analytical Method: V0001780:"Method o f Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Water by LC/MS/MS" ............................................................... ................. Page 63 Exygen Research Page 11 of 110 000034 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 1.0 SUMMARY Exygen Research extracted and analyzed water samples for the determination of perfluorooctanoic acid (PFOA), perfluorobutanesulfonate (PFBS), perfluorohexanesulfonate (PFHS), and perfluorooctanesnlfonate (PFOS) according to Exygen Method V01780 (Appendix A). The limit o f quantitation for PFOA, PFBS, PFHS and PFOS in water was 50 ng/L and the limit o f detection for PFOA, PFBS, PFHS and PFOS in water was 25 ng/L. Analytical results for the analysis o f PFOA, PFBS, PFHS and PFOS in water samples are summarized in Table 1. The overall average percent recoveries standard deviations for all fortifications o f PFOA, PFBS, PFHS and PFOS in water samples were 93% 1 9 , 141% 21, 96% 1 5 and 109% 32, respectively. The overall average percent recovery standard deviation for all fortifications of the surrogate field spike compound, ,3CPFOA, in water samples was 83% 21. 2.0 OBJECTIVE The objective o f the analytical part of this study was to determine levels of perfluorooctanoic acid (PFOA), perfluorobutanesulfonate (PFBS), perfluorohexanesulfonate (PFHS), and perfluorooctanesulfonate (PFOS) in water according to Protocol P0001400 (Appendix A). 3.0 INTRODUCTION This report details the results of the analysis for the determination of PFOA, PFBS, PFHS and PFOS in water using the analytical method entitled, "V0001780: Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Water by LC/MS/MS." The study was initiated on March 03, 2005, when the study director signed protocol number P0001400, The analytical start date for this interim report was March 21, 2005, and the analytical termination date for this interim report was April 21,2005. Exygen Research Page 12 o f 110 000035 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 4.0 ANALYTICAL TEST SAMPLES One hundred and twenty-one water samples, which correspond to twenty-nine sample sites, (Exygen ID C0064404-C0064438, C0064442-C0064461, C0C64467-C0064532) were received at ambient temperature on March 15, 2005 from Tim Frinak at Weston Solutions, Inc. The samples were logged in by Exygen personnel and placed in refrigerated storage. Sample log-m and chain o f 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, was purchased from Sigma Aldrich and was received at Exygen on December 08, 2003. The surrogate spiking standard, 13C labeled perfluorooctanoic acid (13C PFOA), was received at Exygen on April 15, 2004 from the 3M Company. The analytical standards, PFBS and PFHS, were supplied by 3M. PFBS was received from 3M at Exygen on July, 06, 2000. PFHS was received from 3M at Exygen on January 20, 2003. PFOS was purchased from Fluka Corporation and was received at Exygen on April 23,2003. The available information for the reference materials is listed below. PFOA was stored ambient. PFBS, PFHS and 13C PFOA were stored frozen and PFOS was stored refrigerated. Comoound PFOA i3C PFOA PFBS PFHS PFOS Exveen Inventory No.. SP0003800 SP0004184 SP0000252 SP0002401 . SP0002694 Lot# 23116HB 3507-195 101 SE036 430180-1 Purity (%_) 97.64 97 96.7 98.6 101.2 Exoiration E 12/08/05 03/29/09 12/04/06 10/18/06 04/23/06 The molecular structures of PFOA, 13C PFOA, PFBS, PFHS and PFOS are given on the following pages: Exygen Research Page 13 o f 110 000036 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: F 0001400 PFOA Chemical Name: Perfluorooctanoic acid Molecular Weight: 414 Transitions Monitored: 413 -> 369 (for quantification) and 413 -* 219 (for confirmation) Structure: I3C PFOA Chemical Name: 1,2-13C perfluorooctanoic acid Molecular Weight: 416 Transition Monitored: 415 --v 370 Structure: PFBS Chemical Name; Perfluorobutanesulfonate Molecular Weight: 338 supplied as the potassium salt (CiFsSChTC4) Transitions Monitored: 299 - 99 Structure: FF F F F so3 FF FF Exygen Research Page 14 of 110 000037 Interim Report # 1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 PFHS Chemical Name: Perfluorohexanesulfonate Molecular Weight: 438 supplied as the potassium salt (CsF^SOs'K4) Transitions Monitored: 399 80 Structure: PFOS Chemical Name: Perfluorooctanesulfonate Molecular Weight: 538 supplied as the potassium salt (CgFnSOa'K*) Transitions Monitored: 499 - 80 Structure: F FF FF FF 6.0 DESCRIPTION OF ANALYTICAL METHOD The analytical method "V0001780: Method o f Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Water by LC/MS/MS" was used for this study, 6.1. Extraction Procedure A 40 mL aliquot o f the water sample was used for the extraction procedure. After fortification o f appropriate samples, the samples were loaded onto a Cjg SPE cartridge conditioned with 10 mL of methanol and 5 mL o f water. The eluate was discarded. Approximately five milliliters o f 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. Exygen Research Page 15 o f 110 000038 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0QQ14O0 6.2 Preparation of Standards and Fortification Solutions Individual stock standard solutions o f PFOA, UC PFOA, PFBS, PFHS and PFOS were prepared as specified in Exygen method V0001780. The stock standard solutions were prepared at a concentration o f 100 pg/mL by dissolving 10 mg o f each of the standard (corrected for purity and salt content, if necessary) in methanol. From these solutions, 1.0 pg/mL fortification standard solutions were prepared by taking 1 mL o f the appropriate stock and bringing the volume up to 100 mL with methanol. By taking 10 mL o f the appropriate 1.0 pg/mL fortification standard and bringing the volume up to 100 mL with methanol, 0.1 pg/mL fortification standards were prepared. By taking 10 mL of the appropriate 0.1 pg/mL fortification standard and bringing the volume up to 100 mL with methanol, 0.01 pg/mL fortification standards were prepared. Several sets of standards containing PFOA, 13C PFOA, PFBS, PFHS and PFOS were prepared in water and processed through the extraction procedure, identical to samples. The following concentrations were prepared: Cone, o f Fort Fort Volume o f Solution Volume Fortified Sample (ngfaiL)1 (UL) (mL) 0 0 40 10 100 40 10 200 40 10 400 40 100 100 40 100 200 40 100 400 40 1 o f PFOA, I3C PFOA, PFBS, PFHS and PFOS Final Cone, of Calibration Std. (ng/L) 0 25 50 100 250 500 1000 An additional mixed stock solution of PFOA, 13C PFOA, PFBS, PFHS, and PFOS was prepared at 1000 pg/mL and diluted to 100 and 10 pg/mL for bottle spiking purposes. Complete details can be found in the raw data package associated with this study. The stock standard solution and all fortification and calibration standard solutions were stored in a refrigerator (4 2C) when not in use. Documentation of standard preparation is located in the raw data package associated with this interim report. Exygen Research Page 16 o f 110 000039 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 6.3 Chromatography Quantification o f PFOA, PFBS, PFHS and PFOS was accomplished by LC/MS/MS electrospray. The retention time of PFOA, PFBS, PFHS and PFOS was ~12 min, ~5 mins, ~11 mins, and -13 mins, respectively. Peaks above the LOD were not detected in any of the reagent blank samples corresponding to the analyte retention time. 6.4 Instrument Sensitivity The smallest standard amount injected during the chromatographic run had a concentration o f 25 ng/L o f PFOA, PFBS, PFHS and PFOS. 6.5 Description o f LC/MS/MS Instrument and Operating Conditions Instrument: API 4000 Biomolecular Mass Analyzer Interface: Turbo Ion Spray Liquid Introduction Interface Computer: DELL OptiPlex GX400 Software: Windows NT, Analyst 1.4.1 HPLC: Hewlett Packard (HP) Series 1100 HP Quat Primp HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Thermo Fluophase RP, 50 mm x 2.1 mm Column Temp. : 30 C Injection VoL: 15 pL Mobile Phase (A): 2 xnM Ammonium Acetate in water Mobile Phase (B): Methanol Time (mini . 0.0 1.0 8.0 ' 10.0 11.0 18.0 Total run time; -18 min Flow Rate: 0.3 mL/min %A 65 65 25 25 65 65 %B 35 35 75 75 35 35 Exygen Research Page 17 o f 110 000040 Interim Report #1 -Analysis o f Oakdale Water Samples Exygen Study N o.: P0001400 Ions monitored: Analyte PFOA PFOA Confirm Ion 13CPFOA PFBS PFHS PFOS Mode negative negative negative negative negative negative Transition Monitored 413 -> 369 413 ->219 415 -> 370 299 -> 99 399 -> 80 499 -> 80 Approximate Retention Time (min) ~12min. ~12 min. -1 2 min. -5 min. ~11 min. ~13 min. 6.6 Quantitation and Example Calculation Fifteen microliters o f sample or calibration standard were injected into the LC/MS/MS. The peak area was measured and the standard curve was generated (using 1/x fit weighted linear regression) by Analyst software using six concentrations o f standards. The concentration was determined from the equations below. Equation 1 calculated the amount o f 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 - intercept) x DF slope Where: DF = Dilution Factor, factor by which the final volume was diluted, if necessary. For samples fortified with known amounts of PFOA, PFBS, PFHS, PFOS and 13C PFOA prior to extraction, Equation 2 was used to calculate the percent recovery. Eouation 2: Recovery (%) = (analvte found (ng/L) - analyte in control (ng/LY) *100% amount added (ng/L) An example o f a calculation using an actual sample and results from the PFOA analysis follows: Water sample Exygen ID C0064432 Spk F (Set: 032105BR), fortified at 50000 ng/L with PFOA where: peak area intercept = 1170161 = 26200 slope = 1330 dilution factor = 100 ng/L PFOA added (fort level) = 50000 amt in corresponding sample (ng/L)* = 37600 (*The primary sample result was used for all calculations) Exygen Research Page 18 o f 110 000041 Interim Report #1-Analysis o f Oakdale Watsr Samples Exygen Study No.: P0001400 From equation 1: Analyte found (ng/L) = IT170161 - 262001 x 100 1330 From equation 2: % Recovery 86012 ng/L* (86012 n e /L - 37600 n e/O x 100% 50000 ng/L = 97% (values are slightly different from raw data due to rounding) 7.0 EXPERIMENTAL DESIGN 13C PFOA was used as a surrogate for all the samples, 13C PFOA was added to the sample collection bottles in the laboratory before being shipped to the field for sampling. For samples designated as field matrix spikes, PFBS, PEHS, PFOS and PFOA were 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 samples were extracted in five sets. Each set consisted o f one reagent blank and two reagent blanks fortified at known concentrations. The first set contained six sample sites, the second set contained six samples sites, along with a trip blank and two trip blank spikes. The next two sets contained seven sample sites each. The fifth set contained three sample sites, along with a second trip blank and two trip blank spikes. For each site, a sample, a field duplicate and two-matrix field spikes were collected. For each site, a laboratory duplicate o f the primary sample was extracted and two laboratory matrix spikes were also extracted. For the two laboratory matrix spikes, two 40 mL portions of the primary sample collected for the site was poured from the bottle and fortified. Not only were PFBS, PFHS, PFOS and PFOA added in the laboratory prior to extraction, but also l3C PFOA was added. The additional I3C PFOA was added because the levels o f PFBS, PFHS, PFOS and PFOA spiked into the samples were known to exceed the calibration ranges and were not analyzed without dilution; therefore, 13C PFOA levels were adjusted to require the same dilution as the other analytes. For each primary sample collected, between the field and lab, seven individual QC results were reported for 13C PFOA. Some samples gave recoveries for ,3C PFOA outside o f the normal acceptance range of 70-130%. Because laboratory control spikes for 13C PFOA were acceptable in every set, instrument washes were free o f 13C PFOA, at least one ,3C PFOA recovery per the seven done for the sample was acceptable and no evident errors in spiking or extracting could be found, no re-extractions were performed. 13C PFOA recoveries outside o f 70-130% are deemed indicative of matrix effects. Exygen Research Page 19 of 110 000042 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 8.0 RESULTS Analytical results for the analysis of PFOA, PFBS, PFHS, and PFOS in water samples are summarized in Table I. Fortification recoveries for PFOA, PFBS, PFHS and PFOS in the water samples are detailed in Tables II and III. The overall average percent recoveries standard deviations for all fortifications o f PFOA, PFBS, PFHS and PFOS in water samples were 93% 19, 141% 21, 96% 15 and 109% 32, respectively. Fortification recoveries for 13C PFOA in the water samples are detailed in Table IV. The overall average percent recovery standard deviation for all fortifications o f 13C-PFOA in water samples was 83% 21. 9.0 CONCLUSIONS The water samples were successfully extracted and analyzed for PFBS, PFHS, PFOS and PFOA according to analytical method V0001780. There were no circumstances that may have affected the data quality or integrity. 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 sponsor. 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 file Exygen Research archives for the period o f time specified in EPA TSCA Good Laboratory Practice Standards 40 CFR 792. Exygen Research Page 20 of 110 000043 Interim Report #l-A nalysis o f Oakdale Water Samples Exygen Study No.: P0001400 TABLES Exygen Research Page 21 of 110 000044 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table I. Summary of PFBS, PFHS, PFOS and PFOA in Water E m m ID C0064404 C0064404 Rep C0064405 Client Sam ple ID O KLM N -G W -W 3-O 435C310 OKLMN-GW 4N34W >5031<r OKLMN-GW -W 3-0-050310 Dup Samples Analyte Found (ppt, ngfl.) C4 SulfonaU PFBS C9 Sulfonate PFHS C8 SuHonst PfO S 312 162 4750 298 160 3350 303 15 3190 C Add PFOA 6330 6220 5990 C0064408 C00644408 Rep C0064409 OKLMN-GW -W8-O4>50310 OKLMN-GW -W 8-CL050310* OKLMN-GW -W 8-0-050310 Dup 57.0 63.8 60.1 ND ND ND 59.0 290 55.7 275 56.3 284 C0064412 C0064412 Rep CO064413 OKLMN-GW -W 264W J50310 OKLMN-GW -W26-0.05031CT OKLMN-GW -W 2$4W )50310 Dup 73400 75700 71400 222000 244000 214000 13500000 14400000 12200000 78300000 70200000 71BDCOOO C0064418 C0064416 Rep C0064417 O KLMN-GW -W 33-0-050310 OKLMN-GV-W 334Xk5C31 O ' OKLMN-GW -W 33-CM)50310 Dup 28800 28800 28500 92300 84600 81600 4610000 4870000 4540000 1750000 2020000 2790000 C0064420 C0064420Rep C0064421 OKLMN-GW -W 205-0-050310 OKLM N-GW -W 2054M S031 O' OKLMN-GW -W 205-0-050310 Dup 8260 8800 7850 6740 6610 7070 146000 119000 116000 147000 150000 158000 C0064424 C0064424 Rep C0064425 O KLM N-G W -W 215-0-050310 O KLM N-G W -W 215-0-050310* OKLMN-GW -W 2154K)50310 Dup 801 81.2 753 769 37100 4400 258 27000 3510 270 36900 4070 CO064428 C0064428 Rep C0064429 OKLMN-GW -W 20100-050310 O KLMN-GW -W 2010 0 0 5 0 3 1 0 ' OKLMN -GW -W 2010 0 0 5 0 3 1 0 Dup ND ND ND ND ND ND ND NQ ND ND ND ND C0064432 00064432 Rep C0064433 O KLM N-GW -PW 7OO50310 OKLMN-GW -PW 7-0-050310* OKLM N43W -PW 7-0O50310 Dup 4460 4340 4830 4800 5080 5080 71600 67800 72400 37800 38400 38200 C0064436 O KLM N-G W -TRIP1 -0050310 ND NO ND ND C0064442 C0064442Rep C0064443 O KLM N-G W -PW 80050310 OKLMN-GW -FW 8-O-O50310* O KLM N-G W -PW 8 0 0 5 0 3 1 0 Dup 13300 14100 14100 23800 23900 23000 34300 35600 33400 81400 80600 56500 C0064446 C0064446 Rep C0064447 OKLMN-GW -PW 9-0-050310 O KLM N-G W -PW 00050310* O KLM N -G W -PW 00050310 Dup 2110 2140 1930 5160 5000 5140 84400 84900 88800 49000 46700 49900 C0064450 CQ064450 Rep C0064451 OKLMN-GW -W 6102-0050310 OKLMN-GW -W 61C2-0-050310* OK1_MN-GW-W6102-0-050310 Dup NQ 53.5 NO ND ND NO NQ 214 NQ 223 ND 227 C0064454 C0064454 Rep C0064455 O KLM N-G W -W 6104-0050310 OKLMN-GW -W 8104-0050310* OKLMN-GW -W 8104-0050310 Dup NQ N 51.2 ND ND ND 109 207 125 189 118 184 C0O64458 C0064458Rep C 0064459 OKLMN-GW -W 6201 -0060310 0KLM N-GW -W 62010 0 5 0 3 1 O' OKLMN-GW -W 62010 0 5 0 3 1 0 Dup 74.0 74.1 78.0 ND ND ND NQ 95.5 ND 68.3 NQ 132 C0O64467 C0064467 Rep C0O64468 O KLM N-G W -W 200050309 OKLM N-GW -W 200050309* O KLM N -G W -W 200050309 Dup 13900 10700 10000 12900 9040 7860 46600 36300 30100 285000 243000 190000 C0O64471 C0064471 Rep C0O64472 OKLM N-GW -W 22-00503D9 OKLM N-GW -W 220-050309' OKLMN-GW -W 22-0-050309 Dup 36800 32200 37500 31400 29500 25700 45300 34000 28100 317000 301000 244000 'Lsboratofy Duplicate ND = Notdetected at of above 25 ng/L. NO s Not quantifiable = Measured concentration between 25 noil, and the Limitof Quantitation (LOQ) which e SO ng/L. Exygen Research Page 22 o f 110 000045 Interim Report #I-Analysis of Oakdale Water Samples Exygen Study No.: P0001400 Table I. enyBOntP Summary of PFBS, PFHS, PFOS and PFOA in Water CIUM Sample ID Samples Continued Anatyt* Pound fppt, C4 Suifonat P fBS C t Sutforat PFHS CB Sutfonat PFOS CtAchfPFOA C0W 4475 C0064475 Rep C0064476 O K LM N -G W -W 31-0-05Q 309 OW.MN-GW-W31-04WO3O9* OKLMN-0W-W31-O-O5O3O9 Dup 1300 1360 1360 5130 4780 5190 132000 132000 156000 23100 22300 24900 C0084478 C0064478 Rep C0064479 OKLMN-GW-W324M5503Q9 O K LM N -GW -W 32-0-050309* OKLMN-GW-W32-0-050309 Dup C0064462 C 0064482R ep 00064483 O K LM N-GW -W 217-0-0 5 0 3 0 9 OKLMN-GW-W217-0-050309* OKLMN-GW-W217-0-050309 Dup C0064486 C0O64+B6Rep C0064487 C0064400 CC064490 R ep C0064491 O K LM N -G W -W 200B-0-05030S OKLMN-GW-VV2008-0-050309* OKLMN-GW-W2008-04150309 Dup OKLMN-GW-W2012-0-050300 OKLMN-GW-W2012-0-050309* OKLMN-GW -W 2012-0-050309 Dup 2180 2290 2960 ND ND ND 6780 7170 ' 6930 2210 1960 1920 3000 3120 2940 NO NO NO 10100 10800 10300 4700 4470 4420 47100 44400 83000 NQ NQ 128 15500 17800 18800 117000 118000 139000 117000 93300 125000 NQ NQ NQ 59300 58700 60300 48900 46400 51400 C0064494 C0064494 Rep C006449S OKLM N-GW -W 80-0050309 OKlM N^GW -W SO-0-050309* OKLMN-GW-W8O-O-050309 D tp NO NO ND ND ND ND ND ND . ND 302 250 328 00064498 00064498 Rep C0064499 C0064502 CDC64502 R ep C0064503 OKLMN-GW-PW1 -0-050310 OK LM N -G W -PW 1-0-050310* OKLMN-GW -PW 1-0-050310 Dup OKLM M -GW -PW 2-0-050310 O K LM N -G W -PW 2-0-060310* OKLMN-GW-PW2-O4KO310 D tp 5620 5650 5580 641 624 694 4180 4150 4170 '5 0 1 4 S I700 66900 71600 70900 351 383 303 37300 39300 39100 3630 3890 5160 C0064S06 CCC64S08 Rftp C0064507 C0064510 C0064510 Rep C0Q64511 C0064514 C0064S14 Rep 00064515 C0064818 C0064518 Rep C0064519 C0064522 CQ084522 Rp C0064523 C0064526 C0064528 Rep C006+527 OKLMN-GW-PW3-0-050310 OKLMN-GW-PW3-04350310* : OKIW N-GW -PW 34J-050310 D tp O K LM N -G W -PW 4-0-050310 OKLMN-GW-PW4-Q-050310* OKLMN-GW-PW4-0-060310 Dup . O K LM N -G W -PW 6-0-050310 OKLMN-GW-PW6-0-05GS10* : OKLMN-GW-PW8-0-0S0310 D up : : OKLMN-GW-PW10-0-050310 OKLMN-GW-PW10-0-050310* , OKLMN-GW-PW10-0-050310 DUR O KLM N-GW -PW 11 -0 0 5 0 3 1 0 OKLM N-GW -FW 11-Q-0503A 0* 0KLMN43W-RW11-0-050310 Dup OKLM N -SW -0-050310 OKLM N-SW -0-050310* OKLMN-SW -0-050310 Dup 6970 6740 6570 V 8130 7700 7810 7930 8000 8130 13100 12700 11900 . . 6520 6490 7150 NQ NQ NQ 10000 9740 9990 7690 7480 7550 14500 14600 14800 29200 27400 . 26800 8820 10000 8050 NQ NQ NQ 32700 25500 32300 33600 30300 27800 90000 86000 86400 1400000 1760000 1740000 40800 50600 43400 1190 1200 1270 177000 160000 176000 72100 67800 65900 76400 78700 78500 719000 781000 614000 60300 71600 60600 491 529 537 C0064530 OKLM N-GW -TRIP2-0 -0 5 0 3 1 0 ND ND ND ND 'Laooratary Duplica NO = Not detected at or abcrv25 ng/L. NQ * Not quantifiable = Maesurad concentration between 25 r>gfl- anq the Limit of Quantitation (IO C ) which ts 50 ng/L Exygen Research Page 23 of 110 000046 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No. : P0001400 Table EL Matrix Spike Recovery of PFBS and PFHS in Water Samples Sam ple Oeeeripti&n C* Sulfonate PFBS Amount Amt Found Amount Spiked In Sem ple Recovered R ic c v r y te u ~ - < *> Am ount S p ta d fotfL) C tSulfeeetePFH S Amt Found Am ount ft Sam pln Recovered fnofU Recovery m O K U # NGW -W S-O-OM S10 See c, aeoo ngn. Lb SpM O KLM N-G W .W 3-C-06W 10 ICboe444 * j * o, soooo r^n. Lab Spite) O KLM N -G W -W 34-050310 Low Sp ike 5 ppb fCOOeMOt. #900 AtfLFted Spite) O KLM N -G W -W 3-0-OW 31 D H igh S p fte 58 ppb (COMUffT, MOOP FM 0 Spite > 5000 90000 5000 50000 312 312 312 312 698Q 133 67400 ' 7450 134 143 74700 149 500C soooo 5000 50000 toe 162 182 182 5130 47500 5140 54400 09 55 100 100 OKLM fH#W -W 9~0-05031Q (COMMOt 3pk Ev.9000 apA. Lab spite) O fO JH N -W -IW -O -e W W fl 00*440 Sp* F. fm M fl*L Lte SpUwl O nU W M JW 'W S-0-05031a LOW Sp ike 9 ppb 00*4410. soot *i*L FWd Spite > O KU IM -GW -W B-0-OS0310 H igh S p ik e SO ppb fCOOeMtt. #0000 up. fWW Bpite) 5000 50000 500C SOOOO 67.0 S7. 57.0 67.0 7020 70000 7410 70500 139 5000 140 50000 147 5000 141 50000 ND SO SO ND 5120 51400 5610 53300 102 103 110 107 O KLM N -G W W 2*^'O5OS10 (C00*4412Ssh <X 6000 *p*. L*b Spite) OKLAIN-G W -W 28-0-DW 310 (C0M4412 SpS H. SOON n ?L tb Spite) O KLI4N-GW -W 26-0-060310 Low Sp ike 8 ppb {COOS4414.#100 npA. Fkild Spite ) O K L M N -G W W i-8 -O M J W H igh S p ik e ppb (coeewts, so n s p <l f m v ) 5000 50000 5000 60000 73400 73400 73400 73400 73 WO 125000 73200 147000 * 5000 222000 103 SOOOO 222000 5000 222000 147 socco 222000 207000 2S200Q 210000 266000 * ' O K LM N*GW -W 334)-OflGI1D <CP0*H1*spb 1,9000 rtgLU b S^kW O K L M N 'O W -W tt-8-050310 <0006441* $pn J, scoot ngfl. U b Spite) O KLM N-G W -W 33-(M l60310 L ow S p ik e 5 ppb <C006*4lt,5100up, F W S p ite ) M C LM M -SW -vm -O -O BM lO H igh S p ik e ppb (C006441*. 80000 ngft. FtWSpite ) 500C soooo 5000 50000 26000 26600 26600 26600 33600 133000 38700 106000 * 5000 92300 212 50000 92300 5000 92300 102 soooo 92300 78000 122000 65200 150000 59 115 O KU 4N -G W -W 20S-0-05C310 (C0004420 3 (* X. 000 ngtL Lib Spite } O KLM t^aW 'W 205-tM >B03l4 |COOM4 Spk L 40000 n/l Lab Spite) OKUWN-GW-W205<046G1310 LOW Sp ike 6 ppb CCMS44ZX W M tupft.rW d Spite ) OKLM H 4JVM N2O6-O4)W J10 M g h S p * e M ppb {COfl*4433<SOOOOft*1. Ft*W Spite > 5000 50000 sono 60000 8200 6260 8240 15400 72500 tsaoo 62800 143 5000 6740 126 soooo 740 130 soon 6740 149 50000 6740 12500 53100 11BOO 60600 115 93 101 108 O KLM N-3W -W 21 *-0-056318 (C006443* Sfk II, 9000 np<L U b Spite) 0KLM N -G W -W 21S-0-0M 31P (COOI4424 SpkN. H0 noli. Lab Spite ) O KLM M*OW-W21 w - e s o n s LOW sp ike 6 ppb (00004420, $400 S p ite ) 0XLM H -G W 4N 215 4-0*0 31 0 H ig h S p ike ppb <0000443/. 60000 04. Fbk* SpiM ) 5000 SOOOO 5000. soooo 001.0 7200 801.0 67200 01.0 , 6720 aot.o 669CO 128 5000 133 50000 118 5000 132 50000 76 769 760 769 5200 50300 240 48500 90 99 89 98 Saripie residue exceeds the spiking level sfeiUAcarnty; theretore, an w ain * * recovery value eaiwat be calculated ND * Not detected -at or above 25 nfifl- (ppt). N O - Noiquattfifiabl* M easured concentration between 25 ngA. (ppi) and the Limit of &i*nflta(tan (LOO) which fe SOng/L <ppt). Note: Since tht* eummary (able snow* rounded m u lt i, recovery v iIm may v*ry*Hhtty from the valu es n th * raw data. Exygen Research Page 24 of 110 000047 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: PQQG140O Table II. Matrix Spike Recovery of PFBS and PFHS in Water Samples Continued 3 * n ip l, O m crfD tlon AmGunt 9p#w d f a ' 1-) C4 S ulfonate PFB S Amt Found Amount In S em p le R eco v e re d R eco v ery lV L) tntfu w A m ount Spum i l"0 0 C6 Sulfonate PFH3 Amt Found A m ount to Sem ple R ecovered (n#ft.) f#A 4 R ecovery <%> OHLM N -<3W *W 20H W W 550310 (C M * Spie C .< ttO nflA .U b S pite | OKLMN43W4Y2O1O4W5O310 (CQMM42I Spk D. 0000 n * . t a b S pite) OKUAN-4W -W 201O-0-0W 510 L o w S p ik e 5 p p b (CM*490, <000 * . Fiate pike ) OKUMN-GW-W2D1 <M)-060310 H ig h S p ik e 50 p p b IO0NM31. MOCO FI*M S te te ) 5000 50000 5000 50000 NO NO NO NO osso 6B600 700 83600 132 5000 139 50000 134 5000 128 50000 NO ND ND NO 4800 46700 4700 43700 96 97 94 87 OKUM N-GW-PWT4MWOS10 (COOSMS2 Spk e.9000 ru p i U b S p lM I O K L M N -t SW -S * W 7 -C W )5 C S tO <CMM4J2 SfA f . IMOO n t f . t a b Spike) OKLMN-GW -PW 7-W JM510 L ow p ik e p p b (CBOftMM. soeo rtpL F w e Spika ) OKLMN-GW 'PW 7*<W XW 10 H igh S pStbS O p p b iCecsuas.aoocg n * . f* w s > u \ 5000 50000 5000 50000 4400 4400 4400 460 12200 72800 13200 00000 155 5000 137 50000 175 5000 151 5 0 0 0 0 4600 4600 4600 4800 10 50800 9370 59000 90 62 91 108 O K LU N -G W -TW P1-M 10210 Low S pike ppb CC00M4J7, O d PpL Raid S p ite ) O K L M N -G W -1R 1P1-041W 310 H ig h S p i t e SO p p b {CMWA43Sraooce a g l R eid Spike ) 500C 60000 NO NO 640 44400 131 5000 88 50000 ND NO 4600 46100 92 92 O K U H N -O W -fW M -W 0310 (C0004442 Sek G. 900e n * L U b S p ite \ O K L M N <Q M N PW 8^K I0310 (COOM442S{M H, FOQM nf/LUb S pite) OIOJWN43W W W W W W 1 0 L ow S p ik e 5 p p b 10000444. 0*0 f t * . Field S p ite > OKLMN*GW-f>YW-OOS031C H ig h S p lit 60 p p b (COOW445.90000 n * . F ted S p ite ) 5000 50000 5000 50000 13300 13300 13300 13300 21400 79700 21000 00700 162 5000 23000 133 50000 23600 154 5000 23800 135 50000 23800 29700 70300 30000 76100 118 93 124 105 QKLM N ^W rPW B-IHI60310 {C000444S Sfk I, SOOOnod. U b Spite ) OKLM N>GW ^W 9^^)60S1Q {CMieteM Spie J, 00000 n p L U b Spite ) O K LM H ^W -PV n-O O lD SIO L ow S p ik e s p p b icoep4o, seoe n * . FieidSpite ) O K U lH -G W W -O -o M w io H igh S pik e So p pb (00004441,90000 n t f . Field S p ite ) O K lJW N ^W -rttellkM i-M O M O 4COOS44SOSk K, MMOnbL U b Spfto > OKLM N-OW -W 01M ^-P5W 10 (COOM490 Spk L, 40000 R * . U b S p ite ) OKLJ4N45W<W61G24L066!I10 Lo w S p ik e 5 p p b {C0M44K, 6003 K * . F te d S p ite | OKXMN-GW Vyei02-CH>50ait H igh S plit 90 p p b IC0M4433, OOQOO n t f . FUM S p ite I 5000 50000 5000 50000 5000 50000 5000 50000 2110 2110 2110 2110 NQ NQ NQ NQ 0200 66000 9200 74800 7360 67500 7120 70700 144 SOO 5160 134 50000 6160 144 5000 5180 146 50000 5180 147 5000 135 50000 142 5000 141 50000 ND ND ND ND 9310 64400 9350 54800 4890 47400 5040 50600 83 90 84 99 98 95 101 101 *Sarr*>e reeidue exceeds the piking level geMesnSy; ff*refer, m accurate recovery value carro t be catenated NO * Not detected at or above 25 npMPPONQ a Not Quantifiable = Measured ooncertfraftofl between 25 ncrt. (ppt) m d the UtrU ot Quantttattan (LOQ) which Is $0 n * L (ppt). Note: Since this sum m ary table m o w s rounded results, recovery vsluee may vary eHgmty 1rm t i e values in th e raw dat& Exygen Research Page 25 of 110 000048 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table II. Matrix Spike Recovery of PFBS and PFHS in Water Samples Continued Sam p i* D escription 4 Sulfonate P F B S Amount Am tFound Am ount Spiked in Sam ple Recovered RCOvw y (n flit) t e U .. !niU _ (*) Am auflt Sp ite d ew C t Sulfonate P F K $ Am tFound Am ount in Sam ple Recovered Recovery (noJU (nfl/U (*> O K LM N -O W -W tl04-P -O SW 9 {C06M454 9fei U. 90*0 004. Ufo Seite I O K L M fW 5 W -w io * s io [C m U U Sp K K , IM M elLUrtSptt) O K LM N-OW -W M 0 *0 4 1 D L ow Splka 5 ppb (C0N44M ,M M n^LFIaM Spite) O KLM hM 3W -W 1IW -tM tKi3ia H lflh Sp ik e W ipph (COOtetfZ.800W nfeL PWd Belte I 5000 50000 5000 50000 NQ NQ NQ NQ 6680 73000 730 60700 134 SOOO 146 50000 135 5000 139 50000 NO NO NO NO 5050 48000 4720 51200 101 96 04 102 O K LM N-QW -W 201-C-06W 70 (CoosMSa Spk c, woo r * L ta b le > O K LM N-GW-VVA201-0-O5PM0 (C004+4M Spk 0. sote ngfl U b afoe) O K LM hW 3W -W 01-<M SW lO Low Spike 0 ppb (CttSitefl, SM noA.nate Spite > OW J4fW 3W *V82P1-0-050319H lflb Spike 5 ppb (COOM4S1.fOM npfl. FieldSpite } SGOO 50000 500 5000 74.0 74.0 74.0 74.0 6580 65500 077 7550 130 3000 131 60000 121 500 150 000 NO NO NO ND 4610 44400 543 5360 92 6 109 106 OKLM N-GW -W 20--0330t (Ce047 Spk E.seoe n^L LSb SHte ) 0KLM N-G W -W 20-0- 60300 (COOiaUTSex MOOOnyTLU b BfeM ) OKLW N-W -W 2O-O-O0M09 L ow Sp r* 9 ppb (C M M M I. 5D0S t&L TiaM Spite ) OKUW 4*GW *W 2D*0*0503M HtQil S p lk a M ppb tCOOMm,900M s^ L FUI Spite ) 5000 50000 5000 soooo 13000 13900 13900 13900 19400 77100 20900 85000 110 5000 12900 126 50000 12900 140 SOOO 12900 142 50000 12900 16200 56200 16200 48400 66 85 66 71 OKLM N -G W -W 32-M 503 (C0Q04O1 Spa C, 0000 nfrt.U b Spite ) OKLM N-W -W 22-0-&5IM O {COO94471 SJM -H.90000 r^ L Leb Sette) O tO JflN -6V W 24-O S030 LOW S p A * 5 ppb (CMSMtt, 5000 r*JL FWd Spite > O K LM N -G W <W 224*0603M H lflh Sp lka 50 ppb (000*4474, SMMO npL Flete Spite ) O KLM N-G W -W 31 0*050509 (C6044473 Spfc 1,9000 npLLab Spite ) O KU M K-G W -W St-lV O SO (CaeewT* Spk J, eneo - Ufo Spite | OKLM M -OW -W S1 -0-050309 H igh Sp ike SO ppb IC0094477. MOOO nglL FteW Spite > 5000 50000 5000 50000 5000 60000 60000 36800 36600 36600 36600 1300 1300 1300 44100 109000 44000 111000 0450 70500 90900 * 5000 31400 145 50000 31400 5000 31400 149 50000 31400 143 5000 5130 138 50000 5130 179 50000 5130 37000 73003 35000 62203 9090 51200 63200 83 62 70 92 110 0KLM N-G W -W 32-0-D5O M 9 <C9CM47 Spk K, SOOO*0. U B Sptte } O KLM N GW -W 32-0-05040 (C00e47B Spk L,50000 np/l.U b Spite) O KU UM -G W -W 324M H 030 Low Spike 5 ppb (COOS4UO.09 i*fl. FieldSpite ) 0KU U M *Q W -W 32-(M U 0 H lflh Sp ike 50 ppb {C00MU1,50000 A p t FtedSpite | sooo 50000 5000 50000 21*0 2160 2180 2180 0910 67300 10800 66500 136 5000 3000 130 50000 3000 172 5000 3000 127 60000 3000 7400 SOOOO 71C 52600 66 94 96 100 resid* exceeds Ihe level iprtiteantN: therefore. an accurate recovery value carsI'd be cdcuated ND Not detected at or beve 25 neA*<PPb NQ Not quantSatte Meeeured cOTcantrartton between 25 rVL (ppl) end the Umrt at Ojentlteton (LOQ) wNd> W ny/L (ppt). Note; Since thie summary feble show* rounded rssulfe recovery value* may vary styhWy from the values to the raw data. Exygen Research Page 26 o f 110 000049 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table II. Matrix Spike Recovery of PFBS and PFHS in Water Samples Continued Sam ple O ncriotka Amount SpiXKl t>QX) C4 Sulfonate PFBS I I Am M t m Stm pI* Recovered Recovery NW <u <%) Amount S p in e l (mUL) C9 Suifenete PFHS Amt fo u n d Amount M Sim pl ( 0 Fecovw id R ucw w y tn # X ) ... J%) O K LW W 3W -V IM 74>W iCOOeMI2$pkM.MOQnrLlafa Seim} QKLMN-OW-W217-0-06MM (Cm m j m pk hs t o m an. u b spim > OKU4kKlW.W217-<I.ASMO L ow S p lln p p b Field 3pM*| OKLMN-aW-W217-0-OM30* H fch S p ik e SO p p b (CMM4M. 60* eeV FteW Spite 1 5000 50000 5000 50000 NO ND ND NO 6680 86800 7570 71200 134 5000 134 50000 151 5000 142 50000 ND NO ND ND 4880 46500 4590 51300 as 93 92 103 OKU4N-QW-W2O0-0-OW5W ICCW44Ms*i( a . w # na. u b seine > OKLMN-OW-mOOe-O-OMMS C40*UM Spit P, 9000* Bflrt. U b Spike) 0KU4N-GW -W 2MW 4-MU0t Low Splk 5 ppb (ce*M*w> npw Beni s p n ) OKLMN-GW-W20M-0^33OS Hlfl h S p ik e 60 p p b tCOOM*. MOOnILFWfcl M W ) 5000 soaoo 5000 50000 78 6780 67S0 6780 14300 73800 18500 6T9QQ 150 6000 i o n 134 50000 10100 194 5000 10100 182 50000 10100 16000 56500 16300 84000 its 93 184 109 OKLMN^3W-W2IH3'O*OSO300 (co m tm ip k C .W C o eA U 5 * to i OK LM N -G W -V #20i2^-0503M (Caosetet 8p* 0, nooe a p t te e ipwe > 0 K U IN 4 W '-m S 1 2 - 4 3 m Low S p in 5 ppb {CO0M4CLSOM npft. Reid Spite) O K U IN 4 3 W -M a tt-0 4 H K HJph Splk* SO p p b (C M *, WOODn p t Held Spike} .5000 50000 5000 50000 2210 8800 2210. 1 66400 2210 8210 2210 71500 132 , 30 00 128 50000 120 5000 138 50000 4700 4700 4700 4700 6140 46900 6960 53800 88 84 8$ 96 OKLMN-GW-VWO-0-05030 {CWWW spk e, OM npl U P SpWcf * 5000 ND 850 137 5000 ND 4960 too OKUHH-GWWttO"*-a63W {COOeMM Spk F, 90MDne*LU b Bplhe) OK1JMN-CM'WD4M>HOS L ew S p ik e 5 p p b {CMM4U. SOMA<pLRete Spike ) 0KLMR<OW'WMMHtS030ft Hlffh S p ik e W p p b tcoeeewr. m m * neo. nwe t b m > 30000 5000 50C00 ND NO ND 64700 7380 ,f 88700 12B 50000 148 5000 139 50000 ND NO ND 46200 5200 40200 92 104 98 0KLM H-QW W 1*0-0503 icsMMei Spec, n ee n ev u ib *pn) O K LM ^W -PW 1-0-0<W 10 SM U I* Spfc R 80000 nfH. U b Spike) OKLMN-OW-PWI-O-OSOSM L e w S p ik e 6 p p b (00004400, 9000 R*Jd Spite ) 0KLMN-0W-PW1-0-06030 High Spike 0 ppb (CMM901, W npA. FleWISpfce ) sooo 50000 5000 50000 5B20 5020 r 5620 5620 13800 77000 13100 69700! 160 5000 4160 133 50000 4180 150 5000 4180 128 50000 4160 8880 52000 7690 47700 94 96 71 87 OKLMN-QW-PW2*0*050310 <C0M4Stt2 Spk i.eaMnpALabSpte} OKU4N-GW-PW2-0-06310 {CMMI02 3f* J, 60000 ft*L U b Spite > OKLMN-qW -PW 2-0-e310 Low Spike S ppb (C0M4SU4. StM up*. Reid Spite > OKLMN-OW-PWi-S-OSDSIfl High S p * SO p p b {C0e*4d0S. 40000 np*. Field Spite ) 5000 641 50000 641 s o a r - 641 50000 641 7720 65900 7030 64300 142 5000 131 50000 126 5000 127 50000 51 501 501 501 5280 47700 5190 44300 95 94 94 88 'Sample residue weed* (he piting level eigniAeanl^; therefore, en curate recovery value, cannot be calculated nd * NotQetecteCitoratcve 25 r>giL {ppt>. MQ a htotquandMbieBMeeeur3<aoncentretori between 25 no^Lfppti and the limit at Q usntbtkw <LOQ} vhlch i> SOng/L (ppfi. Mote: Since tM i eummefy tib i sbow e rounded result*, recovery value* may vary*l>gfttly from the valve* In ih* **** data. Exygen Research Page 27 o f 110 000050 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study Np.: P0001400 Table II. Matrix Spike Recovery of PFBS and PFHS in Water Samples Continued Sam ple D eo crlo d o n Amount $pik*d (nD C4 8utfofiata PFBS Amt Found Amount in Sam pi* ROCOVWWl R eco v ery tno/L) (%> A m ount Spiked {no"-} C6 Sulfonate PFHS Amt Found Amount In S a m p I* R ecov--w j R ecovery (*U (%> OtOMN-GW-PVWW-060310 (COOMH* 9pfc K.WM no. UO Spike) OK LK N *G W -FW 3-0-0m it (000645 *pk U WeOOa*A. Lab Spike) O K LM N -6W -FW 34460310 LOW 8 p lk * 6 p p b {COOMCM. BOO# ng/L FieM Spike > OKUMN-GW-PWa-lWJWJiO H ig h S p lk * SO p p b {COOMSQ6, $ 0 0 e*CField Spike) 5000 soooo 5000 50000 9970 8970 6970 6070 13800 86900 15200 92300 137 5000 10QQ0 180 50000 10000 165 5000 ` 1QOOO 171 50000 10000 13600 54400 16300 54900 72 69 126 9C 0KL M N -G W -P W 4-04H S 10 {COQMSII Spfc M, 5000 nofL Lab Spike) 0 KUVtN-GW-fW4-(M>5OS10 icoowci o Sait h. #oeoe av l Lab spoie) OKLMN-GW-PW4-9-4W310 Low Split* 5 p p b (C0C645M, seoo n*/L FMd Spike) OKLMN-CW-PW4-0-050310 High S p * e 00 p p b (OOOW91a. 500 ikpL. New Spike) 5000 50000 9000 50000 8130 8130 8130 8130 17400 95000 16300 86900 105 5000 7 0 174 5 0 0 0 0 7 8 163 5000 7690 162 50000 7690 13900 53600 13500 58200 120 91 112 101 DKLMN-GW-PWS-04B0SI0 {C0M4M4 SpkO, SOMa*#L La* Spite } OKLMN-OW-PWS-tWSWIO <CMM514 Spit W,M#oa n y t U b Spike) O K LM FW JW -PW W -0KJ10 LOW S p tk * 0 p p b (0044514. 9000 ng&. Flekf Spike) OKLMN-GW-PW6-0-060310 H ig h SpUt* SOp p b (C0M4M7 .80000 n p l Held Spike) 5000 50000 5000 50000 7930 793C 7330 7930 17200 90500 17100 94600 185 5000 14500 166 50000 1450Q 183 5000 14500 173 50000 14500 20600 58800 20800 59400 122 66 128 OKLM N-GW-PW10-6-0*031 D fCMMrt SpkCrSflognan. u * spue) OKLM N-GW-PW1 0-0-050310 00*4*14 Spk fc S0M0 npA. U h Spike) OKLMH-GW-PWi 0-<M)60310 L ow S p ik e 5 p p b (CBOM83#, 6WOhq/L FId4 Spike) (MOM N-aw-mift'O-CSOSIQ High Spik# 50 ppb (CDO44021.SIXMOi # l FWd Spike ) 5000 50000 5000 50000 13100 13100 13100 13100 19300 70700 19000 74000 124 5000 29200 133 50000 29200 11S 5000 29200 122 50000 29200 34300 71000 33500 71300 102 04 06 54 0K1MN-GW-PW11-G-M031Q (COCMKZSpit E, MW npL Leb Spike ) OKLMN-GW-PW11 -O-DSOJI0 (COOMI215pk A, <9400 ngrt. LN>Spike) OKLMN-GW-PW11-C-050310 Low Spike 5 p p b 4000*41, W -sA PM* *plk*) OKLMN-GW-PW114)450310 Hlgh Split* 0 ppb icoOO40SS. 500*0 ng/L Field Spike) 5000 SOOOO 5000 50000 6520 6520 6520 520 12700 66300 13200 63600 124 5000 8620 124 50000 8820 134 5000 8S20 114 50000 8820 14200 65100 13300 54800 100 93 90 92 'Semple r e e tt* excaede the spiting level irgi*fican#y; fterefere, an accurate recovery value cannot be calculated NO Not detected a t or above 25 K^L iptf). N O * Not quaniiftebi* Measured concertarifon between 25 ng/t (ppt) * * 4 the UmR of Q uartflM un 4LOO) which is 50 ngfl. {ppt). Nook Since th is a u m n w y Ubie show rounded reeu te, recovery value* mey vary nightly from dt* value In ib# raw data. Exygen Research Page 28 of 110 000051 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table II. Matrix Spike Recovery of PFBS and PFHS In Water Samples Continued Sam pl* P-crtP*" C* Sulfonate PFBS Amount Amt Found Amount Spfltad In Sam plo RocovoroO R oeovoiy tW W t*> A m ount S p fta d ("A) C * SuHb m I P FH S Amt Found Amount in SM ipio (") Rocovorad Rocom ry (*) OKLW N-5W ^080310 {Cooeme apa o . saoo n p i u rn 9po > O laM N oSW -o-afio& io (C0M4S33 Byh H, 90000 nglL Lab Spike ) OKLM N^^O-OCaaiO Low S pike 5 ppb (cooewo,K spu ) OKLUN-SWO-OBW^O HlQb S p f c t BD p p b tC0**4$Za. 4OM0 FUid SpMw) 5000 50000 5000 50000 NQ NO NQ NQ 5900 63000 7260 65000 120 6000 12S 50000 145 5000 130 50000 NO NQ NQ NQ 4790 45100 52SO 49400 96 00 105 SO OKLMN-aW-TNlP2-0-06fl3lO L o w S pike 5 p pb (CC0*6n. 9000 DOS.SpllUk ) DRUMN-<jyy-TRIP2*006031 o H igh s p ik e SO p p b (00*04332. WO n U l k | I 500C 50000 NO NO 4460 20100 90 5000 NO 50000 NQ 4970 49000 90 SB Avenge: S ten d er Deviation: 141 21 `Sample residue exceeds t w spWr t a e l e&rtkcarttf, tberetore, an accurate itcovety value cannot be calculated NO ^Md(Heeted<<>rauM25noA-<PPt}NQ Not tpjentflaw - M ured conoefitr^ior* between 2Srttf.(ppQ and fee Limit of QuM ttaawt (LOO) w ncn s do oq/l (ppi). Note; Mace bite aummary UbW hmve rounded neoH e, recovery value* may vxryiUgMty from Uievelu-- In the raw det*. Avtm tw : StM t4vd D w iaU am a 16 lllfllliv- EXygen Research Page 29 o f 110 000052 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table III. Matrix Spike Recovery of PFOS and PFOA in Water Samples Sam ple D escription OKLMN-GW-WWJ-03O310 {C0DS44O4SafeC. COSOIttfL uta Spike ) OKLMN-GW-W3-0-C5O310 (Coset Ipfc P. SWOTngflUP Spate) OKLMN-GW-W3-0-OSOMO L o w S p ik e 5 p p b (CW4449*,50Wflel Ft Sdite) OKLMN-GW-W34HJ50310 High S pike 50 p pb ICSO4440?, m o m gii.fw **pjw i C8 SuHonete PFOS Am ount A m t Found Ammani Amount SpO ted I n S a m p la R a c o v a ra d R a c o v w y SpikMT w (ng*U C9 Add PFOA Amt Found Amount In Sam ple Racovam d n L> (nom R aeo v ary (%) 5000 50000 5000 soooo 4750 4750 4750 4760 12400 73500 10800 84500 153 5000 135 50000 123 5000 160 50000 6330 8330 330 6330 11900 59200 9470 40100 111 106 63 80 OKdkkGW -W t-0-050310 [Co sm o 3ek f , aooo ngu, u b spike ) OKLM K-G -V tt-C-050315 (CWM4M f t * F, MOO*neTLUb Spite) OKLM N-GW -W J4 -0 S 0 3 10 L o w S p ik e J p p b ICOMtMS, COOSnp&.R**d Sphw ) QKLMN-GW-WS-o-OSiiS'lO H ig h S p ik e 0 p p b <CQ0S441t. MOP ngiu nradpOv ) 5000 50000 5000 50000 69.0 59.0 59-0 59.0 4940 55000 5380 50500 99 5000 110 50000 106 5000 101 50000 290 280 290 290 5350 51800 6050 33900 101 103 115 77 O K LM N (SW 'W 2t-0-05O 3i0 {CPM44t2Spk 6 , COMngfLU b 9 * te ) 5000 13500000 9450000 * 5000 79300000 66300000 0KUUN^W 'W 26-<HUO31O (0WM4iSFfcH,seeeene*. u b b rfh i) 50000 13SOOO 7390000 $0000 79300000 68300000 OKLMN-GW-W2-0-0W310 Low Spike 9 ppb (CM44414. MOOrttyt Field 9pHn ) 5000 13500000 9050000 - 5000 79300000 73100000 OKLMN-GW-W28-0-C50310 H igh S pike 50 p p b (COMMIT SOCOCngfL OM Spike j 50000 13500000 7210000 50000 79300000 57900000 OKUWN-GW-WJWr-OMJIO |C0aM1gpt 1, 0 0 ngA.U b S p ite ) 5000 4610000 4720000 . 5000 1750000 1520000 OKLMN-OW-W3J-0-OSOJ10 [COOQMtSSpkJ. SOM nolLUbSpih) 50000 4510000 4730000 50000 1750000 1650000 0KUUN-GW-W31*0-050310 L ow S p ik e S p p b {OoosMte, soaiL fi* Sfris > SOOO 4610000 4820000 . 5000 1750000 2350000 OKLMN-GW -W M-0-05M10 H igh SpOte 5 0 p p b {COO0441. HOPOi p l FMd Spite ) 5000D 4510000 4520000 50000 1750000 1630000 OKLMN-GW-VY205-0-03W10 (OM 44M SpK K. SOM *qlLLib Spi*) OKLMN-GW-WJOS4L050S10 [CoeeMaaSpki-, rT ipa.u& 4pte i OKLMH-GW-W206-0-0W310 L ow S pike 8 ppb ICW4MM, SOWnftO. Field Spite ) CKLM N-G**W 2054W $f0 W lS p ito e ppb (CaceMaa. sao qil fw <i saw *} 5000 50000 5000 50000 145000 145000 146000 148000 136000 156000 129000 221000 . SOOO 147000 20 soooo 147000 * 5000 147000 150 50000 147000 160000 190000 14300) 164000 . 66 * 74 OKLMN-GW.WJ15 -0050310 <COWMMSpkM. SMS [*L UbSpik* ) OKLMN-GW -W 215-0*080310 SpfcN. 5000 flpIL U b SpiM ) OKLMN-GW-W21S41-05031Q L ow S pike 5 p pb jCftOeMM, Ftets Spite I OKLMN-GW-W215-0-050310 High Spike 50 p p b (C0Q044S7. MOWnpL FMtf S p ite} 5000 50000 6000 soooo 37100 37100 37100 37100 52400 96900 66600 101000 * 5000 120 50000 . 5000 128 50000 4400 4400 4400 4400 8850 56700 9860 33200 09 105 85 70 Sample residua exceeds the spiking level significantly, therefore, an accuraterecovery value cannotbe calculated NO Notdetected at or above 25 ngA.(ppt| n q Nol Quantifiable * Measured concentration between 25 ng,t {ppt}and the Umit erf Quantitation (LOQ) which is 50 ngL (ppO Note: Since ihl eummary tab) shows rounded results, recovery values mayvary slightly from the values in the raw data. Exygen Research Page 30 of 110 000053 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table HI Matrix Spike Recovery of PFOS and PFOA in Water Samples Continued S w npJ* O afcrip tiO f Amount Spiked (n tfD li! {a C8SulfonalPF0S Amount Amount R so o v sn d Recovery Spiked (gm?______ c a _____ fc&o-) Amt Found in S im p le ("fl-) C l Acid PFOA Amount R ico v eraci R ecovery <%> O KLM N-GW -W 2O 1O -O -06M 1O (C a to H zs apitCn so m &pflu b e p > OKLM N-OW-W2010-0-050310 |C M M 4at 9 |* o. AMO otfts La > QKLMN-GW-W2010-0-050310 L ow S plke 9 pp b {C0QM430, M S *<*. FU N I 8pik* ) O KLM N -O W ttN 201 170-040310 Hlflt S p M SO p p b {CMW 44H, s o m boa. f m #i pii ) 5000 - 50000 5000 30000 . ND NO NO NO 5170 54600 5270 54800 103 500C 109 50000 105 5000 110 50000 NQ NQ NQ NQ 5290 54300 4710 32300 106 108 94 85 OKU*M -GW 4W -^<W 50310 (C ow H tt * * c, * u * *p* > OKLM N-GW -PW 7-0-050310 (0909# #91 Sptl F. M S bb*>U b df#m ) OKLMN-GW-PW7-04W0318 L ow S pfc S p p b (C ern # , o o n e ^ F ip d 8pnt* > OKLM N 43W -PW 7-0-05W 10 H ig h A pik SOp p b (C0M M 35, S09M n ^ L F*H S O p to > So d o 50000 5000 60000 7ieoo 71600 71600 71600 78500 110000 72600 118000 6000 95 50000 < 5000 89 50000 37800 37600 37600 37600 41900 88100 42800 87100 . 97 . 59 0KLM N -G W -TTO P1 -0-050310 L o w S p lk e S pp b (00044437, SO M np L Ftakl Spilla ) OKUKM -GW-TRJP14WI50310 H ig h S p ili 59 ppb (01094499. MODO A p i. P b ld 8pMb > 5000 50000 ND ND 5700 535D 116 5000 107 50000 ND ND 5360 50500 107 101 OKLM N -G W -P W I-< M 01 1 0 (CM444U tp k G, EMOngfl. Lab SfUt. ) QKXMN'GWPVWM>O5031O (CD0M4413pb H, 9MM ftflit Lab tpM n I - OK LM N-GW *PV4Hto10 U w Splk* S ppb (00944444, M O in p lL Ffekl 8 p u * ) O KLM N -G W -P W S-0-030310 H igh S p i * SO ppb (C000444C. 804C0 npL FiaM 9ptk* ) 5000 50000 5000 50000 34300 34300 34300 34300 38500 89800 38400 63100 5000 m 50000 - 5000 166 50000 81400 61400 81400 81400 61000 113000 59300 82200 103 42 OKUI4W-PVWW W W 0310 (CC044444 Spk 1. OMOnpA U b Opfci 1 OKLM M-GW-PW9-O-O50J1 0 (09094448 $pk 4, S0999rtpA. U M fp H ) OKLMN-GW-PWP^WWOa+O L o w S p tt 5 p p b (C094444*. 9900igA. FWW 8ptka ) aK U U M -G W -PW b-0-050310 H ig h S p i SO pp b tCPP4M#a, eoe n e i. fu ae > OKLM N-GW-W6102-0-050310 (C00944M SpK K, SOM ap L Lab Sfrik > OKUH4CW -W 810Z-0-05W 10 (c w a w * p u . m o n o , u n Stami OKLM N-GW -W eiO2 '0 -0 W 1 0 L o w S p tk e 5 p p b |COO44413.9900 f t ? l Ft*M 9* i# 5 OKLUH-GW -W S102-0-050310HlQhSplk8 50ppt> (C 0M 44M , JMM npL Plaid SpUoi | 5000 50000 5000 $0000 5000 50000 5000 50000 84400 84400 84400 6X400 NQ NQ NQ NQ 83200 136000 98400 176000 5300 55800 5460 53200 5000 107 50000 - 5000 m 90000 106 5000 112 50000 110 5000 106 50000 40000 49000 49000 49000 214 214 214 214 50400 97900 55200 93200 5880 52700 5610 35300 . 96 88 113 105 108 70 Sample ratldua ax caad t tha afiikinQ levs! aipnlflcantiy. tharalorn. an accurate recovery vahra cannot be calculated MO - Notdatectnd a to r abcwo26 ng/L (ppt). NQ = Not quantnabta Maaaured concentration behmnn 25 nglL (ppt) and the U nit of Quantilation (LOQ) wHdi ia 50 n oM ppt)Mctt: Since Blit nummary tibia thaw s rounded raatdte.tscovtry valuta may vary aBohfly tram tha valuta In thn raw data. Exygen Research Page 31 of 110 000054 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table III. Matrix Spike Recovery of PFOS and PFOA in Water Samples Continued Sam ple D escrfcU o n CI Sulfonate PFOS Amount Pant Found A m ount Amount Spiked hi S am p le R eco v ered R ecovery S piked W4 ______ m m ______ r w _ _ man.) CS A dd PFOA Amt Found Amount In Sam ple R ecovered noto * [nglL) R eco v ery m QKLN-GW-WS1O<LO-QSC310 (OMM4S4 Sah M9MWAert. U b S p fte ) 0K L W hW 3W -W f104-0-05C 310 (C0M44S4 Spk H, MOC ngfl. Lab Spike > OKLMN~GW -W 91W -0-050310 L o w S p ik e 5 p p b (C00U 4M. BOMngtLFMd SpHw1 OKLMN-GW-W6104-0-C5031 H igh S p ik e 50 p p b <0*4*4*17, cm m n t. fu m Sp* 1 5000 50000 5000 50000 109 109 109 109 5540 59100 5700 56700 108 5000 116 50000 112 5000 113 5 0 000 207 207 207 207 5290 57300 5470 35800 102 114 105 71 OKLN*<3W -W 1201*0-050310 ICM444M 9pk C, 9000non U ti Spite) O K LM N -G W -W S201-0-030310 (OM444Ct Spit 0. MOMn p L Lab Spike J 0KU4N43W-W821-0-050310 L ow S pike 0.5 p p b (CMfrMtt, m n pLFM d Spike) OKLMF<KaW*WS2014 4 5 0 3 1 0 H ig h S p lk 5 p p b (C9M4441. 9 0 f tp ! FWd Spike) 5000 50000 500 5000 NQ NQ NQ NQ 49B0 50000 670 9000 10Q 5 0 0 0 100 50000 134 500 132 5000 95.5 95.5 9 5 JS 95.5 4950 50800 605 6130 97 10T 102 121 QKLM NW 3W -W20-S- 0 5 0 3 0 9 (C00I4447 Spk E. MOOngn. u e Spue > OKLN hM5W*W204-09M0S |CCde47SptcF. to t nplLLabSpike} OKLMW-GW-W20-O-OSWO9 L o w S p ik e 5 p p b fC40f44M, SPMns/t Field S pite) Q K L M N -G W -W 20445090 H ig h S p ik e SO p p b (CMU470. MOMnot Field S uite) 5000 50000 5000 50000 46600 49800 46600 46800 49900 92800 41900 59500 5000 285000 92 50000 285000 5000 285000 20 50000 285000 289000 235000 278000 264000 0K L M N -G W -W 22-0-0 3 0 3 0 9 Spk 0 , SAMftpft. Leb Spike) O K LM N -G W -W & 44SO SO {C0M44T13j* H, SOHNAtfL Lab SptM J OKLM M 43*<W 2244H30* Low Spike 5 ppb (C0M4473, MOO ng/L Field Spike) O K L M N -G W -W 2 2 4 4 5 0 3 H ig h S p ik e SO p p b (CW44474,30000 n tf. FM d Spike) O K L M N -G W -W 31445Q 309 (CMM47S Spk L SOMn&L U * S p M ) OKLMkMeW-Wai4 4 5 0 3 0 9 90*44759* 4, MMflntfL Ufa Spite) OKUMN-aW-WS1 4 4 BOSOS High Spike SO ppb (06044477, MOMftpfL Field Spike) 5000 50000 5000 50000 45000 45000 45000 45800 5000 132000 50000 50000 132000 132000 44600 99500 41200 66800 116000 160000 216000 * 5000 317000 105 50000 317000 - 5000 317000 40 50000 317000 . 5000 23100 72 50000 168 50000 23100 23100 33000C 412000 324000 286000 26400 71300 65700 96 85 0KLMN-GW -W 32443DW 9 {COOM47SpkK. M0nek. Leb 8pte ) 5000 47100 62200 * 5000 117000 t3K LM H <W -W 3244S0309 (CM4M74Spk U MOM n * L LabSpdte) 50000 47100 115000 138 50000 117000 OK LiW 5W -W 334450309 Low Spice 5 ppb (CftOOUM, MM 1TLFteM SpOt*) 6000 47100 74000 5000 117000 KLMN-GW-WS2-6-O5M0 H igh S p ice 50 p p b (CM4ttt, MPMnelL FMd Spike) 50000 47100 120000 148 50000 117000 109000 151000 131000 1S70QQ * Sample residue exceed the spiking level significantly, therefore, an accurate recovery value cannot be calculated ND 3 Notdetected a lo r above 25 ngA (ppt}. NQ * Noi quantifiable - Measured concentration between 25 ngA (ppt) and the Llmh of Quantitation (LOQ) vrfticfo le 50 ng/L (ppt). Note: Since i d * ummarylaW sh o w rounded result, recovery value may vary HgMiy from the value In the raw date. Exygen Research Page 32 o f 110 000055 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P00OI400 Table III. Matrix Spike Recovery of PFGS and PFOA in Water Samples Continued Sample Oeecrtotkm OKLMN-GWW217-0-tiM3M tceeeeeu si*m ,eaeo ngitu e Spa i OKLMN*GW-W217-0-050309 fcaeeeeiaSe* n .seesBflfliLebsc) O K U M U 3 W A V 2 i 7 O S 0 3 M L o w Splka 5 ppb (Cowim. r *w spe* > OKLMK-<SW-Wai7-M50J09 Hlflk Splka SO ppb {Oboeeea^ s m m no.F W d Sew) Cl Sulfonate PFOS C l Acid PFOA Amoutt Amt Found Amount Amount Amt Found Amount Splkad kl Sawpl* Recovered Recovery Spliced kiSampln Recovered ("VU O W ' D .frtf______ & } ____ i S & L ... ("STM (tlBrt.) 5000 50000 5000 50000 NQ NQ NQ NQ 4790 700 5900 65300 96 5000 99 50000 116 5000 131 50000 NQ NQ NQ NQ 4880 52200 4880 42600 OKLMN-GW-W2OOB-O-OWd09 (COWMM SekO.000 &.LSb SgUe \ OKLMN-QW^f2D08490M* (Ceee44ese a,aowe nn.taban 1 OKLMN-GW-WaMS-<M)M309 L o w Splk* 5 ppb <C0MMM. SWOaa'LFWO SOM) O K L M N-GW^V2004m50je HlflhSpJk* M ppb (COeMe, soeoeneiLfieldSoftie) SQOQ 50000 6000 50000 1550Q 15500 15500 15500 2Q800 69300 77000 71300 109 5000 108 50000 230 5000 t12 50000 59300 59300 59300 59300 04900 114000 73600 94800 OK1^N-<3W'W2O12-O-O5C309 <c o m 4S*Sj* c,sooo non.m e Spike) 500C 117000 143000 * 5000 46900 QKU*N-GW-W2013WK>50ai <cob<iiso See D,eooco g i u b spitwj SOOOO 117000 185000 138 50000 46900 OKLMN-GW-W201 2-4W6M00 L o w 8pfce 3 ppb fCOfliMMt, MMfteLFfeM Spike) 5000 -117000 . 115000 ' 5000 . 46900 OKLMN-<3W-W2012-0*050309 High Spike 90 ppb (00004403.MOMneA. FleM SpOn) S0D00 -117000 203000 172 50000 46900 57700 94700 48500 69500 OKLNN-GW-WSO'O-OMSO {C0664464Spfcfe,M M neALe* Spike) OKLM)NGW-WS0.M503O {CB0044M $pk r,90000epL U b Spfee) O KLWffGW-WSO-O^MSOO L o w Spice 5 ppb toeeeMee.om ngn.n d e spam) OKLMN-GW-W8O-<K0309 HlfihSplk* 50 ppb {CMS44t9, M M o nee.fieldOpto*> 5000 V 'ND 50000 '"'NO '5000 NO; '50000 ND 5280 52900 5720 57600 106 5000 106 50000 114' 5000 115 50900 302 302 302 302 5910 53100 5880 42200 OKLMNK5W>4*WHK0310 (000*440tp k G,M04 ngILm b Spike) OKLMN-GW-PW1-O-&50J10 (00004400 SfcK.M O M n*L Lab StflW) OKLMN-GW-PW1-0-050310 Lo w Spike 5 ppb 4CDM400C, 00 ngrvnote spot> QKLIAN-GW-PW1 *0*050310 HlQh Splk SO PPb (C0MCM1. 00600 BO* FWcl OpU ) 5000 66900 50000 ` *66900 500C 66S00 SOOOO 66900 72000 116000 96900 '95200 -T 5000 102 50000 5000 57 SOOOO 37300 37300 37300 37300 47700 90200 40400 80500 OKLN-GW^W20-05031<r (COOMMt i,M60 ng/L Lab Splka> 5000 351 5490 , 103 sobo OKLMN-GVV-FW2-0-9S0310 (CQ0045Q2Spfc4.0000 ngA.Lak Spike) 50000 351 59000 119 50000 Q K LMN-GW-PW2-M50310 L o w Splk* S ppb {C60eU64r90M ege.F1M Spite3 5000 . . .35.7 . 4280, 79 5000 QKLMK-GW*FW2-O'Q9031<l Hlgb Spike SO ppb (C0004MB, BOOM apA.F M4 tpH* ) 50000 351 40500 50 SOOOO 3630 3830 3630 3630 8720 58800 7860 39500 Reeowy 0*t 97 104 98 85 109 * 71 - 86 . 85 110 106 111 84 * 106 ae 102 110 85 72 Sam ple reeidue exceed* th e piking lev d significantly; therefore, an accurate recovery value cannot b e edcuiated NO s Not detected a t or above 25 ng/L (ppt). NQ - Mm quanttfabte * Vtesauf&d corvc&n*Bori betw een 25 ng/L (ppt) and th e U n it a t Quantitation (LOO)whichIs 50 opT. (ppt). Note: Since this sommarytable howrounded resuRi, recoveryvalues mayvarysligftdy front the values Inthe rawdata. Exygen Research Page 33 of 110 000056 Interim Report #1 -Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table III. Matrix Spike Recovery of PFOS and PFOA in Water Samples Continued Sample C4 Sulfonate PFOS C l Acid PFOA Amount Amt Found Amount Amount Amt Found Amount Spiked in Sample Recovered Recovery Spiked in Sample Recovered Recovery O K L M N -SW -PW 3-W 031P {em etto* Spk K. seso nglL Lab S p ite ) OKLM N-OW PW 3*0050310 tc e e e e w ip * l. seeee ngiu u b sp u e ) OK LM N-GW -PW 341-65031D L ow S p ik e 5 p p b (coo, sqm hc/l f h w en * > O K L K N -W -P W 34'050310 H ig h S p ik e 90 ppfa (cao s * , looes * & . fu m S p ite } 5000 50000 5000 50000 32700 32700 32700 32700 43300 66100 33800 60000 5000 67 60000 * SOOO 55 50000 OKLM N K JW -PY M -W K O ll0 IC00W9 t u t N. MM n tfl 1*6 8plk ) OKLM N-GW -PW 4-0-06031Q <C 0m *1PSrtH , SNOOrroL U fr S p ite ) OKLM N -G W -PW 4-045G 310 LOW S p ik e 9 p p b SOM nafLFW d S p ite } OKLM N-G V W V 4 -0 -0 5 0 3 1 0 H ig h S p ik e SO p p b { C aeeo n . looeo noli- F ie * S p ite y 5000 SOCCO 5000 50000 33600 33800 33800 33600 42500 75700 42200 81200 5000 84 50000 * 5000 95 50000 O K LM N-GW -W 0-0-O5O 31O (C0M514 9g k O.M OOrigfLUh S p ite ) OKLM N -O W -PW l-0-050310 (c e e e ts te spk p, seeeo npiL Lab sp ite } OK LM N-GW W O-O -O SOSIO L o w S p ik e 5 p p b fCOOetCte WOOngiL Field Spite ) O K LM *G W -PW 8-0450310 H ig h S p ik e 5 0 p p b 1CMS4517. WOO n *L P M * Spite ] 5000 50000 5000 50000 90000 90000 90000 90000 97600 139000 94100 124000 * 5000 9 6 SOCCO 5000 66 50000 O K LM N -G W -PW 10-0-050310 (0004491 Spk C, SOM ngCL U b S p te ) O K LM N -G W -PW 10-0-050310 (C004441S tpk O, SOOOOngt. Lab S p ite } 5000 1400000 1410000 50000 1400000 1390000 5000 50000 OKLM N -G W -FW l M N 0M 310 L ow S p ik e S p p b { O ttstsae, o n t*gn- f m S p ite ) 5000 1400000 955000 5000 O K LM N -G W -PW 10-0-05031 H igh S p ik e 50 p p b (COIttCM, 0 1*90. FM d Spite ) 50000 1400000 1910000 90000 O K LU N -G W -PW 114H 3 310 (co a e e a a spx e , sodo npa. Laespnw ) OKLM N-GW -FW 1 1-0 -0 5 0 3 1 0 IC SM te a Spk F, BSOOan^L Lab Spite } 0KLM N -6W -PV * H M J5 0 1 0 L o w SpIK a S p p b (CM 4M K M M nafLPtoM S o d * ) OKLM N-GW -FW 1 1<0-050310 H ig h S p ik e 90 p p b (CMS4B29, sooei nprt.Field Spite > 5000 50000 9000 50000 40600 40800 40800 40000 48900 03100 45400 68500 * 5000 as 50000 * 5000 85 50000 Sample residue exceed (he spiking tevei tignifteantly; therefor*, an accural recovery value cannot be catenated N O s Not detected at or above 25 ngA (ppi). N Q - Not (tuardnabie * Measured concentration between 2 5 npA. {pptj and the Limit of QuanmeUon (LOQ5 which is SO ng/L. (pptL Note: Since Pile ummarytable snows rounded leeuita* recoveryvslues mayvaryslightly from thevalues In the raw data. 177000 177000 177000 177000 72100 72100 72100 72100 76400 78400 78400 76400 719000 719060 719000 719000 60300 60300 60300 60300 138000 190000 196000 204000 77500 121000 80700 118000 82800 133000 67000 116000 868000 40000 692000 747000 64700 105000 63300 88100 26 54 * 96 68 108 * 75 * . 89 * 76 Exygen Research Page 34 of 110 000057 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table III. Matrix Spike Recovery of PFOS and PFOA in Water Samples Continued Sampl* M crlotioa OKLMM-SW-O-050310 (C8H4CM*f* G.9909fttftLa*tyfm) OKLMN-SW-04S0110 <ceetm* * a soona* l ue Spu*) OKLMH-SW-O-OSMH) Low Spike 5 ppb (Casetta, som a^l two aereej OKLMN-SW-0-050J10 Hlflh Spike SOppb (Ceeeem.tow e*.two Sere*> OKLMN-GW-TR1P2-0-050310 Low Spfce 5 ppb (CMMMMI.9eOOn9rt.SpeV) OKLHN-3W-TFIP2-!WOJ10 Hlflh Spin 50 ppb (C00MS3Z.SOMnort.Spike) CISulfonaM PFOS Amount Amt Found Amount Spiked MSample W (ngfU (ntfU W 5000 50000 5000 50000 1190 1190 1190 1190 6270 51600 7220 58000 102 101 121 114 5000 50000 ND ND 8170 57400 123 115 & S 3 Amount Spiked (9*4 C3 Acid PFOA Amt Pound Amount in Sampl Recovered Jns*U (np/L) Recovery <%> 5000 50000 5000 50000 01 401 491 491 5520 53200 8020 44200 101 105 111 B7 5000 50000 ND NO 6040 57300 121 115 Average: 110 Standard Deviation: 32 "Sam ple ewiduft exceeds the spiking level significantly, therefore, an accurate recovery value esnriol be calculated NO * Notdelactedai orabove33 ng/L(ppt). NO = Not quanW bblo =*M easured concentration betw een 25 ngA. (ppt) an d the Lbril of Quamtatfon (LOO) which le 50 ng/L (ppt). Not*:Since lliia summarytablebows roundedreeutt*.recoveryvaluesmayvarysHohtV fromthevaluesintherawdata. Average: Standard Deviation: 4 1 Exygen Research / Page 35 of 110 000058 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table IV, Surrogate Spike Recovery of 13C PFOA in Water Samples Exygen ID Sam p le D e sc rip tio n Am ount S p lk e d (n g /y . T -P F O A Am ount Recovered (n o *) Recovery m C0064404 Spk C C0064404-Spk D C0064404 C0064404 Rep C0064405 C0064406 C0064407 OKLM N-GW -W 3-0-050310 O KLM N-GW -W 3-0-050310 OKLMN-GW -W 3-0-050310 OKLMN-GW -W 3-0-050310 OKLM N-GW -W 3-0-0S0310 Dup OKLMN-GW -W 34>-050310 Low Spike 5 ppb OKLMN-GW -W 3-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5580 53900 431 422 416 4730 34500 101 107 86 B4 83 95 69 C0064408 Spk E C 0064408 Spk F C0064408 C 0084408 Rep C0064409 C0064410 C0064411 OKLMN-GW -W 8-0-050310 OKLMN43W -W 8-04J50310 OKLMN-GW -W8-O-05O31O O K LM N -G W -W 8-0-050310 OKLMN-GW -W 8-0-050310 Dup OKLM N-GW -W 8-0-C50310 Low Spike 5 ppb OKLMN-GW -W 84J-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5840 55900 466 452 483 5550 39400 106 111 93 90 97 111 79 C0064412 Spk G C0064412 Spk H COO64412 C0064412 Rep C0064413 CO064414 C0064415 OKLMN43W -W 26-O-C50310 O KLM N-GW -W 26-0-050310 OKLMN43W -W 26-0-C50310 OKLMN-GW -W 26-0-050310 OKLMN-GW -W 26-0-050310 Dup OKLMN-GW -W 26-0-05Q310 Low Spike 5 ppb OKLMN-GW -W 26-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5430 32900 7720 7660 7540 5210 28000 99 65 * * 104 56 C0064416 Spk I C0064416 Spk J C0064416 C0064416 Rep C0064417 C0064418 C0064419 O KLM N-GW -W 33-0-050310 OKLMN-GW -W 33-0-050310 OKLM N-GW -W 33-0-050310 O KLM N -G W -W 33-0-050310 OKLMN-GW -W 33-0-050310 Dup OKLMN-GW -W 33-0-050310 Low Spike 5 ppb OKLMN-GW -W 334M350310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 3160 48000 262 256 261 2750 42500 57 95 52 51 52 55 85 C0064420 Spk K C006442D Spk L CO06442O COC64420 Rep C0064421 C0064422 C0064423 OKLMN-GW -W 206-0-050310 OKLM N-GW -W 2054)4)50310 O KLM N-SW -W 2O 5-C-050310 OKLMN-GW -W2Q5-0-05C310 OKLMN43W-W20545-O50310 Dup OKLM N-G W -W 205-04)50310 Low Spike 5 ppb OKLMN-GW -W 205-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 4940 53000 279 280 307 4240 38000 90 105 56 55 61 85 75 C0064424 Spk M C0064424 Spk N C0064424 C0064424 Rep C0O64425 C0064426 C0064427 O KLM N-GW -W 215-04)50310 OKLMN-GW -W 215-04)503tO OKLM N43W -W 215-04)50310 OKLMN-GW -W 215-0-050310 OKLMN43W -W 2154W 50310 Dup OKLMN-GW-W215-0-Q5Q310 Low Spike 5 ppb O KLM N-G W -W 215-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5850 56700 1010 434 464 4960 35600 106 112 202 87 93 99 71 The very high PFO A level In the undiluted sam ple Interfered with '*C PFO A recovery. Note: Since thl sum m ary table show s rounded results, recovery values may vary slightly from the valuee In the raw data. Exygen Research Hi ^ Page 36 of 110 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table IV. Surrogate Spike Recovery of 13C PFOA in Water Samples Continued Exygen ID Sam ple Description Amount Spiked ing/L) 1lC -P F O A Amount Recovered (nS>L) Recovery .._<*) C0064428 Spk C CQ064428 Spk D C0084428 C0064428 Rep C0054429 C0064430 C00B4431 O KLM N -G W -W 2010-0-050310 OKLMN-GW-W2010-0-050310 OKLMN-GW-W2010-0-050310 OKLMN-GW-W2010-0-050310 OKLMN-GW-W2010-0-050310 Dup OKLM N-GW-W2010-04)50310 Low Spike 5 ppb OKLMN-GW-W2010-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5390 53000 432 417 510 4500 30200 98 105 80 83 102 90 60 C0084432 Spk E C0064432 Spk F C0064432 C0064432 Rep CO064433 C0064434 COOS4435 OKLMN-GW-PW7-0-050310 OKLMN-GW-PW7-0-05Q310 OKLMN-GW-PW7-0-050310 OKLMN-GW-PW7-0-050310 OKLMN-GW-PW7-0-050310 Dup OKLMN-GW-PW7-0-050310 Low Spike 5 ppb OKLMN-GW-PW7-0-050310 High Spike 50 ppb 5500 500C 503 500 500 5000 50000 5260 51000 341 335 325 4820 33200 96 101 68 67 65 96 66 C0064436 C0064437 COO64438 OKLMN-GW-TRIP1-0-050310 OKLMN-GW-TRIP1-0-050310 Low Spike 5 ppb OKLMN*GW-TRIP1 -0-050310 High Spike 50 ppb 500 5000 50000 510 5100 51300 102 102 103 C0064442 Spk G C0064442 Spk H C0064442 C0064442 Rep C0064443 C0064444 C0064445 O KLM N -G W -PW 8-0-050310 O KLM N -G W -PW 8-0-050310 OKLMN-GW-PW8-0-050310 OKLMN-GVV-PW8-0-050310 O K I WN-GW-PW8-0-050310 Dup OKLMN-GW-PW8-0-050310 Low Spike 5 ppb OKLMN-GW-PW8-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5270 52900 321 322 300 3910 25800 96 105 64 64 60 78 52 COO64446 Spk I COO64446 Sp k J C0064446 C 0064446 Rep C0084447 C0064448 C0064449 OKLMN-GW-tPW9-0-050310 O K LM N -G W -PW S-Q -050310 OKLMN-GW-PW9-0-050310 OKLMN-W-PW9-0-05310` OKLMN-GW-PW9-0-050310 DUp OKLMN-GW-PW9-0-50310 Low Spike 5 ppb OKLMN-GW-PW &-.Q-050310High Spike 50 ppb 5500 5O500 500 500 500 5000 50000 5250 53900 315 317 338 4230 24800 95 107 63 63 68 85 50 C0064450 Spk K COO64450 Spk L COO64450 C0064450 Rep C0064451 C0064452 C0064453 OKLMN-GW-W6102-0-050310 OKLM N-GW-W6102-0-050310 OKLMN43W-W61024)-0503t0 OKLMN-GW-W6102-0-050310 OKLMN-GW:W 6102-0-050310 Dup OKLM N-GW-W6102-0-050310 LowSpike 5 ppb QKLMN-GW-W6102-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5640 53200 424 439 480 5050 32500 103 105 85 88 96 101 65 Not: Sine th is sum m ary tab: sh o w s rounded results, recovery valu e s m ay vary sligh tly from the valu e s In the raw data. Exygen Research Page 37 of I10 000060 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table IV. Surrogate Spike Recovery of ,3C PFOA in Water Samples Continued Exygen ID Sam ple D e sc rip tio n 1JC -P F O A = s s = .............. s a a g a t -- Amount Amount Spiked Recovered Recovery (n g /L ) (rtfl/L) _ {% ) ... C0064454 Spk M C0064454 Spk N C0064454 C0064454 Rep C0064455 C0064456 CQ064457 O KLM N -G W -W 6104-0-050310 O KLM N-GW -W 6104-0-050310 O KLM N -G W -W 6104-0-050310 O KLM N-G W -W 6104-0-050310 0 KLM N -G W -W 8104-0-050310 Dup O K LM N -G W -W 6104-0-050310 Low Spike 5 ppb O K LM N -G W -W 6 104-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5510 54500 398 417 487 4920 33800 100 108 80 83 97 98 68 C0064458 Spk C COO04458 Spk D C0064458 C0064458 Rep C0064459 C00644S0 C0064461 OKLMN-GW -W 6ZC1-0-050310 OKLM N-GW -W 6201-0-050310 OKLM N-GW -W 6201-0-050310 OKLM N-GW -W 6201-0-050310 O KLM N-G W -W 8201-0-050310 Dup OKLM N-GW -W 6201-0-050310 Low Spike 0.5 ppb OKLMN-GW -W 6201-0-050310 High Spike 5 ppb 5500 50500 500 500 500 500 5000 5460 50300 388 391 496 491 5440 99 100 78 78 99 98 109 C0064467 Spk E C0064467 Spk F C0064467 C 0064467 Rep C0064468 C0064469 C0064470 OKLMN-GW -W 20-0-050309 OKLM N-GW -W 20-0-050309 OKLMN-GW -W 20-0-05309 OKLMN-GW -W 20-0-050309 OKLMM-GW -W 20-0-05C309 Oup O KLM N -G W-W 20-0-050309 Low Spike 5 ppb OKLW IN-GW -W 20-0-050309 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 4090 46500 272 270 270 3790 26600 74 92 54 54 54 76 53 C0064471 Spk G C0064471 Spk H COO64471 C0064471 Rep C0064472 COO64473 COO64474 OKLM N-GW -W 22-0-050309 OKLMN-GW -W 22-0-OS0309 OKLMN-GW -W 22-0-50309 OKLM N-GW -W 22-0-050309 OKLM N-GW -W 22-0-050309 Dup OKLM N-GW -W 22-0-050309 Low Spike 5 ppb OKLM N-GW -W 22-0-050309 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 4380 50700 267 280 255 3830 28800 80 100 53 56 51 77 58 C0064475 Spk l CQ064475 Spk J C0064475 C0064475 Rep C0064476 C0064477 O K LM N -G W -W 31-04)50309 O K LM N -G W -W 31-0-050309 O K LM N -G W -W 31-0-050309 OKLM N-GW -W 31-0-050309 O KLM N-G W -W 31-0-060309 Dup O KLM N-G W -W 31-0-050309 High Spike 50 ppb 5500 50600 500 500 500 50000 5410 54200 391 391 371 44100 98 107 78 78 74 88 C0064478 Spk K C0064478 Spk L C0064478 C0064478 Rep C0064479 C 0064480 C0064481 OKLMN-GW -W 32-0-0539 OKLMN-GW -W 32-0-050309 OKLMN-GW -W 32-0-D50309 OKLMN-GW -W 3Z-0-050309 OKLM N-GW -W 32-0-050309 Dup OKLMN-GW -W 32-O-050309 Low Spike 5 ppb OKLMN-GW -W 32-0-0503Q9 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 4840 51000 287 289 328 4750 49000 88 101 57 58 66 95 98 Note: Since this sum m ary table show * rounded results, recovery values m ay vary slightly from the values in the raw data. '? H, H Exygen Research Page 38 o f 110 000061 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table IV. Surrogate Spike Recovery of 13C PFOA in Water Samples Continued Exygen ID Sem ple D escription Amount S p ik e d ,aC-PTOA Amount Recovered (ngrt.) Recovery <%> C0064482 Spk M C0064482Spk N C0064482 CQ064482Rep COO64483 C0064484 C0064485 OKLM N-G W -W 217-0-050309 O KLM N-G W -W 217-0-050309 O KLM N-G W -W 217-0-050309 O KLM N-G W -W 217-0-050309 O KLM N -G W -W 217-0-050309 Dup O K LM N -G W -W 217-0-050309 Low Spike 5 ppb O K LM N -G W -W 217-0-050309 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5410 52500 428 453 468 4850 44700 98 104 86 91 94 97 89 C0064486 Spk O C006446 Spk P C0064486 C0064486 Rep C0064487 C0064488 C0064488 OKLMN-GW -W 2008-0-050309. OKLMN-GW -W 2008-0-050309 OKLM N-GW -W 2008-0-0503C9 OKLMM-GW -W 2008-0-050309 OKLM N-GW -W 2008-0-050309 Dup QKLMN-GW -W 2008-0-050309 Low Spike 5 ppb OKLM N-GW -W 2008-0-050309 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5140 52100 318 326 357 6040 37800 93 103 64 65 71 121 76 COO64490 S p k C C0064490 Spk D C0064490 C0064490 Rep C0064491 C0064492 C0064493 OKLMN-GW -W 2012-0-05Q309 OKLM N-G W -W 2012-0-050309 OKLM N-GW -W 2Q12-0-050309 O KLM N-G W -W 2012-0-050309 O KLM N-GW -W 2012-0-050309 DupiOKLM N-GW -W 2012-0-050309 Low Spike 5 ppb OKLM N-GW -W 2012-0-050309 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5050 50700 344 342 351 5010 37900 92 100 69 66 70 100 76 COO64494 Spk E C0064494 Spk F C0064494 C0054494 Rep C0064495 C0064496 C0064497 OKLM N-GW -W 80-0-050309 OKLM N-GW -W 80-0-050309 OKL M N-GW -W 80-0-050309 . O KLM N-G W-W80-0-050309 OKLM N-GW -W 80-0-050309 Dup OKLM N-GW -W 80-0-050309 Low Spike 5 ppb OKLM N-GW -W 80-0-050309 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5650 52400 486 438 502 5410 41700 103 104 97 88 100 108 83 C0064498 Spk G C0064496 Spk H C0064498 CO064498 Rep C0064499 C0064500 C0064501 OKLM N-GW -PW 1-0-050310 OKLM N-GW -PW 1-0-050310 O K LM N -G W -PW 1-0-050310 O KLM N -G W 4sW1 -0-50310 ' OKLMN-GW -PW 1-Q-050310 D u p : OKLM N-GW -PW 1-0-50310 Low Spike 5 ppb O K LM N -G W -PW 1-0-050310 High Spike 50 ppb 5500 50600 500 500 500 5000 60000 5150 53000 331 350 352 4420 41600 94 105 66 70 70 88 83 C0064502 Spk I C0064502 Spk J C0064502 C0064502 Rep C0064503 C0064504 C0064505 OKLMN-GW -PW 2-0-O50310 OKLM N-GW -PW 2-0-05C310 O K LM N -G W -PW 2-0-050310 O K LM N -GW -PW 2-0-05C310 . . OKLM N-GW -PW 2-0-050310 Dup OKLM N-GW -PW 2-0-050310 Low Spike 5 ppb OKLM N-GW -PW 2-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5420 52600 440 440 431 4680 34000 99 104 68 88 86 94 68 Note: Sin e s this sum m ary table show s rounded results, recovery values m ay vary slightly from the value In the raw data. Exygen Research Page 39 of 110 000062 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table IV. Surrogate Spike Recovery of l3C PFOA in Water Samples Continued Exygen ID ' Sam ple D e sc rip tio n Am ount S p ik e d ("9 /U 1>C-PFOA Am ount Recovered nsfL) Recovery <%) C0084506 Spk K C0064506 Spk L C0064508 C0064506Rep C0064S07 C 0064508 C0064509 OKLM N-GW -PW 3-0-050310 OKLM N-GW -PW 3-0-050310 O KLM N-GW -P W 3-0-050310 OKLM N-GW -PW 3-0-050310 OKLM N-GW -PW 3-0-050310 Dup 0 K LM N -G W -PW 3-0-050310 Low Spike 5 ppb O K LM N -G W -P W 3-0-050310 High Spike 50 ppb C0064510 Spk M C0064510Spk N C0064510 C00645010 Rep C0064511 C0064512 CC064513 OKLM N-GW -PW 4-0-050310 OKLM N-GW -PW 4-0-05G310 O K LM N -G W -PW 4-0-050310 O K LM N-GW -PW 4-0-050310 OKLM N-GW -PW 4-0-050310 Dup OKLM N-GW -PW 4-0-050310 Low Spike 5 ppb 0 KLMN-GW -PW 4-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5500 50500 500 500 500 5000 50000 4640 53100 284 275 294 4080 38300 5190 52400 320 324 313 4870 36000 84 105 57 55 59 82 77 94 104 64 65 63 97 76 C0064514 Spk 0 C0064514 Spk P COO64514 C0064514 Rep C0064515 C0064516 C0064517 OKLMN-GW -PW 6-O-O50310 OKLM N-GW -PW 6-0-050310 O K LM N -G W -PW 6-0-050310 O K LM N -G W -PW 6-0-050310 O K LM N -G W -PW 6-0-050310 Dup O K L M N -G W -PW 6-0-050310 Low Spike 5 ppb OKLM N-GW -PW 6-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5050 52300 304 311 313 4740 35100 92 104 61 62 63 95 70 C0064518SpkC C0084518 Spk 0 C0064518 C0064518 Rep C0064519 C0064520 C0064521 O K LM N -G W -PW 10-0-050310 OKLM N-GW -PW 10-0-050310 O KLM N -G W -PW 10-0-050310 O KLM N -G W -PW 10-0-050310 O K LM N -G W -PW 10-0-050310 Dup OKLM N-GW -PW 10-0-050310 Low Spike 5 ppb O K LM N -G W -P W 10-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 3870 48500 255 249 258 2980 34100 67 96 51 50 52 60 68 C0064522 Spk E C0064522 Spk F C0064522 C0064522 Rep C0064523 C0064524 C0064525 O KLM N -G W -PW 11-0-050310 O K LM N -G W -PW 11-0-050310 O K LM N -G W -PW 11-0-050310 O K LM N -G W -PW 11-0-050310 O KLM N -G W -PW 11-0-050310 Dup O K LM N -G W -PW 11-0-050310 Low Spike 5 ppb OKLMN-GW -PW 11-0-05031Q High Spike 50 ppb 5500 50500 500 500 500 5000 50000 C0064526 Spk 6 C0064526 Spk H C0064526 C0064526 Rep C0064527 C0064528 C0064529 OKLMN-SW -O-05310 OKLMN-SW -O-050310 OKLMN-SW -O-050310 OKLMN-SW -0-050310 OKLM N-SW -0-050310 Dup OKLMN-SW -O-050310 Low Spike 5 ppb OKLM N-SW -0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5180 51600 319 347 312 4400 36000 5270 52000 124 132 505 5320 41200 94 102 64 69 62 58 72 96 103 25 26 101 106 82 Note: Sine# this summary table hows rounded result, recovery valoss may vary slightly from the values In the raw data. Exygen Research Page 40 o f 110 000063 Interim Report #1 -Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table IV. Exygen ID Surrogate Spike Recovery of 13C PFOA in Water Samples Continued 1*C*PFOA Sam ple Description Amount Amount Spiked Recovered Recovery (ng/L) fnoyy (%) C006453 C0064531 C0064532 O KIM N -G W -TRIP2-0-050310 500 OKLMN-GW-TRIP2-0-050310 Low Spike 5 ppb 5000 OKLMN-GW-TRIP2-0-050310 High Spike 50 ppb 50000 494 5520 52900 99 110 106 Avorage: 83 Standard Deviation: 21 Note: S in c e th is su m m ary table sh o w s rounded results, recovery v alu e s m ay v ary slig h tly from the valu e s In the raw data. Exygen Research Page 41 of 110 000064 Interim Report #1 -Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 FIGURES Exygen Research Page 42 of 110 000065 Interim Report #1-Analysts of Oakdale Water Samples Exygen Study No.: P0001400 Figure 1. Typical Calibration Curve for PFOA in Reagent Water I 03MQ6C firour^ H&Mr tovlsib (PFCMSt 'Um * ' ffc jiw io rtO * !J6**0C3* *7.3**004 (r* O ^M I) Area, tounts 0 0 ;, Exygen Research Page 43 of 110 000066 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P 0001400 Figure 2. Extracted Standards of PFOA in Reagent Water, 25 ng/L and 50 ng/L, Respectively X C032TttW - PFOA (Sfrtrdtni) 1 c f 41 ttm * Q224QQC.wiW A r t* 4 4 H 7 ootNTtt $033,636 c p * KT: 114 4 6 m in 11.84 XCD321PM P f O A ^U ndart) 1T3V3WD v n u sanpl 3 f 41 n o n C32405C^iff A u : 7*29$ oaufts ritigM: 12793.?1U eps RT: IlK n t n 11.84 Exygen Research >;*' ?'! Si 5| 4 Page 44 of HO 000067 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 3, PFOA in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively Ann. 97$$ 'P F O A (U rtt* to w n )4 \3 6 f3 6 3 fi i w m p i+ V o f t l 9 9 4 * 2 2 o p i R7: M.&4S m in C * V c 3 fteapent S p k A - J>POA(OC>4I9J)/069.S mu- u m p k tOof 41 fram 0324KC.aM A m : W W < w Ha*ht: 19075.481 opa R L l1 J 1 t n * > Note: A linear lot o f PFOA was used to calibrate the instrument. The two peaks shown in Figure 4 are due to different isomers present in environmental samples. The area counts for all isomers present are included to report one total PFOA value. Exygen Research Page 45 of 110 oooo6a Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 4. Chromatogram Representing an Oakdale Water Sample Analyzed for PFOA, DF=100 (Exygen ID: C0064522, Data Set: 032405CR) C00*462? -PFOAWthitaHHi4t2JH$G9.P ofS7from03t406CB.^W Ap m : H itg h t 7fG G 1& 49t>fl* BT: i1 2 Q m fn 11.82 In tsfiflfy , c p s Exygen Research Page46 of II0 000069 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 5. Typical Calibration Curve for 13C PFOA In Reagent Water (PCPF0^"UnMT,'R*MfeAC1trm&tmfryUlnOB*-Ci**frft.WU) Arsa, counts Exygen Research Page 47 of 110 000070 Interim Report #1 -Analysis o f Oakdale Water Samples Exygen Study No.: P00I40O Figure 6. Extracted Standards of 13C PFOA In Reagent Water, 25 ng/L and 50 ng/L, Respectively I Ar+:XC32*05-f S 3 tOff 1JC cuN rPfP* CA{Si9n5d33aSi}.4f1135^.Wfl3*7R0.t0:llJ36Cmim 2 from<3324OtSCMW <5000-< 11.86 4000 intensity, cps 3000 2000 1000 i2 3 40 6788 Tim*, mm XCS 1 0 4 -2 '13C F F0A CmsnO 41*JX37&.0 amu samp** 3 of 41 fmm o a jW C w f f Aa: 88017 ooums Htifll*: 11438.486 cp* RT; !1<848 10 H 12 13 14 10 10 17 11*5 lntenSty.eps Exygen Research Page 48 of 110 000071 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 7. 13C PFOA in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively I fre#ge*?Cav4roJ f3C P F O A (Vfrhtmwn} 4t9.0f376fi m u A n : Z1 f otumi Hwttrt 96.664 co 67: lf A 3 4 m i 9 of44 hvrt 63t409C.mtr 3*s I R n oM SpfcA- 13C PrOA(QQ419JV3M.Pmu-ssn|)tt lO of 41 fnm 832&Cjj11 Wght: 1 M 7 3 o p < RT: H-S23rr*t 1006 <ft Qu . SflO4 5 6 7 9 Q 10 11 12 13 14- 15 10 17 Tim, rmrv I ftaGMt pk a - 13C PFaA(QC) 4t$JV3700 wnu - Kampfe 116f 41 t W 0324D6CjuN1 A ti; 128964 ooww* M ehC 2038*1 ,018cp* RT; 11,843 mir 2 .0 * 6 1 wa.. to* TSCa> 8 0 10 11 12 13 14 16 16 Tim *, min V ttO>O5-., <J }k Exygen Research Page 49 of 110 000072 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 8. Chromatogram Representing an Oakdale Water Sample Analyzed for 13C PFOA (Exygen ID: C0064522, Data Set: 032405C) 15 0C0064032 C P P O (UakJH3mr}4l5f370 m o . tnpJ*2 3 1*41 from 022406C.uW Aro*; ocv.rH41*903 # 7 f f .059 mi 11A3 Intensity, cp s Exygen Research Page 50 o f 110 000073 Interim Report #1-Analysis of Oakdale Water Samples Exygen Study No.: P0001400 Figure 9. Typical Calibration Curve for PFBS in Reagent Water 034MCR a w i < UftW jtfe (PFMft "Una** t y m t o O ^ w gonq): t 138 n t& tw r Cr tA9$T) Are, counts Exygen Research Page 51 of 110 000074 Interini Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 10. Extracted Standards of PFBS in Reagent Water, 25 ng/L and 50 ng/L, Respectively XC 04M 03* 1 . PFBS tS ti* fr n i) 2 9 9 M 9 9 .0 pentf - 2 o f t 7 WflT 4 $ i i oow/its H t ^ h t } i) 6 3 4 c & * RT: 3J907 <jtni 3.91 .irff I *Cft4M I4 - r r a s (ftandart) ISB-DdO-O rmt - sm p k 3 of 07 Own QiJMOdCA wff A u;7727coM r tp* ftT:34$4ffii 39 Ihn, min Exygen Research y*'; < .. " -j i: t Page 52 of 110 000075 interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 11. PFBS in Reagent Water, SOng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively fio n g tn i Con to ) - P F B S fiJnhno*m ) 399& f99. 0nnM<jn a ftthtd) front O Si4O O Cfi.m 0 Intensity, cp s Intensity, cp s Intensity, cp s omt*MA w ; -H192 Ha)*; 12M .94I apt RT: 3.917 min Time, r&ift * " ^ * 0 O *'&/ & Exygen Research Page 53 o f 110 000076 Interim Report #1-Anaiysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 12. Chromatogram Representing an Oakdale Water Sample Analyzed for PFBS, DF=100 (Exygen ID: C0064522, Data Set: 032405CR) C0064622 -PFSS (U lthrrotm ) 2 9 9 0 8 9 .0 * Mmpj SS QfG7 frAt 0324WSCX.MfT f : 7 7 oow r#f H e ig h t i f <5.406 R T :3 .9 2 4 m ln 3*2 intensity, cps Exygen Research Page 54 of 110 000077 IhterimReport#!-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 13. Typical Calibration Curve for PFHS in Reagent Water (found ttb rtr KSX 'U nw r' Regression fx* wi^hthg); y s h t 04)0101 $ CJ#M ) At, counts Exygen Research Page 55 of 110 000078 Interim Report #1 -Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 14. Extracted Standards of PFHS in Reagent Water, 25 ng/L and 50 ng/L, Respectively * C 0 3 f 0 S - f - PFHS(Stamtwr)3 $9 .0 f9 0 .0 srrtu w n p to 2 of4 * I r a n fcL?4 0 S C j* rff An*: 1 c o tffffr Hltybt 1 4 6 9 .7 4 7 cp* RT: 10 .6 2 6 nwrr 10.62 Exygen Research h' Page 56 o f 110 000079 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 15. PFHS in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively ftf(rtspoMftf fCtoo#tr/bimeorfPjFHS 3 9 $ .o a O G *m t n m p f 9 of 4 f from Intensity, cps intensity, c p s I n o f M t S*< A PfWS amu *arfa 10 r t 4H m m B ttttS C .ttff A m : 3 4 1 * eountc Hai|ht : 422.193 op* RT: 10.5*4 m b 3000 2000 1000' 0 9 I A M 0M spk ' ?rHS (QQ399.IMB0. a m i- 5 fl * 4 1 from W?405Crf1 A f c r . t t t o W u u t r W a tf ;3 *7 7 A lM o w AT: 1C.8Mmi 1 0 ,1 9 ^ 9 10 Tim *, mtft 10.61 ?4' 1-0*4' 0-0 i ---------- 1----------.----------- 1............................. . ~i r 12 3 4' 3 6 7 8 TInh , n iti 14 16 16 17 Intensity, c p s Exygen Research 0 - / / 'i t'i s i * \ * ' v * Page 57 o f 110 OOOOSO Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No,: P0001400 Figure 16. Chromatogram Representing an Oakdale Water Sample Analyzed for PFHS, DF=100 (Exygen ID: C0064522, Data Set: 032405CR) CW64S22 - (Uh m o m r)3 2 9 X>W tra - m ai* 39 < /6 7 fh u ir Q32405CS.wUT * ^ 3 7 ^0 9 *1 ^ 3 9 3 9 5 9 6 cp s ST: 2900- 2900 - 2*0022002000- 1900- 10-39 tu e 1200- 1000' 900- 4CO200- 0 i 32 4 O B 7 9 Q 10 11 12 13 14 15 19 17 Tim *, mir Exygen Research Page 58 of 110 o o o o ls i Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 17. Typical Calibration Curve for PFOS in Reagent Water Area, count ** .. * a : Exygen Research Page 59 of 110 OOOOSH Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 18. Extracted Standards of PFOS in Reagent Water, 25 ng/L and 50 ng/L, Respectively XC $3?f05-f -f*FO$ fStaArd}'4G4j0&0J j* w 2 <X4i fro*r$32406C .i*/y Hiq)rt 1B9Q.120cpc ,97: 12438 rnt* 12m Exygen Research <* ( s ji ' Page 60 o f 110 ooooa Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 19. PFOS in Reagent Water, SO ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively I f h H y ir 1 C&wpf. A P Q S flJAkn*>H*r) 48B.aOO.O mar - 9 **y ji+ 9 o f4 t r+s; tO *46cow fe AT; fi.8 1 0 mi* Q 3}40C *uff 12.62 intensity, cp s intensity, cpe Am : 180532tftts Jt.t373cps RT: t i m * m 12*1 Intensity, c p * Exygen Research Page 61 of 110 0000&4 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No;: P0001400 Figure 20. Chromatogram Representing an Oakdale Water Sample Analyzed for PFOS, DF^lOO (Exygen ID: C0064522, Data Set: 032405CR) C0A0f&tA:S1252C7P&F9OS 0 G43324*qo 87:12.133*6 Of*7 8000 9900 CO 4600- 4000- 390030002900 20001900- tOOO- 900 0` " t ' I 1 I..... ....T ' l----- " 1 !"' I i 1 2 3 -5 5 6 7 9 0 1 0 Tim , min 12.14 12-00 10 1?11 12 13 14 15 Intensiv, cps Exygen Research Page 62 o f 110 000085 Intrim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P000I400 APPENDIX A Study Protocol P0001400 (Exygen Study No. P0001400) with Analytical Method: V0001780:"Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Water by LC/MS/MS" Exygen Research Page 63 of 110 000086