Document dnD95nN5pYOpY3RJqjp2VQv1q

AR226-3642 INTERIM REPORT #1 Analysis o f Oakdale W ater Samples STUDY TITLE Analysis of 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 DATA REQUIREMENTS EPA TSCA Good Laboratory Practice Standards 40 CFR 792 STUDY DIRECTOR Jaisimba 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 s 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: P0001400 Exygen Study Number: P0001400 Total Pages: 110 P \ 000024 Interini Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT Exygen Study Number P0001400, entitled "Analysis o f Perfluorooctanoic Acid (PFOA), Perfiuorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (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. Exygen Research Study Director Weston Solutions, Inc. Robert A. Paschke Sponsor Representative 3M Company Exygen Research //?M Date %?/gr Date o / I|gts Date Page 2 of 110 000025 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 DUALITY 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 Perfluorooctanesulfcmate (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 were reported to the Exygen Principal Investigator and Management and to the Study Director, Phase Date Inspected Date Reported to Date Reported to Principal Exygen Date Reported to Investigator Management Study Director 1. Protocol Review 03/24/05 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 a s i n n s Date `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 of 110 000026 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study N.: P0001400 CERTIFICATION OF AUTHENTICITY This interim report, for Exygen Study Number P0001400, 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: Date Exygen Research Facility Management Richard A President Exygen Research Study Director, Weston Solutions, Inc. Jaisimha Kesari P.E., DEE Weston Solutions, Inc. Sponsor Representative, 3M Company: r^J lS L Robert A. Paschke Manager, 3M Corporate Environmental Programs Exygen Research Date oloils Date Page 4 of 110 00002V 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-I 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 42-02-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, : P0001400 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 of 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 C 0 29 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............................................................... 20 Exygen Research Page 7 o f 110 000030 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: PQ001400 Table I. LIST OF TABLES Page Summary ofPFBS, PFHS, PFOS and PFOA in Water Samples........................................................................ ......... ........................... 22 Table IL Matrix Spike Recovery ofPFBS and PFHS in Water Samples.................. ...24 Table DDL Matrix Spike Recovery of PFOS and PFOA in Water Samples.................... 30 Table IV. Surrogate Spike Recovery of UC PFOA in Water Samples.......................... 36 Exygen Research Fae 8 of 110 ooooai Interim Report #1-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 o f 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 ED: C0064522, Data Set: 032405CR).........................................................................................46 Figure 5. Typical Calibration Curve for l3C PFOA in Reagent W ater.......................... 47 Figure 6. Extracted Standards o f 13C PFOA in Reagent Water, 25 ng/L and 50 ng/L, Respectively............. ................... ................. ................... ..........48 Figure 7. t3C 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 of 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: 032405C R )................. 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 ED: 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 of 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 O O O i> *j 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.: P000140 1.0 SUMMARY Exygen Research extracted and analyzed water samples for the determination of perflnorooctanoic acid (PFOA), perfluorobutanesulfonate (PFBS), perfluorohexanesulfonate (PFMS), and perfluorooctanesulfonate (PFOS) according to Exygen Method V001780 (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 of 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% 19, 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, l3CPFOA, in water samples was 83% 21. 2.0 OBJECTIVE The objective of the analytical part o f 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 of 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, C0064467-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-in 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, ,3C 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 l3C P F O A PFBS PFHS PFOS Exvsen Inventofv-No.. SP0003800 SP0004184 SP0000252 SP0002401 , SP0002694 Lot# 23116HB 3507-195 101 SE036 430180-1 Purity (%,) 97.64 97 96.7 98.6 101.2 Expiration Date 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 of 110 000036 Interim Report #I-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 PFOA Chemical Name: Perfluorooctanoic acid Molecular Weight: 414 Transitions Monitored: 413 -> 369 (for quantification) and 413 -> 219 (for confirmation) Structure: 13C PFOA Chemical Name: 1,2-13C perfluorooctanoic acid Molecular Weight: 416 Transition Monitored: 415-370 Structure: PFBS Chemical Name: Perfluorobutanesulfonate Molecular Weight: 338 supplied as the potassium salt (CiFSCb'K^ 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.: P000I400 PFHS Chemical Name: Perfluorohexanesulfonate Molecular Weight: 438 supplied as the potassium salt (CeFuSOTC^) Transitions Monitored: 399 - 80 Structure: FF FFF PFOS Chemical Name: Periluorooctanesulfonate Molecular Weight: 538 supplied as die potassium salt (CsFnSOaTC*) Transitions Monitored: 499 --80 Structure: F FF F 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 C8 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 of 110 00003& Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: PQ001400 6.2 Preparation of Standards and Fortification Solutions Individual stock standard solutions o f PFOA, 13C 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 o f 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 of 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 (ng/mL)1 <HL) (xnL) 00 40 10 100 40 10 200 40 10 400 40 100 100 40 100 200 40 100 400 40 13c1o f PFOA, 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 000033 Interim Report #1 -Analysis o f Oakdale Water Samples Exygen Study No.: P00Q1400 6.3 Chromatography Quantification o f PFOA, PFBS, PFHS and PFOS was accomplished by LC/MS/MS electrospray. The retention time o f 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 o f 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: API4000 Biomolecular Mass Analyzer Interface: Turbo Ion Spray Liquid Introduction Interface Computo': DELL OptiPlex GX400 Software: Windows NT, Analyst 1.4.1 HPLC: Hewlett Packard (HP) Series 1100 HP Quat Pump 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 mM 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: 0.3mL/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 No.: 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 /mini ~12 min. ~12 min. ~12 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 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 - 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. Equation 2: Recovery (%) = /analyte found ine/L) - analyte in control ing/Lft xl00% amount added (ng/L) An example of a calculation using an actual sample and results from the PFOA analysis follows: Water sample Exygen ID CG064432 Spk F (Set: 032105BR), fortified at 50000 ng/L with PFOA where: peak area 1170161 intercept = 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 of 110 00004$ Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P000140Q From equation 1; Analyte found (ng/L) = fl 170161 -262001 x 100 1330 From equation 2: % Recovery 86012 ng/L* (86012 n e /L - 37600 ng/L) 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, PFHS, 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 dupEcate 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 13C PFOA was added. The additional 13C 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 of the normal acceptance range o f 70-130%. Because laboratory control spikes for l3C PFOA were acceptable in every set, instrument washes were free o f 13C PFOA, at least one l3C 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 o f 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 of PFOA, PFBS, PFHS and PFOS in water samples were 93% 19, 141 % 2 1 , 96% 1 5 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 of 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 DATAAND 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 the 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 Intrim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P 0001400 TABLES Exygen Research .f Page 21 of 110 000044 Interim Report #1 -Analysis o f Oakdale Water Samples Exygen Study No.: P000140Q Table I. Summary of PFBS, PFHS, PFOS and PFOA in Water Exygtn ID C0064404 C0064404 Rep C0064405 Client Sample ID OKLMN-GW-W3-0-050310 OKLMN-GW-W34WJ50310' QKLMN-GW-W3-0-050310 Oup Samples Analyte Found (ppt, ngfL) C4 Sulfonate PFBS C8 Sulfonate PFHS C8 Solforai PfOS 312 162 4750 298 160 3350 303 159 3190 Cft Add PFOA 6330 6220 5990 C0064408 OKLMN-GW-W8-04>50310 57.0 ND 59.0 290 C00644408 Rep OKLMN-GW-W8-O-0S031O* 63.8 ND 55.7 275 C0064409 OKLMN-GW-W8-0-050310 Dup 60.1 ND 56.3 284 C0064412 C0064412 Rep C0064413 OKLMN-GW-W264WJ50310 OKLMN-GW-W26-0-050310* OKLMN-GW-W26-0-050310 Dup 73400 75700 71400 222000 244000 214000 13500000 14400000 12200000 79300000 70200000 71800000 C0064418 C0064416Rep C0064417 OKLMN-GW -W 334M 50310 OKLMN-GW-W33-OO60310* OKLMN-GW-W33-04K0310 Dup 26800 23800 25500 92300 84600 81600 4810000 4870000 4540000 1750000 2020000 2790000 CQ064420 C0064420 Rep C0064421 OKLMN.GW-W205-<M)S0310 OKIMN-GW-W205O-0S0310* OKLMN-GW-W205-0-050310 Dup 8260 8500 7850 6740 6610 7070 146000 119000 116000 147000 150000 158000 C0084424 C0064424 Rep C0064425 OKLMN-GW-W215-0-050310 OKLhW-GW-W215-0-050310* OKLMN-GW-W2154FO5031O Dup 801 81.2 75.8 769 37100 4400 256 27000 . 3510 270 36900 4070 CQ064426 0KLMN-GW-W2010-0-050310 ND ND ND NQ C0064429 Rep OKLMN-GW-W2010-0-050310* ND ND ND ND C0064429 OKLMN-GW-W2010-0-050310 Dup ND ND ND ND C0064432 C0064432 Rep C0064433 OKLMN-GW-PW7434350310 OKLMN-GW-PW74M3503W OKLMN-GVV-PW7-0-05031Q Dup 4460 4340 4630 4800 5080 5080 71600 67800 72400 37600 38400 36200 C0064436 OKLMN-GW-TRIP1 -0-050310 ND ND ND ND C0064442 C0064442 Rep C0064443 OKLMN-GW-PW8-0-050310 OKLMN-GW-FW8-0-050310* OKLMN-GW-PW8-0-05CG10 Dup 13300 14100 14100 23800 23900 23000 34300 35600 33400 81400 60600 58500 C0064446 C0064446 Rep C0064447 OKLMN-GW-PW9-<M)50310 OKLMN-GW-PW94M)50310* OKLMN-GW-PW9-0-050310 Dup 2110 2140 1930 6160 500C 5140 84400 84900 88600 49000 48700 49600 CC064450 CQ064450 Rep C00644S1 OKLMN-GW.W6102-O435031O OKLMN-GW-W6102-0-050310* OKU1N-GW-W61Q2-0-050310 Dup NQ 53.5 NQ ND ND ND NQ 214 NQ 228 ND 227 C0064454 C00644S4 Rep C0064455 OKLMN-GW-W61D4-0-050310 OKLMN-GW-WB104-0-050310* OKLMN-GW-W6104-0-050310 Dup NQ NO 51.2 ND ND ND 109 207 125 189 118 184 C0064458 C0064458 Rep C0064459 OKLMN-GW-W6201-0-050310 OKLMN-GW-W6201 -0-050310* OKLMN-GW-WB201-0-050310 Dup 74.0 74.1 78.0 ND ND ND NQ 95.5 ND 88.3 NQ 132 C0O64467 C0064487 Rap C064488 C0064471 C0064471 Rep C0064472 OKLMN-GW-W20-0-050309 OKLMN-GW-W20-0-050309* OKLMN43W-W2043-050309 Dup OKLMN-GW-W22-0-050309 OKLMN-GW-W22-0-050309* OKLMN-GW-W22434350309 Dup 13900 10700 10000 36600 32200 37500 12900 9040 7660 31400 29600 25700 46600 36300 30100 45800 34000 28100 285000 243000 190000 317000 301000 244000 'Lab oratory D uplicate ND = Not detected et or above 26 ngfl_. NO s Mot quantifiable = M easured concantratfon between 25 ng/L and the Lim it of QuantttaBcn (LO Q ) which w So n jfL . Exygen Research Page 22 o f 110 000045 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table I. Exyo#M D Summary of PFBS, PFHS, PFOS and PFOA in Water C lient Sem ple IS Samples Continued Analyts Found fppt, ng/U C4 Sulfonat PFBS ce Sutfonst* PFHS C8 Suttonat PFOS CS Ackf PFOA C0064475 C0064475 Reo C0064476 OKLMN-GW-W31-0-050309 OKLMN-GW-W31-CW50309* OKIMN-3W-W31-0-050309 Dup 1300 1360 1360 5130 4780 5190 132000 132000 156000 23100 22300 24900 C0064478 C0064478 Rep C0064479 OKLMN-GW-W324MS0309 OKLMN-GW-W32-0050309* OKLMN-GW-W32-0-050309 D ip 2180 2290 2960 3000 3120 2940 47100 44400 83000 117000 93300 125000 C0064462 C0064482 Rep C0064483 OKLMN-GW-W217-0-050309 OKLMN-GW-W217-0-050309* OKLMN-GW-W217-0-050309 Dup ND NO - ND NO ND ND NQ NQ 128 NQ NQ NQ C0064486 C0064486 Rep C0Q64487 OKLMN-GW-W20084KI50309 OKLMN-GW-W20O5-0-050309* CKLMN-GVV-W20084V050309 Dup 6780 7170 ' 6930 10100 10800 10300 15500 17800 18800 59300 58700 60300 C0064490 CC0644S0Rep C0064491 OKLMN-GW-W2012-0-050309 OKLMN-GW-W2012-0-050309* QKLMN-GW-W2O12-O-O5O3O0 Dup 2210 1960 1920 4700 4470 4420 117000 118000 139000 48900 46400 51400 00084494 C0064494 Rep C008449S OKLMM-GW-W80-0-050339 OKIMN-GW-W80-0-050309* OKIMN-GW-W80-0-050309 D ip ND ND ND ND ND ND ND 302 ND 280 NO 328 00064498 C0064496 Rep C00644B9 OKLMN-GW-PYV1-0-050310 OKLMN-GW-PW1-0-050310* 0K LW N J3W -PW 1-0-050310O 4) 5620 5650 5560 4180 4150 4170 66900 71600 70900 37300 39300 39100 C0084502 OKLMN-GW-PW2-0-Q60310 641 501 351 3630 C0064502 Rep OKLMN-GW-PW2-0-050310* 624 491. 383 3890 C0064503 OKLMN-GW-PW2-0O50310 Dup 894 700 303 5160 00064800 C0C645O8 Rep C0064507 OKLMN-GW-PW3-0-050310 OKLMN-GW-PW3-0-050310* : OKLMN-GW-PW3-0-050310 D tp 6970 6740 6570 ' 10000 - 9740 9990 32700 25500 32300 177000 160000 176000 00064510 C0064510Rep C0064S11 OKLMN-GW-PW4-0-050310 OKLMN-GW-PW4-0-050310* OKLMN-GW-PW4-0-0SO310 Dup . 8130 7700 7810 7890 7480 7550 33800 30300 27800 72100 67800 65900 00064514 C0064514Rep 00064515 C0064518 C 0064518R sp C0064519 OKLMN-GW-PW3-0-050310 OKLMN-GW-PW8-0-050310* . OKLMN-GW-PW6-0-050310 Dup ': OKLMN-GW-PW10-0-050010 OKLMN-GW-PW10-0-050310* . OKLMN-GW-PW10-0060310 Due 7930 8000 8130 13100 12700 11900 14500 14600 14600 29200 27400 26800 90000 86000 66400 1400000 1700000 1740000 78400 78700 78500 719000 781000 814000 CO064522 CQQ64522 Rep C0064523 OKLMN-GW-PW11-0-050310 OKLMN-GW-PW11-0050310*; OKLMN-GW-PW11-0-050310 Dup 6520 6490 7150 .. < 8820 10000 9050 40800 50600 43400 60300 71600 60600 C0064526 C0064528 Rep C0064527 OKLMN-SW-0-050310 OKLMN-SW-0-060310* : : OKLMN-SW-0-050310 Dup i-V NQ NQ . NQ NQ NQ NQ 1190 1200 1270 491 529 537 C0064530 OKLMN-GW-TRIP2-0-050310 ND ND ND ND 'Laboratory Duplicate NO = Not detectad at or above 25 njyL. NQ * Not quantifiable = M easured concentration between 25 ng/L and trie Limit erf Quantitation (LOO ) which is 50 ng/L Exygen Research Page 23 of 110 000046 Interim Report #1-Analysts o f Oakdale Water Samples Exygen Study No.: P0001400 Table H. Matrix Spike Recovery of PFBS and PFHS in Water Samples S a m p l* Oaacrtpdoi C * SuKaM ta PFBS Amount Amt Found Amount S p lk *d InSwnpi Rtcovtrtti Recovery (%) Amount Splkad MJ C * Sutton* PFHS Amt Found Amount fnSorapl* R*ccv*r*d Rneuvnry fnflft.) (0*4 t%) O KLM N -O W .W O -tW IW lO <CM *M M 3pfcC,0ngfl-W b9p*a> OKU*N<GW-W9-0-06tt10 ICM W W I* 0 .90M0 itg /LLab Spike) O KLM N -G W -W 3--05C3fO tow S tfik a 5 p pb <000*449*.* m ntft held Spike ) OKLMN-GW-W3~0-W10 H ig h S p ilt* 50 ppb (COMeeer. MM)n^Ln e ts Spike > 5000 50000 5000 50000 312 312 312 312 6960 87400 7450 74700 133 5000 134 50000 143 500C 149 50000 102 162 162 162 5130 47500 5140 54400 99 SS 100 106 O K W W H JW -W I-0-050310 (CtMM440f Spfc , 9400 aqA . L a * Spike} O K LM N-QW-W8-0-4WW 1 & [COOiMfia 3 |*F .flM M 4.La * Spike! OKUWM3WMW-04903ia LOWSplk* 5 ppb (co rn u to . 5oe ng*.Frausp it > OXLJdW3W-WB-0-6S031&Nfflh Splk* 60ppb fC00*M U , 0 W npl FtoUSpille ) OKUffN45W-W2*4<O$O310 {G00M412 S *k 0 , SOOOnpC U k 8pHw) O K U *N -G W -W -tM )W 10 (COOM412 Spfc H, 90000 n * L U b SpttaJ OKU4HKJW-WWLO-060310L ow Splk ppb JCMM414.tiMO ryp/LFieldS p ila ) O K LM N *3W 'W 28-# -M 0310 H ig h S p lk * SO ppb (CMB4419, BOOOtin*n. FMd Sp ira ) 5000 59000 5000 50000 5000 50000 5000 50000 57.0 57.0 57.0 67.0 73400 73400 73400 73400 7020 70000 7410 70500 73100 125000 79200 147000 138 5000 146 50000 147 500C 141 50000 ND HD ND ND * 5000 222000 103 50000 222000 . 5000 222000 147 50000 222000 5120 51400 5610 53300 207000 252000 210000 266000 102 103 110 107 * O KU AN -G W ^ W 33-0-0M 1D (C W II1 I ftp * i, 9000ffp L Leb Spike) QKLMN-GW-W33-0-050310 (OOOSMII Spk J . SO n p i. Lab Spike} O KLM N -G W -W 13-04)6031Q Low Splk* 5 ppb <004*4411. see* a p t Fld d S^ Ira ) O K IJyiN -G V V < W 4M )B 03l6 H lp h Split* ED ppb (C606M 1*, MOO*ngfLField SpHra ) 5000 50000 5000 50000 28600 29800 20800 26800 33000 133000 38700 106000 5000 82300 212 50000 82300 - 500C 82300 162 50000 82300 78000 122000 65200 150000 59 115 0KU4N-W *W 2 0 W )-0 3 i D (COOM430 B j* K . 5000 n p L Lab S p it* ) O KUM N-QW -W 20*4W )6310 (000*4429 Spk L , 90000 n fl. la b S p in ) O K LM N *G W -W 20B^ M )510 LOW Splk S ppb (CDoeeeaa. u m nql r u t *fk > Q KLM H 43W -W 2064M J5C310 M g h Spit* 60 ppb {cooeeeas, so w o p i. n *ie S p i* > 5000 50000 5000 60000 8200 8260 S26A 8260 15400 72500 15200 82600 143 5000 740 126 50000 740 130 soon 740 149 50000 6740 12500 53100 11 BOO 60600 115 93 101 106 0 K LK N > S W -W 3 1 W 4 )5 0 3 M (C90M41490fc M, WOO n p L le b SpOra ) O KU A N -S W -W 2tt-0-06010 |C M *44SpkN ,M 0M np> LLab S p iU ) 0KLM*M3WW21W-0W1Low Splk 6 ppb (C0M442, 5 K npiL Field Satira > O KLR W W SW 4V 21M -D C 310 H ig h Splk* 60 ppb (CeeeeAZF,SU M &L Ftek* S p i ) 5000 50000 5000,. 50000 601.0 801.0 801.0 dO t.O 7200 67200 072 86000 126 5000 133 50000 118 5000 132 50000 760 799 769 709 5280 9D300 5240 48500 90 99 89 96 reafctue exceeds Ihe spiking lev) N pnlfcany; Iheretote, an accurst recovery value cannot be calculated h o Notdetected at or above 25 npA. (ppt)NO - Notquarfiabl* M easured concentration between 2$ rg& (ispt) and d ie Lim it of Quantitation (LO Q ) which is 50 ng/L <ppt>N ot*: S in t* th is uinm ary a b le sn o w * rounded r u u iU , recovery y a k may v a ry ilg M iy from the v a lu e * in the raw data. Exygen Research Page 24 of 110 000047 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 Senspk Deecriotton C4 StiNFoM inPFBS CSSulfonete PFHS Amount Amt Found Amount Amount Affit Found Amount Spiked InSemple Recovered Recovery Spiked bSample Recovered Recovery OH#. (<"-> m tfu (%> ma-) 894 w OKLMN-GW*W2C1MW80310 (Coo*M2oSekC.ieoeAaB-ue 9&uw) OKJJHIN-GW-W2010-^OSO310 (Caoeeeaa $* o, swo# r^uab Sptte) OKUW-GW-W201O-0-0SW1DU w Sptk* S ppb (CM*443*.300# HgA.HeWSpU J OKLMN-GW-W2D1M-06M10 Kfflfl Spfc SOppb iceeea. eeeoo fmuSette > 5000 50000 5000 50000 NP ND NO NO 6500 68500 6700 63600 132 5000 138 50000 134 5000 12B 50000 NO NQ NQ NO 4600 48700 4700 43700 86 97 94 87 OKU*M43W-PW74WMiai0 feoeM32apeUOOCn^LU*3pw | OKLMIH3W-PW7-M5O310 (CM044S2Spftf. fOOMngAiteb Sp&e) OKLMN<rW4W7-C-OSOai0 LowSplke 6 ppb (00*14*4.SaOOnpLFMMSette I OW-MN-3W*PWr43^WW10 High Sette se ppb lCoeem,*eooi) ngn.nieSpntel QKL14N-GW-TOP1-0-010210 Uw Spile* ft pph <C0H44*7,eeoepgA. HeieSpftu) QKLMN-GW-TRIP1-CMIM310High Spike SOppb jcoeauat,fono* ngrt. Rei*spo } 000 50000 sa 50000 5000 50000 4400 4450 4400 4400 NO NO 12200 72800 13200 60000 6540 44400 156 5000 4600 137 50000 4600 175 5000 * 151 50000 4600 131 5000 NO 88 XX ND 8310 50800 0370 59000 4500 46100 90 62 91 106 92 92 0KUS*6W *W S44niO <Ceo4442Sek6. SOMnpL LebStSke> OKUIN*GW*W**0#0310 (COOM4429p* H.KMNMrtlLLa*Bette) OKLMN-GW-PWS-0-05W10 U w SpHtsS ppb (C0OM44.saoen*LFleMSpila > OKUWWW-PW8*PO5031CHigh Splk* 00 ppb (CC0I444S.SCOOOnoB.FbWSette | 9000 GOOOO 5000 50000 13300 13300 13300 13300 21400 70700 21000 80700 162 5000 23800 133 50000 23800 154 5000 23600 135 50000 13800 28700 70300 30000 78100 118 83 124 105 OKUNM'GWMW'O-osam tcoeeu*# 8tt I, SOMngA. Ltb S?Um) OKU*N43W4WMMIHUia (Cmewe S|M4. oeoene^LLe*Sette) OKLMN-GW-PWt-0-d*W10 Low SpQt#Sppb (Ceeeeeee,eoenpLneteScue ) OKtMN-OWHWO-OBOSIOHigh Splke SOppb <000*444*,MPQQnglt FWdSpbe> 5000 50000 5000 5QC00 2110 2110 2110 2110 0280 66900 8280 74900 144 5000 5160 134 50000 6160 144 5000 5160 146 50000 5150 9310 64400 8350 64800 83 98 64 90 0K1JMN-GW4**1IK<4MMH16 1COOO4BSftt K.BOOOneA.Ub atte > OKLMN-OW-WS102-0-0501* (Cooeetiositel.aoeoene*,ut apike) OKLMN43W>WC102-aOOOMOLow SpHu 0 ppb {CQObUCLSOMQA.FieMfSfM | OKLMN-GW-W102-O-0S0310 High Splke 90 ppb (000*4493,*0000 eglLFleid Botte | 5000 50000 5000 50000 NQ NQ NQ NQ 7360 7500 7120 70700 : 147 135 <42 (41 5000 50000 5000 50000 ND ND ND ND 4890 47400 5040 50600 96 96 101 101 'Sample reedueweeds (hepifclnQtevelgnffleanty;thereof, an accuraterecoveryvalue cannotbe ceteiiated NO * Notdetectit orabove25 nglL {ppi). NQ 3 Not QuottftsOte = M easures ooncemraflon between 25 ngA. (ppQ and fte U srtt of Quanttattofj{LOQ1whichI50mjA. (ppt). N ote: S in ce itila a u irw ie ry tab le show rounded re su lts, reco very va lu e* m ay va ry v p itiy fro m d ie wetuae In th e rtm data. Exygen Research Page 25 of 110 00004S 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 templa Daacrlpdon G4Sulfonate f>FBS C* SoifonatnPFKS Amount Amt Found Amount Amount Ant Found Amount Spftad Intemp* Recovaras R*COV*ry spited InSompIo Reecverad Recovery <"4.... <q/14 M tn#/L> Ino/U <n/U c*> OKIMN-GW-Wtl04-0-050*10 (C044M1*W.900 Ute9pte1 OKLMN-GW-Wf1O4-P-030310 (CMMtei SpKN,som nl LabSpite) OKLMN-QW-W1OAO-OW10 Low Spike Sppb (C0MA4M,SOMr\&LFMtfSpite > OKLMftGW`Wia4-P4GOS1Q HiflbSpite ppb fC0flSA487sS0060apt-FI*WSpite \ 5000 50000 5000 50000 NQ NQ NQ NQ 6680 73000 6730 60700 134 5000 146 50000 135 5000 139 50000 NO NO ND ND ' SOSO 48000 4720 51200 101 96 94 102 OKLMN-GW-W20t-C-0OS10 {COPOOSl SpfcC,WOOnpLUbSplte ) OKLUN-GW-W201-8-956316 (C0M4434Spk0. ffWngrt.LabSpft*) OKU4N<JW-W*201-(M)5W10 Low Spite 0,5ppb <CaSS44S0,soe FMdSpite) OKLMfMW>W62610-956316 HlflbSplka 5 ppb (CMM441, Sloe ngfLRaidSpite ) 5000 50000 500 5000 74.0 74.0 740 74.0 6360 66600 877 7560 130 9000 131 60000 121 600 150 5000 ND NO ND ND 4610 44400 543 5360 92 68 109 106 QKLMN-GW-WZO-O-CSOJM (CpOeMarSpbE.SBOOng'LLabSpite} OKLMN-GW-W30-Q-6SOS9 (CWP44P7Spkf, MWa#L UbSpite) OKLMN-GW-W20-4-080306Low Spike 9 ppfa {CMS4M*.500*i l RaidSpite) OKLMN-GW4^20-0-050309 Hltfi 3pflK ppb tCOOMtnLsooooi^l noiaSpite) 5000 50000 5000 60000 13000 13000 13900 13900 19400 77100 20900 85000 110 5000 12900 126 50000 12900 140 5000 12900 142 500C 12900 16200 56200 16200 48400 86 65 8 71 OKLMN<GW-Wa24&030* (C00444718pK0,9009 LabSpite) OKU!N-GW-W220.ft5IMn9 (000*4471 SpKn,50000rqfl*US Spite) OKLMN-GWW2--05M06low Spite* ppb (COOtOft,5000nqfLFWdSpite > OKLMN-GW-W22-Q-MO306 Hlflh Spile ppb <CO0t44?4.50000pH.FtedSpite ) 5000 flo o o o 5000 50000 36600 36600 36600 36600 44100 109000 44000 111000 5000 31400 145 50000 31400 5000 31400 149 50000 31409 37000 73000 35000 62200 * 83 62 OKLMN-OW-W31-0-P5OM9 (C00SU75Spit 1,5000nglLLab Split*) OKLMN-GW-W314-0EO3Qt (C0DC447SSpkJs50000rtpTLL*bSpHw) OKLMN-OW-W11-M50MP High Spike H ppb (COOW477.50000ngff. FtaMSpite} 5000 60000 50000 1300 1300 1300 8450 70500 90900 143 5000 5130-' 138 SOCCO 5130 179 50000 5130 9090 51200 63200 7B 92 118 OKLMN-GW-WJ2-0-50M (Ceoe**7aSpaK,sew pit.LaaSpite) OKLMN-GW-W32-0-6503C* (CMM47BSpKL.50000aprt.L*b8friX*> OKLMN*GW-W324)46030B Low Spite 5 ppb (COOB44M.4000ngfl.Fl*toSpiteJ 0KLMN^0W-W32-0-teW Wflb Spite SOppb {C00M4I1,SOboOP0L noteSpite 1 5000 60000 5000 50000 2160 2160 2180 2180 6910 67300 10800 66500 136 5000 3000 130 50000 3000 172 5000 3000 127 60000 3000 7400 50000 7910 52800 66 34 98 100 'Sjw tpLe re sid lace ad a the apflcing le ve l m rtfleand y: theretom. in accurate recovery value cannot be calculated ND * Notdetected a t Of bo-v* 25 ng/U (ppt). NQ Not quaniiSa&Us = M escured cw cantrafio n between 25 V L (ppl) and the UTO d Quantitationfl-OQ)which 50ng/t (ppt). Note; 9tn ca th i* au nim iry tabte sho w rounded re a u to , recovery va lu ta r a y vary alg h U y from the v a l a s In Uta raw date. Exygen Research Page 26 o f 110 000049 Interim Report #1-Analysis o f Oakdale Water Samples Exygen. Study No.: P000I400 Table II. Matrix Spike Recovery of PFBS and PFHS in Water Samples Continued Sampl* OmctlDti C4 Suffimie PiFBS Amount AmtFound AlRMHlt Spiked in Sample Recovered Rpcavaiy W -> <%> Amount Spiked Cl SuHomrtePFH5 Amtf:CNMKt Amount in Sample Recovered Recovery CnaX) m vu ...... <%) OKLM*FOW-W217-0-O5WM (C0M4413 $pk M.90M no^ Ub Iplke> 0KLMH*GW-W3rt7-0-0603M (C<oa44aapkMtsoeaRafLut4e*> OKLMN-0W*W2174-050300 Low Split* 8 ppb fee**,9*oongi n*w3*"* > 0LMfWJW-WaiT-0-0<JWa High spike SOppb (CDW*,eoeoongfl.FW Sake 1 5000 50000 9000 50000 NO ND NO NO 0630 66800 7570 71200 134 5000 134 50000 151 5000 1 50000 ND ND NO ND 4680 46500 4590 51300 96 93 92 103 OKU*N-OW-WM#M*WW (CMM4M Si* a 8000o0.Ub Splhe) OKUW4-OW*W200V^-0MM9 (CaOM SM SpkP. SOOMepiLLW i Spike) OKLWN-OW-W2MS-0-OSIUOS U rn Spike 5 ppb tCM tM M , BOWngl FW Spit) OKLMN-GW-W20M-0-4M30S High Spike SOppb tCOOSHH, BOOMba*-RaidSp ike) 5000 50000 5000 SOOOO 6780 6780 5780 8780 14300 73600 18S00 37900 150 6000 10100 134 SOOOO 10100 194 9000 10100 162 50000 10100 16000 56500 19300 84BOO 1TB 93 164 109 OKLMN^3WWV2d12-0-OSOaOO fC 0 0 M 3 p * c . s m t * n u e s ik j OKlMM-GW-WiOIM^lSCISW (C*eM4eSpk o , soooea^ L Lab Spiiei| OKLMN-GW<Wa&12-0-OS3( Low Spite 5 ppb (ceoeeMa,eootn y t n*M spn) OKLMN43W-W2M2-C-CH30High SpikeSOppb te w e tw , 59000 n p L field Spike > .5000 50000 5000 SOOOO 22W 2210 . 2210 2210 6600 66400' 8210 71500 132 , 126 5000 50000 4700 ' 4700 120 5000 . 4700 139 50000 4700 6140 46900 6950 53800 69 65 96 OKLUN-Qty'WKMM)B030B (C90$4m spk , twonot. U P S p U ") OKLMii-SVkLWSD-O-OUOO 000*44*4 8 f* F . 9*040 n p l L*U B p tt) OKJLMN-OW-WiC*0*S0009Low 3 p lk 5 ppb <COflB44M. SOM * * 1 R *kJ Bptb* ) OKLMN>4W-WN-O-aS00CftHigh SpikeSOppb tCOOMCtr. MOW ngfLnt0 3pik ) 5000 30000 5000 50000 ND ND NO NO 6850 64700. 7390 .t 69700 137 m o 129 SOOOO 148 5000 13 50000 ND ND ND ND 4960 46200 5200 49200 100 92 104 96 OKLMN^W-PWI4-05031* (C M M M I Spk G, K M n fJL Lab 8pUt) OKLMW4W4W14-O0O310 p t t u ia i * * h , BOOM e l Lee * f* e > OKLMN43W4W144S03M LOWSpike 6 ppb 6*044400. 0 0 n g l " Sp ite ) OKLMN-aW-PWt-O-O60308 High Spike 00 ppb (tsoMsot,joeee el Fw$e*w 1 5000 50000 5000 50000 5620 5620 5620 5620 13600 72000 13100 69700! ISO 5000 4160 133 50000 4160 150 5000 4160 126 50000 4160 8860 52000 7690 47700 94 96 71 87 OKUiM>aW4>Wa-M)S031 (CtWUMaSpfc1.COOPn p l Ud> * p * a ) OKLMKKSW4>m44SM10 tCMM*02 3** 4, fioomft*LU P Spa* ) OIOSdN-gWf*V24o3io Low spike S ppb 90M4SM, M * *1 R*4d Sptfc. ) OKUiN-aw-PWi-o-otojia hhqi>sp* so ppb (CM04MS.aoftcoegft. PWd Spile) KXJO 64t 50000 641 500CT * 641 50000 641 7720 65900 7030 64300 142 5000 131 50000 126 5000 127 50000 501 501 501 501 5280 47700 5190 44300 95 94 94 69 'Sampleresidue w eed * the spiking le ve l signA cani^ ; Therefore, *n accurate recovery value caonet be calculated NO Motddttoecor Steve 25 nqfl (ppt). NQ e tat*iar6iabie * Mewuradconewitraiton brtwaen25flfl/L(ppt)aivittratJmitcrf Quantitation <LOQ) wNch is 50 n g /l (pplL N ote: lin e IN * iu t m *fy table ih o w e rounded re su lt*, recovery valu e* m ay vary *ityh tly from the va lu e s in th e raw data. Exygen Research Page 27 o f 110 000050 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 Sample Descrlptor OKU4N-GW-PW-0-060310 {C0eM8M9pfcK,SOMftfifl.Let Spike) OKLMN^W*PWS-9-0gS1O (COOSiSOSSpkl. SOngA.LebSpltot 0KLMN-RW<FW34>-0S*31 Low 8plke 5 ppb {CCflMCOf. MMngn.fmmSpnte) 0KLMN-GW-PWJ4WM11&HlffhSpike50 ppb {COOMSbt, SMOOepiLneldSpIlte) C4 Sulfonate PFBS C8 Sulfonate PFHS Amount Amt Found Amount Amount Ami Found Amount Spiked li Stempia Rncwwnd Recovery Spiked InSample Recovered Recovery m ("VU (noiU %> (non.) (no-! (ns/L) <*! 5000 90000 5000 50000 0470 8070 5970 6970 13600 90900 15200 92300 137 5000 10000 160 50000 10000 165 5000 ' 10000 171 60000 10000 13600 54400 16300 54900 72 89 126 ec QKLMN-GW-PW44WW310 {CMMS1SSpaM, 9000 non. Lab Spike) 0 KLMN-GW-PW4-0-OSM10 (COMMI8*kN.90100sort.Ub Spike) OKLMN-QVhPW4-0-040410Low Spike 3 ppb (C0C44512,SOOOn*LFieldSpike) OKLMN-GW-PW4-Q-6W10 MghSpfceM ppb {C0W313, WWTO9rt_fleWSpike) 9000 50000 500C 50000 6130 6130 6130 6130 17400 95000 16300 66900 165 5000 7890 174 50000 7880 163 5000 7890 102 50000 7890 13900 53600 13500 58200 120 91 112 101 OKLMN-6W-PWI-M40310 {COOMM4SpkO,9000n^LLabSpike) 0KLMN-CW-PW445O310 (C0M4S14SpkF.MOOOnpLLtbSpike) OKLMN-GVhPVM-OWSIOLOWSpfc* 4 ppb <000*051.SOOO*wt new Spike3 OKLAIN*W*PW6*(Ml60&1OHighSpike SOppb (COOUS17.JOOOOnpl HeMSpike) 5000 50000 5000 50000 7930 7B3C 7930 7930 17200 60500 17100 &46C0 165 5000 14500 166 50000 14500 163 5000 14500 173 50000 14500 20600 58800 20800 59400 122 89 128 90 OKLMN-GW-PW10-0-031D (Coeoeei9pkCteoew'l Lab Spike) OKUMN-GW-PW104-050310 ICOOMOMSek CLSOWOnpiLUb Spfiie) OKLMN-QW-PW10-<MU0410Low Spike5 ppb iCMMMaae,OOagit FieldSpike) OKLMN-GW-PWlD-0-05310 High SpikeM ppb (CDM4021.SMOOepLfWd Spike) 5000 50000 5000 50000 13100 13100 13100 13100 19300 70700 19000 74000 124 5000 29200 133 50000 29200 118 5000 29200 122 50000 29200 34300 71000 33500 71300 102 64 B6 64 OKJLMN-QW-PW11-0'OSW1C {COeSMZZSpkE.9009npl LabSpiket OHXMN-GW*PW11-0-MOJ1C (C0SO22Spbr,eoo nLLWSpike) OKLMN-GW-PW11-0-050310 Low Spflca $ ppb {000*19*. OOMnyLField Spike ) OKLMN-GW-PW1I-0-050314High Spikep p b (cooeesas. sooeoqil neid spike> 5000 50000 5000 50000 520 520 S20 6520 12700 60300 13200 63600 124 5000 8820 124 50000 8820 134 5000 8820 114 50000 6820 14200 65100 13300 54800 10Q 93 90 92 "Sam ple rse ick * exceed iris splicing le ve l sigmAcanAy; therefore, an accurate recovery value cannot be calculated NO > Not detected a t o r above 25 ng/t ipp t). NQ 3 Not duwitHtebte = M easured concenM fcm between 2$ n p t (ppO and h e Urrrtt of Quantitation <LQG) which b 30 ng?L (ppt). Notm S in ce th is sum m ery table e lw w * rounded r e e u ti. reco very v a lu e s m ay vary lig h tly from th* value* In the raw data. Exygen Research Page 28 of 110 000051 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: PQ001400 Table II. Matrix Spike Recovery of PFBS and PFHS in Water Samples Continued Sample CaacflpBon OKUW -sW itwwm <coo*m * * 0.4*00 *9*. Lab8pa> OKLMN^W-O-omiO (C0N4S BpfcH. ONngft. Uri)Bp ) OKU4N'4W-0-W0310 Low $pfto Sppb (COOMO,Mao*v*-*MApt } OKLMN-SW-0-050319High Spit* BOppb (COOMB**OtMftn.FM4S| ) OSuMMUMPfBS C* SuMonatt PFHS Amount Amt Found Amount Amount Anil Found Amount Iptod InSmph Recovered Racovary Spfltad in Sample Rocovurod Racovary w (no. (ngfl.) > ._ .. m in * i%> 5000 50000 5000 50000 NQ NO NQ NQ 5900 93800 72*0 65000 120 6000 128 50000 145 5000 130 50000 NQ NQ NQ NQ 4790 45100 5250 49400 96 90 105 99 OKUWJW-TKlP2--06M1i>Low SpHta s ppb (C0MB>1.6000aalL 1 OKLMtM3W-TiaPZiMC0310 HJQhSplko0 ppb (OOKMSB,WM itf*. 50t*\ 000 50000 NO NO 4480 20100 90 5000 NO 58 S000Q NQ 4970 49000 98 9 Avaraga: 141 Standard DavtaUon: 21 SamplaresiduatwaadalwaiildnB lavai darifcarty, mere, an acculale racavaiyvsluaeannol tiecsfcuMsd NO Moteeisctsdsiorai>ove25neA.(pp(). NO . NotquenMablc.Msesvadoonce'irtraitonbetMeanZSngS.fepQandltielJiritar Quapwaaon(LOO)101B90 ogrt. (ppi). Nota; Mutatataatumnaiytatuashows roundedreauHe,recoveryvalua*mayvaryillgMIy from tha vatuaa Siatto rawOsta. Avuthp; Standard Davlalkm; 6 1C 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 Sample Description Cl Sutton* PFOS Cl Acid PFOA Amount Amt Found Amount Amount Amt Found Amount SpIkMl In Sample Recovered Recovery Spiked InSample Recovered Recovery JoglLt tr&Lj (ngn.) t%t (ngfl.) (null) from (It) OKLMN-GW-W3-C-05O310 <CM M 4ftpk C .< O tO o 0 LL& b *tl) 0KLMM-GW-WMH1S 1 0 (CDOVMMSpk 0 .3MOO ngrt. l*& M M ) OKLMN-CW-W3-0-O5O31OLow Splk#5 ppb ICHM4M,SOMD O l FtoW M M ) OKLMN-GWAV34H15W10 High Spikft ppb {CMM4407, MOM 19II.FkidMM \ OKLMfkGMM-0-09031t (CM444CC Spk P, MMng*L.Lab 5 p lh *) OKLM*GW-W-0-031I> (C M M 4 M *p k F .B M M a 'L L a b M ta ) OKUtlN-GW-W8-C-O5M10 Low $plk* 9 ppb (CMtnn, com m l Fi*m m m ) OKLMN-GW-WMWM310 WghSplk* ppb <00004411, OMOOnplLPMOSpikl) 000 50000 5000 50000 5000 50000 5000 50000 475G 4750 4750 4750 59.0 56.0 66.0 59.0 12400 73500 10900 84500 4940 55000 5380 S0500 153 5000 138 50000 123 000 160 50000 98 5000 110 50000 106 5000 101 50000 6330 8330 330 330 290 290 290 290 11900 59200 9470 40100 5360 51900 6060 36300 111 106 63 80 1C1 103 115 77 OKLMN-GWW20-Q-0M31Q <000044138pfc 6, M M n g fLU b M*>) 5000 13500000 9450000 * 5000 79300000 65300000 OKLWN-6WW2WJ^5031b (00004410 S f* H , BOOM ft. ^>b M M ) 50000 13S00C00 7390000 50000 70300000 68300000 OKLMN-GW^W2*-0-0M310 Low SpJk*5 ppb {C0004414,MMrtpft.Ffrki Oplto) 5000 13500000 9050000 - 5000 79300000 73100000 OKUttl^W-Wi8-0*5W1 High SplkP 50 ppb (CO M M IT MMO ttQfi FW4SpH*) 50000 13500000 7210000 50000 79300000 57900000 OKLMN-eW-W3Wr-050310 <CMM4148pU MOOnpft.Labpika ) 5000 4610000 4720000 * 5000 1750000 1520000 OKLMN-GW-WS3-0-O3W1O (COO94410Spk 4. 50000 Aftll.LbM M ) 50000 4610000 4730000 50000 1750000 1650000 OKLMN-GW-W33-0-050310 U m Spile*5 ppb <00004444MOftapTLR*k4S0k > 5000 4610000 4820000 5000 1750000 2350000 OKLMN-GW-W33-0-050310 High SpOtt 50 ppb {C0004411. MOM npILFM d fipttn) 50000 4610000 4520000 50000 1750000 1630000 . * * OKLMN-GW-wzowaimo (ceosscioSpsn. sms sgiLu s Spu) OKLMK^JW'W205-4V-050310 (C0004420OpbL,4MMnpft.LabMM I OKLMN45W-W2W-0-OWMOLow Spike 5 ppb (CM 94423,5000 n gfl. fltid SpU u) OKLMN-GW-W2054HKQ310 HfflfrS p tic SOppb (C9M 4433,300M ngO. FIvJd M * * ) 5000 50000 5000 50000 146000 146000 146000 146000 138000 166000 129000 221000 500 20 50000 5000 150 50000 147000 147000 147000 147000 160000 190000 143000 184000 - 86 74 OKLMN43WW15-04W031O {CQ0C44MSpk M.00MUp. L ift S p rt*) OKLMNriSW-W215-0-O3C310 (C M M ttS f* N. 50000 A tft. L ib Splba) OKLklN-GW*W215-0-050310 Low Splk* 5 ppb {C044M 00 n p l. Ff*W M b * l Ota.MN-GWW*S154CM0J10 High Spike 0 ppb |C SM 4I7. new SOIL FMdIp ilB ) 5000 50000 5000 50000 37100 37100 37100 37100 52400 96SOO 50600 101000 5000 120 50000 5000 128 50000 4400 4400 4400 4400 8850 55700 9600 '38200 0 105 35 70 Sam ple residue B a se d ll>e spiking le ve l g nifirantly. therefore, ap accu rate recovery vd u e cannot Be calculated NO Oslscurd a<or ibove 25 r^ L (aptl luQ . Not Quaotifippte > M easured co ncentrator hetween 25 rvjA . (p p t)aed the lim it of Quantitation (LO Q ) w hich is 50 n o il Ippi) N o d : S in ce th is au n vn ary U D Ie sh o w s ro u n d K l re su lts , re trw e ty v a lu ta m ay vary slle h tty from the v a lu e s In the raw data. Exygen Research A Page 30 of 110 000053 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: PQ00140Q Table HI. Matrix Spike Recovery of PFOS and PFOA in Water Samples Continued Sampla OwertMlon C8 Sulfonate PFOS Amount Amt Found Amount Amount Spited InSwnpl* Recovered Recovery Spticed w tntfL) .... pgft-i_____ (nflfl.) C l Add PFOA Ami Found Amount InSimpI* tteCOVOFKi Rccovary P W (ntfL) . t%) OKLMN-CW-W201tH3-0Mi0 tcaeeMi*apkc. aooo nn.ub%ik* > OKLMW-GW-W2010-C-05M10 tcee*44at spao, csoao l*apt > OKLMhHSW-W2010^-05&310Low Splkft 8 ppb {CC0*443e. MODe^L RMByte*> OKLMN-GW-W201WFOIOttO High Spfca 50 ppb {cnMMn. som *#. FtoMSo I 5000 50000 5000 50000 . NO ND NO ND 5170 54600 5270 54900 103 $000 109 50000 105 5000 110 50000 NQ NQ NQ NQ 5290 54300 4710 33300 106 108 4 65 OKLMN-GW-PW7-O-0SC310 (C0fe*4*2 S|*E.3WWLUtpa) 5000 71600 78500 woo 37600 OKLMN*0W*PW7"<WMO310 (0WK4 SpkF.sseee aglLUb a#e ) 50000 71600 119000 95 50000 37600 OKLMN-GW-PW7-O4W0318Low Splh* S ppb teeeee*.oe ngruFWdSen i 5000 71600 72600 . 5000 37600 OKLMN-GW'PW7-0-dS03IOHigh Spike SOppb fcoeeteas. seaea as*,new spa ) 50000 71800 118000 89 50000 37600 41900 86100 42800 67100 * *7 * 59 OKLMfMWTTOPi-0-05C310 Low Spike 5 ppb (CflMSter.aao*m^LFtawleu ) OKLMN-GW-TR1P1-0415031IJ High Sptk* 56 ppb (<XIHM3I. SOHOalkFWdSU) 5000 50000 ND ND 5780 53500 116 5000 107 50000 ND ND 5360 50500 107 101 0KLMN-W-W*-O4W0J1CI tco*4tu *f* o. bom.on. u t pa ) OKLMH^5W-PWa0090S10 (CWMWSpk H.twwa npL LabpNNl OIOMIiW-PW-<MWla Low Splkb 5 ppb (CPM4444,X H apl FWU6pn) OKLMN-GW-PW5-9-P30310 High Spile SOppb {00*4445, SONOnpfl FMdOptea) 5000 50000 5000 $0000 34300 34300 34300 34300 3B500 89600 38400 63100 - 5000 t u 50000 - 5000 166 50000 61400 61400 61400 61400 61000 113000 59300 82200 . 103 42 OKLMM-GW-PyrtMW>50S10 <CeOM4W3|B*J,W''9'lUb*i*te> OKLMN-GW-PW-<W>50510 {000*4440SpkA 0 *0A Uft Spilte) OKLMN-CW-PW94W0319Low Spike S ppb (C0M444*.MWo^l FtaklSpite J OKLMN-GW-PW9-0-050310High SpRw 80 ppb tceeewa, SO**rta-nwe se> 5000 50000 5000 50000 64400 84400 84400 84400 83200 136000 96400 178000 - 5000 107 50000 - 5000 1*0 50000 49000 40000 49000 49000 50400 97900 55200 93200 96 80 0KLMN-GW-W6102-0-050310 (CC04M4SOepicK, SON*gA. Lab9*11 ) OKLMN-GW-W6102*0-050310 (C0N44W8plrL.aeNnBA.Lah Spite) QKLMN-GW-W8102KI-05W10 Low Spfca 5 ppb tceeewa.w*a*A.Fteo* > OKU*fWJW-Wi102-0-W0310 Hlflfl Spike 50 ppb (COM*.** eft- FieldSpite | 5000 50000 000 50000 NQ NQ NQ NQ 5300 55800 5480 53200 106 5000 112 50000 110 5000 106 50000 214 214 214 214 5880 52700 5610 35300 113 105 108 70 Sanpte reetatoe axcaads ft*apiunolevel apniflcamfy; therefore, an accurate recoveryvalue cannotbe calculated NO * N et detected a t o r aboim 26 ng/L (ppt). MQ = htol t^a/Hlflable* Measured conoentraticir tsehween25 noA.(ppt) and the lim itor Quantitettcn (LOQ) which is 50 ngrt. (ppt). Mote: Since this nummarytable *how* rounded reeults. recoveryvalue* mayvaryllohlty from the valuta Intha 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 Sarepta PeecrtpUon CI Sultanat* PFOS CSAdd PFOA Amount AmtFound Amount Amount Amt Found Amount Spiked mSample Recovered Recovery Spfktd inSampta Recovered (no>L) (nn/U tao/U |S | fna/U Inaiti inali) Rocovaiy |%) OKU4N-GW-WS104-0*050310 (C90M4MS*M.90OPfla.Ubpftft) OKLMhMSW-WVI04-0-050310 (C0M 44M tpk H, Mtoon*L LibS p ite ) OKLWN^W-W51C4-0-050310 Low Spike S ppb (C90M 4M , 5000 ng/L FtoW9 0 te \ QKLMN-GW-W6104-0-050310 High Spike 50 ppb (COOOUn. CMM ng/L FtaMS p ite ) 5000 50000 5000 50000 OKLMN-GW-WI201-0*050a|0 10099449SpkC,30b Oft, le t fell* ) QKLHN-GW-W8201-0-05W10 (C a te H ttS t* Or*0000ngfL LabSpite} 0KLMN-GWW6201-0-050310 Low Spike 03 ppb (C0044440, KMnpM.FieldS p ike} OKLNhKiWW8201'<M>50310 High Sp4k* 5 ppb (99*44*1, SOW ftp*. Ft*MSpite} 5000 50000 500 5000 109 109 109 109 NQ NQ NQ NQ 5500 58100 5700 56700 4SB0 50000 670 8900 108 5000 116 50000 112 5000 113 50000 1O0 5000 100 50000 134 500 132 5000 207 207 207 207 953 953 953 95.5 5290 57300 5470 35800 4950 50800 606 8130 102 114 105 71 97 101 102 121 OKU4N-GW-W2C-O-OSO309 JCOO*44*7 SpfcE , 5000 nprt_ U Q S p ) OKLNN-GW-W2Q-0-0903Q9 tC d 9 4 4 7$ |*F. 9 0 9 n^LUbSp ite | OKLMI^W-W29^-0S030a U w Spike 5 ppb (090*4449,9099 nA FM d fe d * ) OKLMN-GW-WZO-C-OSWOSHigh Spike 50 ppb fC M M 47ft.M M iieft. FM d Spite) 0KLMfKiW-W22-0-G50309 <C*DM471 &pkG, SOM ngIL LabS p ite ) OKLMN-GW-W22-0-OS0309 {C999M 71 Sp kH . S O fM fttfL L jiife ite ) OKLMM-GW-W22-0050309 Low Spike 5 ppb C0M4473,WOO ft. F ield Sp ike) OKLMN-GW-W22-O-05CMS High Spike ppb <080*4474.50000noA FM d Spite) OKLMN-GW-W31-0 -0 5 0 3 0 (C0eM 479Spk I.W O e n p L L e d S p **) OKLHbJ-OW-W31*0*050309 tC0M 7S Spitt, MOM Latatplte ) 0 K U 4 H -C W -W 9 1 -0 4 5 Q 3 Q 9 High Spike 50 ppb {CM94471,19099ng/L FMd Spite) OKLMN-GW-W32*0-030309 <cooM47i spkK. woo eed. cab spite) OKLMN-GW-W32-0-030309 (C0i44744HkL C9090noA U b Spite) OKLMNM3W-W32-0-O5C309 Low $pc 3 ppb (C80F4AM, WOOngA. Field Spite ) cm iM N -G W w aa-frosow High Spat* so ppb (CMW4S1, B0000 np*. FMd Spite) 5000 50000 5000 50000 46600 46800 46600 46800 300 50000 5000 50000 asaco 45500 45500 45900 5000 132000 50000 132000 50000 152000 5000 47100 5OOD0 47100 5000 47100 50000 47100 49900 92800 41900 59500 44600 96500 41200 65800 116000 168000 218000 62200 115000 74000 120000 . 5000 285000 92 50000 285000 - 500C 285000 26 50000 285000 * 5000 317000 105 50000 317000 - 5000 317000 40 50000 317000 A 5000 72 50000 168 50000 23100 231CO 23100 . 5000 117000 138 50000 117000 > 5000 117000 148 50000 117000 289000 295000 278000 264000 330000 412000 324000 288000 26400 71300 65700 109000 151000 131000 157000 96 65 *50111111* reedu* excaedi m* spUrte levelsignificantly; therefore, an accuiate recovery value cannot De cafculaied ND =Notdetected at of above 25 noA-(Ppt). NQ Notquanuliabl = Measured concentration bcNreen 25 ngTL {pptfand lit* Until of QuanBtation (LOQ) wHlcft 1SOnpfL <ppt). Note: S in M s summerytable shows rounce results, rcovry vatu mayvary sligntly front lha valuas In the raw data. Exygen Research Page 32 o f 110 vi0 0 5 5 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P00014QQ Table III* Matrix Spike Recovery of PFOS and PFOA in Water Samples Continued Sample OeecrlptkMi OKLMN-GW-W217^M55CMfi (001044SekK we ngU.U*ptiie1 OKLMN43W-W217-0-05030* {OMS44S2SekM.SNMnSLefiScllce> OKLMN45WWN2174W5034WLow Splka 5 ppb tCeoe4*M,Wgru FW d See) OKLMK-QWWI7-043090B HfekSpIkaSO ppb <ca4*an * ectiLFMdSetfc) C* Sulfonate PFOS C8 Acid PFOA Amount AmtFound Amount Amount Amt Found Amount Sptfcod feSaapla Ractwarad Recovery Spiked InSimple Recovered (">m____ w n _ J 5 m ________ & a _______i? fla = L (ntfU <ns7L> 5000 50000 5000 50000 NQ NO NQ NQ 4790 49700 5600 65300 96 5000 99 50000 116 5000 131 50000 NQ NQ NQ NQ 4860 52200 4880 42600 OKLMN-GW-W200B-0-050 |CQM44MSekO.M8eJLLah *41) QKLMN-GW-W2009.<M03W {Coesuee%pk p, sow *m l *o Se) OKLMN-GW-W2WW4J5M09 Law Spka 5ppb tC*44M0MB0fLeW *0M) OKLMN45W-W20a-<HJ50309HighSpdct 30 ppb iCoeeMM, Meceril nek*5pn*) 5000 50000 . 5000 50000 15500 15500 15500 15500 20800 69300 27000 71300 106 5000 106 50000 230 X X ) 112 * 50000 59300 59300 50300 59300 64800 114000 73600 94600 OKlMN^WAV2O12-0-O5C6 tceoeneeSeec, eeenpLteeSpile> OKLMN-GW4*2012-0-05C3C (Cees***a<* 6,eeoeo*<yLLabap} OKLMN-<JW-W2012-4W6M0f Low 8pfce 9 ppb tceeseeee,seeseLp w Sene> OKLMN-GW-W2012-^5030High Spike 0 ppb (CMSHfd.N O N ap L FMd *41) 5000 117000 143000 soooo 117000 186000 5000 117000 * . 115000 SOOOO 117000 203000 * 5000 46900 136 50000 46900 * 5000 . *0900 172 50000 40900 57700 94700 48500 99500 OKUUN43VWaO-0-8O (COM4*** * * , 9*00a* L LabSpilw) 5000 OKLMN-GVMIVMMMSOaO (CDeeeoMspitf, s e e e p L u b s ^ e ) OKLMW4W-WMWMl5MOt Low Spit 5 ppb (CSMMOO.000 nan.FtaM p e a ) C^LMN-GW-WSO-CHWp HighSpike SOppb {CMU447, ttOMA L FMM p ** ) 50000 500C 50000 OKLMN-GW-PW1*(KO<U10 (C00644MSpfcS,MOOATLLsb Spike) OKLMN43W-PW1-0-050316 {COOSMOI acritK.060n^yLluto o n e ) 5000 50000 OKLMN^GW-PWi-O-OSDStOLow Spike S ppb < (CMMieo,co t ngn. noiespat > 5000 OKUflN-GW-f'W1-O-05C3WHIQ91SpQcf 50 ppb (C0MM001,00000ngA. FM tf * * ) 50000 to ' ND NO; NO 66900 66900 60900 66900 5280 52900 5720 57600 72000 116000 66900 '' 95200 106 5000 106 50000 114' 5000 113 50000 * - 5000 102 50000 5000 57 SOOOO 302 302 302 302 37300 37300 37300 37300 SS10 53100 5860 42200 477X 60200 40400 80500 OKLMfWW-pW2^WC31<r '6004*00*ok1, 9*00ngtL Lab SpH * } OKLMN-GW-PW2-<W>S0310 (0006*902ok4,60M0nA. LobIp lk * ) OKLMN-GW-PW2-M5W10 tow Spike S ppb (CftoeuM,a m *#n. ro w paw > OKLMN-GW*fW2-<M)3C31C Hlph Spike SOppb (camsos, neeea9x. r m *eu) 5000 351 50000 351 9000 .98.1.' SOOOO 351 5480 , 59800 ... 4280, *0500 103 ,5000 119 50000 79 5000 BO 50000 3830 3830 3630 3630 8720 58800 7860 39500 Recovery (* ) 97 104 91 65 * 109 * 71 . 06 . 85 110 ID S 111 84 * 106 66 102 110 35 72 'Sample residue exceed* the spiking lvf significantly; therefore, an accurate recovery value cannot bo catculeted NO * NotOetectedat oracove25 ng/L ippt). NQ * Not quantifiable Uessured concentration between 25 ng/t (ppt) and the Limit of Quantitation (LOO) which is 50 ngl. {ppt}. >Mo: Since ttts summary table show rounded resulti, recovery values mayvary illghtty from the values in the raw data* 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 PFGA in Water Samples Continued Sampi D M ZW on CSulfon*tPFO$ G8 Acid PFOA Amount Ami Found Amount Amount Amt Found Amount Spiked tn Sample Recovered Recovery Spiked in Sample Recovered W U -fetfU (ng/Ll <%) {aaM tn flO _ (ng/L) Recovery (%). _ OKLMN-GW-PW3-0-O5031O <coo*so4spa k, tow .itUfaSptw} OKLMN-CW-PW3-0-O5CJ10 (cemM eepkt, aoeto ng&Ufa**> OKLWN<6W'PW34436310 Low Spike 5 ppb (CSM45M. SflO#ng/LFNfd 8pUt ) OKLMN<<3W4W34<O50310 High Spike 50 ppfa {ceoeesoe, moos ng/LField tptiie} 5000 50000 5000 50000 32700 32700 32700 32700 43300 6100 33900 90000 5000 177000 87 60000 177000 . S000 177000 55 50000 177000 138000 190000 196000 204000 ., 26 54 OKLMN-GW-FW4-0-0SC310 {C0MS319epk M,5M aoA. Ub apihe> OKUWM3W-PWM-060310 <C0M4iieSpfcH, 90000neL Ufasou*) OKLMN-GW<PW4-0-05Q310 LOWSpike 5 ppb <00084812,9000ne/LFieldpike > OKLMN<-G00W004W4143.-000-000500i3i(1A0 High Spike FloMSpike> 30 ppb 5000 50000 5000 50000 33800 33600 33800 33800 42500 75700 42200 91200 * 5000 72100 84 50000 72100 * 5000 72100 95 50000 72100 77500 121000 870O 116000 * 96 86 OKLMN4aW'PWM*fl00310 (C00045U3pk0. SOODngILUfaSeth) 5000 90000 97600 - 5000 78400 OKLMN-GW-PW9-0450310 <08004514SpfcP, 90000ng/LUfaSplk*) 50000 90000 139000 98 50000 76400 OKLMN*GW4*Wf-0450310 Low SpBce3 ppb <00004114.1000ng*. Reid*pilw) 5000 90000 94100 5000 78400 QKLMN*GW*PW64-05031fl High Spike 50 ppb (CM04917.90000npL FleWSpike} 50000 90000 124000 88 50000 78400 82900 133000 87000 116000 109 75 OKLMN-GW-PW10-0-050310 (Cweie<* c, 9ooo ne/t Ufa*** s 5000 1400000 1410000 5000 710000 OW_MN-GW4>W104-05P3t0 fCOWdSIStpkO, 9000089. UfaOfOta) 50000 1400000 1390000 90000 719000 OKLMN4<30W00-0P4W3910t,M90M00I1*f9i(n.iOFlaLtdoSwplShpi)ke 5 ppb 5000 1400000 955000 5000 719000 OKLMN-GW-PW11W5<050310 High Spike 3 ppb (C0os42i,ttoeeA. Rew spfte) 50000 HOOOOO 1910000 * 50000 719000 868000 840000 692000 747000 . > 0KLMN-GW-PW114MI50310 {O0M4OZ2Of* E, 5000 npA.UfaSetiN ) OKLMN-GW<PWl1-0-O5O3lO SpkF. 000 ne>LLabSpifa> OKLMN-GW-PWI1-0-036310 Low SpIKa 5 ppb (CMMSKK ngfl.RiWSella ) OKLMN-GW*PW11<0-050310 Hffib Spike 50 ppb (CO0C4829, SUN ng/LField Spike} 5000 50000 5000 50000 40800 40800 40900 40800 46900 83100 45400 88500 5000 60300 85 S0000 60300 - 5000 60300 95 50000 60300 64700 105000 83300 96100 * 89 76 Sam ple resid ue exceed s the spiking le ve l eignificaM iy; lhrefon>, an accurate recovery value cannot be calculated NO = Not detected a t o r above 25 np4.<ppt). NQ = Not quantifiable *M easured concentration between 25 ng/L (ppt| and the Lim it of Q uantitation (LO Q ) Which is 50 n g fl. (ppt). Note: Since thl* summaryti bie shows rounded results, recoveryvalues mayvaryslightly from thevalue* in the raw data. Exygen Research Page 34 of 110 000057 Interim Report #l-A nalysis o f Oakdale Water Samples Exygen Study N o,:P 0001400 Table III. Matrix Spike Recovery of PFOS and PFOAin Water Samples Continued SampM oacrlptfon CSSutfonaMFFOS Amount AmtPound Amount Amount Spited In Sample Racovarad Racovwy Spited m (nVU <*) W 4 CS Add PFOA Amt Found Amount InSampt* Recovered (ntPU (nofl.) Racovary <*> 0KLMN-3FMM6M10 (CODMtMftefcQ,4909etTLLehStrike) OKUMN-SW-04G0310 {COfMOMipha <0*00A*L Ub Spfte) OKLMH-SW-O-OSMI0 Low S pite 5 ppb (C00M42I, SONA0LFleWSplINi| OKLMN-SW4M50310High S pite so ppb (Coeitwa.*000*egn. fmi *#w# > $000 soooo $000 50000 1190 1190 1190 1190 6270 51600 7220 50000 102 5000 101 50000 121 5000 114 50000 491 491 491 491 5520 $3200 6020 44200 101 105 111 87 OKLMN-GW-TRIP2-0-050310 Low Spk* S ppb (CMMttt. 9 m bqA Op*n) OKLMN"0W-TWP4*O*O3M10Hlflh S pite SOppb (C09040U,SOSOS00*. Strike) 5000 soooo NO ND 6170 57400 123 5000 115 soooo NO ND 6040 57300 121 115 Araiag: 110 Standard Deviation: 32 "Sample nwtfue exceeds the piking tevei ilgniScantfy; therefore, * Raccurate recovery value csnnoi be calculated NO NottWected al or abewe2b ng/U(ppt), MQ s Not quartiHablA=MeasuredconcanfcaBonbetaken 25 ngA.(ppl}and fiheUntilof Quartftetfor) (LOO) which to 50 ngA <ppt). H o t*: n e e 9 9 a u e en w y taW # b o w s rounded r* u tt* . reco very v a lu e s m ay v a ry *H o H V fro m th e v a lu e s In th e raw d ate. Avaraga: Standard Deviation: 93 1ft Exygen Research Page 35 of 110 000058 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table IV. Surrogale Spike Recovery of l3C PFOA in Water Samples Exygen to Sam ple D escription Am ount S p lk e d ("flA - laC-PFOA Am ount R e co v e re d (nort.) R e co v e ry w C0064404 Spk C C0064404 Spk D C0064404 C0064404 Rep C0064405 C00644G6 C0064407 OKLM N -GW -W 3-0-050310 OKLM N-GW -W 3-0-050310 OKLM N-GW -W 3-0-050310 OKLM N-GW -W 3-0-050310 OKLMN-GW -W3-0-050310 Dup OKLMN-GW -W3-0-050310 Low Spike 5 ppb OKLMN-GW-W3-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5580 53900 431 422 416 4730 34500 101 107 86 04 83 95 69 C0064408 Spk E 00064406 Spk F C0Q644C8 C 0084408 Rep C0064409 C0064410 C0064411 OK LMN-GW-W8-0-050310 O KLM N-GW -W 8-0-050310 O KLM N -GW -W 8-0-050310 OKLM N -GW -W 8-0-050310 OKLMN-GW-W8-0-050310 Dup OKLMN-GW-W8-0-050310 Low Spike 5 ppb OKLMN-GW-W8-0-050310 High Spike 60 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 C0064412 C0064412 Rep C0064413 CO064414 C0064415 O KLM N -GW -W 26-0-050310 OKLM N-GW -W 26-0-C50310 OKLM N -GW -W 28-0-050310 OKLM N-GW -W 26-M 50310 OKLMN-GW-W26-0-050310 Dup OKLMN-GW-W26-0-050310 Low Spike 5 ppb OKLMN-GW-W26-0-050310 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 OKLM N-GW-W33-0-050310 OKLM N-GW-W33-0-050310 0 KLM N-GW-W33-0-050310 OKLMN-GW -W 33-0-050310 OKLMN-GW-W33-Q-050310 Dup OKLMN-GW-W33-0-050310 Low Spike 5 ppb OKLMN-GW -W33-0-050310 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 C0064420 Spk L C004420 C0064420 Rep C0064421 C0064422 C0064423 O KLM N-GW -W 206-0-050310 OKLM N -6W -W 205-0-050310 O KLM N-GW -W 205-C-050310 OKLM N-GW -W 205-0-050310 OKLMN-GW-W205-0-050310 Dup OKLMN-GW-W2C5-0-0S031O Low Spike 5 ppb OKLMN-GW-W205-0-060310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 4940 53000 279 280 307 4240 38000 90 105 56 56 61 85 76 C0064424 Spk M C0084424 Spk N C0064424 C0064424 Rep C 0064425 C0064426 C0064427 O KLM N -GW -W 215-0-050310 O KLM N-GW -W 215-0-050310 OKIM N-GW -W 215-0-050310 OKLM N -GW -W 215-0-050310 OKLMN-GW-W215-0-050310 Dup OKLMN-GW-W215-0-050310 Low Spike 5 ppb OKLMN-GW-W215-0-050310 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 PFOA level In the undiluted sample Interfered with **C PFOA recovery. Note: Sines this summary table show rounded results, recovery values may vary slightly from the values In the raw data. Exygen Research Page 36 of 110 000059 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 Sample Description Amount Spiked (ngiL) 1iC*PFOA Amount Recovered Recovery ..-<*> C0064428 Spk C OKLMN-GW-W2010-0-050310 CQ064428 Spk D OKLMN-GW-W2010-0-050310 C0094428 OKLMN-GW-W2010-0-050310 C0064428 Rep OKLMN-GW-W2Q10-0-050310 00054429 OKLMN-GW-W2010-0-050310 Dup C0054430 OKLMN-GW-W2010-0-050310 LowSpike 5 ppb C0064431 OKLMN-GW-W2010-0-050310 HighSpike 50 ppb 5500 50500 500 500 500 5000 50000 5390 53000 432 417 510 4500 30200 98 105 86 83 102 90 60 C0064432 Spk E C0064432 Spk F C0Q64432 C0064432 Rep C0064433 C00S4434 CO064435 OKLMN-GW-PW7-0-050310 OKLMN-GW-PW7-0-050310 OKLMN-GW-PW7-0-05C310 OKLMN-GW-PW7-0-05C310 OKLMN-GW-PW7-0-050310 Dup OKLMN-GW-PW7-0-050310 LowSpike 5 ppb OKLMN-GW-PW7-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5260 51000 341 335 325 4820 33200 96 101 68 67 65 96 66 C0064436 COO54437 C0064438 OKLMN-GW-TRIP1-0-050310 500 OKLMN-GW-TRIP1-0-050310 LowSpike 5 ppb 5000 OKLMN-GW-TRIP1-0-050310 High Spike 50 ppb 50000 510 5100 51300 102 102 103 C0064442 Spk G C0064442 Spk H COOS4442 C0064442 Rep C0064443 C0064444 C0064445 OKLMN-GW-PW8-0-050310 OKLMN-GW-PW8-0-050310 OKLMN-GW-PW8-0-050310 OKLMN-GW-PW8-0-050310 OKLMN-GW-PW8-0-050310 Dup OKLMN-GW-PW8-0-05P310 LOWSpike 5 ppb OKLMN-GW-PW8-0-050310 High Spiks 50 ppb 5500 50500 500 500 500 5000 50000 5270 52900 321 322 300 3910 25800 96 105 64 64 60 78 52 C0064446 Spk I C006444S Spk J C0064446 C0064446 Rep C0084447 C0064448 C0084449 OKLMN-GWrPW8-0-050310 OKLMN-GW-PW9-Q-050310 OKLMN-GW-PW9-0-050310 OKLMN-GW-PW9-0-05031O' OKLMNK3W-PVV9-6-050310 Diip OKLMN-GW-PW9-(F050310 LowSpike 5 ppb OKLMN-GW-PW9*0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5250 53900 315 317 338 4230 24800 95 107 63 63 68 85 50 C0064450 Spk K OKLMN-GW-W6102-0-050310 COO54450 Spk L OKLMN-GW-W61Q2-0-050310 C0064450 OKLMN-GW-W61Q2-0-050310 C0064450 Rep OKLMN-GW-W61G2-0-050310 C0054451 OKLMN-GW-W6102-0-050310 Dup C0064452 OKLMN-GW-W6102-0-050310 LowSpike 5 ppb C0064453 OKLMN-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 Note: Since this summary table shows rounded results, recovery values may vary slightly from the vaiira* In the raw data. Exygen Research Page 37 o f HO 000060 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table IV. Surrogate Spike Recovery of I3C FFOA in Water Samples Continued Exygen 10 Sample Description Amount Spiked (ng/L) TMC-PFPA Amount Recovered (nfl/L) Recovery w .... C0064454 Spk M OKLMN-GW-W6104-0-050310 C0064454 Spk N OKLMN-GW-W6104-0-050310 C0064454 OKLMN-GW-W6104-0-050310 C0064454 Rep OKLMN-GW-W6104-0-050310 C0064455 OKLMN-GW-W6104-0-C50310 Dup C0064456 OKLMN-GW-W6104-0-050310 Low Spike 5 ppb CQ064457 OKLMN-GW-W6104-0-050310 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 C0034458 Spk D COO64458 C0064458 Rep C006445S C0064460 C0064461 OKLMN-GW-W6201-0-050310 OKLMN-GW-W6201-0-050310 OKLMN-GW-W6201-0-050310 OKLMN-GW-W6201-0-050310 OKLMN-GW-W8201-0-Q50310 Dup OKLMN-GW-W6201-0-050310 Low Spike 0.5 ppb OKLMN-GW-W6201-C-050310 High Spike 5 ppb 5500 50600 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 C0064467 Rep C0064468 C0064469 C0064470 OKLMN-GW-W2O-O-O5O3O0 OKLMN-GW-W20-0-050309 OKLMN-GW-W20-0-050309 OKLMN-GW-W20-0-050309 OKLMN-GW-W20-0-050309 Dup OKLMN-GW-W20-0-050309 Low Spike 5 ppb OKLMN-GW-W20-0-050309 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 C0Q64471 Spk G C0064471 Spk H C0064471 C0064471 Rep C0064472 C0064473 CO064474 OKLMN-GW-W22-0-050309 OKLMN-GW-W22-0-060309 OKLMN-GW-W22-0-050309 OKLMN-GW-W22-0-O50309 OKLMN-GW-W22-Q-050309 Dup OKLMN-GW-W22-0-050309 LOWSpike 5 ppb OKLMN-GW-W22-0-050309 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 4380 50700 267 280 256 3830 28800 80 100 53 56 51 77 58 C0064475 Spk l C0064475 Spk J C0064475 C0064475 Rep CQ064476 C0064477 OKLMN-GW-W31-04)50309 OKLMN-GW-W31-0-050309 OKLMN-GW-W31-0-O5C309 OKLMN-GW-W31-0-050309 OKLMN-GW-W31-0-050309 Dup OKLMN-GW-W31-0-050309 High Spike 50 ppb 5500 50500 500 500 500 50000 5410 54200 391 391 371 44100 96 107 78 78 74 88 C0064478 Spk K C0064478 Spk L C0064478 C0064478 Rep C0064479 C0064480 C0064481 OKLMN-GW-W32-0-050309 OKLMN-GW-W32-0-050309 OKLMN-GW-W32-0-050309 OKLMN-GW-W32-Q-05C309 OKLMN-GW-W32-0-050309 Dup OKLMN-GW-W32-0-050309 Low Spike 5 ppb OKLMN-GW-W32-0-0503Q9 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 Nate: Sine* this summary tabla shows rounded results, recovery values may vary slightly from the values in the raw data. Exygen Research * Page 38 o f 110 000061 Interim Report #1-Analysis o f Oakdale Water Samples Exygen. Study No.: P000I400 Table IV. Surrogate Spike Recovery of ,3C PFOA in Water Samples Continued Exygen ID Sample Description 13C-PFOA Amount Amount spiked Recovered Recovery (no-) (ngfl.) <%) C0064482Spk M OKLMN-GW-W217-<H)50309 C0064482 Spk N OKUVIN-GW-W217-0-050309 C0064482 OKLMN-GW-W217-0-O5O3O9 C0064482 Rep OKLMN-GW-W217-0-050309 CQ064483 OKLMN-GW-W217-0-050309 Dup C0064484 OKtMNLGW-W217-0-050309LowSpike5 ppb C0064485 QKLMN-GW-W217-0-050309HighSpike50ppb 5500 50500 500 500 500 5000 50000 5410 52500 428 453 468 4850 44700 98 104 86 91 94 97 89 C0064486SpkO OKLMN-GW-W2008-Q-050309 C0Q64486Spk P OKLMN-GW-W2QQ8-0-50309 C0064486 OKLMN-GW-W2008-0-050309 00084488 Rep OKLMN-GVV-W2008-0-050309 00064487 OKLMN-GW-W2008-0-050309 Dup C0084488 OKLMN-GW-W2008-0-050309 LowSpike 5ppb C0064489 OKLMN-GW-W2008-0-050309High Spike 50ppb 5500 50500 500 500 500 5000 50000 5140 52100 318 326 357 6040 37800 93 103 64 65 71 121 76 C0084490SpkC OKLMN-GW-W2012-0-050309 00084490 Spk D OKLMN-GW-W2012-0-050309 00064490 OKLMN-GW-W2012-0-050309 C0064490 Rep OKLMN-GW-W2012-0-060309 C0064491 OKLMN-GW-W2012-0-050309 Dup: C0064492 OKLMN-GW-W2012-0-050309LowSpike 5 ppb CO064493 OKLMN-GW-W2012-0-050309HighSpAe50 ppb 5500 50500 500 500 500 5000 50000 5050 50700 344 342 351 5010 37900 92 100 69 68 70 100 76 C0064494Spk C0064494 Spk F C0064494 C0064494 Rep C0064495 C0064496 C0064497 OKLMN-GW-W80-0-050309 OKLMN-GW-W80-0-050309 OKLMN-GW-W80-0-050309 OKLMN-GW-W80-0-050309 OKLMN-GW-W80-0-050309 Dtq> OKLMN-GW-W8Q-0-050309 LowSpike 5 ppb OKLMN-GW-W80-0-050309HighSpike 50 ppb 5500 50500 500 500 500 5000 50000 5650 52400 486 438 502 5410 41700 103 104 07 88 100 108 63 C0064498Spk G G006449Spk H C0064498 C0064496 Rep C0064499 C0064500 C0064501 OKLMN-GW-PW1-0-050310 OKLMN-GW-PW1-0-Q50310 0KLMN-GW-PW1-0-050310 OKLMN-GW-RW1-0-05C310 ' OKLMN-GW-PW1-0-050310 Dup OKLMN-GW-PW1-0-50310 LowSpike 5 ppb OKLMN-GW-PW1-0-050310HighSpike 50 ppb 5500 50600 500 500 500 5000 50000 5150 53000 331 350 352 4420 41600 94 105 66 70 70 88 83 C0064502Spk I C0064502 SpkJ C0064502 C0064502Rep C0064503 C0064504 . C0064505 OKLMN-GW--PW2-0-060310 OKLMN-GW-PW2-0-050310 OKLMN-GW-PW2-0-050310 OKLMN-GW-PW2-0-050310. . OKLMN-GW-PW2-0-050310Dup DKLMN-GW-PW2-0-050310LowSpike5 ppb QKLMN-GW-PW2-0-050310HighSpike 50 ppb 5500 50500 500 500 500 5000 50000 5420 52600 440 440 431 4680 34000 99 104 88 88 86 94 68 Not: Sine this summary tab! shows round! rssults, recovery vslus my vary slightly from th values In the raw data. Exygen Research Page 39 o f 110 000062 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: POOOI4QO Table IV. Surrogate Spike Recovery of 13C PFOA in Water Samples Continued Exygen to Sam ple D escription Amount Splked (ng/LJ ^C-PFOA Amount Recovered Recovery <%> C0064506 Spk K C0064506 Spk L C0064508 C0064506 Rep C0064S07 C0064508 C0064509 OKLMN-GW-PW3-0-050310 OKLMN-GW-PW3-0-050310 OKLMN-GW-PW3-0-050310 OKLMN-GW-PW3-0-050310 OKLMN-GW-PW3-0-050310 Dup OKLMN-GW-PW3-0-050310 Low Spike 5 ppb OKLMN-GW-PW3-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 4640 53100 284 275 294 4080 38300 84 105 57 55 59 82 77 C0064510 Spk M C0064510 Spk N C0064510 C00645010 Rep C0064511 C0064512 CO064513 OKLMN-GW-PW4-0-0S0310 OKLMN-GW-PW4-0-050310 OKLMN-6W-PW4-C-050310 OKLMN-GW-PW4-0-050310 OKLMN-GW-PW4-0-05031C Dup OKLMN-GW-PW4-0-050310 Low Spike 5 ppb OKLMN-GW-PW4-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5190 52400 320 324 313 4870 36000 94 104 64 65 63 97 76 C0084514 Spk 0 C0064514 Spk P C0064514 C0064514 Rep C0064515 C0064516 C0064517 OKLMN-GW-PW6-OO5031Q OKLMN-GW-PW6-0-050310 OKLMN-GW-PW6-0-050310 OKLMN-GW-PW6-0-050310 OKLMN-GW-PW6-0-050310 Dup 0KLMN-GW-PW6-0-050310 Low Spike 5 ppb OKLMN-GW-PW8-0-050310 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 C0064518 Spk C COO04518 Spk D C0064518 C0Q64518 Rep COOS4519 C006452C C0064521 OKLMN-GW-PW10-0-050310 OKLMN-GW-PW10-Q-050310 OKLMN-GW-PW10-0-050310 OKLMN-GW-PW10-0-050310 OKLMN-GW-PW10-0-050310 Dup OKLMN-GW-PW10-0-050310 Low Spike 5 ppb OKLMN-GW-PW10-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 3670 48500 255 249 258 2980 34100 67 96 51 50 52 60 68 C0064522 Spk 00064622 Spk F C0064522 C0064522 Rep C0064523 C0064524 C0064525 OKLMN-GW-PW11-0-050310 OKLMN-GW-PW11-0-050310 0KLMN-6W-PW11-0-050310 OKLMN-GW-PW11-0-050310 OKLMN-GW-PW11-0-050310 Dup OKLMN-GW-PW11-0-050310 Low Spike 5 ppb OKLMN-GW-PW11-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5180 51600 319 347 312 4400 36000 94 102 64 69 62 88 72 C0064526 Spk G C0064526 Spk H C0064526 C0064526 Rep C0064527 C0064528 C0064529 OKLMN-SW--050310 OKLMN-SW-0-050310 OKLMN-SW-0-050310 OKLMN-SW-0-050310 OKLMN-SW-0-050310 Dup OKLMN-SW-0-050310 Low Spike 5 ppb OKLMN-SW-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5270 52000 124 132 505 5320 41200 96 103 25 26 101 106 82 N o: Sine this summary table how* rounded result*, recovery value* may vary lightly from the values In the raw date. Exygen Research Page 40 o f 110 000063 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table IV. Exygen to Surrogate Spike Recovery of 13C PFOA in Water Samples Continued '*C*PFOA Sample Descriotion Amount Amount Spiked Recovered Recovery (ng/L) _ inoH. (%) COO64530 C0064531 C0064532 OKLMN-GW-TRIP2-0-050310 500 OKIMN-GW-TRIP2-0-050310 LowSpike 5 ppb 5000 OKLMN-GW-TRIP2-0-050310 High Spike 50 ppb 50000 494 5520 52900 99 110 106 Average: 83 Standard Deviation: 21 Not: Sine this summary table shows rounded results, recovery values may vary slightly from the values 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-Analysis o f Oakdale Water Samples Exygen Study N o.: PQOO1400 Figure 1, Typical Calibration Curve for PFOA in Reagent Water OXMStC Cnwid W r Hv7.rtb (PFW(t I * ' ItajnMkin o V * I M n O B * J.3OM (f 1M W 1) Area, count Exygen Research ii'iK W ft Page 43 o f 110 000066 Interim Report #1 -Analysis o f Oakdale Water Samples Exygen Study No. : POOO1400 Figure 2. Extracted Standards of PFO in Reagent Water, 25 ng/L and 50 ng/L, Respectively XC032U-t - PPOA (Stmrtarrt) 4*$&$&<> Mtmt 2 o f 41 fro 0324O5C.w# A r r x 44717 ovt/rris H ih jfrt 60 3 3 3 S cf>9 RT: f t 440 ntift 1 1 .0 4 I XCD321W-2 P fOAfSUndirt) 4134010J) *u - anpl 3 f 4im rn 632405C.tf1 fir*a: 7929$ cm ** 13708.770 eps RT: H X Tin in Exygen Research * .?H : ; ; Page 44 of 110 000067 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 3. PFOA in Reagent Water, SOng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively A*jg*rca*ninf P PO A ( tto t* o w < lf4 K O f$ 6 9 A ti mv At o ; 5766 c o e s i * H e i g h t 9 9 4 J t 2 epa RT: (1 fff 9 mt*i R o m 03240CCj* W 11J62 c SOOJQO- 0.00 - -- ^ 12 . .. 3 4 B tpk a WO*(PO4OJ/OI.0 am - sm po 11 trt 4t from Aw; 7WQ3wunts Haight: 10623.T29 ops RT. iMdtmin ......................... > I f >...... .. 7 0 9 10 t1 Tim*, min i 12 I ni I -- I* ..................................y 13 14 16 10 17 <* 1.3 ao. f " 600 4 f aoo 1 2 9 4 6 8 7 8 9 10 11 12 13 1 4 16 17 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 o f 110 000068 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=1O0 (Exygen ID: C0064522, Data Set: 032405CR) C00G4B22 * PFO* 9<rw- 9 n p f 39 ofG7 from Q&40SCX.wiW Am * ;979794eow rfo Height 7f6G-l49qp* RT: 1120 min 11.92 Intensity, cpg Exygen Research Page 46 of 110 000063 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 5. Typical Calibration Curve for 13C PFOA in Reagent Water 032ec G r o u n d J ^ r d D tP*0^ "* * * ^ * ^ * O f ml.31**CO*Jn-OiC3*l O' " M W ) Arta, counts Exygen Research Page 47 o f 110 000070 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 6. Extracted Standards of 13C PFOA in Reagent Water, 25 ng/L and 50 ng/L, Respectively I XCC3SU>0-1 - i3CPFGA {S1ndwn)}4i5,0J37O.C ***tp*2of*1fnMC3240l5C-W>W Are: 33102 c-outfit Height 6<999.<13 OP* RT: i 1JSO min 0000-i 4000' 3000 20001000- 11.86 Intensity, cps 12 3 4* 6 78 9 Tim *, min XCWJ100-2 - t X FFOA&tvvr) 410JV379S>amu samp* 3 of 41 from 932409C.*ff 08017 o*unt* HaiQhl; 1H30.466 cp* RT; 1148 T 10 Hi 12 13 1 4 1 16 17 11S& intensity, cp s 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 W ater, and 500 ng/L Fortified Reagent Water, Respectively fto a g * in C a r i n i fJC P P O A (U ftto m o m ) AW.tUSTQX) a m - s a m p t* a < *44 fr o m Aro: 311 CW<19 HoiQht 36.06400* A7: 1tM4nri* *& | RMOtft S*cA - tJC R F[W (Q C)413iW P mw - s a r* * 10of 41 from fi024&6Cjji<1 A ;W ? 9 9 c < u *s Hwght: 106407:3 p RT: 11*23 mm 1 0 0 .6 ao 540*4 0X0 1 2 3 5 7 0 fl 10 Tim, min | R*acSi* 5J-. 13C0 FFFFOQIA<CK^4lSJV3700arrw: fiiryl l1of 41 fiomMMMCjYW * * i; 12966 amt* HMBht: 2 0 *) 1 cps RT;1LM3mto If 12 13 14 15 16 1? 20*5 M&4 if*a <eo5 I 8 0 to 11 12 13 14 16 16 17 Tim*, min 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) C0064622 >13Cf>FQA iUitkJtomr)Al5jOi37O mompim23 o f 41 toom0324Q5C.wW A r w 4U9C3 oott/rto 7M12 ofi* f t T. H . 5 3 TM <1A5 intensity, cps Exygen Research Page 50 of 110 000073 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 9. Typical Calibration Curve for PFBS in Reagent Water BMBCRGlwrrfUatvRlwIiUb OFFBSE ~UnW Rr5<Mi (1 t r f * 13 IM ST) Area, counts Exygen Research Page 51 of 110 000074 Interim 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 . pFSS{S1*tf9ni)299JH9$.0irm/-wn/U9 2vfe7thm*Xi24Q5CR.w*7 wx//ris H tiht op* ftT; $307 mitt 3.01 t Riandar) 2B0.9i04> w m Mnpfe 3 *wn MWCft.wff 772? w e r H i& t; M .M fitp t FT;3*54flfe 33 Exygen Research Page 52 o f l IO 000075 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 11. PFBS in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively 0knotfotmtf)Reagent Control PFBS fiJn kn e3 9 & J)/9 Q .O tm u -ta m p k 9 o f til front Q3240GCP.*ilt mj Intensity, cpe Intensity, cps 3.66 tpk 9 rr $ coq>M jm m j smu * an* 11 rf I? *wn r u : '96163 c*wi 12O0.$4t c|kf RT:3J17iw > 3JB2 T im *, min 1 1 3 4 i " 0 7 9 10 Time, mift 11 13 14 16 18 17 Intensity, cps Exygen Research Page 53 o f 110 000076 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 12. Chromatogram Representing an Oakdale Water Sample Analyzed for PFBS, DF=100 (Exygen ID: C0064S22, Data Set: 0324O5CR) OJ064G22 fifithnotmj 299JM99 0 - sumpi* /j* ?7S oovrf* iffl.4 0 0 op* RT- 3.924frilit 32 t/6 7 fttM f Q324&SCX.mfT intensity, cp s Exygen Research Page 54 o f 110 000077 Interim Report #1 -Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 13. Typical Calibration Curve for PFHS In Reagent Water 0M4MC Omwd M u r `Umm' +OAOIOI f-O M ) i , r. * . p Exygen Research. Page 55 of 110 00007 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 14. Extracted Standards of PFHS in Reagent Water, 25 ng/L and 50 ng/L, Respectively XC03210Q-1. PFHS {Stlrtir*ta}3$& .0fd0.0 u m / M#npi9 2 o f 41 frotnQ3JM09Cjmtr Art: M tbtftt 1440.74? cp* XT: iG.Ste mkr 10. 10 Exygen Research Page 56 of HO 000079 Interim Report #1-Anaiysis 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 RMOMtCoff; ntd/bvird) jm p f 9 o t * 1 from 0 3 7 -K n C .\rU r 40- a0 20- C 1a> A f l f 3! 1 ^ 3.29 ii , i * l i f f 12 45 79 I k m f u t Sfk A- PfWS ifm off*I 10of *41ftwnttMOSCjiM A te :2d148ceunts Hai8ht:M22.1d2op9i R?: 10.594 nife 1.4 11.79 9 1 firn*, ntsfi It 12 13 40 2TO 13 ,1 0 2 0 14 iM 1 17 I ta M Spk 9 - PFHS (QC)399.1W80.D mu-sam p* II 841 *omKW9C.M A*r.23Sei9oa**ff MogM: 30774.(M om RT:.6Kmfe Q. 2-0*4 1-0*4 0X> Tim. min 10.01 Tim*, rfiin Exygen Research Page 57 of 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=I00 (Exygen ID: C0064522, Data Set: 0324O5CR) C9064B22 - PFHS i m j; 5 7 *5 4 eoitflU a** - 36 4 f6 7 ittuw 2 4 0 5 0 ? . 2339.95 C f* * 7 ; J 0J&3 miff 1 0 .3 8 Exygen Research Page 58 of 110 OOOO&l Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 17. Typical Calibration Curve for PFOS in Reagent Water 02M0JC Qrouod (FfC t> ,T>Mr^R*srtiw (1 / x*waghriao): y 311 a 971*'0D3t* PUBM) Afea, counts Exygen Research Page 59 of 110 0000S2 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 Intensity, cos XCmatOtt - PF09 4W.OWa v n e - sampfe 1 of 4! tw n aa 4 C j itf Atm; 20033oout* H*ight: 2520.702 qw RT: 12.83$ Intensity, cp s Exygen Research Page60ofll0 000083 Interim Report #1-Analysis of Oakdale Water Samples Exygen Study No.: P0001400 Figure 19, PFOS in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively Jfrfcpnf Cow* -PFOSfUAHmuxr}460.0*0.0 jwnr r+s: *0 *4 0 ow H * 87: 2.819 m # 9 of4t 0334O6Cwiff 12.02 VVVy Exygen Research Page 61 of 110 0000S4 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-100 (Exygen ID; C0064522, Data Set: 032405CR) In ten siv, c p s C 0 0 & 4 6 2 2 P F O S f lJ fth m 4W.CM0.0 m m u - 3 6 C /B 7 from 0324OQC& . Mf : 15Q7G& 0OM & W #^* & 3 3 J H AT/ J 2 3 min woo5500- 5000 4500 4000 3600 0000- 2300 2000- 1300 1000- soo ol Tim, min 12.14 1ZI Exygen Research ) Page 62 o f llO 000085 intrim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 APPENDIX A Study Protocol P0001400 (Exygen Study No. P000I400) with Analytical Method: V0001780:"Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Water by LC/MS/MS" Exygen Research Page 63 o f 110 000086