Document 6R5X1y0OJbrQ5120DbQqqa2am

AR226-3636 INTERIM REPORT #1 Analysis of Oakdale Water 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 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 0236-01-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.: P0001400 GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT Exygen Study Number P0001400, entitled "Analysis of Perfluorooctanoic A dd (PFOA), Perfiuorobutanesu1fonate (PFBS), Perfluorohexanesulfonate (PEHS), and Perfluorooetanesulfbnate (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 Date 5f a j t K Date ( tr h \a s Date Page 2 of 110 G 0002S Interim Report #1-Analysis of Oakdale Water Samples Exygen Study No.: P0001400 QUALITY ASSURANCE STATEMENT Exygen Researches Quality Assurance Unit reviewed Exygen Study Number P0001400, entitled, "Analysis o f Perfluorooctanoic Acid (PFOAJ, Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and PerfluoTooctanesulfonate (PFOS) 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 Studv 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 Lydia/Shaffer Technical Lead, Qual: Assurance Unit a sh fits Date 1Note: 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 of Oakdale Water Samples Exygen Study Ko.: P0001400 CERTIFICATION OF AUTHENTICITY This interim report, for Exygen Study Number POO014OO, 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: Robert A. Paschke Manager, 3M Corporate Environmental Programs Exygen Research Date Daft^ 41 Jo lo s 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: P0001400 EXYGEN STUDY NUMBER: P0001400 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 St. Paul, MN 55144 STUDY DIRECTOR: Jaisimha Kesaii PJE,,, 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 of 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 of 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 000029 Interim Report #1-Analysis of Oakdale Water Samples Exygen. Study No.: P0001400 TABLE OF CONTENTS Page TITLE PAGE.................................................................................. 1 GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT..............................2 QUALITY ASSURANCE STATEMENT........... ....................... 3 CERTIFICATION OF AUTHENTICITY................................. 4 STUDY IDENTIFICATION.......................................... 5 PROJECT PERSONNEL........................................................................................................ 6 TABLE OF CONTENTS................................................ 7 LIST OF TABLES...................................................................................................................8 LIST OF FIGURES.... .............................................................................................................9 LIST OF APPENDICES........................................ 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 of Oakdale Water Samples Exygen Study No.: P0003400 Table I. LIST OF TABLES Page Summary of PFBS, PFHS, PFOS and PFOA in Water Samples..... ........................................... ............. .................. ........................... 22 Table n . Matrix Spike Recovery of PFBS and PFHS in Water Samples..................... 24 Table IU. Matrix Spike Recovery of PFOS and PFOA in Water Samples.................... 30 Table IV. Surrogate Spike Recovery of 13C PFOA in Water Samples.............. 36 Exygen Research Page 8 of 110 000034 Interim Report #1-Analysts 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 of 13C 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 ,3C 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: 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 of Oakdale Water Sample's 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 #00033 Interim Report #1-Analysis o f Oakdale Water Samples Exygen. Study No.: P0001400 LIST OF APPENDICES Page Appendix A Study Protocol P0001400 (Exygen Study No. P0001400) with Analytical Method: VO00178O;"Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Water by LCZMS/MS" ......... ...................................... ................................................ 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 perQuorooctanesulfonate (PROS) according to .Exygen Method V0001780 (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 of PFOA, PFBS, PFHS and PFOS in water samples were 93% 19, 141% 21, 96% 15 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 of 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 PG001400 (Appendix A). 3.0 INTRODUCTION This report details the results of the analysis for the determination of PFOA, PFBS, PFHS and PFOS in water vising 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 O O G 03S 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 ED 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 of custody information is located in the raw data package associated with this interim report. Storage records will be kept at Exygen Research. 5.0 REFERENCE MATERIAL The analytical standard, PFOA, 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 Coiporation 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 Exvgen InventofvNo.. , Lot# SP0003&00 23116HB SP004184 ; v 3507-195 SP0000252 101 - , SP0002401 :: , SE036 SP0002694 430180-1 Puritv (%) 97.64 97 , 96.7 98.6 101.2 Expiration 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 of 110 000036 Interim Report #1-Analysis of 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: 1,2-13'C perfluorooctanoic acid Molecular Weight: 416 Transition Monitored: 415 -->370 Structure: O 13C \ OH PFBS Chemical N ame ; Perfluorobutanesulfonate Molecular Weight: 338 supplied as the potassium salt (QFgSOjTC*) Transitions Monitored: 299 -->99 Structure: FF F S03 F FF Exygen Research Page 14 of 110 000037 Interim Report #!-Analysis o f Oakdale Water Samples Exygen Study No.: P00Q1400 PFHS Chemical Name: Perfluorohexanesulfonate Molecular Weight: 438 supplied as the potassium salt (CgF^SCbTO Transitions Monitored: 399 -- 80 Structure: FF F PFOS Chemical Name: Perfluorooptanesulfonate ' Molecular Weight: 538 supplied as the potassium salt (CgFiySOaTC4) Transitions Monitored: 499 - 80 Structure: 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 Cis SPE cartridge conditioned with 10 mL of methanol and 5 mL of 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 *1Y'^fV-.j , S' T Page 15 of 110 000038 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.': P0001400 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 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 (ng/mL)1 (pL) (mL) 0 0 40 10 100 40 10 200 40 10 400 40 100 100 40 100 200 40 100 400 . . 40 1o f PFOA, 13C 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 of 110 J D & 9 Interim Report #1-Analysis of 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 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 of LC/MS/MS Instrument and Operating Conditions Instrument: API 4000 Biorrtolecular Mass Analyzer Interface: Turbo Ion Spray Liquid Introduction Interface Computer: DELL OptiPlex GX400 Software: WindowsNT, Analyst 1.4.1 HPLC: Hewlett Packard (HP) Series 1100 HPQuatPump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Thermo Fluophase RP, 50 mm x 2.1 mm Column Temp;: 30 C Injection Voi.: 15 pL Mobile Phase (A): 2 mM Ammonium Acetate in water Mobile Phase (B): Methanol Time (mini 0.0 1.0 8.0 r. 10.0 11.0. 18.0 Total run time: ~18min Flow Rate: 0.3 mL/min %A T 65 : 65 25 25 65 65 %B 35 35 75 75 35 35 Exygen Research Page 17 of 110 000040 Interim Report #1-Analysis of 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 (min) -12 min. ~12 rnin. ~ 12 min. ~5 min. ~11 min. ~13 min. 6.6 Quantitation and Example Calculation Fifteen microliters of 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 fag/L'i - analyte in control (ng/L)) 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 of Oakdale Water 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 s /L - 37600 ne/Ll 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 duplicate o f the primaiy 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 13C PFOAwas 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, t3C PFOA levels were adjusted to require the same dilution as the other analytes. For each primary sample collected, between die,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 of 70-130%. Because laboratory control spikes for 13C PFOA were acceptable in every set, instrument washes were free of 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 he 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 of 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 HI. 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 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 OO0O43 Intrim Report #1-Analysis of Oakdale Water Samples Exygen Study No.: P0001400 Exygen Research Page 21 of 110 000044 Interim Report #1 -Analysis o f Oakdale Water Samples Exygen Study No.: POOO1400 Table I. Summary of PFBS* PFHS, PFQS and PFOA in Water Enyflen ID C0064404 C0064404 Rep C0Q64405 C lien t 3arrvp!s ID OKLMN-GW-W3-0-050310 OKLMN-GW-W3-O-O5Q310' OKLMN-GW-W3-0-050310 Oup Samples Analyte Found (ppt, ngIL) C4 Sulfonate PFBS C6 Sulfonate PFHS C8 Sulfonate PFOS 312 162 4750 296 160 3350 . 303 159 3190 CB Add PFOA 6330 6220 5990 C0064408 OKLMN-GW-W8-0-050310 57.0 ND 59.0 290 000644408 Rep OKLMN-GW-W8-0-D50310* 63.8 ND 55.7 275 C0064409 OKLMN-GW-WB-0-050310 Dup 60.1 ND 56.3 284 00064412 C0064412 Rep C0064413 OKLMN-GW-W264WJ50310 CKLM N -GW -W 26-0-050310* OKLMN-GW-W28-0-050310 Dup 73400 75700 71400 222000 244000 214000 13500000 14400000 12200000 79300000 70200000 71800000 C0064418 C0064416 Rep C0064417 O KLM N -GW -W 33-0-050310 OKLMN-GW-W33-O-O50310* OKLMN-GW-W33-0-050310 Dup 26800 28800 28500 92300 84600 81600 4610000 4870000 4540000 1750000 2020000 2790000 00064420 C0064420 Rep C0064421 OKLMN -GW-W205-0-05Q310 OKLMN-GW-W205-0-050310* OKLMN-GW-W205-0-05Q310 Dup 8260 8000 7650 6740 6610 7070. 146000 119000 116000 147000 150000 156000 C0064424 C0064424 Rep C0064425 O KLM N -GW -W 215-0-050310 OKLMN -GW-W215-0-050310' OKLMN-GW-W215-0-050310 Dup 801 81.2 75.8 769 37100 4400 256 27000 . 3510 270 36900 4070 C0084428 C0064428 Rep C0064429 OKLMN-GW-W2D10-0-050310 O KLM N -GW -W 2010-0-050310* OKLMN-GW-W2010-0-050310 Dup ND ND ND ND ND ND ND NQ ND; ND ND ND 00064432 C0064432 Rep C0064433 O KLM N -G W -FW 7-0-050310 OKLMN-GW-PW7-CL050310* OKLMN-GW-PW7-0-050310 Dup 4460 4340 4630 4800 . 5080 5030 71600 67600 : 72400 37600 38400 38200 C0064436 OKLMN-GW-TRIP1 -0-050310 ND ND ND ND C0064442 C0064442 Rep C0064443 OKLMN-GW-PW8-C-050310 OKLMN-GW-PW8-O-O5031Q* OKLMN-GW-PW8-0-050310 Dup 13300 14100 14100 23SOO 23900 23000 34300 35600 33400 61400 80600 58500 C0064446 00064446 Rep C0064447 OKLMN-GW-PW9-0-050310 OKLMN-GW-PW&4M)50310* OKLMN-GW-PW9-0-050310 Dup 2110 2140 1930 5160 5000 5140 64400 84900 > 88600 49000 46700 46900 00064450 C0064450 Rep C0064451 O KLM N -GW -W 6102-0-050310 OKLMN-GW-W6102-0-050310* OKLMN-GW-W6102-0-050310 Dup NG 53.5 NQ ND ND ND NQ 214 NQ 226 ND C 0064454 C0064454 Rep 00064455 OKLM N -GW -W 6104-0-050310 OKLMN-GW-W8104-0-05031Q* OKLMN-GW-W6104-0-050310 Dup NQ NQ 51.2 ND ND ND 109 207 125 189 118 184 C0O64458 C0064458 Rep C0064459 OKLM N -GW -W 6201-0-050310 OKLMN-GW-W6201 -0-050310* DKLMN-GW-W6201-0-050310 Dup 74.0 74.t 78.0 ND ND ND NQ : NO NQ 95.5 88.3 132 C0O64467 C0064467 Rep C0O64468 OKLMN-GW-W2Q-O-C50309 DKLM N -GW -W 20-0-050309* OKLMN-GW-W20-0-050309 Dup 13600 10700 10000 12900 9040 7860 46*300 : 36300 30100 285000 243000 190000 C0O64471 C0064471Rep C0064472 OKLMN-GW-W22-0-0503D9 OKLM N -GW -W 22-0-050309* OKLMN-GW-W22-0-050309 Dup 36600, 32200 37500 31400 29500 25700 45800 34000 28100 317000 301000 244000 ' La b o ra to ry D u p lica te ND = Not detected at or above 25 ng/L. NO * Not quantifiable =Measured concentration between 5 ng/Land the Limit of Q u antltaB o n (LO Q ) w h ich is S o n g /L. Exygen Research Page 22 of 110 000045 Interim Report #I-Analysis of Oakdale Water Samples Exygen Study No.: P0001400 Table I. & yan ID Summary of PFBS, PFHS, PFOS and PFOA in Water C lie n t Se m ole ID Samples Continued Anatyta Found fppt; ng/L] C4SulfentPFBS C Sudori* PFHS C Sulfonate PFOS C8 Acid PFOA C0D64475 C0064475 Rep C0Q64476 OKLM N -GW -W 31-0-050309 OKLMN-GW-W31-0-050309* QKLMN-GW-W31-0-050309 Dup 1300 1380 1360 5130 4760 5190 132000 132000 156000 23100 22300 24900 C0064478 CQ064478 Rep C0064479 OKLM N -GW -W 32-0-050309 OKLMN-GW-W32-0-05Q309" OKLMN-GW-W32-0-05Q309 Dup 2180 ` 2290 2960 3000 3120 2940 47100 44400 83000 117000 93300 125000 00064432 OKLMN-GW-W217-0-050309 ND - ND NQ NQ C0064482 Rep OKLMN-GW-W217-0-050309* NO -. ND NQ NQ C0064483 OKLMN-GW-W217-C-O50309 Dup ND ND 128 NQ 0006448$ C0O64486 Rep C0064487 OKLMN-GW-W2OO8-O-O5O3O0 OKLMN-GW-W2008-0-050309* OKLMN-GW-W 2008-0050309 Dup 6780 7170 ' ; 6930 10100 10800 10300 15500 17800 18800 58300 58700 60300 C0064490 C00644SO Rep C0064491 OKLMN-GW-W2012-0-050309 OKLMN-GW-W2012-0-05Q309* OKLMN-GW-W2Q12-0-06309 Dup 2210 1960 1920 4700 4470 ' 4420 117000 118000 139000 48900 46400 51400 C00B4484 C00644S4 Rep C0064495 OKLMN-GW-W80-0050309 ' OKLMN-GW-W8O-O-050309* . OKLMN-GW-WS0-O-05Q309 D l*i ND ND ND ND ND ND NO 302 ND 280 ND 328 00084498 C006449B Rep C00644B9 CKLM N-GW -PW 1-0-050310 OKLMN-GW-PW1-0-050310* OKLMN-GW-PW1-0-050310 Dup 5620 5650 5580 4160 . 4160 4170 66900 71600 70900 37300 39300 39100 C0064S02 OKLMN-GW-PW2-0-060310 $41 ' 501 351 3630 00084502 Rep OKLMN-GW-PW2-0-050310* 624 401- 383 3880 C0064503 OKLMN-GW-PW2-0-050310 Di*) 894 700 303 5160 C0064508 C0064508 Rep C0064507 QKLMN-GW-PW3-O-05O31O OKLMN-GW-RW3-0-050310' ; ' : OKLMN-GW-PW3-0-050310 Dup 6970 6740 6570-, 10000 - . 9740 9990 32700 25500 32300 177000 160000 176000 C0064510 C0064510Rep C0064511 OKLMN-GW-PW4-0-050310 OKLMN-GW-PW4*0-050310* ' OKLMN-GW-PW4-0-050310 Dup . 8130 7700 7810 7890 ; . . 7480 . 7550 33800 30300 27800 72100 67800 65900 C0064514 C0064514 Rep C0064515 C0064518 C0064516Rep C0064519 OKLMN-GW-PW6-0-050310 OKLMN-GW-PW6-0-050310* '... v; OKLMN-6W-PW8-0-050310 Dup ; OKLMN-GW-PW10-0-050310 OKLMN-GW-PW10-0-050310* . : OKLMN43W-PW10-04)50310 Dup 7930 8000 8130. 13100 12700 11900 , ,, 14500 14600 14600 ; 29200 27400 -, 28800 90000 86000 85400 1400000 1760000 1740000 78400 78700 78500 719000 781000 614000 C0064522 C0084522 Rep C0064523 O KLM N -GW -PW 11-0-050310 OKLMN-GW-PW11-04)50310* . OKIM N-GW -PW 11-0-050310 Dup 6520 6490. 7150. -. ..y 8820 10000 9050 40800 50800 43400 ,. 60300 71600 60600 C0064526 C0064528 Rep C006+527 OKLMN-SW-0-050310 OKLMN-SW-0-050310* o f OKLMN-SW-Q-050310 Dup u>'. NQ NQ i; . . NQ NQ NQ NQ 1190 1200 1270 491 529 537 00064530 OKLM N-GW-TRiP2-0-050310 ND ND ND ND 'Laboratory Duplicate NO = Mot detected, at or above 25 ng/L. NQ * N otquantrfiabia = ^ su r d co n ctn tfa tQ n t tw 6 n 2 S n g /La n ijth e L riiit crf Q uantitation (LO Q ) which is 50 ng/L. Exygen Research Page 23 of 110 00004 Interim Report #1-Analysis of Oakdale Water Samples Exygen Study No.: P0001400 Table II. Matrix Spike Recovery of PFBS and PFHS in Water Samples Sam ple . Oeecrfpde Amount! Spiked in a li C4 Suttonale P F B S Amt Found Amount In Sam ple Recovered Recovery Ino-) inm u m Amount Spiked C l Sulfonate PFHS Amt Found Amount hi Sample Recovered fngfL) CnBflJ Rwv<*y <*) OKIMN-GW-WW MBOMO {COOftUMSpit CtW ngflLU b Splks) OKLMN'GW-VW-O-O&KHD ICC0W4C4 S j* 0, 50000 nflfl-Leb Spike) OKLMN-GWW3-0-05C310 la w Spike 5 ppb fCQCet-fQft.H npl. FteMSpike ) OKLMN-GW-W3-0-35031D High S p lk eS O ppb (000*44*7, aoooon fL rWte Spike > 5000 50000 5000 50000 312 312 312 312 6980 133 67400 ' 134 7450 74700 143 149 5000 soooo 5000 5DGO0 163 162 102 182 5130 47500 5140 54400 59 SS 100 10e O K LM N -CW -W I-0-O 50310 (CD0044WSpk E, 5000 ft^/LU& Spike] OKLMN-OW-W5-0-050310 (COOM4M SpftF. awMflO^UA Splkal OKLMN*OWAW-C-WD31iJ LOW S p ik e B ppb (C00M410,9000 n9IL FleW Spike) OKLMfWW-WB-d-OSOaiO High Sp ik e 50 ppb (00364411, WOOng*. FWd Spike f 50G 50000 500C 50000 57.0 57.0 57.0 67.0 7020 70000 7410 70500 73 5000 140 50000 147 5000 141 50000 ND MJ ND ND 5120 51400 5510 53300 102 103 110 107 OKLMN43W-W25-0-050310 (C0MU128kS.tKW n ^ U b Spike) O K LM H -G W -W 2W -0$031C (C00U412 Spk h,, SWW RtfL U b Spi| O K U 4 N 'OW-W2S43-050310 L o w S p ik e 5 ppb (00654414s 8100 ng/L Field Spiki) OKLM H-3W .W 2i-D-O M J10 High S p ik e SC ppb (CMK441S. BCObOn&l FMd 3p*e ) 5000 aOCOO 500C 60000 73400 - 73100 73400 125000 73400 73200 73400 147000 *' 500C 222000 103 50000 222000 . 500 222000 147 50COO 222000 207000 252000 210000 266000 < OKLMM-GW-WA3-0-OWS1D (COOM41S Spk l, SOM rtpfLUb Splhe) GKLM N -GW.W33-O-0S0310 (C0C54416 Spk J. 5000 nga. U b Spike) OKLMN43W-W13-D-056310 L o w S p ik e S ppb (C06A441I. sew nglL Field Sfjke ) OKLM M -GW -W 334K)M 3lO High S p ik e ppb (C006441S. BOOOOngfL Fliht S p # a } 5000 50000 5000 50000 26600 26600 26 BOO 26600 33600 133000 38700 1C60Cf> *: 5000 212 50000 - SOOO 102 50000 S2300 92300 92300 92300 78000 122000 65200 150000 59 115 OKU*N*3WAV2D5-04)5C310 (COM4420 Sp*C K, 5000 ng*- U b Spik* > O KLM N-QW-W205-tW)M31O (CWM420 Spk L, 5 R ffl U b S p k *} OKLMN*GW*W205*04SQS10 Low Spike 5 ppb {CDOU422.800 ngft. fW d Spile* ) OKLMH-GWJW2C6-W IM J1D h S p k e 56 ppb {C0flW4Z3,500TO <**1. Field Splk* } 500Q 50000 sooo 50000 6260 0280 6260 62eo 15400 72500 15200 82800 143 5000 1Z6 50000 1S soon 149 50000 6740 6740 740 6740- 12500 53100 11600 60600 115 3 11 100 OKLMN~S W*W215-0-056310 (C00S4424 Sfk U, WOOn^L U b Spike ) CKLM N -SW -W 215-0*060310 jCMMtt* Snk N, 50000 ngO. U b Spike) OKLMN-GW<W21W-OSQ3ie L o w Sp lk * 5 ppb (C0C6442C, StOO F)*Jd Spike > OKLM H-GW-UV215*0-OJW310 H igh S p ik e 50 ppb ,'CH47, SOOOOft0/L Field SpiXm) 5000 50000 5000,. 50000 601.0 601.0. SC1.C 31.0 7200 67200 . 6720 66SCO 128 133' 118 132 500C 50000 5000 50000 769 769 760 769 5280 50300 5240 ' " 48500 \ 90 99 33 95 'San p te residue- exceeds the apiking level sigrklftcantiy: ihwefore, an w cu rtte recovery value canrsol be calculated ND Notd e U iisd 3* o r above 25 ng0 . (ppt). NQ = Noiquertofable ~ Measured eorcentraben between 25 r/L (ppt) and the Limit of Quantitation (LOO) which i$.SO n&L (ppt>. Not: Since thfc $wnm*ry table ehowe rounded ru u ltt, recovery value m*y v*Y*ftM ty from the varie in the raw data. Exygen Research Page 24 of 110 090^47 Interim Report #1-Analy$is of Oakdale Water Samples Exygen Study No.: P0001400 Table II. Matrix Spike Recovery of FFBS and FFHS in Water Samples Continued Sarnph : Detcriotlort C4 SutfonalaPFBS Amount Amt Found Amount Splksd In Sam ple Recovared Recovery (>m!U (n an j ...... PM....... Amount SpMcad (ton.) Ct Sulfonate PFHS Amt Found Amount In Sam ple Racovarad in *) (ru st) Recovery m OKLMN-OW-W2O10-O4SO310 (Ctt6H28SpfcC. SOMft[lLLb SpOut) DKLMN-GW4W2010-4M)5031 S (CCM42S 3p* D, 3WOO ngft.tab SpiW) O K U W -W .m i< W IS10 Lo w Sp lk* 5 ppb [COM4,JMU (A FkM Splk. ) 0 KUMN-GW-W2 0 1 tMMHSWIO Hfflh Spike SO ppb 100094431.SWObrtgd.n*IS SNIte ) 5000 50000 6000 50000 ND ND ND ND 6500 6&5Q0 6700 83B00 132 5000 130 50000 134 5000 128 50000 ND ND ND ND 4800 48700 4700 43700 96 97 94 87 OKUM M-GW-PW?0-6S&310 fC0SS4432Spiee ,9000119ft. UbSpSw | QKLMN-GW-PW7-0-058310 <COG6*4*2 Spk F, SOOOSng/L tab Spike) OKLWbM5Vf-PW7-0-C50310 U m S p ite ppb (00094434,3HWnpA. FMd Spike ) OKLMN-OW-PW7-O-O6W10 HfcH S p ft* BO ppb |C009443S,OOOCO ngft.Field Spike | 5000 50000 5000 50000 0KLUN-GW -TRIP1-0-0H31D Low Splfca I ppb {C0W4437,COWogtL Reid S p i* ) QKLMN-GW-TR1P1-0-1W310 High Spike 50 ppb (C009443S,5WO0 atfL Fkid Spike > 500C Scoto OKLMN-OW-FWfl-0-050310 {CCCW4425okG.5000n.l LsbSpike) OKUW N-GVMW 8-W S0310 (COOS444S5p* H.WOODr/l Lab Soil ) OKLMN4SW-PW8-0-C5C310 Low Spike 5 ppb (C00W444.3HWnflrt. Fleto Spike } OKLMN'QW-Mtt4W>5031C High S p lks M ppb (C00S4445.90000 up*. FWd 3pik* ) 9000 BOOOQ 5000 50000 0KLW N -6W W 3-0-0S0310 {C0Mi44&ok I, SOOdnotUb Split*) OKUAN4SW4PW94MM31Q ^esserne spK j. com n^L tb Sp*e ) OKLMN-GW-PWS-O-ti50310 LovrSpIkO Sppb (C0fl6444e,M<* n^neta'S****) OKLHH-QW -m>-0-060310 High SpUre 50 ppb (C00M44B,so m ntf. ft#!* Spike ) 5000 50000 500' 50COO 0 KiJWN-GVV-V*702-<>-050310 0 *0 Spk K, SOObnpT. Lab* ) OKLM N -aW -W fil02'0-5031b (C09S4450Sfik L, 50000 npfU Leb Spike) OKLMN<lW-W102^-OSO31O Low Spike 5 ppb {C o rn a c 6W0 n^L Fitta Spila > OKlMN-GW-vyi02>o-05oaio High Spite so ppb ICMS44S3,3WJC0 ntf. Field 8ptt ) 5000 50000 5000 50000' 4400 4400 4400 4460 12200 72800 13200 60000 ND 6540 ND ' 44400 13300 13300 13300 13300 21400 79700 21000 80700 2 110 2 110 2 110 2 110 S290 63800 ' 8260 74800 NQ NQ NQ ' NQ 7360 ! .67500 712 70700 ! 155 5000 137 50000 175 5000 151 50000 131 5000 89 50000 162 5000 133 50COO 164 5000135 50000 144 5000 134 50000 144 ' 000 146 50000 147 5000 135 50000 142 5000 14) 60000 4600 4SOO 4600 4800 ND ND 23300 23600 23600 23800 51 BO 5160 5160 5160 ND ND ND ND 8310 50800 9370 59000 4600 46100 2S70C 70300 30000 76100 9310 64400 9950 54600 4890 47400 5040 50600 90 92 91 106 92 92 118 93 124 105 83 98 64 99 96 95 10 1 10 1 'Sample roeidi^ exceeds thespiking isvsl s^nMcsnUy;therefore, artaccurate recovery value cannot be calculated NO * Notdetected at or above 26 ngll (ppi). QuanfrbstkmfLOQ!wfikcfnt.50NQ =Notquantifiable = featured ooocenvefkw between 25 n^t <ppt>and tiielJrrtt of Note;Sino#this summarytable shows rounded rsiufts, recoveryvalues mayvaryslightly fromtti values Inth raw data. Exygen Research. Page 25 of 110 000048 Interim Report #1-Analysis of Oakdale Water Samples Exygen Study No.: P0001400 Table II. Matrix Spike Recovery of PFBS and PFHS in Water Samples Continued Sam ple D e sc rip tio n Amount Spiked C4 Sulfonate PFBS Ami Found Amount InSom pi* Recovaren Reccuety ........... ( " M - l ........M . _ Amount Spfced (9*L> C8 S v lfe ite te P n tS Amt Found Amount in Sam ple R ecovered Recovery (npn-i (nail.) no OKU*N^W -W *fW -e-OSa31b (CtfoMiM 3pk U, 9000 VL Ufo 9<te I OKUWN-GW-W8RM-9-0M310 (CKHU4H 8pkK, BOOMntfL Lab Spite) OK LM hi-aw-w*io4-o^>m io low s p u n ,s ppb (COO*, iW ) nj/L Fh*d Spite ) OKLWNXJW-WaifUJKoSOSin H igh S p ik e SO p p b (C0C*US7.96000 ngiL Fl*kj pika \ 5000 50000 5000 50000 NQ 6660 m 73000 m ; 730 NQ 69700 134 5000 146 50000 135 5000 139 50000 uo UD `ND m' 5050 48D00 4720 51200 101 96 94 102 OKLMN-GW-weao-wi-esoMO (CHH4$a SpfcC, WWr>eT-LjbSpJte! DKLWN-OW-W82O1-0-OSJW10 (C0M4il 3pk 0 .5OW0 npIL U b Spite) OKlMN<GW<m01>tM)503l0 Low Spike 0 ppb {MQM4M, SOCw l FWd Sf*te > OKLMN'OW>VW2Q1*(Ml5031fr High Spike 5 pp b (C0064W. SlflO *dTLFiald5pflu ) 5000 50000 500 5000 74.0 74 0 74.0 74.0 6560 65500 877 7550 130 5000 131 50000 121 500 150 5000 nd NO ND ND 4810 44400 543 5300 92 69 109 106 OKt^N-QW-W2CMM)&030B (00094407 Spfc E, 0 0 r0. Uto 3 ^ t e ) 0KLMN-GW-W2d-d-0WW (COOM497SpKF. MQQOrtgfL Lab Spite > OKLMN^GW-WWI-iKISCJO L ow Splk S pp b (C00944, 500* no*. Flriri S p ite) OKLMN-GW.W20^^5Q3Ci9 High S p ik e 50 p p b {0006470.3DCKM*.*- FUld Spite > 5000 50000 5000 $0000 13900 19400 13-300 77100 13OO 20900 13500 5000 110 5000 126 50000 140 5000 142 , 50000 12900 12900 12900 12900 . 16200 55200 16200 46400 66 65 68 71 OKLMN -GW-W22^-0&050ft (C00e4471 Sp* G, 5000 nyfluLab Spite) 0KLMN-GW*W224WlMi3Di {COO64471 s p k h .80000 r h .u b spite) OKLN N-CW-W2-<H)&<}3<> l o w SpH 4 p p b (CWW4T4, WOOaq/L FWd Spite ) OKLMN-GW-W2i-O.OM3W High S p H SO pp b (C06M474,50000 npiVFWd Spite ) OKLMN-GW-VMl-a^FSOSO (C60U475 Spk 1,5000 npO. Lab Spite) O K LM N ^3W -W 3t^J5O SO 0 [C006447S $f^c J s000 ^L UtoSfUte ) O K LM N -O W -m U M jM W High S p ik e 50 p pb (C0094477. 009 n & L Field S pite} OKU*N-GW-W32-O-&501O9 (COOM47-S Spk K, 3000 n$n_ Lftb Spite) OKLMN GW-W32-O-&5W0 (CODB447B SpK LSMOOnp/L U b Spite) OKLN-OW-W i2*0-309 Law Spike 5 ppb (C0064440.03 r*/L FIWSpite j OKLMN-OW-WMWl-tWW H igh S p ik e SO p p b {CMM4I1, SOW tiftlL FWd Spite ) 5000 50000 5000 50000 5000 50000 50000 5000 60000 5000 50000 368Q0 38600 36600 36600 1300 13O 1300 2160 2160 2160 2100 44100 109000 44000 111000 , 500C 31400 145 50000 31400 * 5000 31400 149 50000 31400 6450 70930 90900 143 138 .. 179 5000 5130; SOOOO 5130 SOCCO 5130 0910 67300 10600 65500 13 5000 3000 130 50000 .3000 172 5000 3000 127 50000 3000 37000 73003 35000 62203 9090 51200 63200 7400 50000 7910 52600 * 63 * 62 7 92 110 66 94 98 100 Sftfnpleresidue BxcaaC& the spiking ierv^t sjgniftcartfty: therefore, an accurate recoveryvalue cannot be calculated NO * Ntrtdefect^tf oretov*Sng/'L(ppt), NO Not quantifiable * Measured concentration between 25 n^L(ppl) andlhe UmH oi QuaftUttLort (LOQ) which 50 ng/l {ppt}- Note; S lnte thi* summary table howv rounded r**uits, reiajvery valuta m iy vary SgbUy fromthe values ki the ra%date. Exygen Research CK; Page 26 of 110 .000049 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: POQ01400 Table II. Matrix Spike Recovery of PFBS and PFIIS in Water Samples Continued Sample O w riM ton OKLMN-OW-W2tr-045O3M ICMSMI*SpkM.W ng/Llab Spite ) QKUIN-GW-W217-4-0503 (CM44ft*Spk N, *0000 Ub Spite > OKLMN-OW^V217-0-050306 Low Spike * ppb tfttOfrUM,9W ng/LField Spite ) OKLMN^W-WSIT-O-oSOSO* HSflh Spike SOppb (CDOMtaS.S0600nfilL FtetdSUw l OKUUN-GW-W2dOM>4M (CDC444I8Spk 0 .5000ngfl. Lab Spite 1 OK!_MN4W-WtOOa-0-05030* (CMNM4MSpkP, 5COOnpO.Lab Spite) OKLMN-OW-W2&OB4-0WMM lo w Spike 5 ppb (CM*Ua>Btm ngU FWd Spite ) OKLWN-GWWJOOfi-O-OMMi High Spike 50 ppb (Cooeail. 6OQ0On/L FMd Spite ) OKLWN-QW-WJOIJ-O-OBOaOB fC0WSp*C,}0<>CoSA.Ui>5eite 1 OKLHN-GW -W 201I445fl30* (CKWMee3p*co, ooooontft. u& Spite | OKLMN-QW-W20124-0503 Low Spfea 5 ppb {COOM402,9000npft. Flat* Spite ) QKLMN-GW-W2012-04SD3Q Hiph Splice 0 ppb (CDOMW,50000 ngA.Field Spite} OKLMN-QW-W6O4-0EO3O9 flCWMW SpieS , s m n a fl tab Spite r OKLMN-GW-W80-04M3C* (OO06UMBpkF, 96000ntfL U p Spite ) OKUdN-QW-WM-O-OSKHH L w Spike 5 ppb <C0MU4M,SOMngft.Rett Spite ) OKLMKJJW-WM-O-05030 High Spike p p b teoo&ur.&o<Honninm spue* ) OKLMN4W-PW14MKW3W (COOPU9I Sfk 6, B00nplLCab Spite) OKLMN-3W-RWl-0-050310 (COMMAS* Bp* H. 0000n pl Lab Spite) OKU4N-QW-7W144S036 Low Spike 6 ppb (00004500,4000ngflLField Spite) OKLMN-OW-PW14460300 HHJh Spike50 ppb [C&OMKM.50400npA.FMdSpBw ) OKLMN.QW-J>VY2-0-050310 (C0M45O2 Spk1.000 Lab Spite ) OKLMN-GW-PW2-0-050310 (CftOM023f* 00W nrt.Lat>Spite > OKUAN-W-FWJZ-O-OWSID Low Spike 5 ppb (C&M4504, SIX npiL Field Spike) OKLMN-aW-PW2-<Mii03'IO High Spike SO ppb {CMMttS. S0OO0D0IL Raid Spite ) C4 Sutfoneto PFBS Amount Amt Found Amount Spiked in Semple Recovered Recovery (n fl'L) (h0L) in tfL ) .<*> Amount Spiked (iwM-i Ct Sulfonat* PFHS Amt Found Amount In Sample Recovered Recovery tnfl/L) <n#rt.) ... m 5000 ND 6660 134 5000 ND 48BO 98 .50000 ND 66800 134 50000 ND 48500 93 . 0 0 ND 7570 151 6000 ND 4590 92 50000 ND 71200 142 50000 ND 51300 103 5000 50000 5000 50000 6780 6780 780 6780 14300 73800 16500 67600 150 SOOO 10100 134 50000 10100 194 SOOO 10100 162 50000 1Q100 18000 56500 16300 64BOO 1TB $3 184 109 ,,5000 50000 5000 50000 22 W SflOO 2210. ! ew oo: 2210 8210 2210 71500. T32 .. SOOO 4700 128 50000 4700 120 5000 .. 4700 138 ' 50000 4700 8140 46600 SOSO 53800 35 84 65 S6 5000 500 5000 50000 WD ND ND ND 8860 137 647D0. 125 7390 140 697D0 139 5000 5000C 5000 50000 ND No NQ ND 4980 46200 5200 46200 100 92 104 98 sooo 5620 13600 50000 5000 5620 5620 72CXX1 13100 50000 5620 sooo 641 50000 641 500Cr ` 641 >. 50000 641 69700! .. ' 7720 85900 7030 64300 160 133 150 128 142 131 126 1Z7 5000 50000 5000 50000 SOOO 50000 5000 50000 4160 4160 4160 4180 , 501 501 501 501 6360 2000 7690 47700 5260 47700 5190 44300 S4 9$ 71 87 95 94 94 sa 'Bam pitt residue exceeds the spiking levol sig n ific a n t: therefore, en accorale recovery value,ca rro t be calculated ND * ^k#Ctetela*<1^tor^^)cv25r>9M PPfr NQ * Not quantifiable h teyred COncentraUon between 25 ng/L(ppt) ancf tha Lim it of OuBrrtitatkxi (LOQ) vhich la 50 oqA. (ppl). Not: Sine* the* untmary table chow* rounded result*, recovery value* may very from the value in tha taw data. Exygen Research Page 27 of 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 Deeciiptto OKLN-(3W-PWa-tJ-TO031O (0006*90So*K,9000ftfifLLed Spike) QKLKN*GW-FVW-iM)W310 (CO.3pku *00 n9fl. U b Splkt OKUHN-QW'Wa-O'WOaiO Low 8plke 5 ppb {ConttM , woo ngflLReid Sjxt* y OKLMN-GW-PW3-0-0W31& HfflhSptke 50 ppb {Coowsoa $00900*- Field Spike) C4 Sulfonate PFBS Amount Amt Found Amount Spiked in Sample Recovered Recovery W4 fnoiU (%) Amount Spiked m C6 Sulfonate PFHS Amt Found Amount In Sample Recovered tn a iL) Recovery 5000 soooo 5000 50000 9970 6970 5070 6970 13600 98900 1.5200 92300 137 5000 10000 180 50000 10000 165 5000 ' 10000 171 60000 10000 13800 6440C 16300 54900 72 8 126 9C OKLM N-GW*PW4*8-0&0310 (C0 4i 1 l SpkM,5004nofl-Lab Spike 5 QKUflN-GW-fW4-IWSa3tO (COCWiic StfcN. 86900natl U b Spike) OKLMN-QW-FW4-0-0M310 Low Spite 5 ppb (C00MS12,$000ng/LField Spike ) OKLMN-GW-PW4-Q-U50310 High Spice 50 ppb (CWWIA wwcpiu fWd 9p(k) 5000 50000 5000 50000 9150 9130 *130 8130 17400 95000 18300 96900 185 5000 7890 174 50000 7890 163 5000 7890 162 50000 7690 13900 53600 13500 58200 120 S1 112 101 OKLMN-GW-PW9-tLOWS10 4C0A64M4Spk0. DOnffl- U b Spite) QKLMN4?W-FWIMM)50310 {CO064514Spk P.40000 n&.U b Spike) OKLM N*GW*PW8-0-050310 Low Spite 5 ppb (C0C44514.9000ngil Ft*W Spike) OKLMN-^W-PWfi-O-OOOStO High S p ite SO ppb (COOW17,50000 ngO. Field Spike) 500C 50000 5000 50000 7gao . . 17200 793C 90500 7930 17100 7930 94600 185 5000 14500 166 50000 1450Q 183 5000 14500 173 50000 14500 20600 5S300 20800 594QC 122 $3 126 90 OKLMN-GW-PW104L0W310 (C0W4314 Spk CrSDOQn p l U b Spite l OKLM N-GW -PW 104-05031C (C0OO4M-9Spk &, SOMOnpfi. U b Spike) OKLMM-GW-fW104M60310 Low Spite 5 ppb fCDOeeiZtL,8DCHJnpfL FW4 Spike ) OKLMNH3W-W10-0-C5C31G High Spite 50 ppb (COOMSaLSO0OOng/LfWd Spite ) 5000 50000 5000 50000 13100 13100 13100 13100 19300 70700 19000 74000 124 5000 29200 133 50000 29200 118 5000 2920C 12 2 50000 29200 34300 71000 33500 71300 102 34 88 84 OKLMN-GW-PW114LWW10 {COT045ZZSpkE, 9000r>gfLU b Spike) OKLMN-GW'PWH-O-OKJaiO (C0004522 Spkf ,0000ng/LUb Spike) QKLMN43W-PW11-0-&50310 Low Spike 5 ppb {C0M45&KAd n<AFM4 Spite ) OKLM N4JW-PW11*0-050310 Hfgh SplkoWppb (CM4S2S. SOWOno- Field Spite) 5000 50000 5000 50000 520 5520 520 9520 1Z700 66300 13200 63800 124 5000 S8ZO 124 50000 6820 134 5000 8820 114 50000 8820 14200 55100 13300 54800 106 93 90 92 "Sample residue exceeds the piking level signifcarfty; teretere, an accurate recovery value cannot be cateuieted NO Not detected at or aiywe 25 r ^ l ippi)NQ = Not gyeniiieb)e= Measured concentration between 25 <ppri) and the UmH of Quantitation (LOG) which h SO ng/L (ppt). IM k Since thleaunwnery table chow rounded reeut, reccviry valL*rniy very IlgTrtiy bomthevalue Inthe rawdata. Exygen Research Page 28 of l l O 000031 interim Report #1-Analysis of Oakdale Water Samples Exygen Study No.: P0001400 Table II. Matrix Spike Recovery of PFJBS and PFHS in Water Samples Continued Sample . . . Description CtSulfoiuttPFBS SuMcnataPFHS Amount Amt Found Amount Amount Amt Found Amount Spiked In Sample RMovured Recovery Spired In Sample Recovered Recovery w w u (ngJL) p y ....... (non.) fmrt.) i*> OKLMM-SW^-050310 <CtWiSpfcQ, 000 ilpt U b &piW*) OKt_MN^W-C-060310 (coousae sr* h, mmo u b fie) . OKLMN-SW-0-06Q310 U rn Spike Sppb (COOtHtO, ) QKLMN-SW-fi-OKmO Htflh Spike 50 ppb (C0MM329, *H htf/LFkld Spilt) 5000 50000 5000 50000 NQ NQ NQ NQ 5800 63600 7260 65000 120 5000 126 50000 NQ NQ 145 5000 NQ 130 50000 NQ ' 4700 45100 5250 40400 90 90 105 99 OKLAIN<IW-TR1P2-0-OW310Low Spike 5 ppb (CflOSMW,6000 ntfL Splk*) OKUdN-QW-TRiP2-<KJfi03io High Spike 0 ppb fCOWtfSi, Moao n^n/Splk,) 500C 50000 NO NQ 4480 20100 90 5000 59 50000 NO NO 4970 49000 SB SB Average: Standard Deviation: 141 21 'Sample residue exceeds the pikinglevelSlgrlficarriv, therefore. an accurate tecovery value cannol be calculated MO * Motselected el or above 25 rg/l (ppl). NQ * Not quenttflable * Measured concentration between25 np/L (ppt) and the Limit of Qoarwtafiorv(LOG)which te60 og/t (ppi>. Note; Since thl* summary uWe show rounded reeuh*. recovery value* may varyallBlrtty from the value* In the 1 * date- Average: Standee Deviation: SB 16 Exygen Research I Page 29 o f 110 000052 interim Report #1-Analysis of Oakdale Water Samples Exygen Study No.: P0001400 Table III. Matrix Spike Recovery of PFOS and PFOA in Water Samples Sample Description CBSulfonate PFOS Amount Amt Found Amount Amount Spiked in Sample Recovered Resovwy Spiked ("s'L) w .. <no/L) [% ) "Vi CSAddPFOA Amt Found Amount in Sample Recovered (non.) "V) Reeovay (%) OKLMN-GW-WWJ-OSWIO {CDM44MSpk C. SOMntfL Ub Spike ) OKLMN-GWAV3-C-C50210 (CDM44D4SfkD. 5MOOnpfLUb Spike) OKLMN-GW-W3-0-050310 Low Splk*5ppto (CW44PL$0001)01 Relit Spikfr} OKLMN-GVV-VV3-MJ5W10 High Spike 50 ppb CMM4407,SOOMitsIL wdpc* I 5000 soooo sooo 50000 4750 4750 4750 4750 12400 73500 10800 84500 153 5000 13a 50000 123 5000 160 50000 6330 8330 5330 8330 . 11900 59200 9470 40100 111 106 83 80 OKLM^lAMWS-0-050310 (CM44M3<*e, MOOgiLLab Spike} OKLMl*GW-WB-0-050310 (COOS440S8ekF.5W04fliJJi.Ub Spite) OKU*fK5W-Wfl-04)$03l0 Low Spike 5 ppfa (C0M4410, M0*tLFlemSfrfk ) QKLMN-GWAMB-iJ-0503-10 High Spike p p b (C0M4411, WOOnpa. *WSpike> 5003 59.0 4940 50000 5000 50000 59.0 69.0 59.0 55000 5300 50500 95 5000 110 50000 106 5000 101 soooo 290 290 290 280 5350 51900 6050 38900 101 103 115 77 OKLMN-GW-W26-0-050310 (CM4tt3pk G. MMntfLUb ftlke ) 5000 13500000 9450000 - 5000 79300000 65300000 OKLHN-GW-W26-0-OW310 (OOMM4iaSpkH, BMOOnoft.UbpUce) 500G 13500000 7390000 * SOOOO 79300000 88300000 OKLMN-GW-W26-0-06Q310 Low Spike 5 ppb (000*4414. MMnflfl. field Spike) 5000 13500000 9050000 5000 79300000 73100000 OKLMN-GW-W2&4M)5031G High Spike 50 ppb (CtW*44fi, so m nqfL FlewSpike ) 50000 13500000 7210000 50000 79300000 57500000 * OKLMN*GW-W33'4t"050310 (CW441Spk i, MM npft. Ub Spite ) 5000 4610000 4720000 * 5000 1750000 1520000 OKLMN-GW-W33-0-050310 10000441Spi J. 50000 OR.UbSpIte ) 50000 4610000 4730000 * 50000 1750000 1650000 OKLMN-GW-WSi'O-OSOilO Low SpikeS ppb {00*441, SM tfign. Held Spilt) 5000 4610000 4920000 5000 1750000 2350000 OKLMN-GW-WM-fl-050310 High Spike ppb (CM04411,10000r*IL FMd Spike ) 50000 4610000 4520000 50000 1750000 1630000 * OKLMN-GW-W205-CW350310 {CODM420fipkK. SOWng!L UUSpike) OKLMN*GW-W20S4L050310 (COM4420Spk L Mfieonprt. UDSpike ) OKl^N43W-W20tHM>W10 Lew Spike 6 ppb ictoswai, 5000ngO. F ie ld sulk. 1 QKLMN-WW2084HKCW Hfflfir Spike 50 ppb (Co***433, SOcbOngfL FieldSpike > 5000 50000 5000 50000 148000 , 136000 * 148000 .166000 146000 129000 20 v 146000 221000 150 5000 50000 5000 50000 147000 147000 147000 147000 160000 190000 143000 184000 8$ * 74 OKLMN-GW-mi 5-04)50310 {C0W4424Spk M,MOOIHJILUb Spite} OKLMN-GW-W215-04KW31Q (CMfi4424Spk N. 50000npILUb Splka ) QKLMM-GW-W215-C-05031Q Low Spike 5 ppb StW M .iW O^FW dSpiM | OKLMN-GW4AH1WW50310 High Spike M ppb 1C0QO4427, SOofiOngiLFieldSpilo} 5000 SOOOO 5000 50000 37100 37100 37100 37100 52400 * , 5000 96900 120 50000 58600 SOW 101000 , 128 50000 4400 4400 4400 4400 &650 567O0 9880 '39200 89 105 as 70 `Sam ple re sid i exceeds Ihe spikino le ve l sig rifica n tly; therefore, an accurate recovery value cannot be calculated ND * Ncrtdatacted at or above 25 rupL. (ppt|. NQ * No! Quantifiable * M easured concentration between 25 n aA (ppt)and the lim it of Quantitation {LOG) which a 50 (ppt) Nota: Since this eummry u&to show* rounded re*t4t*, recovery value mayvaryaiighpy 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.: PQ00140 Table III. Matrix Spike Recovery of PFOS and PFOA in Water Samples Continued Sam ple C8 Sulfonate PFOS C8 Add PFOA Amount Amt Found Amount Amount Amt Found Amount Spiked In Sample Recovered Recovery Spiked in Sample Recovered Recovery KLM N-GW -W 2010-0-0310 (C m e m e p k C . aow agn.Labpti ) OKLMN-GW-W2010-0-050310 iCOMMat Spko, seoeo ngiL me spue*} OKUHN-GW-W201Q-0-050310 Low Spike 9 ppb (C0Oet49Q, MODngiL FWd spike ) XLMN-GW-W201IH K H K B tO High Sp *8 50 ppb { a m m eoeee ngn. FMd spike ) 500C , 50000 5000 50000 O KLM N -G W -PW 7^ Kl5m iO (C0W 432 Spk e , SOM I10L Lab Spike ) 0KlAtN *6W -FW 7-<W >503l0 (CeosM epk f. a n it Leb Spike ) OKLMN*CW-PW7<'O8(l310 Low Spike 5 ppb tCeWS4, 3W0ns-'Lriete pike I OKLAHN-GW-PW7-0-05030 High Spike SOppb (00*444*5, SDOM nafL riW Spite ) 5000 50000 000 50000 0KLMN-GW-TraPHHHC31C LowSpIko S ppb (00*4427. SODOnfr'L Field Spite ) OKLMM-GW-TR]P1<0-4)50310 High Spike 5C ppb (CSD443S. MODO n^lt FNM 8pliie ) 5000 50000 OKLMN-GW-PWfl-tWWOSIO (C0M4442 Spk G, DOWnpIL Leb Spite ) OKLMN-GW*PWe^<KW0310 {CCCM44I S t* H, S o m nfliL Leb Spite ) - OKUHN-GW-PVW4KW610 U w Spike 5 ppb (C0M4444, sow n tfL Field Spite ) OKUWN-GW-PW5-0-M0310 High Spite SO ppb (C0M4446* WWWng/L Field Spike ) 5000 50000 5000 50000 OKLMN*W-PW*-frb5C310 (C*044444* I, WOOng/L U b Sfifc i OKLMN-GW-PWil-<MK03t0 C44444 5 p *J, 50000 nn. Ut>5pH#) OKLMN-CW^W-b-OSOW Low Spike 5 ppb (CW4444*, WOOnoTLriete Splk} OKUWN43W-FW9--0503M) High Spike 00 ppb (Cw ***w , owe note me**sp>h* > 5000 50000 5000 50000 O KLHKW j W -W S102-KI50310 (Cw ew so 3pfcK, SM npit U b Spike ) KLMN-GW-WB102^0-050310 (CW44W Spk L , KOSCOnV Let Spike ] OKLMN*OW-WV6102'<l-050310 Low Spike 5 ppb |COO84452.5000ApO.Field 8lk| > OKLMM5WW10-0-050310 Hiatt Spike SOppb (CO0A44S.MOOOngIL Fkdd Spike | 5000 50000 000 50000 . ND ND NO NO 71600 71600 71600 71600 ND ND 34300 34300 34300 34300 84400 84400 64400 84400 NQ NQ NQ NQ 5170 54600 5270 54900 103 5000 109 50000 105 5000 110 50000 NQ NQ NQ'. NQ 7B50C 5000 37600 119000 05 50000 37600 72600 . 5000 37600 118000 88 5D000 37600 5700 5350 116 5000 107 50000 ND ND 38300 89800 38400 83100 - 5000 i n 50000 - 5000 166 50000 61400 61400 61400 51400 63200 138000 98400 178000 5000 107 50000 5000 183 50000 49000 46000 49000 49000 5300 ; . 106 55800 112 5480 110 53200 106 5000 50000 5000 50000 214 214 214 ` 214 'Sam ple reeldtiB axesada the asking level significantly; Otarefore, an accurate recovery value cannot bo calculated NO * Not detected at or above 26 ng/L (ppt). NO s Nor quantlflatte * Maasored concenbaticn betoeen 25 n^A. (ppt) and the lim it of Ouantitetlcn(kOQ)wWchls5drip/L(ppt)- ...... ...... Note: Since thie ummary table hows rounded mentis, recoveryvalues may vary eliantiy from the value* In the raw cate. 5290 54300 4710 32300 41900 86100 42600 67100 5360 50500 61000 113000 59300 62200 50400 97900 55200 93200 5600 52700 5610 35300 108 10S 94 65 97 * 59 107 101 . 103 42 96 88 113 105 108 70 Exygen Research Page 31 of 110 000054 Interim Report #1-Analysis of Oakdale Water Samples Exygeti Study No.: P0001400 Table III. Matrix Spike Recovery of PFOS and PFOA in Water Samples Continued Sim ple Description CBSulfonate PFOS Amount Ami Found Amount C* Acid PFOA Amount Amt Found Amount Spilled in Sample Recovered Recovery Spiked \n Sample Recovered WU WU <atfU i%i tr>g/U m 0.1 W t) Recovery f* i OKLMH*GW-W610*-0-050310 (CK444H S*khi. 9000 *VU U b > OKLHhW3W-W5104-0-050310 (C0SS44MSpk N, 50000 ntfL Lab Sblkt ) OKLMN-GW-W41C4-0-0SO310 L o w Spike 5 PPb (CD0M4M. BOMnplL FiM 9pw $ OKLMN-GW<WeiC44M)50310 High Spike 50 ppb iCteSi4.B7, SMM ng^. FtaWSpik ) 6000 50000 5000 50000 109 109 109 109 5540 56100 5700 56700 109 5000 116 50000 112 5000 113 50000 207 207 207 207 5290 57300 5+70 35800 102 114 105 71 OKLMM-<3W-W201-0-OW310 |C00*445Spk C, 50W OtfL U P 8*M*) OKLMN<GW-W52Ch-0-050310 (C ttH ttt *f* D>040 Lab Splk*) DKlMN-GW'WUOI-O-tlSU'ID U rn Spike 0.5 ppb (CMH4W, SWng/LFKMpit* ) OKLMN'GW`W201`O-6$<tt1O High Spike 5 ppb (CWS44S1, sow npiLFMd pika} OKLMN^?W-W20-0-050309 (090M447 Spk C,5800 itgiL Lb Spat* ) OKLWM45W-W20-0-09W0 iCMMMdTSpkF, $0*0nglLUb Spite 1 OKLMK-GW-WZO'O'OSOSOfi Low Spike 5 ppb /COOfM. W ntfLFleW 1 0 KLWN-GW-W2 0 -0-050300 High Spike 50 ppb JCW64470, 0000 noA. FMd Spike) 5000 50000 500 5000 5000 50000 5000 50000 NQ NQ NQ NQ 46500 46600 466D0 46600 4280 50000 670 6600 49900 92800 41900 59500 100 5000 100 50000 134 500 132 5000 95.5 95,5 95.5 95.5 5000 285000 92 50000 285000 - 5000 295000 26 50000 295000 4*50 50800 606 6130 239000 295000 278000 264000 97 101 102 121 OKLMK-GW-W220-05030? Spk0 , SONnpA Uh Spike ) OKLMW-CW-W3!2-O-0S030e {C0MW1 Spk H. 50HMI fi/LLab &pilM} OKLMN-GW-W2 2 -0 -050309 Low Spike 5 ppb (C0C44473, MH r>y/LFtokl Splk) OKLMN-GVV-W224L050M High Spike 50 ppb (CWW4474,MHO n&LFieM Spike J OKLMN-GW-W31-0-05D309 ( C m 475 spk I. 44 n p l Lab Sp*w} OKLMN-CW-Wa*-0-050309 JCW4475 Spfc^ soeec rn^L Ufa Sptto ) OKUAH-QW-W31-0-05030 High Spike 50 ppb {C9H4471. UOMegfL Flald 3pll) OKLMN-GW-W32M)503W icoo***ri SpfcK. 00 nga. i t b ) DKLMN-OW-W32-0-03030$ (CWW+71-Spk L.40999 r*gfLLab *pih) OKLMN-GW-W32-0-0M3 0A Low Spfce 3 ppb (caotuto, woa ngn.n*w 8p** > DKLMN-GW-W32-0-050309 High Spate 50 ppb (CMbUSI, BOOOOn|^L FMd&ptk*} 5000 50000 5000 15000 46800 45600 44600 98500 41200 . .5000 105 50000 - 5000 50000 4580D 66800 40 50000 5000 .132000 . 116000 - 5000 50000 132000 159000 72 50000 50000 132000 216000 168 50000 5000 50000 6000 50000 47100 47100 47100 47100 62200 115000 136 74000 - 120000 146 5000 50000 5000 50000 317000 317000 317000 317000 330000 412000 324000 286000 23100 23100 23100 26400 71300 65700 117000 : 109000 117000 151000 117000 131000 117000 1570CK 96 05 - Sam ple residue exceed th e piking level significantly'; therefore, an accu iate recovery valu e cannot be calculated N D = Not detected a l c r above 25 n fl/L (ppt}. NQ * Not quantifiable = M easured concentration between 25 ngA. (pp0 and the Umft of Quanetation (LO Q )v^ ilch 18 50 n g il.ip p t). Mote: SJac* W s um nw y ta.We show * rounded re su lts, recovery value* may vary slightly from ttu value* lit the raw data. Exygen Research . Page 32 of 110 000055 Interim Report #1-Analysis of Oakdale Water Samples Exygen Study No.: P0001400 Table III, Matrix Spike Recovery of PFOS and PFOA in Water Samples Continued Sam ple D escription OKLMN-GW-W217-0415C30 CC4M4442 Spk til ttOO Lab pika) OKLMN/3W-W217-0-OSCa09 (C06644I2 Sek N. S0Q66 ng/L Lab Spike 1 GKLMN-C3W-V21T4KHi0309 L o w S p ik e 5 p p b <CW44*4,tt<fi*fLFl*WS|>iM) QKLMN-GW-W2ir-iM>50JOB Hlfiil S p lk * S 0 p p b ( W W W , b*m o n o n ^ M d sw i C8 Sulfonate PFOS Amount Amt Found Amount Amount S p ik ed in Sam ple R ecovered Recovery Spfkad t n a ' U ____W D ("fW (%) ( 9 C5 A dd PFOA Airrt F o u n d Amount Ir Sam ple R ecovar! (np/L) (n o flj 5000 .50000 5000 50000 NQ NO NQ NQ 4790 49700 5800 65300 86 5000 99 50000 116 5000 131 SOOOO NQ NQ : NQ NQ 4860 52200 4880 42600 OKLMN-GW-W2Q084)-OK>999 (C0W44W SpkO. 0 0 R01 Lab Spike 1 QKLMN-GW-W200Q-0-05030 (toe4444.j* K ROOM UitiSpliui} OKLMN-GW-W8-(M>5WO Lo w S p ik e 5 p p b {SiiM M H.Ewgngn.wa Spa) OKLMN'OW-W2OOB-(Kl5O30i H ig h S p ik e SO p p b (COMM, sooOb n^L Field 3 p * ) 5000 50000 , 5000 50000 15500 15500 15500 15500 20800 68300 27QD0 71300 106 5000 108 50000 230 5000 1 1 2 ' SOOOO 53300 59300 5 S300 59300 G4800 114000 73600 04600 O K LM N ^W -W 2012-O -Q 503M {C0M44WSpk C, <009 ngA. Lab Sputa } OKUMN-CW-W2012>0-O30ft (COB 00 St* D, <0000 n tf l u i> Splk*} OKLMN-GW-W2O12O-O5O30S L o w S p ik e 5 p p b (COftMOM, 5000 eplL FIMti Se'** > OKLMN'CW-W2012-0*0503W H igh S pike 0 0 p pb (C0004493.90090;a9IL FMd Splka) 5000 117000 143000 5D00Q 117000 186000 5000 117000 : , 115000 SDOGO -117000 203000 W 5000 46900 136 SOOOO * 5000 46900 46900 172 50000 . 46900 57700 94700 48500 69500 O K L M N -G W -W a0'O -050S 0S (CM644 Sole *, 9*00 n p l Lab Spite) OKLM N -G W -W 60-M 50 (CMM4M $pk. F, OCP p p ll U b Spfc*) OKLMfWWAVSO-ii^SOSO L ow S pike 5 p pb (900+406, MOO ngfl l*iaUI 8 pfca) c k l m n -g w -w r o ^k w j o s H lo h s p a t e s o p p b ( c w u - w , soooo n # L FMd * p * > 5000 - :ND 50000 5000 ND ND ; 50000 ND 5 2 8 0 52900 5720 57600 JOB- 500C 106 ' ' 50000 114' 5000 115 50000 OWLMN-GW4*W1-{H>50310 (C0M449I3pk G, 0 0 n ^L Lob Spite ) 5000 OKLM ^rG W -FW 1 -OrOSOMO U W 4 H St* H. BOOMn ^ L U b 9iW* ) 50000 ` OKLMN-GW-PW1-0-050310 Low Spike 5 p p b > - i (CwwBOD. eoot ng n n o u 6p * o > 5000 O K LM N -6W -W 1 *0*050310 Hl0 b S pike 50 p p b (COOftCeai, B0600 ngA. PMd Sfika J 5OCQ0 66800 *66800 66900 66900 72000 ` 116000 86900 ' &5200 * SflOO 10 2 SOOOO 5000 5 7 ' SOOO OKLM N-GW fW 2-0*03C3r |C994SQe $pk t, Shoo ng/L Lab Spik) OKUWN-W-FW2-0-O5O31O (C00945C2 $ j* j. GOMOl>0JLLab S p ite) QKLMN-GWPW2-0-050310 Low S pike 5 p p b - {Goomom, sow a p n fh* space * OKLWtH*GW-PW2-<Kl5C31C H lg h S p lk * 50 p p b (C0064MS, Bbooo npiL Raid Spite ) 5000 3S1 5480 i: . 103. .6000 50000 351 5980Q 119. 5 0 000 5000 . =.9 5 i; . .. , , 4.280. . 5000 50000 351 40500 8 0 ' 50000 302 302 302 302 37300 37300 37300 '3 7 3 0 0 3630 3830 3630 3830 SS10 53100 5880 42200 47700 80200 40400 80500 8720 58800 7860 39500 ''Sample residue exceed* the spiking <eud significantly, therefore, so accurate recovery value cannot be calculated ND Not detected at orabove 25 ng/L {pptjt NO - Nrrt quantifiable Measured concentration between 25 ng/L ippt) and the Limit of Quantitation (LOQ) wttlcb la 50 n g tl {ppt}. >We: Since this summary tibie show rowictod m u t a , recovery values may vary slightly front the values in the raw data. Recovery BU 97 104 98 85 * 109 * 71 . 96 . 85 110 108 111 84 . 106 * 86 102 110 85 72 Exygen Research Page 33 of 110 000Q56 Interim Report #1 -Analysis of Oakdale Water Samples Exygen Study No.: P0001400 Table III. Matrix Spike Recovery of PFOS and PF0A in Water Samples Continued Sample Description OKLMN-GW-PW3--050310 <CWS4S0>Spk K. SOfiOP9lLUb Splk) QKLMN-0W*PW3-(M0310 (C***4W48p*L0W"9k-Leb Spike) OKLHN-GW-PW34MW310 Low Spike 5 ppb (CMSfm. 8409n^LFfeMbplk* > OKLMN-GW-PW3-0-O50310 High Spike 50 ppb (csoeiMs, boooonon. Flaw ftplk*) OKLM)M5W-WUM)5as10 (COOM51#Sp* M, SOMna. Ub Sp)k> KLMN-GW-FW4-0-050310 (C09S4S10Spk N, 9W09n&L. Ub Stfl* 1 OKLMN-GW-PW4-O-05Q31& LOWSpike 5 Dpt) (C00S4812,5000npfLFlekl W k#} OKLWN-CW-PW4-0-KW10 High Spike 50 ppb ICW***13. 80000 nga. PisMSpfiu > OKLMN-GWT'Wi-0-050310 (CowS14fipfco, 6000npfi. LabSplka) QKLMN-GW-FWe-fl-050310 (QMMS14SpkP, 59000tigiLLabSplk*) OKLMN-OW-PW6-0-050310 L ow SpfteSppb (CfiOWil*, *090r& L B*dSpike) QKLMfrW5W-PWC-iHi5031fl High Spike 50 ppb (00**451?, 5000Cn f LFl*4d Spike} OKLMN43W-PW10-6-511 (0004*51*Spk C, 5000 nffil LebSplk ) OKLMN-GW-PW10-fl-O5031O (009*451*pk O, S0090agO. LbSpike} OKLNN-GW-FWlO-C-fiaalO LOWSpike S ppb <000*45, BoaongiL FlOd Splk*) DKLWN-GW-PW10--05310 High Spike 50 ppb (C0954521,50*09 rvgA. FmMO ) OKLMN-GW-PW11-0-05310 (COC54A225pk E, 5000 HiLLebtylM) OKLMN-GW-PWmW)50310 iCM*4S22Spk F. 50000npiL Uk Spike} QKLMN-GW-PW11-Q-0W310 Low SplK* 5 ppb tCM*M, 5000null.Ftod Sill) OKLMN-GW-PW11-0-050310 High Spike 50 ppb (CM64525, soot ngfLField Spike V Ua III C* Sulfonate PFOS Amt Found Amount Amount In Sample Recovered Recovery Spiked tofl/U fn a fU f%) w CS Acid PFOA Amt Found Amount in Sample Recovered tu rn (noiL) Recovery M 5000 3270D 43300 5000 177P0D 138000 50000 5000 32700 32700 . 66100 33800 87 50000 ; 177000 ... SGOO 177000 190000 196000 26 50000 32700 SOOOO 55 50000 177000 204000 54 5000 50000 5000 5000 33800 33BOO 33300 33800 42500 75700 42200 81200 * 5000 72100 64 50000 7210D 5000 72100 35 50000 72100 77500 121000 80700 116000 * 98 B3 5000 90000 5DQOO 90000 5000 90000 50000 90000 97600 139000 94100 124000 5000 98 50000 5000 68 50000 78400 78400 78400 78400 82900 133000 87000 116000 105 75 5000 1400000 1410000 tr 5000 719000 50000 1400000 1390000 50000 719000 5000 1400000 955000 5000 719000 50000 1400000 1910000 * 50000 718000 866000 840000 692000 747000 5000 50000 5000 50000 40800 40800 40800 40800 45900 83100 45400 63500 - 5000 60300 85 90000 80300 - 5000 60300 95 50000 80300 64700 105000 63300 98100 so 76 Sem ple residue exceed s the spiking le ve l sig nificantly; therefore, an accurate recovery value cannot be calculated ND - Not detected a t or above 25 ng4_<ppl). NO - Not quantifiable *Measured concentration between 25 ng/L {ppt| and the Limit of QuaniiiaUon (LOO) which is 50 ng/L (ppt). Note; Since this summary table shows rounded results, r*ocv*ry values may vary sligtafy from the values In the raw data. Exygen Research Page 34 of 110 -00M S7 Interim Report #I-Analysis of Oakdale Water Samples Exygen Study No,: P0001400 Table III. Matrix Spike Recovery of PFOS and PFOA in Water Samples Continued Sam ple D m crlp tio n C8 Sulfonate PFOS Am ount Am t fo u n d Am ount Am ount Sp iked b i Sam p le R eco vered R e co ve ry Sp iked re 0m fn sfL i WW <n -) C* Acid PFOA Amt Found Am ount In Sam p le R eco vered ..J n s A i <nB -> 2OKtM N-svwwsosm (Cm>MS s gpk o . n a r t - L e b s#ik* > O KLM N *SVV -0tO 60310 <ComCH Spk a eeooon^ i. U b Spite 1 OKLMN-SW -O-OKKHO Lo w S p ik e $ ppb (COOS4S2I, sow ft?L Flew Spike 1 OKLMN-SW 4>*O50J10 H K)h S p ik e 50 ppb {C em eat, soooc no. new sp ite> 5000 50000 5000 50000 USD 1190 1180 1190 6270 51600 TZ20 58000 102 5000 101 SOCOO 121 5000 114 50000 491 401 491 491 5520 53200 6020 44200 OKLMN-GW-TRIP2-IW)50310 Lo w Sp R ce 5 ppb (C M ttU f. WOOn 0 i. Spite ) OKLMN-QW-TFIP2-CM}W310 High S p ik e 50 ppb tCPWWOTt.SOWr**. Spite) 5000 50000 ND J 6170 ND 57400 123 5000 115 50000 ND ND 6040 57300 R eco very f 101 105 111 B7 121 115 A verag e: Stand ard D eviatio n : 110 32 *$ample residue exceeds trie spiking level significantly; therefore, an accurate recovery value cam el be calculates ND * Notdelected al or above 29 ng/L (ppt). NO - Not qusnttflablM Measured concanfcrabon between 25 ngA (ppt) and die Umll of Quantitation (LOO)which 150 ngA (ppt). Note: Since We summery table bows rounded rasutts, recovery values mayvary IlgM* from tbs values In trie raw date. A verag e: Stan d ard D eviatio n : 83 1 Exygen Research Page 35 of 110 000058 Interim Report #1-Analysis of Oakdale Water Samples - Exygen Study No.: P0001400 Table IV. Surrogate Spike Recovery of 3C PFOA in Water Samples Exygen ID Sample Description Amount Spiked {m m 13c -pfo a Amount Recovered (nart-l Recovery m C0064404 Spk C CD064404 Spk D C0064404 C0064404 Rep C0 0 6 4 4 0 5 C0064406 C0064407 OKLMN-GW-W3-0-050310 DKLMN-GW-W3-0-D50310 OKLMN-GW-W3-0-050310 OKLMN-GW-W3-0-050310 OKLMN-GW-W30-0E0310 Dup OKLMN-GW-W3-0-050310 Low Spike 5 ppb OKLMN-GW-W3-0-050310 High Spike 50 ppb 5500 50500 500 500 500 6000 50000 5580 53900 431 422 416 4730 34500 101 107 86 B4 83 95 69 C0064408 Spk E C0064408 Spk F C0064408 C0064408 Rep C0064409 C00B4410 00064411 OKLMN-GW-W8-0-Q50310 OKLMN-GW-W8-0-D50310 OKLMN-GW-W8-0-Q5031O OKLMN-GW -W 3-0-0 5 0 3 1 0 OKLMN-GW-W8-0-050310 Dup OKLMN-GW-W8-0-C5310 Low Spike 5 ppb OKLMN-GW-W8-0-050310 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 C0054412 C0064412 Rep C0064413 CO064414 CO064415 OKLMN-GW-W26-0-C50310 OKLMN-GW-W26-D-05O310 OKLMN-GW-W26-0-C50310 OKLMN-GW-W26-0-050310 OKLMN-GW-W26-0-050310 Dup OKLMN-GW-W26-Q-050310 Low Spike 5 ppb OKLMN-GW-W26-0-Q50310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 C0064416 Spk 1 C0064416 Spk J C0064416 C0064416 Rep C0064417 C0064416 C0064419 O KLMN-GW-W33-0-05G310 OKLM N-GW-W 33-Q-050310 OKLM N-GW -W 3 3 -0 -0 5 0 3 10 OKLMN-GW-W33-CL050310 OKLMN-GW-W33-Q-05C310 Dup OKLMN-GW-W33-0-050310 Low Spike 5 ppb OKLMN-GW-W33-0-Q50310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 C0064420 Spk K C0064420 Spk L C0064420 C0064420Rep C0064421 C0064422 C0064423 OKLMN-GW-W205-0-050310 OKLMN-GW-W2Q5-0-50310 OKLMN-GW-W2C5-0-05C31D OKLMN-GW-W205-0-050310 OKLMN-GW-W2O5-O-05Q31O Dup OKLMN-GW-W2C5-0-050310 Low Spike 5 ppb OKLMN-GW-W205-Q-C5Q310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 C0064424 Spk M C0064424 Spk N C0064424 C0064424 Rep C0064425 C0064426 C0064427 OKLMN-GW-W215-0-050310 OKLWIN- G W -W 2 15-0-050310 OKLMN-GW -W 2 1 5-0-05031 OKLMN-GW-W215--05C31 . OKLMN-GW"W21SK)-050310 Dup OKLMN-GW-W215-O-O5Q310 Low Spike 5 ppb OKLMN-GW-W215-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5430 32900 7720 7660 7540 5210 28000 3160 46000 262 256 . 261 2750 42500 4940 53000 279 280 307 4240 . 38000 5S50 56700 1010 434 464 4960 35600 99 65 * * 104 56 57 95 52 51 52 55 85 90 105 56 56 61 85 7S 106 112 202 87 93 99 71 The very high PFOA leval In tha undiluted sample Interfered with ,SC PFOA recovery. Note: Since this summary table shows rounded results* recovery values may vary slightly from the value* in the raw data. Exygen Research Page 36 of 110 000059 Interim Report #1 -Analysis of Oakdale Water Samples Exygen Study No.: P0001400 Table IV. Surrogate Spike Recovery of 13C PFOA In Water Samples Continued Exygen !D Sample Description Amount Spiked ingiL) 1iC*PFOA Amount Recovered fng/L) Recovery __{%) C0064428 Spk C C0064428 Spk D C0084428 C0064428 Rep C0064429 C0064430 CO064431 OKLMN-GW-W2010-Q-05031Q OKLMN-GW-W2010-0-050310 OKLMN-GW-W2010-0-050310 OKIMN-GW-W2010-0-050310 OKLMN-GW-W210-0-050310 Dup OKLMIM-GW-W2010-0-050310 Low Spike 5 ppb OKLMN-GW-W2010-0-D50310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5390 53000 432 417 510 4500 30200 98 105 86 83 102 90 60 C0084432 Spk E C0064432 Spk F C00S4432 C0064432 Rep C0064433 C0064434 C0084435 OKLMN-GW-PW7-0-050310 OKLMN-GW-PW7-0-050310 . 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 QKLMN-GW-PW7-Q-Q50310 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 C00S4436 C0064437 COO64438 OKLMN-GW-TRIP1-0-Q50310 OKLMN-GW-TRIP1-0-050310 Low Spike 5 ppb QKLMN-GW-TRIP1-0-050310 High Spike 50 ppb 500 5000 50000 510 5100 51300 102 102 103 C0064442 Spk G C0064442Spk H C0064442 C0064442 Rep C0064443 C0064444 C0064445 OKLMN-GW-FW8--G50310 OKLMN-GW-PW8-0-050310 OKLMN-GW-PW8-0-050310 OKLMN-GW-PW8-0-050310 OKLMN-GW-PW8-0-50310 Dup OKLMN-GW-PW8--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 C0064446 SpkI COO0 4 4 4 6 S p k J C064446 C0064446 Rep C0064447 C0064448 C0064449 OKLMN GW-PW9-0-050310 O K LM N -G W -PW & -0-050310 OKLMN-GW-PW9-0-050310 OKLMN-GW-PW9-0-0531 O' OKLMN-GW-PW9--050310 Diip OKLMN-GW-PW9-0-50310 Low Spike 5 ppb OKLMN-GW-PW9--Q5Q310 High Spike 50 ppb 6500 50500 500 500 500 5000 50000 5250 53900 315 317 338 4230 24800 95 107 63 63 68 85 50 C008445Q Spk K COO64450 Spk L C0064450 C0064450 Rep C0054451 C0064452 C0064453 OKLMN-GW-W6102-0-05D310 OKLMN-GVV-W6102-0-050310 OKLMN-GW-W6102-0-050310 OKLMN-GW-W6102-0-050310 OKLMN-GW-W6102-0-050310 Dup OKLMN-GW-W6102-0-050310 Low Spike 5 ppb OKLMN-GW-W6102-Q-050310 High Spike 5Q ppb 5500 50500 500 500 500 5000 50000 5640 53200 424 439 480 5050 32500 103 105 85 88 96 101 65 Note: Since th is sum m ary table show s rounded results, recovery values m ay vary slightly from th e v a lu e s in th e raw data. Exygen Research Page 37 of IlO 000060 Interim Report #1-Analysis of Oakdale Water Samples Exygen Study No.: P0001400 Table IV. Surrogate Spike Recovery of 13C PFOA in Water Samples Continued Exygen ID S am ple Description 13C-f>FOA Amount Amount Splked Recovered (ig 4 -L _ (ng/L) Recovery m C0064454 Spk M C0064454 Spk N C0064454 C0064454 Rep C0064455 C0064456 C0064457 OKLMN-GW-W6104-0-050310 OKLMN-GW-W6104-0-5031Q OKLMN-GW-W610 4 - 0 -0 5 0 3 1 0 OKLMN-GW-W6104-0-050310 OKLMN-GW-W6104-0-C50310 Dup OKLMN-GW-W6104-0-5Q310 Low Spike 5 ppb 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 0064458 Spk D C0064458 C0064458 Rep C00B4459 C0084460 C0064461 OKLMN-GW-W6201-0-05Q310 OKLMN-GW-W6201-0-Q50310 OKLMN-GW-W6201-0-050310 OKLMN-GW-W6201-0-50310 OKLMN-GW-W8201 -0-050310 Dup OKLMN-GW-W201-0-050310 Low Spike 0.5 ppb OKLMN-GW-W6201-0-050310 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 CO064467 Spk E C0064467 Spk F C0064467 C0064467 Rep C005446S C0064469 COO64470 OKLMN-GW-W20-0-05C309 OKLMN-GW-W20-0-05Q309 O KLMN-GW-W20-0-050309 OKLMN-6W-W2O-0-O5Q3Q9 OKLMN-GW-W20-0-50309 Dup OKLMN-GW-W20-0-50309 Low Spike 5 ppb OKLMN-GW-W20-0-05Q309 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 C0O64471 Spk <3 C0064471 Spk H C0064471 C0064471 Rep C00B4472 C0064473 C0064474 OKLMN-G W-W22-0-S0309 OKLMN-GW-W22-Q-050309 OKLMN-GW-W22-0-050309 OKLMN-GW-W22-Q-O50309 OKLMN-GW-W22-0-05Q3Q9 Dup : OKLMN-GW-W22-0-5Q3Q9 Low Spike 5 ppb OKLMN-GW-W22-Q-0503Q9 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 1 C0064475 Spk J C006447S C0064475 Rep C0064476 C0064477 QKLMN-GW-W3 i -0-050309 OKLMN-GW-W31-0-050309 OKLMN-GW-W31-0-050309 OKLMN-GW-W31 -0-050309 , OKLMN-GW-W31-0-05Q309 Dup . OKLMN-GW-W31-0-050309 High Spike 50 ppb . 5500 50500 500 500 500 50000 541Q 54200 391 391 371 44100 98 107 7 78 74 88 C0064478 Spk K C0064478 Spk L CO064478 CtX)64478 Rep CO064479 C0064480 C0064481 OKLMN-GW-W32-0-050309 OKLMN-GW-W32-0-05C1309 OKLMN-GW-W32-0-05C309 . OKLMN-GW-W32-0-050309 OKLMN-GW-W32-0-05D309 Dup OKLMN-GW-W32-0-0503Q9: Low Spike 5 ppb 0 KLMN- GW-W32-0-050309 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: Sines this summary tabl shows rounded results, recovery values may vary slightly from the values in the raw data. Exygen Research Page 38 of 110 000061 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No,: P000140Q Table IV. Surrogate Spike Recovery of 13C PFOA in Water Samples Continued Exygen ID Sample D escrip tio n Amount Splked (og/L) 13c -p f o a Amount Recovered <ne/L> Recovery (%) C0064482 Spk M C0064482 Spk N C0064482 CO064482 R ep C0064483 C0064484 CQ064485 OKLMN-GW-W217-0-050309 OKLMN-GW-W217-0-050309 OKLMN-GW-W217-Q-Q50309 OKLMN-GW-W217-0-050309 OKLMN-GW-W217-0-050309 Dup OK1MN-GW-W217-0-05030 Low Spike 5 ppb OKLMN-GW-W217-0-050309 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 C0064488 Spk O C0Q64486 Spk P C0064486 00084486 Rep C0064487 C0064488 C0064489 OKLMN-GW-W200&-0-050309 OKLMN-GW-W2008-0-050309 OKLMN-GW-W2008-0-05Q309 OKLWN.GW-W2008-0-050309 OKLMN-GW-W2OO8-O-05O3O9 Dup OKLMN-GW-W2008-0-050309 Low Spike 5 ppb OKLMN-GW-W2008-0*050309 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5410 52500 428 453 468 4850 44700 5140 52100 318 326 357 6040 37800 98 104 86 91 94 97 89 93 103 64 65 71 121 76 C0084490 Spk C C0084490 Spk D C0064490 C0064490 Rep C064491 C0064492 -C0064493 OKLMN-GW-W2012-0-05Q309 OKLMN-GW-W2012-0-050309 OKLMN-GW-W20120-050309 OKLMN-GW-WJ12-0-050309 OKLMN-GW-W2012-0-050309 Dup. OKLMN-GW-W2012-0-050309 LowSpike 5 ppb OKLMN-GW-W2012-0-050309 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 C0064494 Spk C0064494 Spk F C00S4494 C0064494 Rep C0064495 C006449S C0064497 OKLMN-GW-W80-0-050309 OKLMN-GW-W80-0-050309 OKLMN-GW-W80-0-050309 OKLMN-GW-W80-0-050309 OKLMN-GW-W8W3-050309 Dup OKLMN-GW-W80-G-O5O3O9 Low Spike 5 ppb OKLMN-GW-W80-0-050309 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5650 , 52400 486 438 502 5410 41700 103 104 97 88 100 108 63 C064498 Spk G C0064498 Spk H CQ064498 C00S4498 Rep C0064499 C064500 C0064601 OKLMN-GW-PW1-0-050310 OKLMN-GW-PW1-0-050310 OKLMN-GW-PW1-O-O50310 OKLWIN-GW^PWI-04350310 ' OKLMN-GW-PW1-0-050310 D u p : OKLMN-GW-PW1-0-50310 Low Spike 5 ppb OKLMN-GW-PW1-0-050310 High Spike 50 ppb C0064502 Spk 1 C0064502 Spk J C0064502 C064502 Rep 0064503 C0064504 . COO64505. OKLMN-GW-PW2-0-O5D31O OKLMN-GW-PW2-CH35C310 OKLMN-GW-PW2-0-050310 . OKLMN-GW-PW2-0-050310. . OKLMN-GW-PW2-0-050310 Dup OKLMN-GW-PW2--05031Q Low Spike 5 ppb OKLMN-GW-PW2-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5500 50500 500 500 : 500 5000 50000 5150 53000 331 350 352 4420 41600 5420 52600 440 440 431 4880 34000 94 105 66 70 70 88 83 99 104 88 88 86 94 68 Note: Since till* sum m ary tabl* shows rounded results, recovery value* may vary slightly fromthe values In the raw data. Exygen Research Page 39 of HO 000062 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study Np.: POOOI4QO Table IV. Surrogate Spike Recovery of 13C PFOA in Water Samples Continued Exygen ID Sample Description Amount Spiked " C-PFOA Amount Recovered {ttsfl-i Recovery (*> C0064506 Spk K C0064506 Spk L C0064508 C0064506 Rep C0064S07 C0064508 C0064509 OKLMN-GW-PW3-0-050319 OKLMN-GW-PW3-0-05031D OKLMN-GW-PW3-0-Q50310 OKLMN-GW-PW3-Q-050310 OKLMN-GW-PW3-0-050310 Dup 0 KLMN-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 C006451Q Spk M C0064510 Spk N C0064510 C0645010 Rep C0064511 C0064512 C0064513 OKLM N-GW- PW 4--050310 OKLMN-GW-PW4-0-050310 O KLMN-GW-PW4-C-050310 OKLMN-GW-PW4-0-050310 OKLMN-GW-PW4-0-050310 Dup OKLMN-GW-PW4-0-Q50310 Low Spike 5 ppb OKLMN-GW-PW4-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5100 52400 320 324 313 4870 38000 94 104 64 65 63 97 76 CQ064514 Spk 0 C0064514 Spk P C0064514 C0064514 Rep C0064515 C0064516 CQ064517 OKLMN-GW-PW6-0-05Q310 OKLM N-GW -PW 6-0-050310 OKLMN-GW-PW6-0-050310 OKLMN-GW-PW6-0-050310 OKLMN-GW-PW6-0-050310 Dup OKLMN-GW-PW6-0-050310 Low Spike 5 ppb OKLMN-GW-PW6-0-050310 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 C0084518 Spk D C0064518 C0064518 Rep C0064519 C0064520 C0064521 OKLMN-GW-PW10-0-050310 OKLMN-GW-PW)0-0-050310 OKIMN-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-PW 10-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 3670 48500 255 249 258 2980 34100 67 96 51 50 52 60 66 C0Q64522 Spk E C0064522 Spk F C0O64522 C0064522 Rep C0064523 C0064524 C0064525 OKLMN-GW-PW11-0-050310 OKLMN-GW-PW11-0-050310 OKLMN-GW-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-PWt 1-0-050310 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 C0Q64526 Spk G C0064526 Spk H C0064526 CQ064526 Rep C0064527 C0064528 C0064529 OKLMN-SW-O-5031 OKLMN-SW-O-050310 OKLMN-SW-O-050310 OKLMN-SW-O-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 5200Q 124 132 505 5320 41200 96 103 25 26 101 106 82 Note: Since this summary table shows rounded results, recovery values may vary slightly from the values In the raw date. Exygen Research Page 40 o f 110 00QQ63 Interim Report #1 -Analysis of Oakdale Water Samples Exygen Study No.: P0001400 Table IV. xygen ID Surrogate Spike Recovery of 13C PFO in Water Samples Continued wC-PFOA Sample Description Amount Amount Spliced Recovered Recovery <ng/L} _ fno/L> (%) COO64530 C0064531 C0064532 OKLMN-GW-TRIP2-0-050310 500 OKLMN-GW-TRIP2-0-050310 Low Spike 5 ppb 5000 OKLMN-GW-TRIP2--5310 High Spike 50 ppb 50000 494 5520 52900 99 110 106 Average: 83 Standard Deviation: 21 Note; Since this sum m ary table show s rounded results, recovery values m ay vary slightly from the v alu es In th e 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 @00065 Interim Report #l~Analysis of Oakdale Water Samples Exygen Study No.: P0001400 Figure 1, Typical Calibration Curve for PFOA ie Reagent Water *i QXMCSCGroundWaMfRvvTjdbCPFO<$rUmsc"R*Qf*ionfl *l^5-*0C3x+?.3*)4(r*0jW41) Bxygen Research Page 43 o f 110 000066 Interim Report #1-Analysis of Oakdale Water Samples Exygen Study No.: P001400 Figure 2. Extracted Standards of PFOA in Reagent Water, 25 ng/L and 50 ng/L, Respectively XC032tO3-J-PP.* ! c f 4 1 from O S iAO S C .trf A w 4 4 n T counts Hrtgirt 6&3336 qtw RT: V 4 4 6 min 11.64 XCIJ32HW-2 FF0A ^*>dart)4WWW.lJamu - smpl 3 *? 4Mrom D3245C.arfi A na: 782* oowits K*^R: 12703.770 cm RT: U.W2mn Exygen Research Page 44 of 110 000067 Interim Report #1-Analysis of 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 Co**; PFOA {U ntoow(ii413j0& 6$# am v - a*mfair9 o t*1 tom<>3Jl4C6C.wMf Anw; 5766 ccx/fffc JMgMr994,922 op RT: t1.94e ml* 11.86 Note: A linear lot o f PFOA was used to calibrate the instrument. The two peaks shown in Figure 4 are due to different isomers present in environmental samples. The area counts for all isomers present are included to report one total PFOA value. Exygen Research tlKV; Page 45 of 110 000068 Interim Report #1-Analysis of Oakdale Water Samples Exygen Study No.: P0001400 Figure 4. Chromatogram Representing an Oakdale Water Sample Analyzed for PFOA, DF=100 (Exygen ID: C0064522, Data Set: 032405CR) I C6Q64B22 -PFQ* (U*HiWn}413Jt)t$G9.9*<rtv* Sjwwpl* 38 f t w 0324O3R.wr1f Ar*: 87874 counts fr ig h t' 7 f8 0 1 & 4 9 c s R7: t1 2 0 m ln 11,52 intensify, cp s Exygen Research Page 46 of 110 000069 Interim.Report #l-AnalysisofOakdale Water Samples Exygen Study No.: P0001400 Figure 5. Typical Calibration Curve for 13C PFOA in Reagent Water P324D5C OnHTKj R*v7 t (I3C P F O ^ c"U r * r Regression C* '040341 0 C .ttiir) Area, courts Exygen Research Page 47 of 110 0000*7 0 Interim Report #1-Analysis of 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 P XCO33i05-i - iSCPFOA 2 o f 4? frcni C3143C.w)r Arv>: 33102 counts Ni/rJt5iS.f13<y7* R 7 :11J5C min 6000 -t 4000 ii.es 8 9 10 11 12 13 14 16 16 17 Tim *, min p XCP3ZHK-2 - 13C PFQAC&ntnQ 416,0/370.0 amu swnpta 3 of 41 from Q32405C.<jiff *9017 a u n ts Htitft: tj436.4*cpff RI: 1154? rr*. Exygen Research Page 48 of 110 000071 Interim Report .#!-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 ft*geCoi*irof- fJC F'POA (UnhfTvwa) iMS GKiroa - sanrpt? $ o? 41 ffotTr0324C5C H*fr A r*a : Z 1t o o w t* H a itfrt 56,564 c*>j fi7 : ifA 3 4 * n iit 11.83 Intensity, cps Aw;W fl?8tcoo<*s Haflhtj lOWOT^a# ep ffM IX B in * intensity, Dps A * i; 12M65B oowtr h ^ lt: 23388H13cps RT; 1!.M 3flifc Intensity, cps Exygen Research Page 49 of 110 JO O O ' Interim Report #1-Analysis of 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) 006492? 1$CPFQA *mtr-* |te k flo *w J4 ?5 .0 .i3 7 0 .0 **in p J*2 3 Mf fnom032405C.w!r A n : 418903 e&trrfo WWjpAt R i: l i . 855 m h 11,89 intensity, cps Exygen Research Page 50 of 110 000073 interim Report #1-Analysis of Oakdale Water Samples Exygen Study No.: P0001400 Figure 9. Typical Calibration Curve for PFBS in Reagent Water fyT ' ttfWOSCR O rcxni u o u t R*v1 jU i (P F9 S ): "LM a f R w u sto n (1 *#**!<'. y 135 x -tD C H C /ir > Area, counts Exygen Research Page 51 o f 110 000074 Interim Report #1-Analysis of Oakdale Water Samples Exygen Study No.: POOOI400 Figure 10, Extracted Standards of PFBS in Reagent Water, 25 ng/L and 50 ng/L, Respectively P*SS {Staa<f*ri)259jM99.0 2 ofSTfrov? A m : 421 i vxifrts tf&sht? ti)6 S 3 4 c fi9 RT: 3307 min 3.61 I X C 04W S* - PFBS CSMhdtri) 266409.0 *mM- rapfe 3 of 57 'rem Q3M05Cft.iff A w 7H' W r tW *; lT.i4 ej fm 3 *5 4 fl*i Sfl Tim e, min Exygen Research Page 52 of 110 00Q07S Interim Report #1-Analysis of Oakdale Water Samples Exygen Study No.: P0001400 Figure 11. PFBS in Reagent Water, SO ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively Cewrinoi - P F B S f l J t t , 3 9 9 . 0 J 9 & - 0 jw u . sampkt 9 o f B T from Q324t><5CR.*r/f (pM kxoitw fra) I ftogft Spk A- P FIS ( Q C ) 3 S 9 m u a n y! 19 of 97 from 03M05Cfi.wft A t i: 4 wnte hW^T. 1D6.400 cps R7:3.6S2 min 3 65 Mi:f9>92<unta Hwjht: De.W RT: 3.017 min (Qf>. fOOO H& T9 C 300. I, 0.53 1 3-02 i 3 .1 0 A4 2i 4 5 .0 2 .. 8 .7 9.05 11j03 8 0 10 11 12' 13 14 15 19 17 Tim . Exygen Research ; * Page 53 of 110 000076 Interim Report #1-Analysis of Oakdale Water Samples ' Exygen Study No.: P0Q0I400 Figure 12. Chromatogram Representing an Oakdale Water Sample Analyzed for PFBS, DF=100 (Exygen ID: C0064522, Data Set: 0324O5CR) CQQe4522 - f>FBS Unknown) 2$9JM9$.Q mstu * 38 o fe 7 frtrtt 0324&SCJt.irr Ar9:877&oouitiv WWgiri 215.40$cp# flT:-3S24m)n 3432 intensity, cps Exygen Research Page 54 of 110 000077 M erim Report#!-Analysis of Oakdale Water Samples Exygen Study No.: P0001400 Figure 13. Typical Calibration Curve for PFHS in Reagent Water W 2W C Grcimd irftertsr RtvT.ndb (P f K3> ` linear* Reijnrssioo(*1 t x ' y - <WSx +0OCM01 $*C-96&8) Are, counts Exygen Research Page 55 of 110. 000078 Interim Report #1-Analysis of Oakdale Water Samples Exygen Study No.: P0001400 Figure 14. Extracted Standards of PFHS in Reagent Water, 25 ng/L and 50 ng/L, Respectively ' PFHS (S&Stt?*r3)S$$,<>fdG.OMfrta mirnpl* 2 o ( 4 i fm m Q 3 2 4 0 5 C .w ilt A r t : 12966 GQdltti XT: 10.626 rnirr 40JB3 Exygen Research Page 56 of 110 000073. Interim Report#!-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figur 15. PFHS in Reagent Water, SOng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively . p f h s ( U n k n o w n ) * m t awnpM 9 o f* i kem M 4 P3 C .fr {JoVwt not found} oa . 3000 * 2000 c f 1000 RM0MC Sfk 6 - PFHS (QCJ MO WSOJOvtw- sampte 11 trf 4\ ffvn KT2WC.il * '.2 3 8 6 1 8 Mcrntt W*s*<:39774.188op* RT: 10.886* 10.50 110.19-* B 10 11 12 13 14 . 1a 15 17 Timt. mift Exygen Research er}'!- > Page 57 of 110 000080 Interim Report #1-Analysis of Oakdale Water Samples Exygen Study No,: P0001400 Figure 16. Chromatogram Representing an Oakdale Water Sample Analyzed for PFHS, DF=JO0 (Exygen ID: CG064522, Data Set: 0324O5CR) CQ064H2 - PFHS (Uttkno*n}3$9X>&0to MMtt - * i m&f 33 CF67 !h>m 0324v5CR.wifr A w : 373S4-otxin1* H+tgHf: 2939.956 c p s XT: i0363frtk> icjsa Exygen Research (ft $ Page 58 of 110 ooooai Interim Report #1-Analysis of Oakdale Water Samples Exygeix Study No.: P0001400 Figure 17. Typical Calibration Curve for PFOS in Reagent Water 0324D5C Orouiid V ttrR *W .rtb(FrO S> '^ r"R *jn issic> n O /x*i*iglrtW>$): y * 329 >+C>1<nC03$->*OS**} Exygen Research Page 59 of 110 0000S2 Interim Report #!-Analysis of Oakdale Water Samples Exygen Study No,: P0001400 Figure 18. Extracted Standards of PFOS in Reagent Water, 25 ng/L and 50 ng/L, Respectively - PFOS j w s jfn p lt 2<*<41 fi-wrr 032406C.*ifT A r* ,:1 $ 4 $ ev* 'rts Hakfirt 1B9QJ2&opc R7; 12&3B fahr 1 2 .8 4 Exygen Research Page 60 of 110 000083 Interim Report #t-Analysis of Oakdale Water Samples Exygsn Study No.: P0001400 Figure 19. PFQS in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively t0#48 owwrf# iWffW11ifi3.3?6 Cpss R7: t2,81$mt* 12.02 intensity, cpn * v a .Z lW tM * S nW F *:37i,tn cps BT; 12.Biir>r> 1**1 intensity, cps A m : 160532oaums Htfflta: 15it8.73 cps RT: 12.328 mb Intensity, cps Exygen Research Page 61 of 110 000084 Interim Report #1-Analysis of Oakdale Water Samples Exygen Study No;: P0001400 Figure 20. Chromatogram Representing an Oakdale Water Sample Analyzed for PFOS, DF=100 (Exygen ID; C0064522, Data Set: 032405CR) CAQ0w&4;G1252075P$FO>oS*(wUfenkHnovwignh)t46330.3M32904.&C<0 K- *T:*iin2p.f1*363tuCir/t&7 0324QX#.w#r eooo-i 5500 5X0 3000 Intensiv, cps 3 A S 6 7 8 0 10 11 12 13 14 19 10 17 Exygen Research Page 62 of 110 0 0 0 8 S intrim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 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/M S/M S" Exygen Research Page 63 of 110 000086