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p. 111 3 729 INTERIM REPORT # 23 - Analv03 of Sediment Samnles STUDY TITLE Analysis of Perfluorobutanesulfonate (PFBS), Perfluorohexanesuifonate (PFHS), and Perfluorooctanesulfonate (PFOS) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Program , DATRAEODIREMENTS EPA TSCA Good Laboratory Practice Standards 40 CFIt 792 STUDY DIRECTOR Jaisirnha Kesari P.E., DEE Weston Solutions, Inc. 140{? Weston Way . West Chester, PA 19380 Phone: 610-701-j761 INTERIMREPORT_C_OMPLETION DATE May 2, 2006 PERFORMING LABORATORY Exygen Research 3058 Research Drive 1W - State College, PA 16801 Phone: 914-272-1039 : w STUDY SPONSOR 3M Company 3M Building 0236-O1-B-10 St. Paul, MN 55144 Phone: 651-733-6374 P OJECT Protocol N: umber PO(?01131 Exygen Study Number: P0001 131 Total Pages: 110 _ BEST COPY AVAILABLE [WhOi4f, bDu,uenf] 000134 Interim Report #23 - Analysis of Sediment .SampleI3 . E.xygen Study No. : PC001131 GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT Exygen Study Number P0001 131, entitled "Analysis of Perfluorobutanesulfonate (PFBS), Perfluorobexanesulfonate (pFHS~,. and Perfluoxooctanesulfonate, (PFOS) in Water, Soil, Sedimept,~ .Fish,, Clams, Vegetation, S,xnall .Mamm~1., Liver and Small Mammal Serum Using.-LCIMSIMS for the _.3M,,L~ecatur. Monitoring, Program," conducted for 3M Cor.q.pany; is being performed in, compliance with EPA TSCA Good Laboratory Practice Standards 40 CFR792 by Exygen Research, with one exception. The laboratory control and control spikes for the direct injection. method were not recorded promptly at the time of extraction. (-;Z/fi 2!4~ - hn Flaherty f Date Principal Investigator Exygen Research . Jaisimlla Study Director Weston Solutions, Inc. Date Exygen Research Page 2 of 110 0001,35 lifterim Report #23 - Analysis of Sediment Samples Exygen Study -No.: P0001131 QUALITY ASSURANCE STATEMENT Exygen Research's Quality Assurance Unit reviewed Exyger, Study Number P4001131, entitled, "Analysis of Perfluorol.utaitesulfonate (PFf3S), perfluorohexanesulfonate (PFHS), and PerfluorooctanesuTfonate (Plk'G5) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal "Liver and Small Mammal Scram Using I,CIMSfMS for the 3M Decatur Monitoring Program". All reviewed phases' were inspected for conduct according to Exygen Research's Standard Operating Procedures, the Study Protocol, and all applicable Good Laboratory Practice Standards. All findings were reported to the Exygen Principal Investigator and Management and to the Study Director. Phase 25 . Final Raw Data Review and Interim Analytical Report Review Date Inspected Date Reported to Date Reported to Principal Exygen Date Reported to fnvestigatar Management Study Director 0510210b 05102106 05l0210b 05l02106 ~ o` Date Note: All in-lab inspections will be documented in the QA statement for the final analytical report at the conclusion of the study. This QA staternent involves only the review of the interim report and associated raw data. Exygen Research Page 3 of 110 000136 :Interim Report #23. - Analysis of Sediment aarnples Exygen Study No. : P4Q01131 CERTIFICATION OF.AI;LHENTICITY This interim rt:port, for Exygen . Study Number PD0011.31, is a true and complete representation of the raw data. Submitted by: Exygen Research 3058 Research Drive State College, PA 16801 (814) 272-1039 Principal Investigator, Exygen: ohn Flaherty Vice President Exygen Research Exygen Research Facility Management ; dfx Date sz, Z'4 Date Jaisirnha KesW- .E., DEe Weston Solutions, Inc. Sponsor Representative, 3M Company: Exygen Research .53 q6 Date ' Date Page 4 of 110 000137 Iiiterim Report #23 - Analysis of Sediment Sacnples Exygen Study No.: P4001131 STVDVJ NUkTCATION Analysis of Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) in Water, Soil, Sediment;Fish' Clams, Vegetation, Small Manunal Liver and Small Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Program PROTOCOL NUMBER : P0001131 EXYGEN STUDY NUMBER : P0001131 TYPE OF STUDY: Residue SAMPLE MATRIX : Sediment TEST SUBSTANCE : Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) SPONSOR: 3M Company 3M Building 023b-01-B-10 St. Paul, MN 55144 , STUDY DIRECTOR : STUDY MONITOR: Jaisimha Resari P.E., DEE Weston Solutions, Inc. 1400 Weston Way West Chester, PA 19380 Michael-A- Santoro 3M Company 3M Building 0236-01-B-10 St . Paul, MN 55144 PERFORMING LABORATORY: Exygen Research 3058 Research Drive State College, PA 16801 ANALYTICAL PHASE TIMETABLE: Study Initiation Date: 11l05/04 Interim Analytical Start Date: 04127106 - Interim Analytical'TerminatiomDate .- 04/30/06 Interim Report t, ompletion Date : OSl02106 Exygen Research Page 5 of 110 Interim Report #23 - Analysis of Sediment Samples, . . . , , , Exygen Study No. : P4001131 .PROJECT. PERSONNEL The Study Director for,this project is Jausimha Kesari at Weston Solutions, Inc. The following personnel from,Exygen Research weac associated with various phases of this interim portion of the study: . Name Title John Fiahert3!, , _ Karen Risha Vice President ,- Scientist Paul Connolly Technical Lead-LC/MS Christine Edwards iechnician Mark Amrnerman Semple Custodian ~ Amy Sheehan - Associate Scientist Brittany Kravets . , Technician ~ Scott Crain . ... , ,. Technician Frances Crespi . Technician Devon Ingram . Teckrnicaan Christa Gallant Technician Exygen Research Page b of 110 000139 p. 117 Interim Report #23 = Analysis of Sediment Samples Exygein Study No.: P0001 131 TABLE OF CONTENT'S PaLe TITLE PAGE ... .................... ........ . . . .. .. ......... ............ .... . .... ............ . ............ .... . . . ................ . ..1 GOOD LABORATORY PRACTICE- COMPLIANCE STATEMENT .... .... . .................. ...2 QUALITY ASSURANCE STATEMENT . . .......... ...... .... . ...=......... . .... ...........:. ...... ...............3 CERTIFICATION OF AUTHENTICITY .. . ... . ..... ....... .... . ..:. .....:...... ::...... ..... . .....:..:.:. ..... . .. .4 STUDY II)ENT3FICATION . ...... ..... . . ..... .... . .... ........... .... . . .... ...... . . .... . ..... ... .... . ..... ..... ........ ...5 PROJECT PERSONNEL . ........... ..... . .... ...... . .... ........... ..... . .... ..... ... .... . ..... . ...... . ..... ...... ..... ... . .6 TABLE OF CONTENTS . .... ............ . ..... ..... . ... . .... ............ . .... ..... . ...... . ............ . ... . ....... ..... . ... .7 LIST OF TABLES .... .. . ... . ......... ...... ....... .---. . ... . .... ..... .......... .. ..... . ...... . .... ........ . ... . ...... ....... . .. .8 LIST OF FIGURES ... .... .. . ............................... . .... .......... ...... . .... :....... ..... ............ . ...... .......... .9 LIST OF APPENDICES . . .... .............---......... .. ..... .... ............. .... . ..... ....... ............ . .... ...........10 1 .0 SUIbIMARY ........ ... .. . .... .... . .....---............ . . ..... .... . .... ...... .. .... . ..... ....... ....... ..... . .... ...........11 2 .0 OBJECTIVE .......... ... .... ..... .....----. .......... ....... .... . .... ............ . ... ......... .... . . ...... .... ...........11 3 .0 INTRODUCTION.. . ...... .... . ... ....... .......... ........... .... . ...... ...... . .... ........ ..... ...... ...... ...........11 4.0 ANALYTICAL TEST SAMPLES ....... .......... .... . ............ . .... ............. ...... ...... .... . ......12 5.0 REFERENCE MATERIAL ... .... . ..... ....._.......... . . .. . .......... ... . . .. ....:..,.... . ..... .. ..... .... . ......1.2 6.0 DESCRIPTION OF ANALYTICAL METHOD .. ........... . ..... . ....... ..... . ................. ......13 6.1 . Extraction Procedure For Sediment............. . ... . . . ........... ..... . .......... .. . ..... ........... . ... . ..13 6.2 Direct Inject Extraction Procedure For Sediment.............. . . . .......... . ............. ..... . .... .. 14 6.3 Percent Solids Procedure For Sediment ........... . ........... ..:.. . . ::......... . ................ .. . .. .. ..14 6.4 Preparation ofStandards and Fortification Solutions . .. ..... . . ........... . ... ......... .... . .... . . .. 14 6.5 Chromatography ....:............ ..... .... . ... . ..... ............ .... ..... ....... ..... ........ . ... . ........ .... . . . . . ....15 6.6 Instrument Sensitivity ....... ....... .... . ... . ..................... .... . ....... ..... ........ . ... . ...... ........ .. . ....15 6.7 Description ofLC/MS/MS Instrument and Operating Conditions..... . ...... ...... .... . .... 15 6.8 Quantitation and Exarnple Calculations .... ....... ..... .... . ..... ....... ...... ...... . ............ . ... . ....16 7.0 EXPERIMENTAL DESIGN ......... .... . .... ..... ..... .....:..... . ...... ...... ..... ... .... . ..... ........ ... . ....20 8 .0 RESULTS ........ . ...... ..................... ..... . ..... ..... ........... ..... . ... . ........ ..... ....... . ............ .... . ....20 9.0 CONCLUSIONS .. .... . ................. .... .......... . .... ..:.... ...:. ..... .......: ..... ..... . . . .... ........ .... . ....20 10.0 RETENTION OF DATA AND SAMPLES ......................... . . ..... ..... . ................ . . . .. ..21 interim Report #23 - Analysis of Sediment Samples Exygen Study No. : P4401131 Table 1. Table II. Table III. Table N: Table V. LIST OF TABLES Pa&e Summary ofPFBS, PRiS,aud PFOS in Sediment.Samples ..... ....... .. .... ..........23 Summary ofPFOS in Direct In'ection Sediment Samples ....... ............ ..........24 Matrix Spike Recovery ofPFBS, PFHS and PFOS in Sediment Samples .....25 Matrix Spike Recovery ofPFCjS in Direct Injection Sediment Samples .......26 Total Percent Solids in Sediment Samples ......... .... . ..... . ..... ....... . ...... .... ..........27 Exygen Research Page 8 of 114 000141 p. 119 Interim Report #23 - Analysis of Sediment Samples Exygcn Study No. : P{1001131 LIST OF FIGURES Figure 1 . kneTypical Calibration Corve for PFBS in Methanol .. ....... ..... . .... ........ .... . ..........29 Figure 2. Non-Extracted Standards ofPFBS in Methanol, 0.Z'n&/rnL and 0.5 ng/mL, Respectively ... ...... ..... . . . . ... ...... ......... ... . ....... ..... . ... . ........ .... . .... ......30 Figure 3. PFBS in Reagent Blank, 0..4 nglmL Fortified Reagent Spk A, and 4.0 nglmL Fortified Reagent Spk B, Respectively . ...... . .... ...... ....... . .... ...... .....31 Figure 4. Chromatogram Representing a Sedinnent'Sample "1Analyzed for PFBS {Exygen II}: C0172892, Data Set: 042b06F) ....... . .... ........ .... . ............ . ... ........ .32 Figure 5. Typical Calibration Curve for PFHS in Methanol .... ........ .... . ......-.... . .. . ....... . .33 Figure 6. Non-Extracted Standards ofPFHS in Methanol, 0.2 nglmL and 0.5 nglmL, Respectively ........... .... . ... . .................. . .... ........ . ... . ........... . . .......... ..34 Figure 7. PFHS in Reagent Blank., 0.4 nglmL Fortified Reagent Spk A, and 4.0 nglmL Fortified Reagent Spk B, Respectively . ............ . ............ . ... . ..........35 Figure 8_ Chromatogram Representing a Sediment Sample Analyzed for PFHS (Exygen ID : C0172892, Data Set: 042606F) .......... ............ . ...... ...... .... ...........36 Figure 9. Typical Calibration Curve for PFOS in Methanol .. .. .. . ..... . ................. ............37 Figure 10 . Non-Extracted Standards of PFOS in Methanol, 0.2 nglmL and 0.5 ng/mL, Respectively . .......... ....... .... ..... ............ .... ........ ..... ...... ...... . .......... . .38 Figure 1 l . PFOS in Reagent Blank, 0.4 ng/mL Fortified Reagent Spk A, and 4.0 nglmL Fortified Reagent Spk B, Respectively ... ........ . ... . ...... . ... . ....... . .... . .39 Figure 12 . Chromatogram Representing a Sediment Sample Analyzed for PFOS (Exygen m: C0172892, Data Set:042806B) ...... .... . . . ..... . .... ........ .... . .... ....... ...40 Exygen Research Page 9 of 110 000142 , interim Report #?3 -Analysis of Sediment Samples Fxygen Study No. : PODD1131 LIST OF APPENDICES PaQe Appendix A : S-bady protocol P{)001131(Exygen, Study No_ P0001131) with Analytical'Method ~T0001782: "Method ofAnalysis for the Determination,o_f Perfluornoctanoic Acid (PFOA) in Sediment by I,CIMSIMS", and Protocol Amendments .... ....... ..... ......... .... ...... ..... .....41 Exygen Research Page 10 of 110 000143 Interim Report #23 =Analysis of Sediment Samples Exygen Study No:: PO01131 1 .9 SUMMARY Exygen Research extracted and analyzed sediment samples for the determination of perfluorobutanesulfonate (PFq3S~}, ., pp, uor,ohexanesulfofiate, . (PFHS), and perfluorooctanesuifonate (PFOS} a~corc~ri~ to ~xygen Method V0001782 (ppeudix A). The limit of quantitation for PFBS and' PFFIS in sediment was 0.2 nglg. The limit of quantitation for PFOS in sediment was 2:0 nglg. The standard sediment method (V0001782) was originally used to extract all of the samples. Use of this method yielded poor recoveries for PFOS . Because of this, a direct injection method (Section 6.2) was used to analyze for PFOS. Analytical results for the analysis of PFBS, PFHS and PFOS found in sediment samples extracted with the original method are summarized in Table I. Analytical results for the analysis of PFOS found in sediment samples by direct injection are summarized in Table II . The average percent recoveries standard deviations for PFBS, PFHS, PFOS in sediment samples were 85 t 19%, 99 29%, and 93 6%, respectively. Fortification recoveries for the analysis of PFBS, PFHS, and PFOS in sediment samples extracted with the original method are summarized in Table III. Fortification recoveries for the analysis of PFOS in sediment samples by direct injection are summarized in Table IV . The total percent solids for sediment samples are detailed in Table V. 2.0 OBJECTIVE The objective of the analytical part of this study was to determine levels of perfluorobutanesulfonate (PFBS), perfluorohexanesulfonate (PFHS), and perfluorooctanesulfonate (PFOS) in sediment according to Protocol P0001131 (Appendix A). 3.0 INTRODUCTION This report details the results of the analysis for the determination of PFBS, PFHS, and PFOS in sediment using the analytical methods entitled, "V0OO 1782: Method ofAnalysis for the Determination ofPerfluorooctanoic Acid (PFOA) in Sediment by LC/MS/MS ." The study was initiated on November 05, 2004, when the study director signed protocol number P0001131 . The analytical start date for this interim report was April 27, 2006 and the analytical termination date for this interim report was April 30, 2006 . Exygen Research Page I 1 of 110 .er~~~r 000,144 Interim,Repqrt #23 - Analysis of Sediment Sampl,es . Exygen Study No.: P0001131 4.0 ANALYTICAL TEST SAMPLES Three sediment samples (Exygen ID: C0172.892-C0172894) were received on wet ice on April 22, 2006 from Tim Frinak at tJVeston Solutions, Inc. The samples were logged in by Exygen personnel and placed in refrigE7ated 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 standards, PFBS and PFHS, were supplied by 3M. PFBS was received from 3M at Exygen on May, 13, 2005 . 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 . PFBS and PFHS were stored frozen and PFOS was stored refrigerated. Compound PFBS PFHS PFOS Exveen Inventory No. Lot # SP0005726 101 SP0002401 ' SE036 SP0002694 430180-1 Purity 61o) 96.7 98.6 101 .2 EN&ation Date 12J04106 10118106 10131107 'The molecular structures of PFBS, PFHS and PFOS are given below: PFBS . Chemical Name : Perfluorobutanesulfonate Molecular Weight: 338 supplied as the potassium salt (C4F9SO3-K) Transitions Monitored : 299,-* 99;~ _. Structure : ' . PFHS Chemical Name : Perfluorobexanesulfonate Molecular Weight : 438 supplied as the potassium salt (CbFl3SO3'K+) Transitions Monitored: 399 --3 80 Exygen Research Page 12 of 110 0001-45 Interim Report #23 - Analysis of Sedirmnt Samples Structure: F F F ~ F . F ,F F F .-I .F' .I . F F F Exyg'en Study No.: PC001131 _ PFOS Chemical Name: Perfluorooctanesulfonate . Molecular Weight: 538 supplied as the potassium salt (CgFl?SO3x+) Transitions Monitored: 499~-4 80 _ Structure: F 6.0 DESCRIPTION OF ANALYTICALMETHOD The analytical method "V0001782: Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Sediment by LrIMSIMS" was used for the analysis of PFBS and PFHS in sediment samples. A direct injection method, detailed in Section 6.2, was used for the analysis of PFOS in sediment samples. 6.1 . Extraction Procedure For Sediment Before the samples were weighed for the extraction, they were mixed thoroughly by vigorously shaking the container . A 5 gram portion of sediment was weighed into a fifty milliliter centrifuge tube for the extraction. After fortification of appropriate samples, 35 mL of 1% acetic acid in water was added to the sampies . The samples were vortexed and allowed to shake on a wrist action shaker for --60 minutes. The samples were centrifuged for -20 minutes at -3000 rpm, The supernatant was then loaded onto a Cls SPE cartridge conditioned with 10 mL of methanol and 20 mL of water. The eluate was discarded. Twenty milliliters of methanol was added to the sediment samples left in the centrifuge tube. The samples were vortexed and allowed to shake on a wrist action shaker for another 30 minutes . The samples were centrifuged again for .-20 minutes at --3000 rpm. The supernatant was then loaded .anto -the same . Cta , SPE. ~cartridge . The eluate was collected into a 500 mL NalgeneBottle~ The column .was washed with 4 mL of methanol. The wash was collected in the same bottle as the eluate. Approximately two hundred milliliters of water was added to the bottles . The samples were mixed by shaking and loaded onto another Clg SPE cartridge conditioned with 10 mL of methanol Exygen Research Page 13 of 110 000146 Inztrim Report #23 - Analysis of Sediment Samples Exygen Study No. : PQOD1131 and 20 mL of water. The eluate was discarded. Approximately five milliliters of methanol was added to the cartridge, Five milliliters of eluate was collected into a graduated 15 mL polypropylene centrifuge tube. Each sample was analyzed by LC/MS/MS electrospray. 6.2 Direct Inject Extraction Procedure For Sedhnent Before the samples were weighed for the extraction, they were mixed thoroughly by vigorously shaking the container. A one-gram portion of sediment was weighed into a 15-milliliter centrifuge tube for the extraction . Ten milliliters of 1 % acetic acid in methanol was added to each sample. The samples were then shaken by hand, vortexed, and sonicated for thirty minutes. The samples were then centrifuged for -10 minutes at -3000 rpm. Each sample was analyzed by LCIMSIMS electrospray . 6.3 Percent Solids Procedure For Sediment Percent solids were determined using the procedure indicated in Exygen method V0000427 . Approximately 20 grams ofsample was weighed into a, pan. The weight of the sample plus the pan was recorded. The samples were then dried in an oven overnight at 104 2 C. Then the samples were transferred to a dessicator and allowed to cool for -15 minutes. Each sample was then weighed again, including the weight ofthe pan. The percent solid for each sample was then calculated . See Table V for percent solids results. 6.4 Preparation-of Standards and Fortification Solutions A mixed ' stock standard solution of PFBS, PFHS ; and PFS was prepared at a concentration of 1000 ~LglmL by rlissolving 100 mg of each of the standards (corrected for purity and salt content) in 100 mL of methanol, From this solution, the following fortification standards were prepared: Conc . of Stock or Fort. Fort Volume Solution (.NS)/m'l (ML) _ 1000 10 10(? 10 10 10 1 .0 la 0:1 10 ' of PFBS, PFHS, and PFOS Final Vohune (ML) 100 loo 100 . 100 100 Final Conc. of Fortification Std. (pglmL) 100 10 1 .0 0.1 0.01 Exygen Research Page 14 of 110 Oppl~7, Interim Report #23 - Analysis of Sedinjerit Sarnpl6s Exygen Study No.: P0001131 A set of non.-extracted calibratibrr standards containing PFES, PFHS, and PFOS was prepared in methariol, as specified in Exygen= method VOOOI782 . The following concentrations were prepared : '. . ., ' - Conc. ofFort Fort or Calibration Volume Solution n mL 1 (ML) 100 1.0 100 . 0.5~ - ' 100 4.2 ' j 10- 1 .0 5.0 1 .0 2.0 1 .0 ' of PFBS, PFHS, and PFOS Final Volume (n*) Final' Co'nc. of Calibration Std. (ng/mL) 14 ~. 10 - 10 5.0 14 2.0 10 ' 1 .0 10 0.5 10 0.2 The stock standard solution and all fortification and calibration standard solutions were stored in a refrigerator (4 t 2C) when not in use. Documentation of standard preparation is'located in the raw data package associated with this interim report . 6.5 Chromatography Quantification of PFBS, PFHS and PFOS was accomplished by LC/MS/1VIS electrospray. The retention times of PFBS, PFHS and PFOS were -0.56mins, -9.4 mins, and -11 .4 mins, respectively. Peaks above the LOD were not detected in any of the reagent blank samples corresponding to the analyte retention time . 6.6 Instrument Sensitivity The smallest standard amount injected during the chromatographic run had a concentration of 0.2 nglmL ofPFBS, PFHS and PFOS . 6.7 Description of LC/MS/MS Instrument and Operating Conditions Instrument: API 4000 Biomolecular Mass Analyzer Interface: Turbo Ion Spray Liquid Introduction Interface Computer : DELL OpiiPlex GX400 Software. Windows NT, Analyst 1 .4.1 HPLC : Hewlett Packard (HP) Series 1100 HP Quat Pump Exygen Research Page 15 of 110 0 00148 interim Report #23 - Analysis of Sediment SappIps Exygen Study No. : P0001131 HP Vacuum Degasser HP Autosampler . HP Coaumn Oven HPLC Column, . T'hermo Fluophase RP, 5:0 :nm x 2 1 mm Colutnn Temp.: 30 C Injection Vol.: 15 gL Mobile Phase (_A): 2 naIl4 Ammonium Acetate in water Mobile Phase (B): Methanol Time tnin %A %B 0.0 65 35 1_ .0 65 35 $ .0 25 75 10 .0 25 75 11~0. .. 65 35 1$ .0 65 35 Total run time: -18 min Flow Rate: 0.3 mLlmin Ions monitored: Analyte PFBS PFHS PFOS Mode negative negative negative Transition Monitored 299 --> 99 399-),80 499--),80 Approximate Retention Time rnin -0.56 min. -9.4 min. -11 .4 min. 6.8 Quuntitation and Example t;ak:irlafnons Fifteen microiiters of sample or, calibration standard were injected into the LCIMSIMS. The peak area was measured and the standard curve was generated (using llx fit weighted linear regression) by Analyst software using six concentrations of standards. The concentration was determined from the following equations. Equation l calculated the amount of analyte found (in nglmL, based on peak area) using the standard curve (linear regression parameters) generated by the Analyst software program. Please note that the equations in this section are presented in a different order than the equations in the method (V04U1782), but this has no effect on the final calculations . Exygen Research Page 16 of 110 p. 127 J Interim Report #23 -Analysis of Sediment SampTcs . -- l:xygen Study No.: P0001131 uation 1 : Analyte found (nglmL) = (Peak area - intercept) x DF Slope Where; DF =Dilution Factor, factor by which the final Volume was diluted, ifnecessary. For samples fortified with known amounts of PFBSyand PFH&prior to extraction, Equation 2 was used to convert thfe amounC of 1?FBS' and PFHS found in ngJmL to ng/g (ppb). Equation 2; Analyte found (ppb) = LAnalLrte found (n,glmL) x final volume (S mL)] sample weight (5 g) Equation 3 was used to calculate the percent recovery: Equation 3: - Recovery (%) = (,analvte found (ppb) - analyte in control (vnb)l x 100% amount added (ppb) Equation 4 was then used to calculate the amount of PFBS and PFHS found in ppb based on dry weight. Equation 4: Analyte found (ppb) dry weight = Analyie, found (ppb) x [100% l total solids(%)] An example of a calculation using an , aotual.,.s,amlsle ,follows (calculation is for PFBS only) : Sediment sample Exygen 1D: C0172893, Spk F -(Set: 042G06F), fortified at 4 nghnL with PFBS where: peak area 353819 intercept -592 - slope 42300 - dilution factor , . - -. < <. 1 nglg PFBS added (fort level) _ 4 amt in corresponding sample (ngJg) _ 2.41 final volume (niL) .5 sample weight (g) - total solids (%) - 54.37 Exygen Research Page 17 of 110 000150 Interim Report #',13,-- Analysis of Sediment Samples Exygen Study No.: P{OO1131 From equation 1 : Analyte found (ng(mL) _ [253819 - (-592)1 X 1 423f}0 = 6.01 n.ZJrni~ From equation 2: Analyte found (ppb) , _ (6.01 ng/mL x 5 mL) Sg = 6.01 ppb From equaflon 3, % Recovery = (6.01 ppb - 2_41 ppb) x 100'0 4 ppb = 90" 0 From equation 4: ' _ Analyte found (ppb) dry weight - 6.01 ppb x (100% 154.37%) = 11.1 ppb NOTE: This value may be slightly different than that ofthe raw data due to rounding . A slightly different set of calculations was used for the direct injection samples analyzed for PFOS . - Equation 1 : Analyte found (nglmL) = Peak area - interc t x DF Slope Where: DF = Dilution Factor, factor by which the final volume was diluted, if necessary. For samples fortified with known amounts of PFOS prior to extraction, Equation 2 was used to convert the amount of PFOS found in nglmL to nglg (ppb). Eauation 2: Analyte found(ppb) = Anal e found mL x volume extracted 10 mL sample weight (1 g) Equation 3 was used to calculate the percent recovery. Exygen Research Page 1 S of 110 000151 Interim Report #23 -Analysis of Sediment Samples ; -` Exygen StudyNo .: kt1001131 Equation 3: Recovery (%) _ , (anaiyte found Cng(g) - analyte in control fn 1~)) x100% amount added (ng/g) Equation 4 was then used to calculate the amount of PFOS found in ppb based on dry weight. uation 4: Analyte found (ppb) dry weight = Analyte found (ppb) x [100% I total solids(*/o)] An example of a calculation using an actual sample follows: Sediment sample Exygen ID: C0172892 Spk D (Set : 442806H), fortified at 400 nglmL with PFOS where: peak area = 152371 intercept = 3720 slope = 22700 dilution factor - 100 nglg PFOS added (fort level) = 4000 amt in corresponding sample {nF,lg) _ 2360 volume extracted (mL) - 10 sample weight (g) = 1 total solids (%) - 66.54 Fram equation 1: Analyte found (nglL) - - = f 152371 - 37201 x 100 22700 From equation 2: Analyte found (ppbI). = 654 ng/mL ' _ (654 ng/mL x 10 mL) 1 .9 = 6540 ppb ., , From equation 3: % Recovery , . _ (6540 n" - 2360 npljz) x 140% 4000 ng/g 105% From equation 4: Analyte found (ppb) dry weight = 6540 ppb x (100% / 66.54%) = 9830 ppb Exygen Research Page 19 of 110 000152 Interim Report #23 - Analysis ofSediment Samples .. . ,Exygen Study No. : P(i401131 NOTE: This value may be slightly different than that ofthe raw data due to rounding. 7.0 EXPEIRIIVIENTAI: DESIGN For sediment, samples designated as laboratory matrix spikes, PFBS, PFHS, and PFOS were added at a known concentration to the samples in the laboratory after the samples were weighed for extraction. The sediment samples were extracted in one set. The set included one reagent blank and two reagent blanks fortified at known concentrations . The set contained three sediment samples . For each sample, two laboratory matrix spikes and a duplicate were extracted . Due to poor recoveries, the three sediment samples were extracted and analyzed using a direct injection method for PFOS. This method is detailed in Section 6.2 . 8.0 RESULTS Analytical results for the analysis of PFBS, PFHS and PFOS found in sediment samples extracted with the original method are summarized in Table I. Analytical results for the analysis of PFOS found in sediment samples by direct injection are surnmarized in Table IL The average percent recoveries + standard deviations for PFBS, PFHS, PFOS in sediment samples were 85 + 19%, 99 f 29%0, and 93 6%, respectively. Fortification recoveries for the analysis of PFBS, PFHS, and PFOS in sediment samples extracted with the original method are summarized in Table III. Fortification recoveries for the analysis of PFOS in sediment samples by direct injection are summarized in Table IV. The total percent solids for sediment samples are detailed in Table V. 9.0 CONCLUSIONS The sediment samples were successfully extracted and analyzed for PFBS and PFHS according to analytical method VO(}01782 . The sediment samples were successfully extracted and analyzed for PFOS using an alternative method, which yielded acceptable QC data_ Exygen Research Page 20 of 110 Opp1s3 hiterim Report #23 - Analysis of Sediment Sainples . Exygen Study-No ., P0001131 10.0 RETENTION OF DATAAND SAMPLES When the final analytical report is complete, all original paper data generated by Exygen Research will be shipped to the study.director. This does not include facility-specific raw data such as instrument or takperature logs .~~ Ezact copies of all raw data, as well as a signed copy of the final analytical report and all original facility-specific raw data, will be retained in the Exygen Research archives -1'or the period' flf time .specified -in EPA TSCA Good Laboratory Practice Standaitls 40 CFR 7'92 . Exygcn Research Page 21 of 110 000154 Interim~Report #23 - Analysis of Sediment Sampies Exygen Study No . : P0001 131 TABLES Exygen Research Page 22 of 110 p. 133 Interim Report #23 -- Analysis of Sediment Samples Exygen Study No.: P4001131 Table 1. Summary of PFBS, PFHS and PFOS in Sediment Samples Ervom IP C01T2E92 CD172892 Rep C0172093 00172893 Rep CU172894 C0172894 Rep Client S b ID DALSD-BPP01-G-0000 DALSD-BPP01-0-0000' DA1I-SD-BFP02 .0-0000 DAL-SD-BPP02-0-0D00' DAL-SD-BPP03-0-0000 DAL-SD-BPP03~0-0000' C4 Suffonah PF9S vrfluaroomrr:Monau Ana" FoueO Aiee6sed (ppp~ npl9) Aearoa.q o w +r- x 3.14 40 3.10 40 4.43 30 4-84 30 9.B7 30 8.73 30 Ci Sulfionsb PFHS ttirlluorchRmwissuftaft Anoly6t Found Assessed {PPb . "WO) w k Acowsal' "r- % 84.3 30 a6.1 30 74.3 30 64.7 30 139 +SD 123 5D CS Su)fonsle PFOS PwllroroocianusuMaa Analqta Found Assessed (pDti . np+p) wi t Axuraay +~- x NR NR NR NR NR NR NR NR NR NR NR NR 'Lenm+oy oWl ;a% NR = Not reported due 4o OuWIkY control re" f+ilues. See Tabk II !or re-rnrlysis results_ Exygen Research Page 23 of 110 0OO1 .S6 Interirim Report i#23 - Analysis of Sedimwnt Samplcs . ., , ~ _Fxygen Study .No .: PO101131 'i,abie Ii;, Summa>!rya~f 1PFQS in Direct Injection Sediment Samples Exygen ID C0172892 C0172892 Rep C0172893 C0172893 Rep C0172894 C0172894 Rep *Laboratflry duplicate Client . Sample ID DAL-SD-BF'P01-0-D000 DAL-SD-BPPO'-0-0000' DAL-SD-BPP02-0-0000 OAL-SD-BPP02-0-0000* . DAL-SD-BPP03-0-0000 DAL-SD-BPP03-0-0000* CS 5ulfonate PFOS .. -Perttuorooctanrsuifonate Rnalyte Found Assessed (pPb~ ng/g) Dry Welght Accuracy (+1- *- 3550 30 -3520 30 4160 30 3840 30 11900 30 12000 30 Exygen Research Page 24 of 110 0 00 157 p. 135 Interim Report #23 - Analysis of Sediinerd Samples Exygen StudyNo. : P0001131 Table 111. Matrix, Spike Recovery of PFBS, PFHS and PFOS in Sediment Samples Sampls ImauM Spiked C4 iuUMetn FFS6WSt Wd Anrt Found , In Sqnlpb n wal wt - . Amowlt RecAvw4d wll ra. Recpnly x CB SuMonste PFN81IW1WN 1 iOmt.Fau1W . Mm"t in 8a" RLoaowErnd R n wst wl. Wat rt % Ci SIIfanIMa PFOS VlhtWa Arm Found In Swppia wet wt. . Amount _ Raoorahd wat wl. Raaowry % DAL~o-erPOio-oooo , (Cpf nmapy C .4 PPlr Ihlly 4 ZOO . - 447 DALSD4BPP0I-Q-0ODO 0a17UNa0 a4oosa,nof 400 2.De 2e2 66 50.1 4" SO - DAL"SD-BPA01-0-0000 1M72n111kE.4ooonn1P3puU 4000' 2.08 2870 67 68.1 _ , 8190 128 , NR - - NR NR DALSD-BPPU4-0-0O80 FoV21S3lnto.4nNSpft) " 2.41 DAL-SD"BPP02-0-0080 NS- 00 Q AS ppeeprl 40D 2-41 DALSD43PP02-0-0080 (at7wa Ilrt u, romwv adli 4000 ,2.41 8.02 00 - ' - - - , " - 374 03 40.5 .. 316 78 - " - 3620 95 40s 5090 120 Ni HR NR DAL-BD"BPP00-0-0000 OCDI7lrilck 1. a hb spew a+Laa13aa03-0 .0000 {oor w SON J. 400 rar eMwd DAL.,SD-80-0-0000 (CotrrErEqiIL4wopvvloIr) 4 400 4000 1 4.39 4.30 4.30 7.71 83 380 80 - 01-8 4840 121 01 .8 283 4600 ae - 111 . NR - - NR NR AvemsqW 0 Standard DwIaYan: 1f Aww I!l Wandard D4vhtlo~ 1! -Srnple rar07ue nsasd@ ia+oUli WwW$4(0A=nWY I3msokhro IrwKrw*fnr.. .. arsuna racoveyvru .raved e4 ealddrl4a ND = Notdceeele'star abms h*L"ol QIwIMbYon P .O*d02 npp(wdwwlyYR1. NR rR0tIlpOitlC d~e tr 9uWKyoDMld roiW (iINroR S!~TiOI! IY IOr1a+1~7M ~11yNabs : iha OftslwntinarY1i6b ahows,eunded IuWq,rncovwrywFeo nnYyiyalphlr p*ntly nslns Intlw rewr dMa. Awwqw: NR 3andwl Darlalloa: NR Exygen Research ` ` Page 25 of 110 000158 lnterim Report #23 - Analysis ofSediment . San$les Exygen Study No.: P0001131 T'abIoIV. Matrix Spike Recovery of-PFOS in Direct Injection Sediment Samples Average: 93 Standard Devlatlon: B *Sample rosidue w=edsthe epiking level significantly (3x apking levei); therefore, an accurata neoovsry velue cannot be Calculated ND = Not detected at or abovetheLimit of QuanleFation (LOO)of 0.2 ngfg (wel wafpM) . Note! Since ado su mmarytable shwvs Founded results. recovery vahm may vary sliphtty from the valws In the raw data . Exygen Research Page 26 of 110 0001.59 Lnterim Report #23 - Analysis of Sediment Sarnples Exygen Study No . .- P0001131 Table V. Total Percent Solids in Sediment Samples Exyqen ID C0172$92 C0172S93 C0172894 Sample ' Description DAL-SD-BPPDI-f}~G[)Od DAL-SD-BPP02-0-0000 , DAL-SD-BPP03-0-D000 . . . Total SoMs (% 66.54 54 .37 44 .46 ~~tY~ : Exygen Research Page 27 of 110 0001.60 Interem Report #23 - Analysis of Sediment Sarnples Exygen Study Na,: P0001131 FIGURES Exygen Research Page 28 of 110 ooo1si p. 139 Interim Report #23 r- Analysis of Sediment Samples Exygen Study No-: P0001131 Figure 1. Typical Calibration Carve for PFBS in Methanol oaeoev s .e~~a~ .ree (r~BSx " un~rr Ryrurelon P~ rx Y..~onthpz+~ . axt.+ooo x+ .oat (~ " o.acca~ 4_40 " 4245 4AO6 3 .8a6 4 3r6 .Q- 3 .4e6 3.2*6 3.066 2.866 2Ae6 ~ C 0 A m c` 2 Exygen Research Page 29 of 110 000162 Interim Report #23 -- Analysis of Sedirnent Samples Exygcn Study No . : FQ(1D1131 Figure 2 . Non-Extrafted Standards of FFBS in Methanol, 0.2 ng/mL and 0.5 ng1mL, Respectively ssinas~s-PFSS ~+dara~a as~~r.~~rra .Mmmrr. a!mt'otrdr, Odaca~!Fwff ara&: SW cor.Il. Mi90te sos.*o0 W xF. assRW& a 2 13.74 T 8 0 10 71 12 73 14 75 10 17 TIM-L min SS007nd4'S " fFB3 (. . Sta0 nda0 0 rd)C 299 aunu -sampia 2 rf 46 *gm 042p00FariM , Area : 200D1 count ; Htipht: 1 .40a+003 opt HT : 0.550 min a Q c m Exygen Research Page 30 of 110 000163 p. 141 , blerim Report #23 .- Analysis of Sedimebt samples : Exygen:Study ria.:.PD001131 Figure 3. PFBS in Reggent Blank; Q~4 ng,ImL Fortified Reagent Spk A, and 4.0 nglmL Fortified Reagent,Spk.B; Respectively , a~ conaow ~~~~~.. -PM ~INx fY. ~.*idJ eum+~o+rr) t~~usFio-s~ir~ r. ,pw m ; . v 1 S'. ' 13.OCi N Q u G C 4 4--- 0- _- -7 S D ID 79 72 73 74' 4 Tlma, min , Roaysnt BpkA . PFBS (QL72GIa.DWDOD am " sample o 6145 from 04260DF .witS Ns~ tDY7D wuntr Holyht: 1 .06e+003 oPf RT:O .dlf7 mih O .E+D 4D a u . cro c $ 7 8 G 7D 1t '12 13 14 46 16 1T Tinma, min , Reayrat SpkB " Pros (QC)200iDlOD .D amu-samplo 70 of 44 hom 042EODF .wi1f Nma: iD8227 oounls H" IpM: 9 .71s+004ays RT :O.DD7 min CM , 1 .L10s44 4 u ~ c COOQ .00 0.00 D S -(r-lo 41 72 73 14 to 1E Timt, min Exygen Research Page 31 of 110 000164 Interim Report #23 - Analysis of Sediment Samples Txygen Study No.: P4,001131 Figure 4, Chromatogram Representing a Sediment Sample Analyzed for PFBS (Exygen ID: C0172892, Data Set: 042606F) , o~myQ.~~s .ow,.)rra~xo~.. .Affawl.aroeOnM..0rMw,.ra w.=: aaa~w.a Hrr~~ aso.+ooo~a" ar. ~.sro~riw o.ey a s u C C Time . min Exygen Research Page 32 of 110 00Q1f;5 p. 143 Ynferim Report #23 -- Analysis of Sediment Samplds Exygen Study Na. : -POOb1131 Figure 5. Typical CaUbratioa Curve fvr;PFIS ln `Metha~noI D4Z008FSadimani.rdE(VFH3~'LinearReyresion(4Je wNyhliny):y- 7ip0*a004M +-7 .1 OM (r - GANG) 7 .306 7 .0115 Q .Soa 0.046 - 5-5615 - 6 .045 4.'S46 ~ m 4.UaC - O ca cma 3 .585 < 3 .046 . ss .a 2405 1 .6~f - 1 .DSS - O.Dp- Cononnta0an,nplinL Exygen Research Page 33 of 110 000166 , , p^ 144 Interim Repoz: #23 - Analysis of Sediment Saankples _ P.xygen Study No.: l'OO41131 Figure 5. Non-Extracted Standards of FFHS in Methanol, 0.2 nglmL and 0.5 nglanL, Respectively . , sSrMslli " POW tstr.dad)3Mwaa@@eAr " se"ta tafIS itop oowiFmlr a.~~ m~ecorar ~a~ r~s. .r~~ere ~:" u~~te 9 .40 ?oa a 4C0 i ID 3W J 200 700 0 0 90 Time, min 580014606 " PFNS (5landaId)300 .OIH0.C amu " sample 2 0 45 tram 042OO6F.wW , Area : 33083 a*unfa Height 1.73*+OD3 q5 FM 9 .40 wWn 0 .40 7600 u CuL 1000 F c 600 0 hx3+gen Research Page 34 of 110 0001(;7 p. 145 -Interim Report #23 ~ Analysis of Sedimerit Samples Exygen Sttiiiy No,: p(1001131 Figure '1. PFHS ih~ReagehtBlanlf;'U.4 figfim~. FortiRed Re2lgent Spk A, and 4.0 nglm~; FiirtiffM Reagent Spk B, Respectively , Rasl.~tceatrol "i+A~18Nl+troualj]skbsri~ poet not fmrd) =,~.r+i~pJ~!aafTSfro, ~.l~iiil~.+rJn' 0.3e 12 .47 n ,13.13 12,31 '81 2 .02 440 5,~ ---- 9 .9B 11 ~~ I ~ f ~ 6~ j 116D6 VV cc 3.30 0.77J .06 8'~ l /}l4fl ~Y"~y~SU! U LV 5 e 7 8 0 10 11 12 13 14 1d 15 17 Time . min Reagent SpkJ1- PF1i8 (. QC)30 00O= area -urpple p 6148 fhem 04230pF.wiR , Area: 27M ooantc Height, 1 .60e+003 opc RT :0.3q min G .3D a u t 0 10 11 ix 93 14 Tllwr. nNa ' Reagent Sph B " PFHS (QC)9W .0l80 .0 am " sarnpla, 10 of 46 fronm042006F .uJ11 Arnr. 27E07" eswftt NoipAtt 1 .d0e4-004 epr RT : 9.40 min a V . ~ . C C GAD 16 17 Exygen Research Page 35 of 110 000168 Interim Report #23 -- Analysis of Sediment Samples- , ; Exygen Study No ., : POO01131 Figure 8. Chiroas4atogram Representing ~a Sediment Sample Analyzed for PFHS (.Exygen ID: C0172892, Data Set: 042S0bF) , G772~lQ" PF7~ ~ArRrow~r)~llA+dOlO~r~ "p+~A i~ol~5lFiow if~iOiF.~Wt1 Anr. 3Kr.i9 wwns Wait 2?3b+OOLi ape A'T: !N'! rtir 9.41 180P " 1000 " 1400- w a u 1200- N Lm low C Ow . 40D 200 F,xySen Research . Page 36 of 110 000169 'Interim Report #23 - Analysis of Sediment Samples ~ ~ Exygen Study No: : =P00{1113 l Figure 9. Typical Calibration Curve for PFOS in'Mithanol o42aoee s.d . ni .rde Srvos~~ "Wn"pP Rrapr,esi0n (11 fir weiphunpx y" 2.zv.+ooax+a_rz,.oo3 (r=o .ooaAS) 2 .526 " 2.4ed - e 3 D u u 4 6 a 7 a 0 10 CsnerntralFen . eplmL Exygen Research Page 37 of 110 p. 148 Interim Repart #23 - Analysis of Sediment SarnpjIes,, . Exygen Study No.: PO901131 Fignre ] O, Non-Extracted Standards of PFOS in Methanol, 0.2 nglmL and .0.5 ngImL, Respectively , 55Ail45li "PFQS J9hredrrd) 4WM0 "ra "mmwJ+ !af45lrow MWMvff Arn: 1V3! eowarb Wolf. "a1*+N2 eps RT." i1Iaijr 11 .42 800 R OOo Q 400 ~ d 0 1 2 3 " 6 0 7 8 0 10 Time, min SeQU94596 ~ PF 09 (9tandard) " .019D .D srtw - sample 2 045 lrnm D42900B,witt , Area: 12226 oounb Height 7.72*+002 op RT : 11 .4 min Too - Ow . i s00 4oo 300 200- 11 .43 '1000 1 1 2 3 4 !S 0 7 8 Y 10 Time . min Exygen Research rage 38 of 110 000171 p. 149 Interim Report #23 -AnaIysis of Sedirnek Samples txygen Study N . :-P00O 01131 Figure 11 . PFOS in Reagent Blatik,' 0.4 DglmL~ Fortrf ed Itcagent Spk A, and 4.0 nglmiJ Fortified Reng'eiCt Spk, ,B.) Respectively , R.~r~r: car~ - ~s n+r~r~r.wr~ s~ov~o a.rr- -is+.~e'~ o~~ riorp ioa~ Ares: 330eowrffifs ftvyft 211r+00lcAr R'F" 11.5 win ' . 11 .46 m a 'c81 m c 7 8 D 10 Time, Min , Raapaat SticA " PFOS (OC)400 .OUB0.0 amu " sample O o0,46 trom m428006mi11 Area : 70080 meets Height: 0 .21e+002 cps MI : 1t.4 min 000 m a ca 400 t1 .40 m 200 c 70 . D 1 2 41 6 0 7 B 6 10 11 12 1B 14 16 10 17 Time . min Rerayeat 9yh B- PF08 (pC) 4OD.Wr00 .0 amu - sample 7D 045 from 04III308B.wilf , Arac D3701 commit HaiyM : 0_07*+OD3 cps RT : 11 .4 min 0000 tno anm c 2000 c D 11 .41 10 . 10 B 0 f0 17 12 13 - 14 16 ' 10 17 Time . min Exygen Research .: ;yv~;, : Page 39 of 110 000172 Interim RWrt .#23 - Analysis of Sedinmat SanTies . Exygen Study No.: P0001131 Figure 12. Chromatogram Representing a Sediment Sample Analyzed for PFOS (Exygen ID: C4172892, Data Set:042806B) , C07J2rP2-PFOS~~ArR:o1wJA&@APLIarr-nrpfaliNISNar M06B,wfA Area.- 5MeOratr IkpAt 4M+M2qr RT." li.Serlr 400 380 . 300 340 . 320 no . 280 260 240 Qca 220 -EIf 200 c m 180 1C0 140 120 100 11.40 00 40 29 0 13 14 16 10 17 Exygen Research Page 40 of 110 000173 Interim Report #23 - Analysis of Sediment Samples Exygeri Study No.; FM1131 APPENDIX A- Study Protocol PQ001131 (Exygen Study No. P0001131) with Analytical Methods and Protocol Amendments , 4 , f Exygen Research Page 41 of 110 0001"74 hsxerim RePart #23 - Analysis of Sedirn~.~nt Satnples - ~ , , . _ .: .'Exygen Study No.: PO001131 Esy;w Plosocol Nwrbw. PM 1131 STUDY PROTOCOL Study Tide: ~ Analysis of Perfluaroliutaneaulfonate (PFBS), Perfluerohexanesulfonate (PFSS), and Perfluorooctaneaxlfonate (PFOS) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LClM51MS for the 3M Decatur Monitoring Program Ezygen Protocol Number: P0041131 ParfomiltgLsbQratav : Exygen Research 305$ Reuafath Drive State, College, PA 16801 Phone : (814) 272-1039 r Sp,onm Iteot+esentative" Midasl A . Santwv Director of Regulatory Affairs 3M Building 0236-O1-B-10 St Paul, MN 55144 Phone: (651) 733-6374 Pagr ! af 65 Exygen Research Page 42 of 110 Df)01'75 Tnterim Report #23 -=Analysis of Sediiri6t Siuniplea p. 153 Exygen Study No:~N001131 Ezyten Protoeoi Nwnber: POOOI131 DMTRIBUTION : 1) laieimhs Kesari, Stndy Direetor, Waton Solutions 2) John M . Fiebe :ty, Prineipal Investigator, Exygen ltcaearch 3) hficllscl A . Seatoro, Spormfr lieprasentativa, 3M Company 4)Ecnul .Rsa,esrch Quality Aeawrnw,~o Wt 10- Exygen Research =tt,~ 3 Page 2 of 6J Page 43 of 114 0001'76 Interim Report #23 -Analysis of 5edimem Samples , Exygdn Study No . : P0001131 Exypq Protocol Number: P0001 !31 PROTOCOL APPROVAL Study 75tW Anal* ofPafluorobnttnesulBoMte (PF$$), Petflnomhexanoeutfonate (PFHS), ad Paftuoraoctanaulfonate (PFOS) in Water, Soil, Sedimant, Fish, Clam, Vegetation, Small Mammal Livers and Small Mammal Serum Using LCIMSIMS fart 111e 31vi Decatur Maritoring Program Exygca Pwtocol Nwnber : POW 131 . 115 D . Date ~/ - ?"- kY ' Datc Page 3 (d 65 Exygen Research Page 44 of 110 00017'7 p. 155 Interim Report #2-3 - Analysis of Sedirtrm Satiiples~ `- Exygen Study No . : P0001131 Hxyaca ProtDODl Ntua6er. P0001 131 TABLE OF CONTENTS TITLE PACE .. .. ... ., .. . .__. .. .. , ., .,., ._ ._ ::_'.._._ .~ . .. . .. .,. ...... .._' .._...,.. . .. . .. . .. ... .~., .. . ...... . .. . ..__ ... . .. .... ...., ., .. ..1 bIS'fRl9lf1'[ON---. . ._.. .. ..,. ... ... .. : ...._ .. ..:.... .. . ...... . ._ .. . ... ..~ .. . ... .. . . . . .., . . , .. ... . .. . .. . .. . . . . . . ... ... .... .. ..... . . . . ..2 PROTOCOL APPRDVAL_ .. ._,., .. . ...... .. ..._._. .., ..__. . . . . ... .. ._ .. . .____. . .. . . . . ... .. . ... .. . ... ... .... .. . ... . . . . ... . .. .... . . .... . . . . . ..3 TABLE OF CONTENIS . . ...... . .. .. . ._. ._ .._ . .. .,. . ..~., .,_ .. .... .. . ... :. .,_. . .., ., .,.. .. .,.. .. . .. . .. ._. . .. . . .._ . ...... .. . . .. ._ . . . . . . ..4 1HTRODUCTION..... .. . . . .., . . .._ ..._. ._., .., .. .. ...,. . .. . ., .., . . . ..... .. . ., .,.,., .,.. .. ...... .,.. .. . . .. . .. . ... ... . .. .... ... . . . .. . .. . . ..5 TEST MAT&RIALS .. . . . .,.. .- .-... . . .. ... . . ... .. . . .. ... .. . . . . .. .. .._ . . . .. ... . . . ._ .. . .. ... . .._ ..--- ..__ .._ .. ..---..----. . .. . . . ., .. . . . . .. . . . 5 48JBCfIVE ._ .... ...... . .. ... .. ..... . . .. ...W . . . ._ . .__ . ..,.._ .. .... .. . ..... ., . ._.. . .. ... .- .... .. ...... . ..... .. .... .. . ... .. . . .. ... . . . . ... .. ..... .,6 THSTiNGFACiLfTY ... .._ .. ..... . . . . ... .. . . ... .,.. ..... . .. .... .. ... .. . .._. . . .. . ... ... ._ ... _. ...--- ..__ .. . . .. . .. . . . . ... .. .... . . . 6 STUDY DIRSCPOR ..... . . . . .. ..--- . . . .... .. . ... . ._.... . ...,. ... . .._.. .. .. . .. . .._. ... ... ... ._ .. . .__. ... .. .. . . .. .. . . . . ..__ .. . . . . . . . . . . ... . . . .. . .. . .7 SPONSOR RSPRBSSM'ATIV6.... ., ._ ... ._..... . .. ... ...... . .. .... ... .. ....., ., ... .. . .... .... .. . ......_... . . .._ .. ... . . . ...,_ .. . .. . .7 PRINCIPAL INVES774ATOR.. . - ... . ....... ... . _ . . .. ... . . ... , . .__.. . .._... . . . -, .. ._ ._. . .. ..7 EXPERIMENTAL PROP0S813 START AND T8RININATIOTI DATES . ... .... . .. . .. . .. .... ... . . .. ... .. ... ... " .--". . .- .. 7 IDENTIFICATION A?iD IUStIPlCA9`ION OF THE TEST SYSIEM .. . . ..... . .. ..., .. .,. . ., . ._.. . . . . . . . .. . . , ... . ... 8 SAMPLE PROCUREMENT, RECEIPT AND RETENTION . .. ... ._ . ...... .. ...... . . .. .. .. . . . . . . . .. .. . . .. . ..... 8 SAMPLS mEN1TFfCA'f'iON .. . .. . . .... . .. . .. ... ...... .._ .. .. ....., . ..... . .. ...... . ..... . . .. ... ...... ... ...... . ..... . ._ . .. . . . ._.. . . ., ....9 ANALYTICAL PROCEDURE SUMMARY..... _...__.. .. ...... ... .". ...... . ...._ ...._ .... . ...... . . ..... . . .. ... 9 VERIP1CA1iON OP ANALYTICAL P1tOCEDURE . ..... . .. .. .___ .. ._ .___._ .. ... . .. ... . ... . .. ... . . ..._ .. . ._ .. . . ..... .9 METHOD FOR CONTROL OF BIAS .. ... ........ .._.. .. . .. ... ., . ..._,..._ .. . .. . . .._ ._ _ .. . . . .. ... . .. . . .... . ...... .. . ... __ . l l STATISTICAL . . .. .. . . .. . .. . .... . . I OL.P __.... .. ...__ .._._ . . ..._ . .__ ..__..-. . .: ...._ . ..._ ._ ... . . ..... .. .... . ... . .. . . .. .__ . .. . ._ . . I I RHPORT .., .,. .., .. ...... ..... . . .. . .. ..._. ... . ...., . ..... .. ...... . . ..._. . ..... .- ... , .. . .. . .. . .. .... . . ... r .... .. . ... .. . . ..... ..._ .. . . ..I1 SAFETY AND 0sAZ.Tx_... .. ._ .. . .. ., ...,_ . ....__ ..... . . . ...._ .. ... . .. .._. . .._. . .. ... . .. . .. . .. . .. ... . . .. ., . ..._. . .. . .. . .. . ... .._.. .. .- . . 12 AMENDMENTS TO PROTOCOL _. . ._ .. . ......_ ..... . . . ...... . ..... . .. ..... . .. ... ._. . ..._ .. .._ ... . .. ., . . ._ ... . .,_. . .._.. .. . ... .. . . ..13 DATA RECORD 1CHEPING .. . .. ... ., ... ., .. .. . .. .. .. . .. . ., ..._. . . ....- .. . .. :.. ......_ .__ .,_ .. . ... . ._ .. ... . . . . ._ . .. . . . . ... .. . .. . . ._ . . 13 QUAL1'1YASSURANCH ... .... .. ... .. .., ., ., .. ... . ...._ . .. . .. .: . ... .. ., .__ . ., ...,.___ .. . .._._-- .. . ... . .. . ., ..- . . ..,.. . .. .. . . . . ... . .. . .._. . ! d RETENTIUN OF DATA AND ARC}DIMiG .., .. ..... . . .. ..,.., . ,. . .... .. .. . .. . . . . .. . . . ... . . . . .. . .._ .. ... .__. . .. .... .. . ._ ... . .. ...- 14 APPENDIX 1, ANALYTICAL MEl7i017S . . .. ..._ ... .. . . ._.. ._ ., ..___. .,._. :,_. .: . ... . . . . .. . ..__ :._ .. ..--_ ..., .. . ... .. . . .. .. . . I S Page I ofdS Exygen Research Page 45 of 110 000178 ltlterir.iReport #23 -Analysis of SediraeM Samples Exygen Study No . : PtJ0a1131 Exyyea Proloco1 Nuner_ POOB 1131 INTRODUCTION Tlre puapoaa of this atMy i+ to parform analysis for perfluorobutenesulfonate (FFSS), parfluomhexaaosalfunNe (FMS) and perIIuoraoctanesulfonate (PFoS) in water, sail, acdiaenl, fist1, clams, vegetation, small nummal i9vas and anaU marranal serum man LGIMSIIuIS for the 3M Decatur Manitoring Progrlola. The si+by will be audited for compliance lwiW EPA TSCA Good Laboratory Practice StinkUrtis 49 CFR 792 by the Quality Aasuraace Unit of Exygen Research. TEST MATgRIAIS The teat materials are perttuarobutantvtllfanate (PFBS), pp:tlualnFlexanawlfaaabe (pFHB) NW petfhwlvootanesulfonate (FFOS) and are all supplied by 3M . FFHS Chemical Nam: PewfivorobutwesuffoWe Molccular Wdght : ?38 supplidd aa ft potbsein>3f Malt (C4FqSO3V) Lot Number 101 Pwity: 9b.'r9i Transitions Monitmed: 299 -+ 99 Shui:tlire: F F F F F~~ 503' F I F I F F PP'HS Ghaoicsl Tlarm: ParGuc.roliwcrnesuifoscate Moleculnr'rWrdW 438 enpplied as the potassium ealt (C6F'izS03x4) LruortiNturm9besrs:xSEqOC Transitions Moaitoae& 399 -+ 80 struclure: F F F F F F F--~+_~ kSC 3 0- FF FF I F F F Pate S of 65 Exygen Research Page 46 of 110 0001 79 'iin'terim Report #23 -Analysis of Sediment Sarllples' ExygenSti*No.: ~P00p1131 Ssnen Protocol Number: P0001131 r", PFOB Cbanoiica! I3snto : Perfllwrooctanaanlfooata Molecular Weight: 538 applied ae the potassium ralt (CsFl7SO3 K+) 1 .atlVumber : 27T- . ` ~ ,. ~. _ Pttiity: 86.9T~ ' . . . , Tril;aitions ilsmitored: d99`'i 4'9 F F n` - F F F -F. F I F S 3- -F F F OBJBCE'IVE The pnspoac of this study is to perform sulysis for perfluombutanesulfonato (PFBS), paQuorohexanasulfoaltk (PFHS) and Pertluorvactanesulfoaate (PFOS) in wafer, soil, sediment, fult, clams, vegetation, am" mammsl livers and small mmanmel senm for the 3M Dzcatw MoniEosing Program using the current versions ofthe Mowing Exygm analytical methods : VODD1780 : V4001781 : V0001782 : V0001783 : VOOD1784 : VD001785 : V0139178F: "Me" of Analysis fbr the, Determination of Perfluoroocianoic Acid (PFGL4) in Wata' by LCJM$/M5" . . "MNlod of Analysis for the AetCm>insKipn of Perftuaruoctanoic Acid (PFOA) in Soil by LGMSIMS" "MWhod of .Anafysie for the Detemainatioa of Perlluorooctanoic Acid,(PPOA) in Sediment by LCAdSIMS" "Mefbod of Analysis for the Determination of Pertltiorooctauoic Acid (PPOA) in Fish and Claw by LC/MS/MS" "Method of Analysis for the Detamination of Perfluorooctanoic Acid (PFOA) in Vegetation by LC1M5l1vIS" "Method of Analysis for the Deterniination of Perflnoroootenoic Acid (PpOA) in Small Mamenal Liver by LGMSIMS" "Method of Analysis for tlap DoWminstion of Portluoroootanoic Acid (PFOA) in Small ?Aammel SoAUn by LCIMSIMS" TESTiNG FACILITY Bxygen Researoh 3058 Research Drive State Cotlege, PA 16801 Phom: (814) 272-1039 ' Pate 6q161 Exygen Research Page 47 of 1 I O 000 1 80 Interim Report #23 - Analysis of Sedimept Samples. . _ , Exygen Study No.: POGO1131 Hxyrta Proeocol Dlunaba: P000] 13 1 STUDY IYUREC'M Jeisimba Keaai PA, DBE Weswn Solutions, Inc. 1400 weswr. Way Wed Cheater, PA 19380 Phonc:(610) 701-3761 Fax: (610)701-7401 j .ke=iweelonroh*ions .com SPONSOR R'gPRESENTATIVL 1Vlshaei A. Saw= 3M Conipsny Diroraor *fRcpkWry Affairs 3M Suilft023lr01-11-10 St . Paul, MN 53144 Mac (6Sl) 733-6374 I,- PRINCIPAL INVESTIGATOR John M . Flahety Faygca Rcnr+arch 3058 Revauch Drive State Collego, PA 16801 Photlo: (8 14) 272-1939 john .flaherty@elsy8r-com PROPOSED FXpER1MENTAL START AND TERMINATION DATES It is gropoeod that 11x malytiaal pawtivn of tiris etudy be conductad from October 01, 2(10d-t Der~raber 31, a0(15. The actual experirmtal stnn and samin.tion aarai rvill tie 3nclwdod iu eLe m~al r~port. . Page 7 oj6S Fxygen Research Page 48,of 11Q 00n1 .$l ' Ititerim Report #23 - Analysis of Sediment Sainples Exygen Study No.: M001131 Exygen Ptorosol NuGtber: FeOQ 1131 IDEN7TFICA'TION AND JUS7TFICATION OF THE TEST SYSTEM Tim following an the test ryatqoas for this stady: , " Wata (groandqater and surface uAter) soil . " SodimCat gish Clams Vagetatiovt " Small Mammal Ltvv Small Mammal San= The samples will be collected by Westett Solutions. The central samples will be purchased and propand by the testing *ility. Purchase and pmccWng details for the control samples will be included in the final report associated with this vtumdy~ 1 The test "am were ehoson to aeceas .the onvironmental impact of PFBS, PFHS and PgQ3 in the Decatur, AlAbt$na area. SAMPLE PAOCUREMSNT, RECEIPT AND RETENTION Water. soil, sediment, fmh, clam, vegetation, small otarnmal liver and small mammal serum samples will be received st BUM directly frm Weston Sohrtiotg . The detsils of sample pwmeamt for this study am outlined in the 3M work plan entitled "Phsae 2 Wodc Plan for Sampling Environmental Mada." The mmtbe[ and types of samples collected -will vary depending availability m the field. Tltc WW number of samples received and analyzed fnr each matrix will be documented in the final report associated with this Itudy. Water, soil, slid sediment samples will be used as received witLout farthcr processing at Exygea. These samples will be stored refdgeruted at 2C-8C. Fir14 c1sm.. veSetqtion ad small mammal liver samples will be processed aceardift to ibe uppropriate analytical method (see Appendix I}. These srrnplos will bo btond froapa at S =10'C. Smdt mammal wbolc Wed samples will be cintrifagad III the field tat the time of collection end the serum 6raction will be used far tlte sttdy. Small tnamumd senan will be storod fro= at S-IUrC. The receipt and processing of the samples will be documented in the final repoit and raw data associated with the study. Page 8 q165 Exygen Research Page 49 of 110 OUQ182 Interim Report #23- -- Analysis ofSedimelt-SampIes - Exygen Study No. : PO001131 Exyjea Premool Nsvnber: P0001131 SAMP#.E yDP1VTWK:AT-IflN Prior to atawlpris, each sumple WiZl be assigned n laboratory sample reference numbtr. The referer:ce aumber will bie unique and will distinguish eerh laboratory ample that is proooesed tbroaghout the analytical procedure. Ctlsoosstogr8phie det8 will be identified by the laboratory sample reference number. Sample . stoup e.orx'btMns and locations will be documanted throughout the stndy. ANALYTICAL ]PROCEDURE SU1IIMARY Rcfmences~ VOd0178o: Vp001781 : V0001782: V40O1783 : VO00i784 : ' ;VODI)178i : VObo1786: 'McdW of Aaslyris Sor the Determination of ParIluarooctanoic Acid (PPOA) in Water by LCUS/hIS" "Method of Analysis for the Determination of Pertluorooctamroic Acid (PFt}A) in Soil by LCIMSIMS" "Metthod of Anslyeis for the Desertninatiout of Per1]uorooctsnoic Acid (PFpA) in Seditnent by LCJMSIMS" "Methad of Malyru for tho Doterrnination of Perflnorooctanoic Acid (PAOA) in Fish and Clams by LCIMSIMS" 'Method of Aaalysis or the Dctemdaetion of Perfluorooatanoic Acid (PFOA) in Vegetation by LM"S" " 'Method af Analysis for the Determinotio.ti of Perfluorooctsnoic Acid (PPpA) in Small Mammal Liver by LCIMSIMS"" "Method of Analysis for the Iktermination of Perfluorooctanoic Acid (PFC1A) in SmaU Marnawl .Saruni by LCMSIMS" The above mothodi uae analytical conditions capehlo of separating the isomos of PFF3S, PFHS anti PFQS. The final report will include the isomers summed into total PFBS, total PFHS, =d total PFOS found. YERFLCATION OF XPfAYTiCAL .PBDlLEDI7M A laborstory asntrog stlmple will be used fir the prVaration of fortified control smepleR. 'f=oe teat subatrqco will be made into solutions as per the metlfod, and added to ft matrioes via s mieropipeue. For water smpling,-Exygon will ruPPly one bottle, per sample collecuml . The bottloa will be 500 mL precleroed SeilSpee Premier wide mouth HDPE bottles. These bottles have beeod rostinely used for fluoroclemical sample Psgr 9 of 6S Exygen Research Page 54 of I 10 000183 Interim Report #Z3 -- Analysis of Sediment Sarrtples Exygen Study No. :- PO001131 Ex,Sen Proncol N: umber BOOOt 131 r coUection at the testing facility and havebo~ altiown to 5e free of PFHS, PFHS and PPQS. Sansplce will be added to= contain" to a voltunotric fill line at 200 mL . A lkid d+pFisate, a low field spike and a high field spike of each . aanoe -will be ieotlected 1'he low tcod high, field spike bottles will contain PFBS, PFHS and PFflS as weIaa perfhuoivocbnoic acid (PFOA) and 1 .Z-13C perfluoroOCWwio ;acid (it : PFOA), . ~ PFOA and "C PFOA we included m the Aolulicne used to spikethe'aamples . Vie reaults for PFOA and t3C PFOA will not be reported in this study . BacySen will supply one field blank (oontral wator) and two field blank spikes (control water fortified with PFBS, PFHS-amd PFUS at~a low and itigh level) for'every twenty samples collected. At the teating faeility, each water lattrple (excluding field duplicates and field spikes) will be eatractad in duplicate and will also be foriified at a bow and higb concentration with PFBS, PFHS and PFOS and processed through the described procedure to determine method accuracy and to cbcck for biaa. For aotl, sediment, clama, and vegetation, Bxygen will supply one 500 TnL precleaned Sc"rl5pec Premier wide mouth HDPE bottle per sainple collected or a zip-seal bag All containaralbaSs used for sample oolloction will be shipped to the sample location. Samples will bc added to each container of bag io ft field . At the testing facillty, web :ample will be extracted in duplicate and will also be fottifled at a known concentration with PFBS, PFHS and PFpS at both a low and high level and poocaed thtotFgh Ow described procodum to detemine method socnraoy and to check for bias. For amall'~maaqnmal liver, Exygen will supply a 50 mL polypropylene cetitriAtSe tpbe. For small nttnunal serum, Exygen will supply a oolleetion kit for each satnple containing scram separator tubes (red top), vacutainers, oeedle holders and aeodles, transfer pipcttae, and polyptWylene tubes . At the testing facility, each liver and serruin Iunple will be vittBCted in duplicate and will also be fortified st a known coacentration with PFHS, PFF15 and PF05 at both a low and higk level and processed through the dGecdbod procedure to determine method accuracy and 6D check for- bia& Low and hi ikin levels for each matrix an defined below; matrix Water Soil Sediment Low kla 500 4 n 4 Laval HI h Ikin Level 5400 n L ;p Awl l 40 n NO C110110e - - Ve etation Small Memtnal Javer jo nff/Ji 14' 14' ]b a 100 nova 100 n 100 n 100 n ~ Small MUntnat Serum 10 100 ng/ mL - . POP 10 OJ'dS Exygen Research Page 51 of 110 000184 Itnte:im Repqrt #23 --Analysis of 5editrwa: Sum1S1c-s , Exygen. Study No . : P0001131 Exyw Pmmunot Nweber ; ?MI 131 ltecavoriea are aetieipated to, be batsvept 70'fo and 13(ft of the fortified leti^ds; hmYOVpt, tbe m7tect,procis}oe rnd accuracy -will be dotemlined by the enat*a of the quality uontrol ouqplet descn'boc! above. A statement of accuracy will be included in the final raport. M~T~4;a II~C1F C~riT~'~L t~F ~1~ Control oftin will be addressed by taking rapresmtative sub-sarnples from it hpaxigenoaus tnixture of each matrix from untreated control samples, and by st(AlyLilly, At )feast Me ldlCli of fottl$e8tions. S1'A77SMAL M1~ETlPlOj5B Stntirtica will be limited to those specified in the mbject methods and to the cakvlation of average recoveinim as aqtplicable. GLP STATFWNT All aspects of ihia study shalh be Oerformed and rr.ported in eomp&anee with EPA TSCA Good Laboratory Practice Standsrda 40 CFR 792 . The final tcport or deft package (supplied to the Spomeorj altall contain a statement that the study was conducted i eomplienoe with cuereest and applicable GLP sutldatds and will outline any d.viations :n the study from those standards. This slatenunt will be signed by the Study Director and Sponsor Repreiplt8tlve. . - 1tEfipRT A final report will be prepared by the principal investigator or their designee at the conolution of the study. The =port will iucladG, but vfi11 riot be limikx! to, the Collowing: e The " w= and addrm of do Str-,dy Diractor, Sponsor Representative, and of am testing famlity, s A st&UsnaYt of GT.P eotnpHanee (any related doc=cnWon. such as chain-of-custody records. must be in the study records) . Page ! 1 cjQJ Exygen Research Page 52 of 110 000185 Ititerim Report #23 - Analysis of Sedimont Sarnples Exygen Study No.: P0001131 ExyQea Yrotocd Nwaher, p0pp1131 s The signed and dded ststentent by the Exygen Research Quality Assurance Unk iegarding datL's of study ffispections and dates findings waft reported to the S'tudy DiroOtor sdd'Mmagement . . A deaeriptioa of the exact saalytisal conditions employed in the study. If the object method was followed axactty, it is necersaly to include only a copy of the sualytical mettiod" Any modficstiow to thi method will be incorporated into the report. If the inethod is photo-reduced, the project number and page number must be included on each pap. . " DWripeionof the mobilmoulation and andoperating conditions. All txxoits from ali aft analyzed. Control and fortified samplea will be identified mid the data table +ta'iD Include wrriple umber and fortification level. a Rbpresetrtative cltmtnatogratas for each atralytc i each matrix, including duonwtogams of a standard and a control wimple, and a chrornatogram at a fottification level . The location of the analyee peaks will be clearly identified in all chroatatopame. ^ a A]1 circumstances ttnt may have afttod the quality or integrity of The data will be documented in Ow roport. a' Locations where raw data vA the final report aia to he archived. a Additions or corrections to the 6nmi repoit s>tall be in the form of an amendment signed by the Study Director. The amendment rhall clearly identify that put of tlre report that is being altered and the reasons for the alttrrations. 7rie sntendtnent will be signed and dated by the Study Director and the Sponsor Rapresentative. . All applicable requirements for reporting of study results as per 40 CFR 792.183. SAFETY AND HEALTH a Laboratory penomnae] will pncticagood saaitadoaand heahh habits. . Bvpy reasonable pneesation shall be taken 'to prevent inadvenent exposure of pummel_ aud .the .awitoameat to the teat or referetce suboteme{s). ' 00*1 Page 12 of 65 Exygen Research Page 53 of 110 000186 Interim Rapprt #23 -Analysis of Sediment Samples ; ; Exygen Study No. ; P0001131 Hxygra PrpWel IHianber Mot13) AME"MMM~'! TO P'R{)WC(?Is' All eignlgcw dtalsga to the sstalytJCal protocol outlined here will be expressed in writiug, signed and dated by the Study Director and Sponsor Representative. Amendments usually will bc issued prior to initiation of study plan elsaage. However, wheat a cbanga is requited without sufficient time for ft issue of a written atnatdment, that change nay be cffocwd verbally with supporting documentation .signed ttgd . dated by, the Study Director and followed with a written . itpa~a~ .MA soon, si,pQeeibie. In this case, the effective date of thg w~itti=li . ~ndment will be the;,~te of the documented change- Copies of the sri~ied ~ents will be s~ipended to all distributed study plan copies . The original aaatdment will be maintained with the origiaal aptdy plsn: Any deviations frora.the study pin or from the analytical method as provided will be documcnled and reported promptly to the Sponsor Representative. DATA RECORD EXIMPING Rccorda to be, maintained include the fallowinS (is appropriate): . Sample tracbngslkeq(s) . " Ssntple receipt seooebt.,. Nome history, and chains of custody . History and preparstion oft<tssldards (dock fatifice_tion, calibration) . Description of my modifications to the method R . .IttArun+ont run sheets, bemh-atreets or logs " Analytical data tables " All chromabog<gphic and iostrumentat conditione . Sample wdtracfion and analysis dew . A complete listing of gtssiy personal, signnpu'e: and initials " Chropoaogisal presentation of ail study coaeppondeace " Any other documentation necsxwy far the reconstruction of the study C11r0lilf1tll$rstns- All o>aromRtosrams will contain the following : , Sample, identification, iajection date, arrow or other indication of the area of iaterest, and irdectioa number corresponding to the run. . Additionally, fortificatioas will include the amount of analyto addad and the sample rwmber of the sample that was fortiSed. s Analydicsl standard chromaoogrini will additionally include the coac=trati.on (e .g., hglmL} pov es ofas Exygen Research Page 54 of 110 .., Interim Report #23 -Analysis of Sediment 5amliles ' p. 165 Exygen StudjIwTo :: P00(}1 131 en e RESEARCH 3a58 Researach Drive - Phone: 814-272-1a39 State College, PA )6801 Fax: 814 "231-1580 DEVIATION FORM X Project Specific Deviation Facil4*0tvistion P s1of2 Dote, of Occurrence: W206 Exygen Project ~ : P:OQP;13f Deviation # : 5 Client Projeet ~ : NA ' Reference # : OB-076 ulst Mist Tno: (Mch+de Vik ior methais and SOPs) GMP GLP X _ Protocoi , , Method . , SOP , Other V#: NA None Notebook refergnce: NA samola Dosah~t~: . , . . Lagin# : : .. ' L00081 B9 Container #.' NA Lot# : NA suffmMy of l7rrristbn: The three sadtrnerd samples In,L8181 (CD17289~-00172s84),wene ~yoxlraded using ~e sediment tnethod .V0*1T$2: PoarrecoiferiGs were obtained for PFOS . A end '~C PFOA . Because cf thi, the study epodsof requested'the use of an apernative extraction for these oampounds, ~ tottorvs: Direct Injection Method : Fieforo the sampies were weJghed for to extraction, they were mlxed thoroughly by efgorouslyshatiin9lhe ooatelrbr. A aneVfem portion of sediment was weighed into a 15-mdhlder centrifuge tube for the extraction . Ten mfpillters Df 196 acetic .acid in methanol was added Weach s. ample The samples were then shaken by hand, vortexed . and sarkaled for thirty minutes . The samples Were then centrifuged for -10 minutes"at-300Q ipm . Each sample was analyzed by LGMSJMS slectrospray. Using trys,rnethod acceptahla data was obtained .ioifPFOS, twt. .the recoveries for PFOA and "G PFAA were stitl poor . . Another ellema1vs iribthord was . .; then usW for PFOA and ft PFOA, as blows: Alternative SPE M: ethod The samples that were prep9tei! In ,08L 6eetic acid for the direct injection method were used for this extraction . fivs7MIIINtn of each sample, was allquated into a 50-rorL polyprapytene centrifuge tube and the voNune was tafusn to 40 mL with water. The samples were then centrifuged for -10 rnirautea at -3000 rpm . The supernatant was then loaded onto a C,s SPE cartridge conditioned with 10 m1 of methanol and 5 mt of water. The eluate was discarded . Approximately f'nre milliliters of rnethariot was added to tlie carttridge . Fivb milliliters of Wets was collected into a graduated 15 mL polypropylene cen4rihtpe tUtm Each own* was one" by LGAASIMS electrospray- Cause: ~ Preparation - Analysis - instnxnent ~, Client Request X Other 1Cmti More usable date woo obtained . 00 4' 1 LIBRARY 10: Vaoo1640-d l;xygen Kesearch 1 ADMINISTRATIVE FORM Page 1t)9 of 11 U 000188 Interim Report #23 - Analysis of Sediment Samples CKE11 EH31 236 18 651 733 1958 DrOi-wI 4t :Mor Fr"4ilin0 SGLITJOlt Exygen Study No. : P0001131 05/01 ' 06 13 :46 N0 .106 03l03 + M14 F.01lI09! F-9i1 Exygen Research Page 110 of 110 000V1- 89, Interim Report #23 - Analysis of Sediment Samples p. 167 Rxygen Study No.:-P.0001 131 3osara~e~rat Dr~. P ,otte: ai~-zn-i o~9 s~u ton~, Pa 168M Fax: 31+231-tsao RESEARCH PROT't)Cr~L 7tA8EAiDMEN An~endrnent Nuwber:,~ . ~0l~1YS,D~: ~19I05 Exygen 3Wdy Number; POQQ113t ` CUrn! Study NumberIJMI , Psps 1 of 1 t~C~f'1 R7N OF AMENDED S~N 1) Malyrcal PrOOedtu's Stmrttary Vd001780:9ecilon 9.1 2) YsriHa tlon d Artaydcal wrooadtro AMENDED 19 -- f) Add b Sec~on 9. i: 3scdon 9.1 .8, IUterr m e rwipltfs d standards may be used 60 preperta akarrsb# concentrations dsiodk solutions ae neosssaty. Altantate levels d faAwc atitxti solutions may also be propsrad. 2) Low and high sprtktpWyells dfm nn&W s foreach matdxmaybe altered dependIng an sample :aze eraailable foreotbadion aw War b caw snslyte conowdrafta s psdsd i the aemples. i) Higher oonanlraUo n of siardards need b be propavc! In orderb spike the sample 6attYR dhiplbr leweh . 2) Tn.ssrrtpw size avaraers !or small trtarrwtttN NW and germ VMS alnl" UM eo p+clod. svUft b ft praiieWaftd bwrs M ft prdoaoi puls Me .prted concW*WI rt lower 1b1rt ft detaag n WK Also,ft andyis Istnels In the Found water sarnple so ~cGed bWM fN exceed to Pre4slarmined spactnD levels lisMh Me prdDO01. WW to Wells h be sarrlplla great/ exceed Me spiki v levels, en acstuabe rscovsry VOW cannot be caloulried far thr QC sample, HpFnr tplcfng levels h to botthsw1Kooaerthe dnalybscw=ntnidona eowscted in tlta waters: . ample TM LOC Is i00 ngrg tora0.1 p earnple d:rnel nwrrxtwl lher and is 1000 nphtit tor s 0.81 ml. sample ds n d marwnal swum M yrwr tereis dsoft iarto watersampleswIB ensure 1f+ai mom OC ncovety date can be uso d. . f . bwir11p~1or 81Dn~4+~ sp o ~nnnt bn~ r -- a,aun pt MW" Ir V ab~' 6V 1109 Ode QJ DAM 6) qrpen OAU R Mow ! a5 Ode I lr LJ6nARY ID;VV0001 2266+ ADUMSTRAnYE FORM Exygen Research Page 107 of I 10 4001`;6 hatexim RWrt #23 -Analysis of Sediment SanVles , Exygen Study No .: A4041131 309 Rese&rO MW StsLe Coll~gt, .PI116801 ARCFE~ Phorie~ 814-Z72"1034 Fat%: 814-231 "1500 . Amendment Number. Effect" Data: Ex'lrgen Study Number PROTOCOL AMENDMENT ' -2 ~ P0001131 - (3ieni St+uty Muh~ber. . ~, .. ,. . . . D~~1'ION (3F AMENOND ~~!I 1y Rapart, pmp@ 1t d45 2) TOO Maledals. pW 8 of 85: PFOS tr"Uon mon8oaed 490a 9-D. Pep 1 of 1 None 1) Irrbea0~iFOm Ornl repOrl, In11M1tl~~iat~ed`' - Zf PFOS aandNon naMlored mapr Ow be 409 a ao. . 1d)ieD'unewtmocteWn.xde.tem6iwnaa**F.woQrgKoad~abm,1amk%WhiOmIbAr%n4krrepOoWrb 4Jo iesuaa m aIaarft z) The API 4000 LciMSIMS sysens ~sa hs 499 ~ 90 PFas eWWRor+wNh gnwdw own" tw to 409 -* 0e transhlom ~pA~r flre snmv 1) The COl11t1w11 be aW b lstxha ad Ihi~alAwr dab mw' qpio*. 2) The ,86 a 80, ~ldan an be oeWdid wif1, w*mlir :enal~ly; Omvars, 9mg batlar dramdo0raphy. 9~uar ~ DOW is ~Bown o p . /-N. M~-OS ' ~ ~a at' . . . . Exygow f2ALd Rsdbw Idlld LI6RAR1' ADMWiSTRAWYE FORM Exygen Research Page 108 of 110 000191 Interim Report #23 -- Analysis of Sediment SaAfples p. 169 ~ Exygen StudyNo.. P0001131 Eayseo Pmtncol Number: P0001 t91 13.o eu .Wse .adrfib : " ' 17 .1' ' !31' .. }33 . .. , .~. ~ - .Cfh`eeOWOa"M ~~of MOM ftM .s~ib ~ rFMOA mmn we~kn~h +xx~wb ir t]i9 xr~a) ~Yea lax.afaew. ~aaia.. hidha! blria a~le ~ee ca~aria rJOA u Lrsb ~axaer IAr tls LOQ . IF a Nuk oEeYies"lFOA s 11w11 p~rYr !m 10 "L. Urn a new b4mk aarqkaewtDbW~uit~iwiAirwGw nt rw w~rsvxcrod, Rabwtlr of toiYivl ay0ow ad wa6ix V!w oM be batrrwe 70_ .1SOx of Yuir' Yr&ww w1x& If a wWol o.A& nUlla lM axliic: w ~f r~{s fbonU be n~ s~bbbaaadddxxAx&dd..s Aiq awbix~~!suts6de 70- 130X dWW lrnYonnd by ft no" 10 oaa4ibx i( ro "axu+csion 's U .! ' 17.3 Iss rAiTedibrall" alrird head ls Iw a wok" axsgw h' wxt tw Htaw am 7w6 pqy be axbiaad 4w we eakeLUan D! Me awliirtinn eir.e Nomr, IYe tedl auadKef willeattmxmdw*1hM could ba ei8ndad mY1faN aord 70li Yf14a bid wcbatClRaadxrdx iAlaaad" 7abiW .m00WpWxdzxaameb~aplauixnsta(wla)af.ar. anxli"Yndsolwl eaw.vypaFObweeMNh*.-LsW,A*dboe IFpwp1111e xlW pur be am is xdjwe b1ftwIplt aFerxfoe, xod The Yrdud~aranievw aw oFan~lw q~ fa ~aaalne0, Ra~,~os tcs b.r+wr W."i wd .w w~w aa mitt ..ps olwi t+lf; .ilpia an w~btial rs H ia~don uo. a~iu sxsndsdis limii .i~ o+~!YP~ Nn I>twltw wl mwt w wwiys.d. ~aR CGIadrnoy l " l 1!r tLa mUori~ ~qrsflxa a aJradwa ttw nard ofR'OA bwd fia nrmL. hrri an pa* on) w&4 9u xlrdr,* xtie"t Iww rxgaxaon Frxmatwxl ' ' pmawd by Iw Min Lieu xal+rw psoFxw: TFOA 5ord (npIaLI - Llralc rxa . nree(aet x DF x aiiqimA fecmr s DF +pxpp by *hick an SW vaie rax dlmad !f>retixnry. Allqpol {klw- 20 , ia.7 Fer~wIIr bid" wmbbwre waasr Of FFOA prim m exbfetloe, nfs Iw A1Yad"faqyleb,atcxlwiYx iw prxwxraoavsy. 4woraqr (JO . lbnl. .ht~lfwadfP.+mla - .ra~.lb,naia~ooeAl{nroiL)1 , lao asdfdxdlad("~ImLt ry,aefr PSsse 64 ofE3 Exygen Research Page l 05K of 110 OOOi92 Lntenim Report #23-7 Analysis of Sedimei4 S=W-CS rxygen Study ND.: P0001131 TixySee Pro*" Nnn6w POOO1171 et~e~e ~IIIIIt~ Mood GrIkap-wo " . MYRALAtlt'PA00 bierme! SwmM 3.C+MalblS M~iod N~Bp V000171i I .ia '.~1M b/owom p"w w o .-pt tw ewmwt af PROA faw4 n +yymL w . ' . AOA St" (A*) . -. , . . MA "_ -4b YOM wi Exygen Research Pop Iv Pqge 63 V61Y Page 106 of 110 000193 p. 171 Interim Report #23 - Analysis of Sedifte~tSsaripleg ~ 3 Exygen StuEdy~No' : P+~OOI 131 Ecygae Ptmosol N: umber PUDDI 131 . _ ~4Yl1! .lt~rrl. r~ . 14wri0 oC Ir ' . MOWN. .rrvmole A..,AL maws a i6r~"IIrDai I~ ed8w!lilsr.oosueoie Acid (1'PON in Sma11 Mumid BasuAbyLCA4yMB !A ~qiard tnpewion 9.1 Slaodwd SmetIRo~titir~m SaLriao 9.E .1 Pesprg ttbsk.asYlioa at-100 pylmL afPFOA hy weighi~ f0 wa 0/ Ilaalylkal Audwd (aottaaaA fotlwiEy)rd dilme io 100 mL riJ ~IrLed ~ a 123aa1. LGPl:lalw. 9.1.9 A !A ~ai.lwplkwion nlaiar9CPPOA Is prepwed by bringinY ~ a1. of On 100 pjhaL salatiaa Ie a And volane of 1 p0 whb eudwwvi ka 123t1,LDPH lallh. E.9 A 0.l okoInL 1hl6riiaa lonioofPlOA ir i~npred by bapsIY tlLofthr i .0 pBAotLaolufka 1a a lfoa! roLnoe or i00 wnh manaml ia a 125 sL LDM Wqla 9.f-~ ZLt alselt rei ~li~aslai~w an lobe atopd ie i ro5ipenlor u aprox+e~abt tI'C ~i ws ilaWa fa a a~a~a~ pwtipd oT6 na~w:c f~ >IYedre[p~u.~a. 9.7 BpaadardC11llratia3alpmor 92,1 tA~ ulihnMn sdWa am prlprad In matlnrai via Afton orAM 061 prd. ]brdlerioa aoiotloa . 92 .2 IM f011wfed is a qVlal laamplb: aidSpanl earalatralian may be plepmia~ wdad. V1- 11110116- 0"-- ---- ----- - -- ------FvW 10- .aE.Krrm . velar Mod lo cw~ae~wele d9a11oabldedJ O.w) (.N)a SnyrnL,Z in ~.e lo! s.a !9c . . :.e 10o :.0 lo! . is 1].o0 )on Joe 1 .0 o.s zq lo 100 0s 1.0 10 100 6.1 9.2.3 S1w drrl+waYOa bpladb in 125-n1. laPB armw " moulh budtlw p 2'C 1o 4?C. u! Ioit woIIlYi. 9.2.0 Aldmali iolona ~d aaaoaabYlan< ofatrdaod" mq La prspa,W ,la rim" la0 balcb9aellt 169 ]0 .2, Baai hneAwfqlw abaeW (pyliulW 20 or lea) amre iaaMde " km w nolsarY oonYiW am ewo uopatad oonsoll !tii]bd al known OOa01a1V111110aa{!ID a0adO11p" 1a "AI4' VIOCOdUral noorty for to baecA iGql/t'Imrua * Wl q0 Lrowwrp dlPliralu and apha will be wesif n1 in Ow qualiy a~ ple for " projop. F.re i af! r+ Pop 62 of 03 lnteriTri Report #23 -Analysis of Sediment _Samples . p. 172 Exyg.en Study No.: .PiM}O 1131 T1% 8xySea Prom001 Number P0001131 by/uA11111ib 7 - (M1o/ NWbWYM17a6 WOMAN-91- SOD vIr . T ; Mm_'Awd (r 1tr,18wwb y LCNarMs ) is sm .u 11.0 31mpk 8xaodom . . tt.l . blD..xol .earn .p1.1.1.aealnLVelypmpyleDeoenoilly .lrba(ronify u arakd none W an/ mia wdQ. NOIY to M, '- vohlloao or mum 112 A~df~~pn,r1r~ot~2QICGptybtly . 11 .3 vow 11e utaaa f1.1 Tpprft ?. 7s1 i. 0 pn w~qk rrb* . fylerbb pipqa iap a Is IDL , a~plrbb araiyr ~ ll3QddSDd .otaor6eibiaardahalrlhr-40mi*ABmarria"rcaoedwRer. . R1 .6. CSj,'! Wu6wa14110Dqslbr-3aritawlw . . ! 1 .7 . DOW GY alpmtmt two a SO mL "apaYllt arlriMp tube mad add 75 a.d w,qn. !(A C9blBka .lw Caw 0'E trlr!dlh (1 0, i aL) Y!?wW 10 mL metmo1 ToYpwad9yStILOlH?LC+Iwr(-2d1ap71rc) . ibaotktoolcerlnmdy I1 4 LOW Ararepa rl opldb(wpd CH 6l8 rtCidae . DiaatH ekac! 1A0 Ilqrlt afdl -4 rL a[ amhaeDE Colkta Z mL of aim irD a gaduuaf lA n11,pWlayylwa awmifiye oft (gad wha - 21aLd. . 1 : . .1' /mrlyasnmpoaYSeleelrapr13 LCIMEIbiS. 12P A'ireeW0brj4vltg Al Slyaet Na fimme roux Dfnli IArdrd, wqlpk and IbltilNd mwiph wan 'be LCAiM1! qon. A p1!bnqlp0 qapda/ Rx1A ynDde aad Polbw atl 12.2 dllGA orsumpaomDa m a 1aw1 Aveor mm cDnomvatios kvds ~ pcar tia'~ sasLda! is an wlytial a ". 121? AR acKt sst otulibw5w ta!ndards mut be kehdd at In byinlanY wd a t'r_ ee~-!caawpk ar. ftSdWa aanl bt ialapaned bclwaea e .e.y S~ io aLv#h, AM no alfwaWrR, r wNo am o( DaGbtitiDD slardaeda my be a 'C &M bollwift of a W tOIIoYfad by Di11brafiD " aaldhilllC inlu+laut+rxy i10 wylu bo aocant lbr n ~eoand ~u o! wnC~rdsl In wdlar cwl e~l6ndm st~mda+e m~n~ b the OM and IM lqienioD ia a ~tqri; ca. l2.4 TJu Saw rhodmd oonu 8r quadwion . Lioear aluidvd curvm are BaaaelaLllrtby a1k1a by liuwr eep- ruC Ira Weybbnj or Auk area ra~w WiYrdop "ndw oaroppbrtioD wios MwLynx 13 (a cqnivaenV MR ., .n nM~a f7.3 S~k rrgmcr Iborld no MAW wnNed rqponrw. My uayles IMI wood nreara..rprra Ir .aabc mnaQ almd .d nrllryraed . rW s 0n 1.0pop 63 OJ-65 Exygen Research Page 104 of 110 000IL95 p. 173 Interim Report #23 - Analysis of Sediment Samples ' Fxygen Stady No. : P0001131 &xnenProoocol Nunober. Pooo713) M7MMWAO" . . . It4q"MrnbwvOD0Ui0 IWt)w~+~ r!~!p Dr4lrirpro slkt~ Mid Mmmd Ssr Dy LCIN>hu9 w)iMSm11N )A Sttpa , TSri nlwhod i~ ro 1r ~yd Rr Uu irohiw w11 l~a~la~ of Irtluvoxuporc UM b!' ~ Freletnrop Liquid CMsuo~pop Y eauAld u a trdrm blue SpeoaoeMRie D~teoar(LC+M39~fS) in aowU mnMm0l ~pwll. 2 .0 Bwly 11 Alhrayi olam oh a6wefslY plfltitieet 21 CaowB ta 4pptoytiue 3I9I73 betbes lradlloi aY ehanicu ICr propx aklr 3D Eogh A~qauwur Atlas I pL oftwt urplp Rretpmsm 131.12 Nm up* rivalubK.ip ewbd !6r manlp ampla. Hovpvw. Rnwn prlpp w~l " I~II q dbwk 4 f~q1~111Yt1~+ 01 ro011711o1paaWn belwe we. 33 3~wpls ao1lWallan Foordlwa Will be Itwr36d ill TLe Wwwpw" pun for ikiq P-1- 4A RwpmYaed11*nk* s.i Waht-lpLCraOr ., . 4.2 ifMYrA-HrLCpoh 4.3 Aandnils-fRLCVwM 4.4 AMlqNIM Mues -A.G$ Rwr[ psds 4d Fw0mvUbooiaAr14-ApprAl*4l S.0 4YSromrtrd1**erMft 5.1 A ho Padaaapoos h"i qnmnoEryY uPabb of Dwa4iItt wp lo 2 w{iwlU pqdppedwib p wiWs vehmu vioeler tIpe61p e[ iqj" 5.200 pL carAGdm auodwl Mm Sywemaelw (LCIMSANa 5.2 AdNafe salMpt nw /Ya 16e Iuk bWVWap *n/ qwlrtiHdoe. S.) AodyYed lulrla ap"afwrfq to U0001 S. Sd !Q mLdlpwilrprlVWlwrl ouril4ye wlbp. f.5 15 m1.6iqewYlrpelypopYlweooasi4ye mbr. !.i DIPorLipsipn*w(l0.100aL.1OP200uL). 1.7 123-Ot.1D8 rlnw.molull boulw, S.i 5.9 ZaiqmLod"krvHOPL"mC.v.i.wl k!L s_lo Aoo1powr .tloaloooNC.x3d lalooply,wurmlvm.brnp.. S.1 l S~tiko 6&p 14i Vu 6 w (1E) ICIi WE taWdseq. 5.12 fTErinluetMIrllM. S.13 Ymaxa. hrt.r Pap 6o 0/61 Exygen Research Page 141 of 114 000196 lrii+erim Report #Z3 ---_Analysis of Sedirx=t Samples p. 174 Exygen Study No.: P0001131 Fatygen Protocol Nmbw PM 1131 ^ sri,t .tw~ 1w.+1w.r~rrowl~w . . AiY:, :.Y'nC~u. syCriloD tN14e+letNnllain~ro.Dwawl6~do.NI& jaw[t amrt rs LcrM&Us t~ wswwi s.t4 . . s.ts ` ~ cawi~ll,~ ~or~ 1 s ro>,. a"brorra.. wa. r 3op t~t. a:o' , cbm.,vs6,>ft s1+wt . ; . ~3 ~ .. lllnlrital Csbm FlooObrC 11Y OuyMrr 8efadfCL 7-1 mm A 50 0mt. So ;,Q,Ok f270S0l2130) ' - 6X , 16"Footow 7CC 63 ; .6ipL'Ll!hrw(A) : 2niiIArn%rIYumAwWeiaYar 6A -1A41ptYarsQ} : lAellrwl , 6.3 i: . G~dr ihqt- IWAIEW %A 0 .0 65 1.0 63 _ 1 $0 23 *P 23 - ' 2i! 65 Flow RW HIA MAW 75 0.9 33 0.3 73 0.3 73 0.3 33 0.9 5,6 bjCaliw YWrIR FS p!. (wbC f~n6rd le r aorCh r SD 1tL1 . 6.7 '4~ lWcArr-rdendave4rdeNibntionaun . 5.11 AuYTaYr r Z3 yoirwR Tkoibvr oaotdlqrnaw oekdrd u a qlidv r+d mCy bseltwl~d ro oAa w aptisadvslla I~F.S'-~>siee. 7.0 MWA ay,wt. 7.1 MoOat lleopom aP b1aptiYe 111Rh1 Cwdq mmdwria0413 -r 360 mh for "W. roe C6ova ooo6aiCwt w inftded r s 6aWe ard MW Eo Chrrpd in owda to Opmew " Una ".ft. i.1 f[wtlnltrtdB"tr Rl 16ohBelki+s ''&1 .1 Z~rY Ytaclli~eC r~ hl 7wilUf to pIp1YW by eddin{ MI SC & of mrrimt arWs b ]00ntLKrwtr- .~Y~OIirYa~aimp'1G1MOrC0 . Pap 3 .r7 Page 81 0/ 65 Bxygen Research Page 102 of 110 00019'7 Interim Report #23 - Analysis of Sediment Saanplt~s Exygen Study No: : POOO1131 Bs"ep Pmtoco) Ntmber: POOt1713i meow wmY.r vM5 .-. . At~__LY fICAL HMO= . - n ' " ~ - ~~e iwedLrraaefa~ole Aeld {FIroA) in SmNI htw"Lirclr LCTl311 "S 14.2 Fa au*Y~1 fo~~d x1m Iraowo r~wtq c(plpA prtor m exnadm. we ~KM~ b ~ ILsy1[e0M Mswey. ~r+er ~!i) . .Lww rrh~r reisatww- ~wiratoraaao~twita~nwl awuP..aamtopa" loo 143 =MYw~~ ~q~Wea 1~ p~ypc " s ~moyoi afPFOA faa~a w nymL w ., . ~ l1" SD .odyipb)- ,rP1.+woW (i1 Exygen Research Fy,7.9 7 Page SB 0165 Page 99 of 110 0p0198 Interim Report #23 - Analysis ofSeditnwn4 .Samples Exygen Study No. : POdd1131 Bxygsa Pratacol Number PWO1 131 f.TiA4YiTCAL MH7nOD iiiatNROW. VOOD1736 ND1YodNAm*i br Rr D~Mrr1rMY~ ~t~k AM IPPPwI Is SwwJl - Iwlr~d >arw >hr LC!lY1VMS +YY7Ya1'fi~ft FapUr. 6xYlrlYmh M kwmab Dive Soft MIINw, PA 16W1 11ppaW 9Yc p. :al Omawly iAaled xwae#.?1' W.pxyLP Rowurk as Aatt 6o Flsh .h" Da. Va t1wi.lak cynYnn. HcYlm A~ib ell Exygen Rcsearch 70a! 1yu. 7 page 59 005 Pagc 1(}U of I10 000IL99 Interim Report #23 = Analysis of Sedi:frvnlt Simples " < p. 177 Exygen'Study No. :-FOfl41131 ^ Aoft HxMea Peolxol Nutrber. PooDl 331 wuePrlr4 ._ _. . . ..__ . ..-, . ; . wwneaNwek~vaoo~ss . - -. IIa+ .~~" y~ot ~}repwpoe4noic Add {PF4A) in Snrl1 Minn* Lkrorby LCdySMS 10.0 mild" I* 19.1 ' Erek WA of taaqlaa ataeeed (lypi+lly'0 a IM) =oq iaIYde a Isra aa! ~l aaw_004" d1" 010191" aaools_aools Portilhd au known .movwy 1b, me back . ( . 10.4 L~sb Air AM ~~Lbo~Yaey diqlied. oai epum wv be spanned , . , . . . . . WOO ~p1,P aa~aaa;y4a be q4 ryplest . 11 .0 Say" Fame pa , u.l weqk ~ .1, on~lpl. w . so,.k I~ls~nl~ ~^~tr r6a tfufy .. , lw~dr+, 2e~Ua lii aai lais MM , liew 90t akwxate waf6Db of hva may be ~tawe/ iqe~qra Lr waFU aim VAM" jar MW lf] - AiiwrstelbaweqLltraQodwkrefloa~L ,11'.3 " ~~be weOA riu~s Waato~ar "r-t mmme. .- : }1*< . ,~ ~~ ,~ s 3F ,le ppKa no a lf mL "' '11 .5 ~1 :6 .I,1.T - ._ l 1.9 "6.9 1.1Q li.ll . AdA S IaLef rleoil9saod aLL1a tnr .20 atiwwlw m uwrio+edon alrka. `C~eai6~a fL n~kes r-7000 qm mr-S ewnees. ' ~~ fla a~aaalal kYa a 90 raL ~tyosabls apMiNOe wbe nd a00 33 rYR. Opdo.abilil~w Va Ca WE olAddllla (t 6, 6 ML) 1y 9awias 10 m1 lnpkspal ONSMwd by S W.of tP1C+w7ee(-7 6eaIhu} t7n nol iet aol,um,m, iky `L7~/7kesrepkfoaor~3iar6Cte~1!errtid1 Diaasdaluam . BI" r .-*2 pOIaq~ clam elof duaim a gadun0_ - 2 m1). IJ1uel)za.lwpplae rftelecl~aIeq (LCJML%B- ~~12g , L~amaloryLy . - Iz1 Lq ;:bf Iha rr. ~a.l ac .aek tY.tnd. uoople .oa ~Ai6.+ wnyk uao a. -- - i_'~, !IN qrwem. A calllria. .dedae must pveoe4 .ad fitlow .n 12.2 21046mol1'rQAewrwOep1~7rk1wt1lwamoneonnn1eetiemlark wtll N iosle6r7 huo Iaalyqclq wt 173 losepike aR dab'4nWiaa Wadeek mwtbe inch" pthc besinaina end u 6r Wof assnrb at SWWWOs must be iaMnpaved bat-van away 7-i u qwooplm 11n r iI1wWivq am outin sat of oulbwuon :wduuds nwy khow" Y ria bagwil" of a wt kUewe6 by calikaiop staurds inwpene0 ~wY S-l0awptr (n aaoma forsaead wo! aundrasi le - +ilYer c: aw edikr+da wodr& MM bc ft Rwt sd ho i,yechoe in a so" IK It6 1ke "Yooat'.terarA aatrna for quunYduoo. 1.ioFr qredrd ourvem re ' -Swnaed llte&e aaqle b9 Baura " a,uy Us +wiyktipj otPWkarw r.e. s or7 Pogsr 56 oj6S Exygen Research Page 97 of 110 000200 Interim Report_#23 -Analysis of Sediment rS, ~ples , . p. 178 : . Exy$en Study No. : P0001 131 Facy=ae PAOlocof Nirnher! Mp1131 6qi~sr~rck 9fd6a! _ ia bI Nrho/ IIuWrV1s11~IS ACi3ib'I1CAL ~11110C s lssiiat~I~~rAea1~ ) ir ~aosU w_nlls as_Ibtqka inedlld aosaordois wtet NaaaLy~ 3 .3 Isr pui+itarl lky Sew fwAam alould PA swam slada[t ~a~os~. Any ariples AA aowd at~dsd mper~akvaldOr RRhu diltiee0 r10 rwadpad 13.0 Aaosplap Q111& 13.1 L1uumb/d swtfaw a /nL dm dwi/bw laa at i6! saw Ow a pwrw af -At9 sos TIE "tl< w ~r awwlpoods lo do "OA anioa . whik Nor dw~li4c im (iW wlg !e0lawa Ib sew etewWn Obxida . 13.i bteelol blab aws ml aonhio 4'1DA at lerala swar thaa ae l.04. 11 a Mde eaMir PPDA it Iewh rtYt itr 10 w& dw a mew blanb ~ple VAN %P elYisltd MA lY mYo IN am be a4zracai. t9 .1 2 eOr.iasof ca .ol spka ad aua6 4Yoa, mm b. b .rvwen 70 " 130% of Aa'v Swwra wluas. If a wnbel yft A& ouleide 11!e eepriabh Iimin, da ptiw ael a[ rqlll. sYeade ba r."exerClld . Aar MMic epiKc oruioe 14 1)01i 110d1 be evelwled by IM audyrt Op delateae if ro-mSnoNon ir wrtaWd. 13.4 Any nh%Wm dasi!d *ad a b s atslilldwl oalller by uwr4j on Huge Beee TW, myy be laelulad !au !w e4kWa0ias of du uhleadoe owe flaweno, No 1s41 som0w of es1bllfial sllndads Ou! aosld be excluded art astvowad70% of dr WA nowhworapedsz& Wee" us rie eslwMll eosAloaoi ) aa aliherls. anva+ NWAewm must be aim W a. 09071 if dbtralion sorb Odl ousede aae Ivnla . *en /"% sXwpliw pap amus b. ohm m adJr Werawwai oyasliw. and ft annAlOs ar Ila eYwt wt @frmpllarborld be nudlsed. 134 AeUlllws d", et~wa IfIaArW led lplplle MR Jot d011 motc 4rs t"%wilhle aelrbsod htt Ifrtlewian IirK dfiA srcaade tug limit wti!fiin ueealyfiral aiatwoOr ad xnwt6a nl~ulYbad. 14.0 O51001060e6 l41 UwAs "ISs~Mo~aqwllonncakWIStIramwatoSPlpAIWM(ina~llm4 bow au !rY aa4 -105 to Esdnd muw (1'ww rsya-on par+wKas) lor1"YyflelGss LYN loltwM ytopsa; tPOA 1Dw14OWit) -MVAJML_kMMWj s aF a diqua fiVM at*o 0! - fleiorbywbfd! re And Ydawe WE dlluled . ifneouaary. AYllust pelar-10 nyeKv Pop 57 oJa3 Exygen Research Page 98 of 110 000201. Interim Report #23 - Analysis of Sediment 5a."nples = p. 179 Exygen Study No.: PC041131 Exyjaa Pr00oe01 N. umber Pfl001131 POW ar.ewwY .r .voawM : ill~ldt bfrS~si' ` . . af M==W LtrnrbyLClYSIIAa Add MA) in Small 6.0 , 9.0 3~9 Owns" P*vn;L 5.10 . AMW4yW (30a1000 pL ud 10-100 yL), wht dl4%opb)s tips. s.u . wrlrfiVhY vrf ae (Ip tQ1 : SPB eroddl4w. ~.u . sre ~aa.wallai~aa s.13 ruw .mlnr. s .1+ wdr"scn.e 11311111. , $15 c.mi~e.o~+n~.or~a u~1. varrwr~a~.~,b~. .~ 3000 ~. t~u6err,~~k B~uot f .l Ar1~alColssat 11oopYtr Rl (Ksywss Seisarilfe), 2 .l aun x SO mm . fp Oft VISSWI30) 62 91pslsalre !0`C 6.9 . ' 14ok1k /,hw (A) ,". I roN Amewn$ml Aeeeue e wrw 6a' LfeijIqfYw(y) : 16s0unol ~-S ~rl~lutPpi~e: Flow RM15 6~9 ~ " 0.3 Y,q 43 7S 00.i i.0 75 0.3 2&0 121S 73 0.3 213 4S 33 03 66 lsjeelioaYoissk . IS YL leda Da hlauwti ton much r 50 pLl 6.i l]urdul* lwtAw-mptna1r41aW a%iwtioncostie. LS 140 T%*. - 23 "am, TIWAM OOMMbllaYikla6P611r api{/r jM1 MW be 04owdin nnder b Ii I 61wH!l 11511I1M 6l8AiSlYsoo . 7.1 ~ 8lsqco~sslr NysYrs11111M ade, awilurhu ~13 -r 369 sds Por Tlr am" sqodiYw am islwl6s0 r a SAW and may Te 4um6ee ix orter ,n a~ b MSrLb syslan ?".3d, Pass 34 0jQs Exygen Research ~~c" ~Rt~f " ~ Page 95 of 110 000202 Interim Report #23 :- Analysis of Sediment Samples . Exygen Study No . : PO041131 HxyBen Protocol Number PCOO 1331 >~ 9IINYi A.~fAL~a77CAL -M--- 16v e( bfrmd Lirvrby LCdkSIYS ~z~~l~ ' Adt (lFOA1 in Small LO ?wprallmot6alrtlaos, L1 HolYir?!W 8.1.R 3 eMI_. .iow .eaw i. .+m< iu pnpan0 Dy IIIdia= 0.1 54 Y of rllrmdum aomam l01008 plLefwMer . wWnrlsrilraw meybe popmri . 9A 61rda1 ~ 9 .1 , BN~d amelMFmllflcrdoll Somliea D1 .1, Pupa aseek aoirlion of-l0a yB+mLefPFOA by weighina lo w$ yralty,Ht >~iy (eereOfY f Mtiqr) a/ dilute m 100 mL with alatllm6l ins325-ai.LDP1 boola 9.1 .2 A 1A p-+aL lmi5euioo aolalios of ?i0A !r ' by brhrinL t . mL ofUm 1001~1. aoktiw m a Rod rolmAe of !00 wbb Meenwul Ix &173 aI. LDPE bonla. 9.13 A ql ~Aml. feAlieatiae ~o711dCU N I~FOA y yrajtr0 br brinjb~ 10 , ad . a(Mm BAIyfaJ. aolulbnl0 a SrW Won of 100 wi01 maCmwl in a 113 a1 LDi! boule. 9 .14 ~ bOdt Ird SKqAqqaa IW~w ca m brslond in a nfiltaamr N WgndmNly 1'C and rr alabb !ora maximum VwW of 8maxbi . lYamolfehlaafpvIqnim r 9.7 SluedrdCdibnliar8oi41tior 9.E .5 4.i3 . _ LC~M6IMK eaYdallos ~ slsya~rad In mdFwnol +la diplliq+ adflm 9.l ~rmL heifiodios aolwfiow. 1Us S+Ibmiiae bafypial oer9ic adiftaorl oommiseioos MY 'x FrIOKia.n .rJw4 . Wto BaMir tdlyadd 'T6~ 1W 1110 vainllt [nud si ?A 11 Oiluld r 1 ICY IN -FIM - Lumeisuien cas 1,0 1 .0 S.0- 10 to 10 lag 01 ~l,` kQ k0i 0.1 ~ ia 1]3" L,D)B rnow~moudl bYW atYC m1'Crp m wx awyRa. MA AIYnWnveLalnw r1d emeetr+damu nf gUedrdt nyy be pmpred a fft.a .fr Page SS 0165 Exygen Researeh page 96 of 110 0002013 Interim Report #23 -Analysis of Sediment wamplCS - Exygen Study No, t P0001131 ExyVn Protocol Nuruber. YODOI 13 3 ANALYTICAL METHOD MiUo "1iwbuc vOD017p Mole! rtCAWiYler IUs D~Iwwkfllw dh~Orrnanrde AM "CA) in SMn . . YrmmN LWer by IiCISd6JNS M$7deW TO-1 YrMW , El" 1rOrw! MR Rrrs6 Ddve BrIpCnl4Je,?A 16a1 App-liy: ~~LyUC~~ 1 7OdOieJ~Ltws.LCdti, 8triw ~a~weF ,2,14 ~~ allilaty , viorPnridO i wp- i ~m ltrere5 1 6124104 Dna Ado"610 D .a Ibal Paw 7 h. Page 32 Of6J Exygen Research , Page 93 of 110 0"204 p. 182 Interim Report #23 - ~ Analysis of Sedir:=t.S%r.ples . , ; Exygen Study No. : P0001131 Earysau Prarocol Nuxt6w : FM 1131 r^ av,.eM-wa MOW"e.wtwonira . - AMi .i77CaL DtMOD oiAkhtla iav Iiw Tiwat~eroes el~lfowae4rie Aeii (tFOA) in Small arnW LMerly I:cAMM IA am" Uk rmdOll is so be w4da* Ibe 11e ibolwoa rd qrrYYtiou efperfluoraetaeoie will by IGt Paloearue Uqd Qawrlopaplpr oaOld to a trams Mas 9pwsalv~iaDheelaeQ.ClAD~idS1 ie eot~1 or0u11irer. tD .Sa1w . . . 2.1 La AAw7eo6ewwwltlalerweypnpioea CR+dt tLe appeepeib 111S WE . Dao~ioD ~y eLmica! ihe ptoptr are, 7.0 3wa~h R~i .'aacse 7.3 At fews li ohnl umpb be p~ewwe. 3.1 ' $f(rpW,eioald be peoeeaad bellies weaaedan. Maw th Uvanm ample is a iaaiSroca+aar~Damopidree(ll; dry Iw. Dieoe die wmpiea ia ocuwiaen ad'i.nw ape' it Ibru apwr eremisk oo bil low for acbaa diosire ea6wom4w. amd we rwe ft wmplee in *min emrye well Iwo al, aealyeu . AIMtaalaly, i! elrn Is ee iwYllkleet usown of ample (AM Our. 4 ;;, Uu no roeNAV4 is mummy d Uit ample M 00 Died 04 suplow 3 .7 Saeirk pDNeiioa DreeaOtrr wil !e paoifind in the eampuaD plan fw 11** 1104- r 4.0 1(eaetttaaI4Bpladw0a aa wwr-~.c waa ~x laeerd-i~cc ra6e Y.) iteeloaluf6 -1?LCpade "A Atiehlodmmllw6a-A.Ci.Room OnW 4s rr.7ewmoemwieAaii-SOaFAldrioh S.0 wommwadltlwpimtoh S.a A k'* pRftm+ww 6q(id t0awaMWMapL cepalie af pAMFinj nP to 2 eolwam evippe/ VA a vaiaWa volien iejeowe amp" alinjaetinD !"20U W, ed+elad to aIniem Mw Spavaarls (LCJ1AS1W 32 A dMdr maslYp me OMa br Ceat iA~tw[~a wA qarroxtan. 5.3 Andy" laweeaap" ef+aadiqln6.ODODID. SA 11Q pL iitparLiepl~pWyhoemisye tabS.S iBetLliaperl~lepNyprArloatiom~till~yetrba S.d DiOanlbadaopiletetlO"100a1 (OD.700u1.). S-7 t2S~1 .1.DP8 arww-mon& fotllr. s.s 3 ML errlazceNat. r,r.iL4, 0-1 Page 39 oJ 63 Exygen Rescarch Page 94 of 110 fl0O;205 InteTim Report #23 - Analysis of Sediiii-fit Sar ;iples ;1 ` ' p. 183 i Sfiddy No--.! T'0001131 ExMt. Protoml rhttn6er: POOOI 131 u6A0t11.a&rnvooornO AAALh'TMAL.N,S'Tllpp ". _-d . . .Ae~iii>~W' - -o - --- -- ~ AeN (PF1~A) IR Wptoum ii.L .,,1+1~0'ol .oraawoeianrmms+twpleietr.wca.oenilUrl~.. li.! shag m.rql .+PiafOt-IDyr..tae .wdp"keloo,k,loos 1l-tu a. sD ML foqpne~yur Who o.ar.w,R ,w,,b o .MDDD ,pm ibr~ 1t .;f D..r Ow .A.et aft to .w . 70E aolw.a cuA.a rh . .4aq. inw * . ._ mew /w9 WYc md mehiw wit ft .IuaN I=n the initial 11.12 11.17 lt.1s - l1:1S = ha6 1" OP 11,1 6 .r,r 11 .11 .pk ,Ydi 74 Lup. .r toe~ Yu do wAmet Q 1h. rv4hw+ eu1 .a w~/o,watw~Ac.a w.ur.,.MS " wrr e.wa-(* cwc~ Lhb 110 !rd roluer, by alOin T ML W 3% reoibia WO !n sadupeW OD I~~t~A~! Urk tei wriil4 olrAl~ralw. 7Yi~ArAo ttt4reb or 1~LC+i~~ rioj oiwpertbe pipw . !1trh~+!~+01w~f ~4c~r GG.HS+1ds . ti.0 Q~ciwt~arty" , " 1't .l 1nJea &e O.w . .,mrr or .ef *qea.a, ..mple aoa ihwtie.e . .mpls isle Wk LCAifi+WY a~u10. A caUlrwioa trdrd awe'eapda viL fopow al! 9tomlr! ofTlOA a~aadlo` o0 ot lort [Ws or own oa~wnuMion kvels - ' m~rt bb iob,ludd w o ral~"fied ~e1. 12-3 Ai re&e ra of enoao~d cYilotiia Amluil4 mun be ioelu0al at tlx 4~iss md at &s sii or a awo0ir oA, Fauncad it~ mm bc iYtai0wNdblbw~l 1v1iy SlD ral(11~. At ar alese~6v~, aR maim sat or . "emald ,pYO~ea ~tr0edn my t ipJooht r Oy Eoyanif~ of t ta bumew"~di ir alad~a eahladm w~ Weapaad evay S-i0 "10 .(to wmmtK ibraapeaad nt of RhrYd Ybmdris) . Ia pdwrar, ~xtr~emi ea4hntiu~,~* ~lba /n few id hot iq~Otion ima ~k ~rl" 12A Lha Nwtr rlridtr0 mm Rt 9~a Liwir snndrl e,rvn re " Osy~fp.Rr do pwbw by Wrnwenloo utd~ VA oai3Ltin3 ofi~ ma in plllndlh itnlr0 ~ortradoo ntia~ Mrsl.yns 3.3 (or qwolent! . w~saqa4+o. t2.3 , I~b,wtpcnw oAauld not wt~ad ,rdad ,vpas. Any ,rmpleo eou exam ar~otd repot~r rYooldLo lirWerA+3md wd romalyrcd. 17.0 qaapdrs~~ 23.1 (hirlwfre 00 ivw a put ofo rrf~ We w 369 rrw fioaa o prea~ af31~ r~ 'ltie 113 aew fu~t as~~mpoode 1o gm "OA aoioe, wlule he - ' dryhtar toa {769 rw) ~o~ Ow bnof eohoa Aiwciba Ty'a of 7 /ti ft! ~Of 6S Exygen Research C~'!`6'( 1 (, ~ Page 91 of I10 ooo2os Interim Report #23 4-Analysis of Sediment Samples . -p1. 84 Rxygen Study No. : P0001131 I", EkyymPwsocal Number POW] 131 p~alYtrel M~ytsf Rsd ANAL1TGCaLAlL7HOl4 Of ' b) LCl3iSIYS IItON N~rk~ V0031id Aeid(PPOA)iaVqsatisn !39 . 33,3 1]A 13.5 :34i . . wa16od IYeOts>n* ma. eemraie PD4A m W* raw mm 9w LOO. it 0 W~llt 01~111pC PPOA it 1~1h4 /I~trl f>tr 0-3 /~,llwn anewblank sunple awrM obaiwd ad Ilw aamodembesww"eud. 1lgewaiw o[srasoj Raw rd mmuia apibw man bo belmeew 40-IM of dwb Uauw rdtir. If a eaobd fP!>ti bb wRUdrr 16s OeeR"k lidsr, ihe sMbe frt rrfawrilw ~YolYdbs rnsofbe101 . Any aYbwIw sodod lwM6 SO bb 2 xnirdW What` by "Oft t1e FIW lnae 7erL now be wseiudN bas tir ab:aLdqe of Iho eahrnion rrvr. liotttars. llw WW me" of taLlmiow ObawYadt AM vodd be axcMdcJ want ON aew l0%elrLs 1041 rbv*falnwdrdv iyOeM . Top msebt's sadLd-1 (R) tor eaftqliou Curves P601W main IM, 30.!!9 (Rr i4!!7~ 7f Glihntian rwala fan wtlrida tbow linita thm Map" Ihy1 a" be jam b i4ue inwimment opetawon, and 1,e nwy+aer 4w rdhwwe r1t dpmplw dwl/ benwr17Adlqlmdmt dalw igWmiw& rd 20111048 m+rl ON deNl awrs than 3 4 % wi*M M ana*n) EVIL f(mullim dw Alift OWN& " limit winiH w rallOwl val dw VIP- w MW be romb=& to i4a LTw#A5ftwh*4wx~ a as Peak MM) -i" do WdwAbNLYM I I an" (MMU FIVISMOR P"MeW pqpw 142 FPCkA Amed (Mb) - mwbwmwoo DF - ftW by WWO dw Od VdM WE Chh" it nomMY- 143 Irw moon *ASA wilb knowo amems afPFOA pW so emmriaft. dw atlowlag spoutm tg ankAms do ~mrcwua rowvwy 10--y M - WAI MMYwhww Owg - M!bt huridin Owngi (r4VIA , IOD ana"addod(WS) F*,w 7.f ; ~Oft Page 31 of 6J Exygen Research ' - 4 Page 92 of 110 U0020'7 a Interim Report #123 - Analysis of Sediment Samples p. 185 Exygen Study No.: POGO1131 001- &I<yrn Protoco1Nwnhar. rD001131 .._ , l4~qArreoL. _ . .._. . ._ . , . 1r~6uo Nnw vmat7N . .--AN resatt Ml7Aao , 11Wr~ Asdylullbr 16a ' ofTwlIIIOrooaraio Aeid (1"FOA) in Vqrbtion _ . 1YLORR~ ib aberrswdlsfau wirrd~d r a ~IIWrle nqbe mr~ee in ada w ' 9,0 Ptvawlt4ar" i.1 bfobIY Fbw tl .l 2 rA0 muneshooaeelW ;a WoUr y pepre9 by ,M;of o. ISa l of ' twooehost Miles to 1000 ad. ofwalw. L7 Hs4aceoa 9olYdaa t.].1 37Lroorbk ri1 inaoMrd ispqpwibylifaolviog 2sorrarbic . +of0l430DOLd7pll~ael L2.Z 30lI 1~y~lr0~a 6! 10h~alm is p9- d by britl/rl= 3 mL aC~wMlpddlaltlarerilne qolaal volirlr of 10 mL with t. om" Alorrnnon wlraw"be Iwpwod . R4 SdOdYd /apa1"tio 91 Slrdncd StoddPoAiiaabaa folrrinn A1.1 111tlwti &alock wlulkp o(-100 yy8ul, of PF0A by woyhioj 10 mg el'ralyiai ah~i~ (oal+~ebd br paiNy) and Oilltta to lOD mL wilb rlabre la a 1254RL LIVE bob. 9.1.2 A 1.0 "%L hean.alm .olwlon or rroA is rr+rr"d M Waina i ml. ohhs !00 MInoi asledep p a 11W volume of 100 with inarlrwl . Iaa i27 rd. LMboW, 9.1 .i A ai p@WLlkdlc,arsootllua,of tFOA is pnpaw by muq ;kg l0 m.l o111w 1.0 Iy4sL roluiaa a a Food volume of tOD wirh rodrrbl in a !2i mL tol'8 bortla. 9.1,4 A0.01 y,jraL mrddwioR pidiey oIFPOA is Peopled by 116.64 10 rL of no RI pWrl. anleEim in a Anal volume of 100 ~filh ahlYrW lo a12imL LDiBlorqa, 9.1.5 IM dock.rd bMe0fom rW4eea w iv be arorod is a ra8ipearor ai aprasilanly 9'C ad an Bob Ar a masmur'eleQ ar i somuw 5voa dls " ofiwpanieo. 9.2 Iqnd~d(SIi~Yka ~Yltolla ,3,1, I,bM9+Ali aihlrraloa krlidr an )Anpu*1 m ~.Miawl ria dilation Drum 1 .0 WmL 6rlifrlion aoblrloa rw4w /1, page 48 olas Exygen Research *,r~t ~ ;' 00020$ Page 89 of 110 Interirr~ Re~rt #23 ,-.Analysis of Sedimear.t S~les . . , . Exygen Study No.: P0001131 Exygen Plaocol Vumber PDD01131 t^ l .7 .2 711s iibwYII is s b'pbwl Iamnole . ratl6ulowl ooeeRraaws my be pr$ l on"" EZ_. .a.. dltdtaplir Va"r lolMioa{7~ta _wf .L DihNdr (rIL~ 100 rwI Co(mr.pn-.fN.}ow WOS 11 1S 100 O.D23 . . l.E: ' IA JOD 0.91 , 0.0 le uD o.oos am Iv am Do6u Al so no Dxt 0~ 1D 111 S 9.2.~ Slen all rrllfrds ie IYimL E atvlow.aoawb banks . rt 1'G to !'C. W b six eWtFw 9.2A Attiawwlut~s adsvonoYrtbme ef lilaiada 1~7 Oa pwpueY r rWld. 90A BaklBelUy }QA Hae1.lsYee ar .rlpw at~eraa (O~Ir+lly ZD er Iw) mua aeIUAG u Iau m, IrYmdti 9D&VW a/ lm 1mwlYti nootloll 6ni6d r known eempuftfiw (JoLooetrul spike) b eeily prooeAral wcomy 6x do brult 103 Raqidl"Jrqot tos ddqd and Ir6auotY dMliaaia md Ipibw rvitl be epeeifiao in *0 qtpk asrmum plw fbr f1tH prV/ee. ILQ ~mpb8~thaet(aa Il.l I4 .1 `i i .7 1 t.e L L.9 Wei~ ! 1 of $oas a~L hro 50 m1 polrp~yltae eatrifuge te6et Ik~y sawlW, nptaaa Ud mO alix wa1ly. Add 3a mL *faealodltiL ari eTeb aI a wtifl aaUOCi siveter fur-tS minutas, Ca~6ifa0 3a !a nL PKYPWy1ws pOw saR+6tiai " n -2000 ram Fer'",W~olea, ltielc rd at+aiitim 6y SP8 tole rE~ tl,eppraMpri6 flaeb. raet oltu 1'D mL 6M tuYm in wqmwae willt 2 6 flmisil. 2 i ailiu pl . 2 Y akbeW iet 1 a LC-144 Caeditlea in eoluww wiik 20 a1 of ntwwnel. OW ^.'ts mL Of wff04iiira. Dkqld Ix wYtKS. Do WO dlow Ux oolwan lo I1.6 Sykalo 11r 12S m1 paYWhMod flulb by teips; wB1 the Mri dinamo7ftmajigilllwlktIsitwiukYioa. Riretlsf4qkWith tolueneones, l6tlvaed IsY~Ilrmol gfrw dnay, Diy 6M bob eompkaly tefwe me . ;Ibtby Rb-d1jjmR*i6 aeRwql otnttioppl. 11.7 YlwW Af!"aman a aeordLiwwad Ps ooBmas Dow lnaie as =WAvi . S! prF111pW Out CMef ft i1I11b In the 12! mL uUml7ed peu-slope . fak. fty. s.!' A Ptg.I9of 63 Exygen Research Page 90 o 110 000209 Interim Report #23 = Analysis of Seditinm: Samples p. 187 Exyga4 Study No . : P{1001131 h Bxygen Protocol Number: PM 1131 ' '~7~'' 1rQedwd' " H~Yo"1h~oYR YODM>M .itiAl .f IICALMETHOD A~l7sl~ br tAa bwael~a ot by LCMyMd ' Aeid QFOA1 in Vsseuteon ~ .0 ^!'T~ k . ' Awa medod 111 Balm arOb3d fbr mskoirSon aod dwn4mdon olrgwaoaasiorc +~ b ~ ~~~ ~~ ~F+lh7 ~aPbd to a wdw M~s lp~stiwroie D~tms (L~IJiS) ia YWnrtion. zA Siley - . . , 2.1 Ai.,ay.or.~ .Y . ..r.i.raswyyr.w., .- s2 Cmwu ft ppeapdsk MW hdix. iuaAli,g.Rr cheaso.i for proper gettcy ynxrdon. ~ .i Aslwamfetlrrdrrriwwnwotks as s~rh diouid'iayroer~r+wbn .mnalon rLe. W . bases .mpb i. s f,cd pve.nor aeiba;aqea. vilr dry W . Place nir ..,.p4s in eoaagina, w,d *ara IM A baM danF wmui& m AVOW INN ra6c. dioxide wtifficanAas. !ml ad VWa Ow >.oplq b lro:en mrye mil tim. 3.3 3+edtfb alYeYen jivooairrw will be ysoilGd in IM srmplwS plan for this Pro- 4.0 R.yraBapddMDdWft 4.1 Wow -1D'LCdnda 4.2 Aewminile-IWirCVads 43 Cwbn {110P.OQ m16) - Raqmt 91110 4.1 AHlhroi-HAbC~N 4~ sdie.putso,M .rn)-wysr,ba ~.Y u s.,.Kr~acwa-~+p .4sa. 1 .e0001-30icAPS& L9 LA ..ai+icadd-Rw/M wh ..~i r.ia.-K....rw.a. 4 .17 AmopdumAeIu-A.C6.RwWet(inb 1 .13 Arlhwoodsoaie Arid- MrwKA)MA ! .0 ipWpomotaed8qupmYt 7-t A YdY psrmu~s dquid adosdwaplL eqwk of Pmpia= up 1e 2 MuiYasY ywWd wii a rrldblY VOW= IyeeOOr aspebic of tajooaiad S "2W I+l.ewn~aed m almdwa 1tw i~ObooA~r ~LCIIdil1A61. !.2 A dnk@le oWYG m++dYt br3adc hpaWgea aad qiqetludoL S.9 Air)yica1 bdmaasap" otvowilingaa 0.00001 s r .., 2.1 7 Pcg 46 oJ63 Exygen Research Page 87 of 110 000210 ?uterirr. R.epart #?..3 .-Analysis of Sediment Samipl.es . p. 188 Exygen Study No . : P0001 131 ExMn Prolooo! AkLrnber : POW 1131 Emu Imm" fINW NYSMi V00017ir i A<4:LYi7CAL {IICTRO:D Adetbrd af r'fw+y.Ba d* ;hp Damk6tis afihwAawmdeoie Aeid (MA) in vergam) ' by LC1kISILI5 ss.s4 a.uq ".pi.f.+.1t11+r..an..r.. y .6 S1Oueu~~:eO~1 rYlePa7p~PY~smtrilnleThle~. ~,7 uou~i.wlro~rraKw~aww. stt a~Ipawl.aiw~tow(samou1,.11o-2oa+1.~ i.! ll^iaw, LM swwwarsrotqr. O.tc ~ct ~Ihuw.rya. !.1'1 DlvawblepwUw, 7.1., lltipoldpcnw (100"t/i0 /L=110-1001L)6 wdtklbpowDb Kp. S.ls s1~ rWld!d6.udu.rv(AM1riWMC. w~"k+ra.aaaASrlTq. xrs CawktpSp*leormicaft 20at.aM7wPYm wbaat3aooqm . LO >.'~aw"PqYe tylw E 1 1aaly" Qdmm linYOw 1! QLqalar SeWnti11c1, 2 .1 mm x 70 nm.lN (P1N:i3306-06217M !S: Taf7p:1%m 7C"C S,) A(ODik Mm (A1 : t m11 Aw+arimm MOO to Wow fA MS:SuPtw (ij t Ms&" 4.5 (Inow Flop r more.i.i xa x Flaw RAN 35 013 1 .0 se 3s 0 .3 1.0 23 TS o .3 2R0 25 75 0 .3 72 .5 LS 3f 91) 6 .6 lhjrelia Yafism 1! NL(ar bsiwwwd low iardM .11 !0 NLx 6 .7 Q1Milwoe Frlt Am-rctmd nardrd atibetice nasva 6.i bnTqM : . " 37mbrJOL The 16orf eolYtinn aw iiom10e0 n s Ooide ant may he m=01d in ouder to ~*priuYrL71A Ijd@a 1A MWMf O~er 1.1 IA,Idx )?11a[I~aY Nqp4v11GlAt nOdE ~ Ol3 -a l69 rol: int ry. )ari Page 0 7 of 63 Exygen Research Page 89 of I to Interim Report #23,-*Analysis of Sediment Samples p. 189 Exygen-Study Ni).*: P0001131 Exyyra Ptotoaol Nuasber : PD001131 14.3 Fm rppr ftdisd witA 1c~cwa meow ot 1FOw piw so o~:e.mros. we do *Ngwiy swoon" to calwlqr $0 Pwasit nomy. ~~YI%3 ~ ~w "is~lfY~rAWy1 " ~pmu~diasa~ad(n~'dl .]OD " . +rtra .d~dlnlril n Exygen Research ftps .rj POgs 44 of63 Page 85 -of 110 00012 1 211 interim Report #23 - Analysis ofSedimeat Samples. . . . , , . . Exygen Study Na,: P0001131 Exysea Pcatoool ?. Amber P0001131 ANALYTICAL METHOD MAad 1ie+lrr. VOOG1Ti4 MeAMd *fAraY Iwr Aie DWwoltitlr O1 hrllerererNO Add (lI0A) 1 . VAehSlw by LCML4Ni Anyuar r.gft haft: &crwa.wne "18 RewwA Drive Spas Co11WlA iN01 ? +rA OrrNV~` pipti CawroRY TeilmicN H.eWw,MId; EtyprRae+ee6 ~dT DAu lvicehw4iL opwnkm, & " n Rsmrai Exygen Research TaMt Pffln: 7 Page iJ oJ6J Page 86.of 110 0002IL3 p. 191 Interim Report #23 = Analysis of Sedirtient Samples ' Exygen Study No.- PCOO1131 sxy$co Protocol Number : roaol131 M.+aiaY.Yr VOOOr+o AidALYTlCA1.IKRTiOD ' 'a naiawaaYiuourrwntwoocl .nic Aai/ (rrQA) in fun .na 11 .7 -raixiw,e b. Jill, ML polyvAhrl"n. wbo o.m.la;" ,attpI. W -moo . ~ Toe-la .i,.le.. n ,t jDaeaar up attract a. ro a ~ue .e.6 sra ew,aw slaw ~a. the ~ or . du pne.ae~d Mdc. Couea ON dole in tae 1ss ML :iaaize6 pearsDape MUL u .s Add lo nt of sneeoalulle to the arqde In n SO rai. neau;flp abe. dloaioriYw Mr eeea ft OM raft anu1110iar far d0 Mwrds no naae a. dwoiaar .ka-a0sL uf awti.idL we do lie.. 1 Y.10' . Own the aaawla again far -10 vaiauosae a vKiat4ccan ddmr. 11.I1 lYbeiWlaiaala~=fnc-lhourmaR. ll.u r.orle. a . so ml. pelypn,rleaa hh.e eanainiy maple at -:aoo Mm de-toadawr 31.13 Ca01ot r =VIM OM 11a< 110MVi g/9 mhmio. Co1wd dr dnrls id* Ihc oi /ewvAfped lbrk apd combine v01 die slow 6vm the initial 11.14 "PN*" 7i?pd oraaa4akrib moaO fir 1in wlana d ooanbipe the dwle in t!W arw par4hapo1 flaet. : lqJS AM s+ enW of I-0ened in Ove !a 69 pear-shaped Ink and 11 .1f 1t~ fin~alvolaa,e.~badydi~yi at~4r+eoalrc(~.e~ lametlrmol to IL9"P'r1W0 fiat wa4rwbl to odxldlwoln. M17 'ha"afar do moml0111K.C via1a uaaqAsIwaYWyqda 11 .12 AYdyae soIpha oft I ~ I 1' LCAMM- 120 Clro:reagwlqr IZ .I w,a s. a~. .ooa.e araaeh wnin+. wapL .ea Aadiea >smrk i~ro 6w LJCAMIAIIZ W. ake A qlilrrtioa aeudu6 faaat proada and 60ow a0 12 .2 gain8aai sfrlGA earavanday 1o at Iwl fin or nwan aoacetralioa lweh irobe iu la6ad ia raaaly7feal rl . t2.s 1b, walfea.ue ofealBheatias aa+deda moo k iaMW K rra b .pmaiuj ad ai the ad of a aispb v.at ina6aNr auul k 6wnpuw between awry 5-10 yrmpLa. As as rllwoatiw, an atis wl of eah3radon padaudf mry be Wowed. "el 11w Dapaa'vg of a art followed by oaULelOioa eWdiNi hnrivawa6 waey y-10 samples (fs aeeppn Jim a second sat *(saardteis) to wither MN aY~raiou rm6aW arm h td Ilea WA Ian bqtopon in x M"wert. 12.4 -UY'lialw a`aird sairr far epuaaYbYai West aNadW awtip we y~eri'fw IhW anntyle ly Hone regelwiwe palaill th w9iglaka or peak am ` vrew wllieaiiw Sallow saaowrowtiaa ariq lluet-Ym 3.3 (or aQaivw1eM) iedwaw syalm iy.anre Page 42 of65 Exygen Research `,(+ra+ Page 83 of 110 000214 interim Rqport #23 - Analysis of Sediment Sam,plcs . . . Exygen Study No. : P0001131 Exypn Pmtoool Nufnber. P0001131 13.3 laqy .w~A~ dee16 we ao0aw nudud Is"osm Any ialpplea ma , sseaob Wnd~l n~onu afiwb tr AAhor dihwd aed rwuJyaed. 11.0 Atehlral?Ysia , 1S~ 17.7 11 .3 11A 133 11.6 An~ro~w srq drw a pw~lc efe rrjY~c iw rt 36! anr hsm a pwu~t of "Ul am 1W 433 sow parent plnayeols w du IFOA nio. wLilt dn dwoor b(30! amllfbwaeew Unionofal"mtdbKka. IlAo~t MOM son sa onYia R+oA a! brnlb paw tlm do LOQ . Y ~ Week Needed "OA at lwd ~urrY &M 43 101. *M s ne+~ blr~t ""I: arlleoYaiw!md 16a~Yswaa~bnslracbi RMWWw obewtel apYon aed MINOR ayboa mug be MOM ?0-11014 of IbW lulwa rnpm. Ita oalbw rPia rua ouedds e wopalle ]iM1n. uro wltw as ~f wilw alwldbs>r~eerd. Any eelkaYa aodvi llwlni 10 6e a rriaded eaAbr by .inb the Flu,, tnor r.a Mr b. aalead Rv d. vak .laiO . d the wfibrat1oR carvc H .M, O *. ,wl .lowbw Of oal+lIro. AMiM elra cwla w ..kd.u . .u m mr+2nx orrnarl mmbw orar.aa .d la;.alaa. 7b oomlalk~l awllclmt (it) 16a tdibnMimt oelvw aauwe0 am !e 20.l93 {li yo9ts). R .r6wwa. Met" &u o+Ud. *WO lieu., men inrapLU SP rue r ItYr h "UK iauruot apamion, end ft aondlada win wlehmm ofNOON eladd ha rwm4yaw . )h~aCM dime hKwwq mlkao4 aed wuVUs mm not du0 mor than t"7i wi1MO baedylidl M if C0lpllkll tlqi0 dnA pcaadt thil time Wilhih r eryrwur w..m.ow , .wwde aan.lt..e . 14.0 cllwwun. la.l SJ~iebCswL6KurYaaleWw~Wathad0_toiPFDASbnee(inavm4 bard an prt ONO riAS Or MUM" we++ (MOW npawM pRIwmslaal pwiwabi by Ihe Mine Lyn arBw+Yeyooysa! PPDA fo~d (VtiL) ~ ~JOIC~tI 142 l1~ Aa >~Yaw~/ ~rYio~ fo aomet 11n raomnafYPCk1 lboiW in nysL b MA 6014 TTQA "wa09bl " ~~+ ~WKti<1 pp -hclw bywhuh &S9pa1 valess wm d1Y0K, ileacwary. tqpt,tY Pqge I3 oj 63 Exygen Research Page 84 of 110 0 00AZ 15 Irlterim Report #23'=Analysis of Sediment Samples p. 193 Exygen 3j4 No.: P0a1131 F-xypn Psobocol Nnmber: POOD1131 &v,.Iwrlei . Aqrlysis hr . . wr .a N. .W . vooeIo AMALY'CICAI. 'IHOD DO-bad- ofTwaaacoq.iaio Add {1tpA3 is Fub and t0oa by LCAASAAS 7.0 MEMO Spomi ? l . ~ EbelraprayNsSWn btRM made. wsmriy 41 ; ~ )69 mix for ' 7Lsaboacca~Ytfams sw Iof~Wad u a pi0a wt wty is ahnpi ia mdsr b IapiLrbs to LSt1AlS sY+ema i.0 ~n~otEduWr Ll. MAW PYsan Xi.t 2 rY armoaei9r aaawa bralsr is p..prd by a"eS 0.164 s of Urnomvo aosm b low ML otwew. Ss Ifaeaafl+ .lnl.akr 5.2,.1 7% aaofie MW 'r aarwol b'rspva ry diwt+dnS 2 seluoe,bic adA it 100 MLOimwlamap IJJ - JOli DWIN0046dilUwsiaN ie blnae 9a peepras by brinpaS 3 ,nL , afAimdaydiollnwihats a 6ns1 rolms oJ 10 wL with soAiene. All~ ~aWan maybbpeprsi. 4,Q 9 .1 8madrd dUOlMlo~iaa Soh~tix 9.1.1 9.1 .2 9.33 9.1.4 9.13 re"it woaca"ae+r-tao,&ra<l . .iPYOA by r..i&rig lo m, of a-lylid a-fti (eswaawi be wity) WA dauwa to 100 ml with medmoi in a 12k4 LM bvide. A 3 .0 p#ml. Dr6ljnYa suW4iao orPFOA is rrepad by briaSina : mL dfia 100 pyal. whRioo b a IIad rolawu of l00 with momw in a t77 e~l. iDPELu~Ia A " 1 Iqyml, im6A uos solrdna of PPOA is prepaae bY briWn lu Al. otlba 1.0 p01mL sokdon b " &a volumt of 100 with mnonW in a M =4 LOPE book. A a .01 p&qat . 9utinraeaa aeL,ros of rPpA is pmprsa lY brie=;na 10 ML Of Ow 0.1 wjfaL aalNbp b a Goal wbac of 100 +riUb aslrrlfa a l75 mL LDlB boMs. 'fba warl ed ani/aa6w o]dous as b be warai in a nRipiratov au sprmbaWl) 4'C aai rr stWbb for s aokiuompniod of 6 raawM 80mYa dba ef pn, oadm ryr a elt Ptrgt 40 oJ63 Exygen Research Page $1 of 110 0002'i6 irxterijt: Repart #23 - Analysis of Sediment Samples Exygen Study No.: POGO 1131 YOOMIL ExppnPromcd Number PD001 131 U *MdrlCr0kvioofof~Waat s.t,l I&lNWLL! c9beadw "ririh am p"rad iu rqednnei via dIuuai ctf tla i .0 ~Iml" brltlleYim aol~cm S.its '6b hroniy i a tninl arlVlac addiYarl ooaoamaiaw my bs q~i " ~aa0d ------- VMS[ neex~i5r . .. r.lwa~ nuwwti ewioeafrauo0 ~ .e,1 ~w~mw !A. fA l00 OA3 IA 23 l00 O .OSf Is ~ IA 100 gal in 10 ,~oas iv 1n4o0 o0A.9O0u5 DaAl M w10 H3o" e0..000010 9.7 .3 SAuo ad aibtalLa ipwdird+ is 12S-mf. LDPB omccvw-mwlh . . o2'Cesf'C.nptoeaavaat)r . louln 9.1 .C Ali1fY10 Vq114p01 i0lCOn00~adOnaofRaidads maybt PnPuad u WDOOO ;.0d euc43at'01 113.1 Ink3AAeraa9pb.aocuaear (+Ylkar 20 av 1m) must Y,eha. a[ lert 00 Ulnrrt eaomoel god tM vRlOaoed 00111csy MW n lnswa ooacwa.p.si~ ~~p ~Yv~"e~Ure.verylbrae eru. 102 k,qoi,.nuea fer lhit and whaaerrr +uplieats a.+ y" +vtn be r,xNflxl im lbe quality ranoarpla br do pdao[ . IlA 31ntpWEsEoeCm 1 ..1 wiiOR s M ot sew au.p1. ieb so m!. polnaowleao oawit40e t. ab (fI0!! ;@lrdr4 nNra rid&" mix weft 11:2 A9i3Oai . dasslouikila d drb on a wdY 0090 likdar fir -i 7 mbuaa ILS Plop op, ailuiaasaweiw-tiew. ,1tA W and arditiaaela3l81ulwadalhialeathalw4Yapedltwtk I L3 Fee ow 26 ML 9P8 alt" is aqMcs wils 2 g Dudr't, Z i r6" p6 2 Y ,aaoo~4 sd t I LGi98a Cadilio* tAa aalaaiur *ilk 20 ml of secYmoi. am 70 rw nf aw~riM. Disease YI lnalw. Ds am albrv the colusri to xl,i SAwbo As 123 aL 1anwhaPa/ frlca by riming .dlh file 30% OppebpViebbmaWw is alum aoiadn. Abu Yrc Wk +riWi mlwne awe, 6/wed Yt meArwl 10n0 ti-}Dl Day 6a fl-Ica eooplaoly befmo we. qMwhy virrryin.0 Orwii a ~Yaa+aHaiewp~ h0esrrM /^ Page 41 oJ'6S Exygen Research Page $2 of 110 00021'7 Interim Report #23 - Analysis of Seflirrienf'&ai~les ' ~ Exygen~Stddy 1Q6 : PQ401131 Sxy/au Proiaaol Number FM)13 k MoLod of Aal il@dWd NWMWr VCOOi7p AAALrr]cwi. MsrHOa lbr i!e DaKmierioaofleOwroNpOoio Aeid (PiOA) in Fish a.e Cum MZ+OfEfM3 lA swp . This softd b n wat,l4yd for do bobeiN "1 qwohuos of pa&aovcuuwic wit by HO lRfurrors Lfqnid Llmmrepapiy ooupld to a mailm most BP"brMtrJr Aaberft {LCJNYAM ie 6i Mad GLaa . ',r ; IA saw 2 .1 Ahrwobw~o 11bIIYwAA0qAlCliwl. 2,7 Cloonit Ib gproqeinlc MM 6dPe 1iSd1hq riy demiett Gx prapa Hfoty Prrewdar. 1.0 $siplel~qirut: " ." . , 1.9 3.7' : ' .. Aryrit70~~o~f~1~I~fbrsrsaatkti dryh~ 1Yl~ ie~rre .rd 6a6n aotCaaliaa PlOa Ns bum potPl~ 1n x ~D~~.Sw,MtbeSrtrS rrim *Y ia: ft" Iht, riynPin in ooepirm oi "lpw~lq *pea Mmp oveei&M ID saw for vuhm diorrlde aalGsamm. '9aA a6 pea ft ""In In Aarw .mnte rmi1 lime or 3.3 so%h ee0eelba Frowdutn wYl be tpwilbd In 14e w~yFleS Phw for An p'o1rr+. ' 9 .ltw"d "Ododl 4.1 WOW-iWLCpm& 4.2 AoeYpitriw-I$LC poft 4.3 C"a(17WOOow* -Rw/nts+" ". " Meamad -RPM M" is &TaOW460.M-&)- Rowe via 4.6 Pla;dtso.l6a~)-nrpon~.d. V E00doei.C-A3h -]twaotpWv 4.i 1" 00WA-iRI+C paf 49 LAsemYisaail-=wFoejmb 4.]0 inadiyldiddoroa7w-Reqmtpde 4.11 SeMur-RwrrRswe a12 AmommarsAOrMr-tiae.]t.praaac 4.13 PO&KONM* AGM -sPM.AWdCh fA fatruuuolsd8qripwil 3.1 A "FI rm~w liqwd r7romaAFwh sp" W pWaqPuql .P to = nivwY eqippN ri66 s radslb vrolun iqwlor top" of iapewy 3.2Du ptaommld lo a Wdn 1!r Sp~amu~rU.C11R9IMS7. !i AArvin lUwAm mw iM1lsDisk imigmam wd iwAutm 33 Awlytie " bdoron cup" alrwdiq q 6.OB9o1 S. p. we Pqrt i8 q) 63 Exygen Research Page 79 of 110 000218 interim, Report #23,- Analysis of Sediment Sanvlcs D. 196 . , Exygen Study No ._ P0001 131 ExyamlromoolNmnher: p0001131 lippreru:f ~, ANA9 .\'tICAL METHOD bli6+d~~G~1re~ wwes~ MO." vlr :70 Acid (MA) u Fuh r:! $A 1<as7wyco~lati 3.7 7Lw~dwr. . *%tS ii5mL .pw"" cpcilaitc. 3.7 3"a~AqmcLbMbpcQ" IrwewYlRptrbr. s.~ is nLSW0.iv.r"bPROrrM- ONOF.P tub.. !.9 : DLporhlc nkmplPft(AtfRii, IOC"100uL). 3.E0 1'tf" rri.LhISprswwweearlattfaL i.l l 3 aL Wrr HFLC viN IcH. s9,.137a DAiwqpoow.lehb*r9(u1Mca.mD,jL.ria1oa,L),YA& rj,o ..ri.tijiL 3.16 strs t.b ., (Pr.) (s.w1u OIL w. Hnsn7n s.1s s .1a . wcnmsddWtiwe"arapc.bwlr..erspredeisomLpdyp.opyn.Aenrrwzaor;m . 6.0 - CuoeywasAicaWam 6. 1 A"" lywO.Cd .~- Ykopw RP W.ynau seaWao). 2 .1 mm . 50 trip. s,: nsm.essi3al 41 'YwrpMerk 3a'C 6 .3 11ebiM 1Lw (I) : 2 MM AmaMsM Aowa ht WOW 64 rubA PhIN (a) : MWAePl 6.5 GvwiectT"rm /^' Ftow Raw DMRWM %A OLD " 45 IA 65 10 IS - 2Q,p ZS ?Ly 65 12 bd&W 35 0.3 G) 1713 0.3 7f 0.3 33 0.3 6k >ej~ Volv~ IS ri. (m be ioneard w ae wuek es 59 pL; 6." T]~raoLllsn . 1K1~Arw w peno~l ~~d edi!entioa cuive. 6.e x,wtfmc-umiin :ew. - thteYaa aWitfowa~e ap~dad r Ryaidc aod ml3b* e4cnyd io minto eplirolwUtF"f.Csyrrw r.,n3 .n Page 39 of 63 Interim Report #21- Analysis of Sediment Samples ~ p. 197 Exygen Study No.:-P0001131 Hxygen Praoool Number P0001131 -tr< .a ., . : dAMW WMw~' - -- --- -- IYIy~11~r1isv00011p Ad pPOA)la 3adiw.by 13E RaiNk0" Aisw hiMw imdwb ud moon mm nol dnll mm Ilre t4!%Iiiaa!rylyCalYw. ]f=lMdwtira M11raeMdb ftrr Iimt wKhie , " ;`aadyliwl r~ ts mr wt amt Lwmdyaed. -14.fl hlad+6w. )i.l uw dr k1lor.ihswwtial w doA+ri tll~+~ol~u alrFOA abrna (ik ~hlli brll OIP pot w-Y OWN Ilu -d" eww (q- Ippdw iv-en) J 1~[rlad bir 'Y liwl.)ms roA717~ Pear. }lQ11 lW (11ymL) - IPaA'!u ".ILlwaetl y pp i1" OF-11iawlr whiri as Bow volor wu &mW, Ittmow~r. 143 Ax w~ brddd ~rAq mows ~orott oflFOA P~r iv acutcrioa, wc 16s~lIUa+~i M~ ~s c~ad~ISUr pa~t~vwr. (wwraNlyNYasa ~I~ ~Is 6roccroitsV~l~ ,l00 t~a- iw>~r.t'ftba~~~Guwrf. . a. P.~+ooa.arwr an .momuof rroA ~u .a in nyr.r . u PPO,hAwW {nb)- QFQS~411WmSJ=~-mole +MW(s 1) l44 Ur Ib iYbwinP puw[w C~f moawr~ lo c~lplf~b g+ amowt of PFOA bir.d a P/b Lrrrd aa dry wi* PPqA !u~ (p/D~ dqr w+l~t' PPOAlound /ppD) a [lOOSL l ~qal toi~[Xr] l7or7 /~ Plop ,i6 rrf 6S Exygen Research Page 77 of 110 000220 ' interim Report#23 -_.Analysis of Sediment Samples, Ex.y;en Study No . : POOdi 131 Hxygm Profa4 N. umber FOODI 131 ANALirTtC.AI. MMOD MAW,wlbr: Y00017i7 MwYd ~[A~a~ hr1N ~fs~Ur ~f~ AM ("DA) in MA ' a~d CLs ly Ldlf~Ml~ Aury~Tru,V r~o^ axrw ~k 309 PWWWCh Otin SIW CoA~.?A 1610t r APpqweO BY- !~ l'- .3[ Nod Qwee4 irefuqo~lY.eidtr, :.GAf3.lsY1~~111~ccL ` vi,.lnniwuw oqwwowr,EeySrawom6 r9lZr.Lc,L We pop r . Fxygen Research Taw rwC It rap 37 of ss Page,7$ of 110 000221 Interim Report #23- Analysis of Sediment S"ples p. 199 Exy9en Study No.: P0001131 T Exygen Prae0col Nuuiba: P0001131 w~.aa.aa . _ wWra nrt6w vca~ra ~~rth1 el Ol I.CJiA1I1m (FFQA) in $sdimem by )1T !wn IA1 s~ti6ntios ~1uiy b I2ymL LblB s~owalalal ewlks ~e Z,C aPC.y a ra aarha 9.1i Allmrr relllrr r6 elooariuomt al lae6udo maybe prepeal tt rW~t ]0.0 9~Ie1fArly . 10.1 bah atlah of rmplr nmfaei vypiodly 21 or IM) nuel iluL6s ,t bal eer trwre6 aereol rd tws ruYloa ooeErofb feett6e6 ot Iam~ Ww~tldot~ (~ wWl aYtells ~wIQ' P~eesiaH I~ra7 ~rtYe lnM. 101 1"lumPaa >x &id w01t4on1ay Apitaat rod yyilnt will 6s WW&q al~~rlil~ ~waa Pln forioarajeR, 11.0 5=Wb SYOader 11.! 11~7 1i.3 [[A 115 11a l l,7 11 .i 11 .9 11 .10 ' 11.11 ~rd~ ! 6 otampl. iolo 10m1. oolynopytmts ameikso otb. troniry a hrdd, ~e~leetw rd mix rel~ . Add 3! al. o! !10 oee4e at* eig, vr.s and "s an a vr+tm oetios tlrku lff .0 mlwwa CmflYp be e " r r d060 qw hr-20 cdoWa. CaadifeA Iw Cr SiE aaidaw (1 6, 6 al .) by Purim 10 rnL laetlmool flloasi6r10m1 . sfFDLC wlwf-2 d+ophw} Do aa Iw aolumo nm dq" LOW (/reftl} go wqls ft tL sooditiapW Cu BPF cntrid6e. Dipwd . A/d 30 sL o! mMllrmt lo Ihe ndWmaLA In Ihe boatp e! 6m So a9. smhNp ai6a Cop, Yam md arks os s xrim wlion dtJwr for -]o msrYN . CwCilYp IAe w" el ti1000 eps fir-tolpipurL Doug 1b trnlrwt mb pw own 8!8 ereidM. Co" ple slume. . We69s ep0am w94 " eI . O(mlq~p6 Cellst tbe shWe sR0 edi k eo fiie llimAeplls~hdisAA 11 .11. C13o~tiou . noaml en IM s.airp p s 6 mt,) by paWft to ml. tnelMna rWem.ahy70m1.oraeLC+,w(-s6npr..a). oeanlaooWswra,ary AM Am mrhrlel to -70o mL of neue re ksd em Me eaeoed oadidwKd 11.17' Bhft vrli -3 md. tOD% a" WL Cbbot 7 mi, of oluus into jnduated It-* IASlraltyLrpinlepPrlerwyrluiwftodwuMOMopMnay6aLC(1S1udd8AsdoSl.ame - S mLy i.,, s .r, Pae 34 oj6S 1n3=im Rapart .#,23 -Analysis of Sedimmt Sanc:ples , :Exygen Study No . : POOOI 131 n 1*11 Exyjen P=oEOCd Number: P0001 131 ya],r,Ru ,a wfAacl,lWa hesrwrr>,wvooa]m AIiAiLY'17CAL i~R'i'~DY Dalraitawioo~>~Irio~e Acid (PPGA) in SedimeM by 1R0 Cddamrlor"ky 97.1 Iy~X dre utwarouri o[nol rtndad, rrySa alod foRiRad wapla iMO t!e y,-JM= "ohm A aYlhtatid Wodrd mwr yseedc rd Mow all 122 121_ , ' 11" 9rndrtdn ~fl94}A nntpoeti~b at kW &a er more ceeeerutwica Vevels mot ia bDeludod Is s wlyliwl wa AA. atl]tre wt of wceaaad ealibrnfow aloodoch awa be iaelrded a ihc bqO1p/nE end It Yr ad O( A ImPls u1. iuedrpa mual be inlempened .I+Os~ wtry S-l0 wlp~lu. As ca tNwoWve, an wnee aa of cuihrrwr~ rIwfuOr my 1L We" et doe lylaniq o( a rot bIlowrd by WfbrnJon nrldwiY WrpMecd wary 340 anapla (to oooarw for a axoad ta of tlaehely, In eidlx sow catilrica uaodrdc trnnr be Oa cat am taw icetica isaatMpb wl. lln isarr aqodrd corm hr qvrotdtrtiun. Lfawr nrndard u+rrea we ~>brflrafdybbYl~Crte~~cavAilhwpWiuyolpethaes n_oec caillhooldne shodad moeaulafon woring MniL)an 3.3 (or OqUiralent) U .S . . 71aepI0 ~aqryw tirald t]ot 110044111 ME[" .eoiaeua. Any aanpln shu stoaall ntnird mOwnr AwW 1e Ihrlbrr dlluad and rarWlaei. 1S." AcagtanaClftwM 13,f G%ramcayMsundew a pcak af aiu&s iaa at 7f9ARMSassynanl r.d"13 am 71e ili re pns! e~ryC~dt to Ow PPOA anion. wAiie the 60&K hot (C70W! OM) nynwu-r- ~ do ho a(osboaaiwdb. 7b,2 Monk OrdrYs PFOA aa brvb srR tLov 04 qpiaI, fAww a aew bin* rwPlo arrs b&MiW 610r wtki wl sact b w~snwad. 1]3 Itreavrir e[eourollPamnd erlia +Ifw mre bo luwra 7C" 130X of iwr door wkr . Na ortepl qb 1YlL wuWa do aaorpablb 11mib, do aeWee ea1 al =NOW dlot111 !a iv"iupcrlrl My metnix VOW eoufae 70. 130X, rbrl Yc own" by do wlyrt 10 Inanatyt if rsotowriwa is rRrlwl 14 .4 IuW atflslfw rpodwl IbtwW Im bo s etrlMpd wlliw by aesy tlw Hup Older Tat. my Ya weLM IM do takulatAn of Ow alibntion cura . Iiottlaar~,fw IoW wwbar of etaactad odihntioa "aadoode dua cwld be amldad UM not moand 20% of Of WW amber of axlYacted xandwdr at ~aardYir aeaelrt IR) !r to*t~lae tuna Alawood mug he I0992 R' 10n3). Tf wllndoa nwhr !11 asnida thew ]imnc, tuen appvplwlY RIlM MW Yd Mn p WJ11K *Aauwapt OppWOn, mod Ma cnndai Or1Ye ebvrtarl Of YmpIMchoYld 6e enaONymd~ hW6.W7 Pap 3SOJ'bS Interim Report #23 - Analysis of Sediirient- leg p. 201 Exyg~sStudYNo:: FD001131 Exylen Probmo( Number. P000 )131 !nw,lwwob , ..n 1~Se~d o 71sit ~- ' " iliiW Mu"r VOp1T{t ._ MA~ 11~ dFelY~oocqrie 11eiQ (PF011) ip SOfmrx by LC/tAw1A,9 sa~ ~o~.. > ; . . t>vri.*~*A .. 6.0 Wemro~yNcSrar i.l 11~1 CctwenR: Pla~bew ~! ~ian 7ciqdDc).21 maa e SD mm. sk a r >.+. (IY" am-M130) W ?aeyamme: wC 4.J MahOr r4w (I) : 7 U!t Auooolr eaulela ww. 6.4 WbibPhw(a) : 14mIInqi 6.3 Obwihot*X*m Plow Rote Iin~Liob} . 9iE !fS UtlGmial O.a as 0 .3 l-v Ias 3s 0,3 :s 7s o .3 ` 20A 25 75 0.3 ss 0.3 s.b hjmYo1~e: ts PL (aab. maa..l m u rirc! uso pi) 6.7 Qwr~nYliw. Pwk Aiw-eahanY ~hnd4d aNibrxi~a arro . &.1 lh~'ISnr -23mosew . TM opf~4~ do 1aiC qwimm. PAW* mdosybachwwdit, **w to 7.0 Mi+1Qiyan 7.1 ldo~.`LwcYO~payN~6w~ KRAlmodr . ~eqimaiq~ 113 -.3G9 esh6oc PFOA. '1bDiLovb ~esl~daar Ss WBadri u a pdd~ ~A e~y WahwpE in Wdc w wnmft Ow balbM sjlia iD )"nPrati4rMSeLtim~ ".l 61o1~'Y PAw f,7.1 3 n" mmebm won is won b p""Cpl by addaij 0.lbb y of ~au~r anwtrb 1000mL ef~raw. nr.l rh Page 32 ofd! Interim Rqport #23 - Analysis of Sediment Samples . . . Exygen Study No . : Pq041131 FacyQe Peosocoi Number. PM ! 131 a,~ep..ai mom m .r . vwotn: AKAlurncAr .>9frsruoa ls4e~idcflE_+~dysle far tFs D~s+ca~caa~~o0awi0io Acid (PFOAS M Sed~aam by u Fau~Riw8olWimle RZt 1% w11e aeiA i0 wan ia ptapnad by addi0li te ad. ef ncelio aoid to IOODaLvlwnlr. A1laens v0oas nny Ix itWr~ !.0 Smc~rdh+ya~w !.1 SIW011liloiIRaAlSutioa9aMiw -9.i .1 ' lsrpnt a mink aohiNeo of-100 plhnL ot TFOA by we;lAiuyl1d we 4f'a0dyfi013 ausilq{rOneeiod fa pOwiyl and dilate e0 100 ML wiOW 9a.1 rAYliaropl&ila.ar1W3r3raAr@L1eL.D1a!a1a<nIeOeWao. rproArI .6 by Winging 10 s,t in a eIntnw,cllaxo,s~a,b~aotn,l.eol. uros~. . ibet,~a vr 10o wius nn~el U .1 C. 1.C ppiei. bpiGeqioa wbqionOf iFOA it pmpmW by Winging 141 me . of9r 14 pohnL asidom w a fod vel+iue ef 100 with swimc) in ' s.12Si%LLpl86aV6a 9-1 .A ARlpgOLion1lWfasfOhltknof"spAitpatqanedbykinpnalo . tH.olfle ]A y~L wbalsn u a 1fsa1 volwir of 100 wh n~anel ie R Y2! o1.LDrB6onb. 9.11 . GM M esL. iylaL fn65a6oo a1 do 0.f p,,haL adm{ai advmm or ?FDA b to a soma rpor3qmwneodobry1b0r0inwgiitnhg n .yhra in a 12! mLLDM bottle. f.iX '13a ro* and fetk'Aaeior aolrelenan to !e aloead ix a rMipraror at - Mmii0aldy 0'L' a00 a "h" AK a ~YO pRiod of 6 mmOw 5w tr OW ofrlpaNlbw !3 MEAemF7dIbwtSoaSolrimi 01!.t 6CAI1ilLif taY6a11w pmadrb aw ptpwiin wwomao)vi*Minim lI;y10.0) Na1LRldOpY0401WtiilOti 3U 71r lqewla0 to a "1W aaanlr a9Bwnr1 eonoeatratian may 6e .. sfmm0iaa. .e_o._e~" _ Fwl a! 1ad6rtiaa ~trld,l' Yohm d1 Dilald b bai) iAaerMHr (6uNeL) j00 t0i< 1100 10 s : 10 100 S too I )00 to 100 to 100 to --- to 10.0 f.0 2.0 1-0 a .s 0 .: _ r.p sof+ page 33 afd3 .'Interim Report #23 - Analysis of Sediment Samples Exygerr Study No .: Y0001131 HzMa Prosooot Number. P0001131 ANALYTJCAL Man-HOD Ife&WNurolwe VOG017i2 R~Iwd~6A~w>tir Iw D~" o(hr0ewyactrvli Add ~riK1N k ' . ~ h u'n~tsr~ N-tyUwl Tatiss Yewlq. 8aMe Rari M1 140011A WK BawcApe~,lA teeot ._ AID-ar9T . r~tc. --.1. C_._t~.. Teedwl lwft. LC IAti. tawa Arnrah ~. I dp no" , V'we PidideK ~eR~t~r lward~ p.. .~.~s.b~,ls~ T lExygen Research Toattagr : 7 Page 30 of63 Page 71 of 110 ooo2zs Interim Report #23 -- Analysis of Sediment Samples Exygen Study No .: P0001 131 6x"enProtocol NuznDer. F000! 131 sqr,taaw.w~eb 4Mw r~ . .a ..vooei m ARAI,Yrscru. Narpon MmbodafArMYW lps"efPffNorooatmoieAaid(PF4A) in Ss&nattby iA 9sa" '?!tu a~kad is f~ 5a a~plOyr~ ~r qte 1aolqioa wdaurrtila[iao efptrtlnawaUnoic aw Yr: No d~Fct~aa+a Litril C7itoWuaPWhY aoupled 10 a tadua Mau *U0mmaltie DafaebrUA7!l91111<1iaawdiat Z9 9aAq . 7 .1 :.ra~ya abasw a"1 WoiamY P~ 2 $ Qocuoit Am iyyoopiala kms baOxslWadlYft say Obeoiai! Am Few aaftlY 3.0 90x& RuvinxTmt 7.1 A1 kaat 30 So11at ww"k fv aatraeoua . 12 No rppb pwtawftia yaa"ler P1d'anal pmppa, 3.D ' SimOlaa rma0 raOdOratad thould be a8oaad ro oquilibnie ro room 3A Al iamlr RUN batloror011Y eelrad bafae bmw moplad Porn axtnebon . 3 .! SropU osYaotia+ Fto0a4wa will be peilld In 1!a tatpftPtci ta ehis 1go140 Rayaftatadila~tadt 41 Wow-HPLC iida 4.Z _ Il4sald-w[.Craia 43 Awlio Add-Raapal sadr 44 AmrwfumAoarn-ACA,Raymt0tala 4,7 PulU.tMOoebeoloAdd-]IpNa.AldtieL SA laaaaratt w0 Y4*9004 S. I A ~k PwI areaa W ohm-SRO eap6la e( y-pi~ ~ +o 2 foirawlr qoY* WO a rtYrlb wAer iq9oomreolY of ugattini 5.200 yLabwrslatta alte0aw IVal~aeeondsG1d9MS1. 5.3 A-- b onilad nw dala 6br peat Ialqalian aqd 1uaatiMtioa . !3 AaalYAwlbalwwoWNke[epr4ifo0 .00001 j& SA f0 ad.4ipawWalolf'PrPY~ ~~ K~ ss is mLetvaaaway0oiYaePyru o1rlhoa atbu. sr a~.~n.;~.atsa~oaat,tooaao.l.l . s .t 5 .1 1:2x31-Lwd1a; r.DP:a.om.o:wd-nmiu. ,rb. oa s .P Jy4iaablaptpawe. 5.10 :5twqi0wlw 41W I000 PL ad 10-100 pW. WIN OitPonbla apa. 5 .11 Waft SA PYc Vim t to (14) 1C10 6PE wtbid~ 5 .12 !PE vaawn mra4lAlA, r.r 1.0 Popit of6S Exygen Research Page 72 of 110 000227 Interim Report #23 - Analysis of Sediment Samples p. 205 Exygein Sttiidy No.: P4D01131 T E=yg.n rnomool N=ber: roov1131 nra....~ . Ma~bedOfIMrlrD Marwwwbwweot:an .. ~DI~LY[ICAL Mi'Y1iOD do W 611xfktotooewwieAadd(PFOA)ioSuUby Piln8ld aalmetbo alrodrOt sad be itiread at On befuaog of a as lelfo'e'ad b!' wko4d srbYrilion wdrb iilatay w+W -YY S-]0 tanRko 68 auaid Ax a "cow ut ofossae1oA dommdadb7. b oida c+oa. enteaere arlrimwt ~HSw 4t+t wa0 bwt injoc4oo is r wmpk u1 . 1'J.I _ Un imir okodatd ew+o far qwpitYion Linar btrodoid oarva an , ji anlai 1br b! w1)t1 by iarrWaEion pawq lAe -40w&*( VEmb . r~swLL~w adndawl onrwenWaa aofn{ MonLYrA ] .3 fareqoiralenn wAdwq7Wa ]23 see* rrI ar doom M am" atratid waporw- Any aa+iV* tAai ,.., . roaorlaums4 ~w ab.oY bs [d6 .dikwd od tpndnd . 33.0,'Asio~{kiRiia L'. t7. f ` Q~aialo~wo mwta~ a M~ of a /wplu ion at )6~D amu Mmn a Wnn or 413 au Time 413 sew pwt pptfaalOda ip dia "F0A apjpq ahlk ow dw#bWj'M'.PB9"awlnprswiw rw low otwb~ 6oxido. 13-7 Uitlfnl biwlta aim no eobkia PFQA at kvea pwW tbe i!. l .OQ . if . blrkweYbts'!!GA at lbrdo gwlwtltiaol0 Egg, Wsa a ~ bLnk swnyk io~t bo olulrd rnd tha w~ut ewnb" sr~tbra+ad. 133 iGaoradu Keowuol apkat ad euhia ;iloaa oaat bW 3amraen 7p.130'K of tlar laeka rulwa If o eoebol qaor AIL ooaddo tho acatpablc lwitr, tAe . . am" aol o1 rrola ahod4 be n-Woosa& Any mwia aplO owaip 70- ala~e. ~ .~tu a .~.wawa by Ow LWW m 4ssrtnkno if r.-atra3im n .atera~ai. 13.a Atq aaY'bnMee 11amdnd blup lo be a alaHaflbN *r11 by wial the Huge EaK Tral. aq! bo aaobdod Oos eho wkWdba o! NO tNibtufon Curve, Howwu, 0w NO nnYor d wAaold oab'Ln6on ltbdnda dmg Could be oebie6 ar1k ad =sed 7B% of ft OW ,puobar o! oatrnoad armdards igirebrd . 19.3 '!ho aoawlaliat ooellfoiut y !br aliYwioe ourw 4enankd must bR xeM R' io.sta). r a.waa.. n.air su r" that umirt, then %Ywopinoe OP sa[ In WINE to SOW inaucoer opauioti and the nrarai ae Ywntwael an .ta~Sa. .bwsd ss,arwlysd 13.6 xraukn saow btveaa aAmabad. OW umplaa Saw Our difl eare IMa 3 4 % rWa saoalYYed nia 1f~aotk" 6at0 Ot1R anada Qiiflvait,w'whia _ e! stil7pr+2 ~b bn fke wtmoal be twmlysa0. lPi.f7 001. Page 28 of 63 Exygen Research Page 69 of 110 0 Interim Report #23 - Analysis of Sediment S.q;mlrs p. 206 Exygen Study No.: PtN101131 XittygpaPmboolIVUteber. PODDil3l EsP~~ A(abi~iArtyrn~forlh~ A.IAL'Yi1CAL MRTlM tim Y.ud]. Wad vOmr+lt Aeid A>inSoahr ?19 Cclart~iar ass .i . rrn ~ s~ .;ruiea a wl~ m. ~mowK ot tPOti bur tis OWL, h~a aa v~ ~") wiws a~e saare caw ttin~ ~ .ra .iae panuNaa) Sae1sA b7aMr Lym wlraro pmVm: DF-Aqer bywAmOw Ikrl .ok~ .ar diMrd, itx~awry, M1 Fm wmp6a MAW ne1h low+ra OoaMb oi8P0A pna io amctiax we dt bqow:4oqurre w calaWwr*wj wowm +.oovary . AKOyryClt~ " [IarEa~qi~iam~,l " mt)ftis~iisoee1~i .~ .x'~ aWbdtedhYu ~~a. tbr ua ~, wumar~.a..~ w m~ arFOw r~ mw~ ~o ari tMbN rFOA *r (vrb)- "-wIC "e4ft ($ A) ItA UK to domwly .yuniM 10 Mluaue di. reoea of PFaw rwna in ypu w.aoR+awdzbL rPOA ftwa drr) ty.dzM-rnoA %wa (ps) i Iiooao!. nul sokafKll MW 7.0 Paw 7f+of4.t Exygen Research Page 70 of 110 000229 Interim Report #23 - Analysis of Sediment SatrVles p. 207 Exygein Study No.: P@001 131 h- sxyyen rrolocol Nomber PmDOIU 31 AxUrecAl. ' ~iaim of . .~p~.~ 1Y --~rird6a ' LCrt~qfilS ]6"lir#rY6s6i7f1 raek MW (lFQA) ia soil Sy 9.0 ' Ssu6ndPwtr4" 9.! Slm6rd BbettPsniliradw tfolatioa . 9.1J RqMo;aloek roYwMef+lOD WmL of PPOA 6y wei6ltrsg 10 Mg of aaal~lipS q1611pd (eowsted 6 Pud4} rd d~lrk w 100 mL witk ' . 1rl~l in a 1Z5~sL LCI'H bE1110. ' '9.} :2' A N p61mL RnHionioa Oak" of TPOA b pro'sied Iy "ie6 11) . w{. of do lOD pOArL mltioa lo a ilaal vohxm of 100 whh mmh-i In a 12! oU.IAPE btlk. ' " 9.1 :] ` A 1 A yy'IaL 1'a46oaliataWWO6 Of MA it prop" 4y Wm=in6 1 J ' sL of fYe 10 pae,l. =IWtian a a 6a61 roJums of 19ID wiih mnhrnol n, a 127 af.1= ia61r. 9.1A AOQf K#imi.lbniuoariam nUpio6af ItOA ;pqwd by Mlnin Kw nl . of pa IA 1g%L qhRq1116 0OW vOfasfeof 100 with msilrnol la IMS mLLAFB YavIb. f-LS A 0.01 lyr.t.rufi6rases .6>tY6a of PFOU1 i6 p[e+panea by xin;oj 10 pL of Ss Ql p/lel. aolriio to a 6ail YOIVRIC Of 100 wiiS sr6anl in s127m1 LDPBlottb. 9.1.6 1Laa~OtfaA1EI1610aSb61Dk61661 Y6 p!a /101ad Y a IOf1ij01a9of it apympdanldr +'C w1 am wbh for a iantumun yaiod af 6 awntho . . ., tian 11w Eleoef pnpanwiaa 9Q lhd~id CYh~1oa isw6iar AL1 T:C4dWA e610sYion 6trrfa6 w pnpand in fiPi.C waw. Tlc - ' eai6"tioa rtadrdt w qx+owwd daoqs6 pr plnetian yeoeeA~re . man" 10 OMWIVL 93.t MW kib"bq is a VOW wa6qik addFtlarl oaiweuwion may be ~ed r oae" Rod p60MRapP rsa6xqm vow" of Cwowsnlqaaf atFti++ YIN= Va66odCwral oJllatia, toliiaa tnebl (kL}.' - famla (a) _ im~dad lasil" Calihncion sh~ID LaacamJ+W 0 6 +6 1" lar ~6 w M ~6 Is ` 400 ~0 16a . 166 a a1066 ~09 ao6 o ~6 0 Xiponddyy-0 :f xc=Nayy.1 So xr:.a,wMyy~: IN xtaa.aayy~~ z+o xclo,.d0yy3 a66 LM xxcctmim.arier~rac " Us euocY$ oo6osWionatAa atilr" 6f6aeffra is oqiw! so 6m !in Inifial . . oaaope4iY!be, Awlo rl0oasaaatratiaa of 6w m4adar0 Aud1K1FS ex,nciiar (BAE} . XC+oet0ara16 a6ltifoa anedrd. ~ . .y? , Pagr 26 oJ'OS Interim Report #23 -, Analysis of Sedimeot Sainples , . . p. 208 Exygen Study No:: P0001131 h T' Exygen Proax-al Nwaber. PM l l31 eqrpaamra r.+rrn,wwvoaol'" i 9,2 .3 A Sao araadrd OWN (nWll Mask) MoLb"MAM WO each nR af Raadsia aaoaoafd. 92.4 Ws dl ascrrr olihn6ool stand" In !!-mL polyyropyleue wbes vt]'C w BC, ;m lwo wwt:a. 9 .2.11 AWpWe vOh~ela d oopomhYiana of wradwda may 6o prsprcd u no" 10.6 H.W1$alUv ]ai - lecla ]s~ d ~ph sauad (h7KSllr m ~a) mw iocmae . lasl w scryan ar" a] iswltd tAaudc Win I m.L ormeYreoq am two ,vpm aenlroll "rY1bd at trm aeacwmaliwa pab aanaol spike) vc6lr paadinlnoovay kedeYWa. RU Rapiewmda Par add md Llonbey di0i0atn ad 40Mwill De ipoeiRed io IEuqoiq rrruplaa to dWnpnjaet. (1.9 SnsplaBdiY+aeeloa ' 1l .1' WIi01 ! g of iapb iaoa JO mI . pelyprapylr o~atihgr "a (krlilY u mafad,rtplwlidrmis w.r) . a 2' !la'M S alG m[awiawol aodiaka w a wlial wtnn dutas far-t! o~iuutsa I13 SYsmft !]rtnlw lo w ubwoaie bob said wuieala In -t! m. imes . . 1]A MM go ,o],mo, .p Is w ML r]ta wader io ds. so ML pulypoplMae awbUWa. ds ll .! Cmti6p for --IasierYWat-]DOOIp+L 11.6 ftL1fYou'Ib Cu 9PE eatRldgr (1 1. 6 mL) by Puafqg 10 e1L neqnol (utlcpW by 9 af. o(11= atr (- 2 dwylwo} Do aot Ml oolamn :nn dry IT.I lmwd (4roenq Ow mnwyle as dim eaadititwqd Cu SpE oneidyc . Uiaurd cAlas . 113 1!luln WA -$ ML !00% aallraol. Co11W S ML of dwte WO yaduulal 11 mLpo6yplrpllule eeaWilye Mw (lfaal volume - S ml.). 1J.9 . A=r~rer+wppbswiageMt .'urYgLCI1,t9IMS. 120 I3uomampr~v ' 12i 1~oit i~! ~a amwot uf sCl Aeda~ uw~ple aud lortiAed "np1! Ia10 Nee i.(yidBtd!' Mno A aaBElWon 111odrd meal proDade WA lbNow +ri 12.2 STi1d3u<d'umeNktbPLGAeoeIMPwftIe Y lutMn mri aeMMIMafoq 1Lveh awu~ 6u iar~~dd ia asaa]yYudrc W An rhr ad a! ariaelud wISEstiuw aaoi" awr 1~ ieAided u A* 6pbry ap K ft wa 0( a nullq aea 13ta<xd Rrdwda mm be lawnpaurlbuwue every $-1o rEpW. Am m allssaliv% r enr+e um at nrsarr Page 37 of 6} Exygen Research Page 68 of 110 000231 Interim Report #23 -Analysis of Sediment Sar4lcs~ ~ p. 209 Exygen Study-NU.i"PDi}01131 fi EuySen protppol Ntmlber. P00p1131 Bs"mtr.rr.A _ . _. _ . . . _- . - . . .AhALYI1CALM&TWD ~~Awa~u' 16r Bue Dawsioliw - , .. I,CIl1LSIMs 16"oiflr+rv0001+1! Acid"") in $Ail by ID 'Ibk wrllr~ i46s ~ykpl hr Ihs6sLAwrtd ~rdYOaw olycttwrssc++na ie mad by MO Pwimrme lxsfd Chambpaply osrpled to s uoppy Mug Syo~anaa+o DQeabr (1.C1WlIAIB)ie sa1 2.0 9 .1 AUq+*lrerslW IWwsmrypatoaK. T.I OnruM ~e ~qrop~qta AQp,7 L~Mi blWill(: WY eh~mlui forprppsr safaay pbCwMp1" 3 .9 S1ISple11,1qulmeeit` .'.: 3.1 ,At kw SS sollqtaYiyls fs sxpwfion. 3.2 Nos~rpl~pYSewilyir,sni~lpraHlamplq, 3.3 SooaYlw alwpl rbl,w34d *Add bs allowd to qui4lrsee to wom t~aaw . 3.1 All arnylM meet he Ibma%* mixed Y+o brry smpFed for taAeeGaw3.S SampL eolkGlat I uirp will he ~pxi5~d la the snlpliap pin !a W: pOwt ".0 'Asyaw riA 6ued~td~ ll mast-1!r(+DSNs 4.2 Msm" -IRLCg+ds 4.3 Aaaekp 11oeY-AC.1I. Ap/p Osls ".i lrrEyorwamaieAcid-SmunwAIbo4 !.s Lrnm .* will B"peami 5.1 A lwp fsnia- Ilquid ehronueoqih upsbk d pwnpip3 up l0 7 salsa qrippd wiW a wl" vokrols !owa cop" sP isjecupe. )-if* pL asreW tss rar Mom Qpseuamrola (LCAwS71d) . SP2 A O~rks oo_eotllp n new_ dIq Ow prtlelyapoaand Qurokdas . ar w"q to DAM S.4 SD~mVanhte wlyPssAylr ootrillqe n~n sa is ML mws.bb r.typr.vy..=,Wh,.we. 5.6 mlpoawa1ao-i1 1 (saluoot, loa2ao.t.). 5,7 125.m1.L1lPBames+meYt13SC6ee. 7-1 2aaLoksHAI~CrWYit. s-y Dl.pa.sbk pip3 .14 Ameaplowelve[1M100D pL rd 104OD pLy *ilb dirpordle dp. 5 .11 1Vnen 89 Pdc Va 6 as (IS) 1C1 " SP8 eqniidpn . 3 .12 S?E+nsmoilold . 5 .13 L1MrmielwA. nw2 er1 Pop 14 ofa! Exygeri Research Page 65 of 110 0002~32 hctcrem Report #23 - Analysis of Sedimicrat Saxlnples , . ., : Exygen Study No. : g0001131 Exygaa Protocol Nmaber: P4pOl131 e"Mnww ~~eeK.Mr vaoo1ni L_ ANALrMAl.AES7IOD ~d ~RAti~lIr~is iRAr tir dewe~ioodoa ofY.illriiaodroie Acid(MA) Soil by 0.14 WrJslon9ae i1w. 5.11 tweiawwH6b af mdpRipO JO aL polpPwpYwwrba d l000 wm. f.G ' Cbemmwviu irrra , 6.I F1 E.3 R.4 A+1lYea0 Cilms P4qph3w RT (Ysyrimo 5dm41kL 2.1e 150 mm. )a {MN: S2lOS4m30* Tmpmwr1c 30'C MObio nwr (A) : lAalelo 4hw (8) : (AMIN"rivamm 2mA1 AmmaJum Aawxla ww . Itfrhd Fbw are vIina ss ss n ss 0o33 25 7S 03 2Q0 23 7S 03 425 66 33 03 6 .6 Wwdmvalwne ts pl.tea heisarrad to umroR w SO pLy. 8 .7 QmdwOm AdcAaa-bcwul*edudcdilxa+namve . 6 .9 A1m1YeW +237doWAL r 7M dMro oo0iidaw We ln1F6d r l W66 apdmey be obwyid io order m ap"wOrrl!'1Cayner. '+.0 MMS Cvmm 7.l ~Wd` 8beftay~r NriYn'o MRM med~. woppotiq3 "13 ~ ]69 rw+: tor 1PCV- 71" WpmVpifditiw em UkOWdaa a mW& wd msy 6e clwyed in ordm to o~eln$o4~Wia vAo LO PrVessm of BONN= 9.1 ldul& Plow 0 .1 .1 2 p( rmawidro~ ~ is w .r b yvav~d br ~e ai74 s or r~urima aerr~ o iooo mL a~wa~a. TOWmmmwbspw@L r.niwr OINk Pop 23 qr65 Exygen Research Page 66 of 114 000233 kerim Report #23'- Analysis of Sediment 8arnples p. 211 Eacygen Study No.: PDO01131 B:ygen Proloaol Naalbw. P0001131 Aaft wr s..w wrr.iMrw vaon~ MFALlfTICAL i1al71bD ~'Tirady0TwIe . LCJMW>G Acid pronJ in w.v ry 112 f4t ~Plw fe~dbd wiA tew~ rtomb of TFOA pww a nineNm. air . Ihe 1blbriq~ ~ bf~llYW! I~a ~wllaeowry, ~r(KJ~ Ebdl :..a,+ .~cw~l - ~r.ma~~awn~l "` ~am+adu 0.1% Exygen Research r.,. +.rI rage u cpfas Page 63 of 110 000234 hiterim Report #23 - Analysis of Sediment S3mples Exygen Study No. : p0001131 sxyta, Prowcoi Number: roaol131 FIdW orAaay.h ar err seWriArM drrrarrwtuNk Add Err+oAl ft sNl by LC1MOd6 +w~~17~ ~~r ~rv~ ~ le7t 11ww~h Drivs Bobpollq.0 4A 16901 wPPCewd Dr- AL -k=~ L cnww ` TaIriW Lesds. LCdl8.8+W 0E"JB4 Drr 1ho 011- Exygen Research 7pqtt+Wc 7 Pace 23 qf6J Page 64 of 110 Interim Report #23,= Analysis of SedirirncrA'SatrnpTes p. 213 )Exygen Stddy No.: PDUU1131 .r"` ell $xygn Protocol Number, P0001131 B"SPOW4 _ u ., AT4WYTtCAL NRTNOD siAtalrUlflbaOfpYlfl~d00Cf u.e.ero.~..vooeizro Aoid(PFOA)uWaurby 9.23 l.2A A2S I A Now uauAM aolwioa (myna bkpt} n=pLZMMO wMh each M a(aa,drda adma1i Slam ata aCec110 pibfetioa raodlrde iu Me1l. pDlypmqylne tubes a1 Ylao 6"C, aylalw w*aba. AYwyft wlmea re aaoanstrmoba of aurdrdt may be pnpaal as J010" 10.0 Baa38atL* iQl 'U& brA b1 rpolwro~are4d (hpiaJy 20 a iew) " inc" ai Iwac min aeapM ee~et (wtllD/ blank wft FPLC water) and two mymi 40Rtrdr QOINfiae " boo" CaGOe~oa1 {hb cwwRl =pib01 to senlr pcoadral "aewry fanbabnsb. 102 , ior Sdi ad Lio+atvy inpiiais ud epiUea wiII b. spaei6M " ' In ,bayaal6yassoan.plmfm,bbpwjacl. 1t .4 l~pla8itqpi7il t1 .1 1f~weo p mf. alwaple ar a pbrtier efs~yla iAnae ro 4D s! witk wum !me 90 mL palypapyhn awaiAye awbw (hr* r maaar, nplYes be and wix wN} III Canada Yu elm 9eB eKVidOea (2 y, 6 m[.) by paashig iR inl . n~aAanoi Jb8aw.diy! as. .rluLC .aw(-s ' vw1 wc~ vo aw It aoGsaa rwi aq Ila tara wmpla oa eonAtiaa4a e aee etbidV. nl.esd .lur.. . .ttw ehrrWVh -s ML 109% mdrnoL L1aAact s ML of aiura We yaanauec " u.aa.pobprapylwa o~uailfa0 . Mba (ead ronuoa-s ut .) . 113 ArlyssaceplasmiqdettaepVLCIbMAiS 1:.o civemalov4phl7, - -- 121 hod do arsmsoamt ofwh arniard, wnp7e ssd feefEed uimp)ciMo cbe LCA&118 ayalea A oibntisn Randad rnuat pncaee wA bllw W -dyad aAla 122 91miewdaof ('PdA daerrpaadlo6lb r lnat f" er mom nmieannason b+reis sst be mob" In an RNOPbwd ML 1t.7 Aa vaoro, ad ae aYaAad eablration am"* most be iaebmdN n ibe bqimiq and at 16o and of r aaniplo aa . 1shrAwl euneni. oww he iolnIpanal twa+w mmy !4tl ao41aa. As d altauaqivs, n atin ra of ataeW aal- erim "mdude tny be ir0eae6 ae dn bejiaain4 of a sei lbW/rW by allaelW =000den plbYdl bpala/MYa1/ "OU 3-t4 amlplCs , (lp atww'1 kr ~.@wrai re of otaaand aueerdq. In either come . "uactod OyLrWq fYaAaads mirlba ibe AM sit LM ilioetiaa in ataipkael. 12.6 l1w Saw e6aeard anna hr raanUYlfGa Utter viadftd owes at yeasa~i forltv rut~uby 16uafwjfaaliall Wag 1AC rdflde/ o(Pe+b aen P.r f of , Page 20 of 65 _p. 214 Interim Report #23 - Analysis of 5edirneat Samples , Exygen Study NQ. : POpd1131 r Exypa Piotocol Numbar : PODD1131 ssvMnwwree 16ntrt! aAMNIlM D.-*A tw,eseNinraer veeevp AN-A~ ltCALt1ZTdDD dlerlaoboAenole Add (1POA) in Waterby i,pY911t6 w1ir allbmiee onduld aoeea aYr~en e6iaiLlart .yex 1.3 (oreqeirakr) IO*IVrNl3rla I2 .S ?Ymple wqao rhuY r1 aoosod slradait: nriaowe Any eml9ls that, e~owd ahr~el+wPolwe s~wt! he frrasor fiiiwol d ra~Wyred 13.0 AioeilpfseeGtiSerla 13.1 QeorprpEre mw Ynr a prh oft ArqLev iara at 3"9 me Mn a pucni 0(413 aw . S1u 413 aiwr pnM carta~nde to Our P!'OA eefoe. xbik On "wllear ion (3 mir) re5r+eru d61aw efaa,bo divsi0e. 33.2 IGNiod With MW rot ceedia t'Fpw at le,el. psow ilm the lAQ. IF a liI* oorddwF PPOA r Lrda ~s " r tWe !0 sqL, dust a arts bknk wnpk 20111111 hsebuird ad Yhe wiln,et sa~~u ye n,a,lesered. 13.1 Raw""of Is" epitw rd =Wk ;it6eprop he 6nwese 7lF 130% of *air bnra r61wb re Oenkul spasm TaUe aqi& ihr sowyl "ble 1'riq. on eatiw w1 or eoeple dierM be w-atncle6. My mnntis spite out" M 134% eheehl b mlwmd by do sr13s1 to dolamiee if we:Yadian is 13.4 Aay oNibnlloe OnOlli kind r6 be a stnlnkal oseMw by ad" che Ylute ]rnor Tell, My le 6ordedW km d~ r111kuteuon of but cNibnasa curve. 1owsar, IM aut aiebtr Of rctneotd pflbniae shndrd6 +Iw wuld be accyded omR ml eseesd 70% of so Ow ~r1er of estracied crsnAarda 13.5 7he eredYka oes0deti (R) hr eelhorstloa eewa paeraled mw be 205" (11' lra9tsj it .h'1ssaae Milts rall nA+ide rrcae Will. the. sppnp;r . ae" mw 6e Lt.r i. Was ir.vuemi olaveiUM, apo tK 6laaiw~r a Iwe idwe~ ro~er~5w .lw~ld b. nw1~ 1IA flelelfiall Uele1 Wwem YrAnda Md fefplee MUM ea 4A11 more than #A%w101se6mIpIeYm IfrasaftlmtliwdiR6ree6de0ikliaritvrlrAie ao Iwlydr"1 wotlan lbawt merUa , eenebbd. 149 C1loulrxias !al We IYe follori0 e~pelkra a eYwlne Oe rnort af P'PQA founA (ia ngft. Yeesil w Ppt eml oft fm elddnd OM (liaar roWe+siaa PMcnans) gaernle3lyle Mw LM soRven posaro: ?FflAhold (qil .) " tjrdmiss.iedoc+t5 x OP An" DP - how by w1de1, do Awl roAwr who uYwd. if aeaweqr. 1011060" /'4. Par n ofOS Interim Report #23 - Analysis of Sediment Samples p. 215 Exygeri Study No.: P0001131 Exysen Protocol Number: P0001111 _!wr .~...~'+ ` ' ' ' n"rw H""~ "~~7+~ A4ni.Yncu. Aa'rsroa . ~p ir tpr .~n ' - el)sllMoool=io Naid (PFOn? In WruT ey LCIMWNs als srawwwar+i:w,t~L ~ s.l~ c~ ~~roi.or~iraiy so ea. vrbwwyt~ wws s ~ooa ~ . "0 Cw"1dftwwFM1 pot" 6.1 MrbdeN o&-& Tlwylwe RP f16crsm BoivwMe~ 2.1 mm a mw sr e.x T(o"w41pS..2r".5m-3wrncO, 6.3 .- llabiWplrw{A} : 2 s1I Abeeetra Avievais Water O.i lWbilaflpw13;1 : 3*ft" O.S ~ fseQre: rX0a6ql flA O.p sf 1 .0 0 s.~ 2s 70.0 2S 22.3 65 Plrw xYp 7LA smUMd Is 0.3 3S 0.3 7s 0.3 7b 0.3 3S Q3 64 ryeodoo Vohowe 15 pL (e~ Maater~t b r aueA ~ SO pL), f,7 QurpM0im Peak Am -~lmdAWdEledihnKosnere. 42 . Rue I1mW. " 23 mfuMn. ' TIN ibpY6wqdL1W41RVmEppdW r rr Mad Si nay Draehm/W in oFdw ID 7.4 My11! 9rhon 7.1 hbdi: " SIxuaPb7Nrl~~ b(RM mO6R 010Gimfiqiq l ~ 369 Mi. The m*Vt. bOC'YHOY an IRIIII/Od Y a 1pide and may 4e eh+e{d fn order to ~deiaw qrc 1d.i>~S syowen. 8.0 1"wlwdm otiolutfaor 1.~ Mol~i ~Lw LLl 2 EM aooimudre aauts !o wrler is prapiusd by rddirpl 0. 134 191 . .m,.a .err. b 1000=L .r .nea. ~s...~~ma...rLa rKwreO rw. ~W': /'1 Post /a of 65 Exygen Research Page 59 of 110 000238 Interim Repart #23 - .Analysis of Sedim,e.n,t.Samp)es:. `,p. -21.. .6_. Exygen Study No . : POOOI 131 h 8xyseq Pratocd Number. A0001131 1.r,wal.wr1 IIti1.d r4rw wdonU At1AlY17CA1.A1S7NW _ ' 1ldk~d ntAa~i 'Iha ~ Aoid (PPDA) i, Waxr by ,l.0 sordrdT]qraallm t.i %lWW lleaklJwB4iadn 13iAl' oa l.1.1 -?WPM a aledc adktfida ot-1001pynaL Yf PYQA bY wvitbft 10 09 adrdyOeal aYiaiut (aonaaal br yurity} and dlrle lo l00 mL wilb wAdmolba 1]l-=L LDPB bdnb, - l.12 A 10 paiwl .lknif4" aelo`as of f4'OA !a yaeioad by brinpai lU uL o(1r 100 ypLl.wha6m to a lul rakqee of 100 rit4 meMeni .;~ ~iqil26fN.IO_TBkOsY._ _ . 103 od. of~ ~ to a SaY "Nwra of~with~medwniin il IZ! dl. ti7!! bWRb. . l.1 .4 A0.1 ~weL.lbidlhrke aoOWae allFQA is prparrd by liridyaii 10 . a9i. dtYa 1.0 M,~+atl.~ lo t "W voL~a of 106" mumm in R t33 Al. LiDl'BUolllo. 9.13 A 0.011ayr1. thBiSeNioa ao]ulan of PlDA in rreprw! try 6rin jsy ]0, ML of pia 11.1 Nyhd. aolulp+i 1o a Cuua vokirm of 100 with erdrd ha 126 r$. LDlrB besie . 9.:.6 TM SO*at lenilleadoaisluetoar sw op bt akrW iw arel4i=ernor d ypeeaisdaly4*C atd ara atWU for "mlximmu parmd of d awr.tks tanie db elpaymam. 4.Z 3ardriC.+~adrlal~riaas 9.2.1 LCAMtUM1 alkweim WndrL vin P4pwW In 11r1.C wrer. 'la aWaYai SWAMia in Rnaa~wd Adono qe aocpaotion PMCWure . i ", 'eMPEIPUL 9,L2 T, he lolmwios in a OVW aaaupb: addOhpd eoeaqroanon my be PPpwd asnWad. Find CaaeuMIkW2 .lwNlo9a Yelwuf dMDOa"iarf 4. 166++i aCAwdEatiaa llaiaae Yrieiild Ctiuud 6aLaieeiass~,~, tyLl EaawNdNJ Gh'htiiaa lmdwd 1D lrertalel 9 ~ w a XQawddyy~0- io . . lw .o u xo~+a~r .~ ilo0 :40a0 r4o0 l!ooo XXAcamn.w+fbtyraa mb loo a no xc>vardria t~ soe 40 lor ' 410 ro wo low xxCrxmvaWrWr4rY-.s6 Tlaatrneui eaoewYYis ofOrnlhntia SWAM i2 ftiul U SK aa iaidat aaaaipief~ Cee On aaoparrice eftV mundwd dmie0 tlr pctracaon (S?E~ adarasch AMdIML hae a d' Pop 19 of 65 Exygen Research Page 60 of 110 000239 Interim Report #23~- Analysis of Sediment Samples Exygen Study No. : P0001131 Exypo Y7oloeal Nomber. P0001131 AXALY77CAL METHOD M1"OdNMY1rs VO617ip H"oddMdPw lYw am liwwwl~llw eflraw"ceeek AtJd pPOA1 d Water ` , b LCIIMbIms AWyuW Twtioj?rOW Pspw SOSI AaurrL A[" Stab Conrp. !A 16M Appwed 87: Pwiddaelyr . ; Tecbikalla0yti ILGl13. BiMM ROiaMh . ~er . Exygen Research Terd Fyrc 7 Ptega 16 nJE5 Page 57 of 110 000240 1nteriwReport #23 -Analysis ofSedimen,t 5avpIes : :, p. 218 : ; Eacygen Study No.: P0001131 Tvcyyee Protocd Number: POOaI 13 1 e~aluww UAW *.rrvaaaw NaALV~ncu .usrnoa LtaShoAof Anlypa Ibrlao1: dPIrADanxuqieAed(PFOA) ia Wrv by LD Seepa ma somai ia as In w141 )ri1 for So irohtiaa Ed oa+amioe of prllumooelaoofe Ow by S4b lUJImmerw UqrW Chaw"Oym10' o0upw to a andem me" s/OCNpweLi0DoiK'b: (LCAumJ lil rallf. 2 .0 1lafaly i.3 47rvtyaallafY1n111~6Wa1Mypeaaien. 23 ~`aon[31 ~r a3peonirs 10DS bHC1r 8Yd1rL a><Y elwnleal mr p~opar ulhy 34 SWO RaluharW 3.1 At Irnt OeLorerl aaleIIt iraaaelioas 33 ft taaflflsprooua" is Avow foriraer aaolplr . 3,7 Sa" !ko do" wliiypab0 ihowli be allowcd m a4ui1i6rmc w Pam 3A .:L samplo aemt 6e IfioroqMymbW 0ab~s beiuS w+plad forexuoeilon . 33 Asy trlplm mompleig 1rWes cAonld be aeplrlNllod ei -3DOD 1pm Ix -S IofwOa wd to aalimmlot end foctlr mmtnotim. 3j6 Sat/la oefLoiaw pumilwas +M be apaei8d in Me plan for Lka (>tiJ~ 4-5 MOSEL Ed &22&k 001, 4.1 Wdw- "PLC Old* 49 iilaeltwel-I1pLC ra6 s.3 A~AalYa-&C.S.YAASI "tQtW 4.4 TarlhmporAaaioAmid -SSgmrAldriol S.D 111167ra1p1m4LqWpmod f.1 A il# illrb~ WaY dhpmkopol1 Wwb1a of PrmphW W to I aatvon aQuippd rMS a wdYY vNma wpm mpaY]o of injanina s-IOo pL Oa1~a0pd 10 iladl<H~12~a~a~a ti.ClAfN1dS}. S.2 . Aimce ro oolhd an' AW frPaY *rteyaWn+nd qaWSUe=. S.Y Aralylier 1wImeanpalla of=oftg Is 8.G0001 g b.4 -30U1 diaDao"4a17oPfmaraRqhDeabaa s.7 ls aot6iW.wYirpelylpPyINS olsol6ya OWL S.b uqaoa4xwlaop}eu(3aoonLtoD4oonL). SPY s.s :1w2rs.aCohLwwiFreLaCa+ewlo.1idvta. aleloma.. DAbapemnbllj OaP(END,DOw.a .o 10-w004 rwaetapoaarl.bw. 5.11 Watnsap h41he i ao pl) ICSI3T8 arti{pa yyr1I7 I^" Pap17 oJ65 Exygen Research Page 58 of 110 O. 00241 Interim Report #23 -~ Analysis of Sedimt;nt Samples Exygen Study No. : P0001131 Exygea Pcolocoi Number : P0001 131 " fla W oftim dOC1AAt"JlIatl,on Ilw Jollovill7~ ~51l41btS win be included in each analytical set a nm iheet listing tlte samples tobe riua in the set, and an itut:untrrtt conditiotn aheet desc'bing the xtstrttrnaatt type and operating Catditiotss., ' . QUALIZY ASSUBANCE , '1'be QA Unit of Exygeo Rwean;h a!ill' i"ect iha attdy at intervals adequate to no= cotnpHanco witli Gi.F'a, and .wn'Il repot~the fttWiqp of audits to the $tudyDfrector, Bxygsa Matngaueut, land the Sponsor R. epresentative RETF.N'I7UN OF DATA AND ARCHIVING AA hard copy taw dw, iwhtding, but not linuted to, tht original ebroenatograms. waddhtxts, carespoadatce, and results shall be included with the dab Package submitted to the Study Director.TLese will be archived with the oriPW gladly plan, rtaaedanenta, final report, and ail pertinent inforanation itom dw Sponsor The testing fact-lity shall keep all electronic raw data and any iaatruuteru, equiptnent, and tdorage 792.195, An exact r.opy loofgat'hefomrattehreialpseraiuobdmiotfietdimteo 'specified the study in 40 CFR direetor will also be kept at Exygett Rtradiriat. Sxygcn will obtain peanisaiaat frrnn the study director belbrt discarding or manning samPlea- . .. , Exygen Research Pagt If of63 Page 55 of 11 Q 000242 Interim Report.#23 - Analysis of Sediment Samples , Exygen Study No.: P0001131 8xygan Pmsocol Nwuber: POOOl 131 0-- APPENDIX I ANALYTICAL METHODS V0001780: V0001781 : VOOOt78Z : V0001783 : VOO01784 ; VOOOt985 : V0001786: "Mathod of Andyais for the Determination of PeMuorooctawic Acid (PFOA) in Wow by LCIMSIMS" "Method of Analbeid for 11w Delarmineaion of Perfluorooatanoic Acid (PFOA) in So~ by i.Cl1RSIM5" "Method of Analyns for the Determination of Porfluorooctanoic Acid (P'FOA) in Sediauru by l.CMSJb1S" "Method of Anaiyaic for the Determination of Perfluorooctanoic Acid (PFOA) in Fish and Cl"m by LCMSIMS" "Method of Aaolym for ft beiermiaation of Perfluarooctanoic Acid (PFOA) in Vegetation by LCUS&W' **Method of Analyait for the Ihlomiastion of Perfluorooctanoie Acid (PPOA) in Small Mammal Liver by LC/MS/Mr "Method of Analysis for the Determiairion of Perfluorooctanoic Acid (PPOA) in Small Mamaul Sam by LGMSIMS"" I--- Exygen Research Par is oJ6S Page 56 of 110 000243