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P. 1 INTERIM REPORT # 23 - Aua . b of Spdimet Samnlaa STUDY TITLE Analysis of Parfluorotautanesulfonate (PFBS), Perfluorohexariesuifonate (PFHS), and Pexfluorooctanesulfonate (PFOS) in Water, Soil. Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Senun Using LC/MSIMS for the. 3M Decatur Monitoring Program DATA REOUIREMENTS EPA TSCA Good Laboratory Practice Standards 40 CFR 792 SnMY DIRECT Jaisimha Kesari P.E., DEE Weston Solutions, Inc. 1400 Weston Way West Chester, PA 19384 Phone: 614-701-376 1 IIYTERIM REPORT_!COMPLrnON DATE May 2, 2006 rERFURMIN G LA,,~_RAT4RY Exygen Rrm rch 3058 Research Drive State College, PA 1680 1 Phone: 914-272-1039 STUDY SPONSQR 3M Company 3M Building 0236-01-B-1{} Sl. Paal, MN 55144 Phone: 651733-6374 Protocol Number : P40t?1131 Exygen Study Number: P0041131 Total Pages: I 10 . p. 2 Interim Report #23 - Analysis of Sedimeni Samples Exygen Study No. : PC?00113 1 GOOD I.AB99ATOR-Y PRACTICE CCMPLIAN CE STATEMENT Exygen Study Number P0001131, entitled "Analysis of Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonste (ffHSj and PexfluozooEtanestttlfonate (PFOS) in Water, Soil, Sedimept, Fish, : Clams, Vegetation, Spa1tMamm*.. Liver and Small lbtamma! Serum Using -LC/MS/MS for the -..3IvE , .latqr . lwioniioring, Program," Program," conducted for 3M Corppan:y; is being pqrfius~ ia;conRpdiance with. EPA TSCA Good Laboratory Practice Standards 40. CFR 792 by Exygea Research, with one exception . The laboratory control and control spikes for the direct injection method were not recorded promptly at the time of extraction. .< , . . .. , - " ._ . . ' j, . " . .. Flaherty Princi* Investigator Exygen Research Date Jaisimha P .R., DEE Study Director Weston Solutions, Inc . /~~ ~ +S/I('/ ~ 641 Michael . Santoro Sponsor e1pmentative 3M Com any Date Fa:ygen Research Page 2 of 114 p. 3 I~tercm Report #23 - Analysis of Sediment Samples Exygen Study No . : Pfl41131 9UALrrY' ASMArtCE. SUMMTI Exygen Research's Quality Assurance Unit reviewed Exygtri Scizdy Number P(?001131, entitled, "Analysis of Perfluorobutanesulfonate (PFBS), Perfluorohexactesulfonate (PFHS), and Perftuorooctanestttfonate (PFQS) in Water, Soil, Sediment, Fish, Clarns, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MSIMS for the 3M Decatur Monitoring Program" . A1I'reviewed pitasesr 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 Analytiml Report Review Date Reported to Date Reported t o Date Principal Exygen Date Reported to bum Inve.s'tig~ j+~anam1 Study Diz= 0 5102106 45I02J06 05/02/06 05/02106 L ' Air T 'cal LeaA Quality urance Unit 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 ,statement involves only the review of the interim report and associated raw data . Exygen Research Page 3 of 110 p. 4 Interim Report #23. - Analysis of Sediment Sarnple4, Exygen Study No .: P0001131 CER MCAT1C}N QFA "fHENZTCITY This interim- report, for ExygelZ- Study Number PQ001131, is a true and complete representation of the raw data. Submitted by: Exygen Research 305$ Research Drive State College, PA 168 01 (814) 272-1039 Principal Investigator, Exygen: ohn Flaherty Vice President ; Eacygen Research Date Exygen Research Facility Management : Ric A . Presiaent Exygcsr R Date. Study Director, ton Solutions, Inc . Jaisimha KesAlFf., DE Date Weston Solutions, Inc . Sponsor Representative, 3M Company: Michael Santoro TI Date Director Regulatory Affairs Eacygen Research Page 4 of 110 p. 5 Interim Report #23 -Analysis of Sediment Samglcs Exygtrs Study No.: POQO1131 STYJDY: MEN'TMATIUN Analysis of Perf luorobutanesulfouate (PFBS), Pcrfluorohexanesul#bnate (PFHS), and Perftuorooctanesutfonate (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 PROTOCOL NUMBER: P0001 131 EXYGEN STUDY NUMBER: P0001131 TYPE OF STUDY : Residue SAMPLE MATRIX : Sediment TEST SUBSTANCE : Perfluoiobutanesulfonate (PFBS), Perfluurohexanesulfonate (PFHS), and Perfluorooctan,esulfonate (PFOS ) SPONSOR : 3M Company 3M Building 0236-01-B-10 St. Paul ; MN 55144 STUDY DIRECTOR: Jaisimha Kesari P .E., DEE Weston Solutions, Inc . 1400 Weston Way West Chester, PA 19380 STUDY MONITOR: Michael-A. Saiatoro 3M Company 3M Building 0236-01-B-10 St . Paul, MN 55144 PERFORMING LABORATORY : Exygen Research 3058 Research Drive State College, PA 1680 1 ANALYTICAL PHASE Study Initiation Date : 11105/04 TIMETABLE : Interim Analytical Start Date : 04/27/06 Interim Analytical ''feriaination'Date: 04130/06 Interim Report'-Completion Date : 05/02 1+06 Exygen Research Pap 5 of 110 p. 6 Interim Report #23 - Analysis of Sediment Sampte,g. . Eaygen Study No .: POOb 1131 PROJECT PLF.SEIME L The Study Director for,this project is Ja:simha Kesari at Weston Solutions, Inc . The following personnel from Exygen Research were associated with various phases of this interim portion of the study: Name Title John Fiaherty, . Vice President Karen Risba Scientist Paul Co;rnolly Technical Lead-I,CJMS Christine Edwards Toolmician Mark Ammerman Sample Custodian Amy Sheehan Associate Scientist Brittany Kravets . Technician ScottGrain Technician Frances Crespi Technicia nnDevob3grwTchia Christa Gallant Technician Exygen Research Page 6 of 110 p. 7 Interim Report #23 - Analysis of Sediment Samples Exygeis Study No. : P0001131 T6F CONTENTS Pase- TITLE PAG_E .............. ............................ .......................... .... ......................... ............ ........1 GOOD LABORATORY PRACTICE-COMPLIANCE STATE1biENT . . . . . . . . .. . ... . . . . . . . . . . . .. . ..2 QUALITY ASSURANCE STATEMENT . . . . .. . . . . . . . . . . . . . . . : . . . : . . . . . . ... . .. . . . . . . . . . .. . . . . . . . . . . . . . . . . .. . . .. . .3 CERTIFICATION OF AUTHENTICITY . . . . .. . . . . . . . . .. . .. . . . . . . . . . . . . . . . ... . . . . . . . .. . . .. . . . . . . . . :. . .. . .. . . . . . .4 STUDY IDENTIFICATION . . . . . . . .. . . . . . . . . . . . . . . . . ... . . . . . . . .. . . .. . . . . . . . . . . . .. . .. . . . . . . . . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . .5 PROJECT PERSONNEL. . .. . . . . . . . . . . . . . . . . .. . .. . . . . . . . . . . .. . . .. . . . . . . . . .. . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6 TABLE OF CONTENTS . . .. . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . .. . . .. . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7 LIST OF TABLES . . . . .. . . . . . . .. . . . . . . . .. . . . . . . . . . . . .. . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . .. . .. . . . . . .. . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . .8 LIST OF FIGURES . . . . .. . . . . . . . . . . . ... .. . . .. . . . . ... . . . .. . . . . . . . . . . . .. . .. .. . . .. . . . . . . . . . .. . .. . . .. . . .. . . . . . .. . . . . . . . . . . . . . . . . .. . . . 9 LIST OF APPENDICES . . . .. . .. . . . . .. . . . . . .. . . .. ... . .. . . . . .. . .. . . . . .. . . . . . . .. . . . . . . .. . . . . . . . . . . . . . . . . . . . .. . . .. . .. . . . .10 1 .0 SIJMMARY . . . . . ... . . . . . . . .. . . . . . . . . . . . .. . . . .. . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . .. . . ... . . . .. . . . .. . . . . . . .. . . . . . . . .. . . . .11 2 .0 OBJECTIVE .. .. . . . . . . . .. . .. . . . . .. . . . . . . . . . . . . . . . . ... . . . . . . . .. . .. . . . . .. . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . .. . . .. . . . . . . . . . .11 3 .0 INTRODUCTION . . . . . . .. . .. . . . . . . . . . .. . . . . . . . . . . . .. . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ... . . . . . . . . . . . . . .11 4.0 ANALYTICAL TEST SAMPLES . . . . . . . . . . . . . .. . . . .. . . . . . . . . . .. . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . .12 5.0 REFERENCE MATERIAL ... . . . . . . . . . . .. . . .. ... . . . . . . . . . . . . . . . . . . . . . . . . .. . ... . . . . .. . . ... . . . . . . . . . . . . . . . ... . . . . . . .12 6 .0 DESCRIPTION OF ANALYTICAL ME'THOD .. . . . . . . . . . . . . . . . .. . . . . . . .. . ... . . . . . . .. .. . . . . . . .. . .. . .. .1 3 6 .1 . Extraction Procedure For Sediment . ... . . . . .. . . . . ... . . . . . . . . . . . . . . . . . . .. . . . . . . . . .. . . . . . . .. . . . . . . . . . . . . . . . . . .13 6 .2 Direct Inject Extraction Procedure For Sedimont . . . . . . . . . . . . . . . . . . . . . .. . . ... . . . . . .. . . . . . . . . ... . . . . . . .14 6.3 Perccnt Solids Procadwe For Sediment . . .. . . . . .. . . .. . . . . . . . .. . . :. . . . . . . . . . . . . .. . . . . . . . . . . . . . .. . . . . . .. . . . .I4 6 .4 Preparation of Standards and Fortification Solutions .. .. ... . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .14 6 .5 Chromatography . . . . . . . . . ... . . . . . . . . . . . . . . .. . . . . . . . . . . . . . .. . : . . . . . . . . . .. . :. . . . . . .. . . .. . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . .15 6 .6 Instntment Sensitivity . ... . . . .. . . . . . . . . .. . .. . . . ... . . . . .. . . .. . . . . . . . . . . . . . . . . .. . . . . . . . . . .. . . .. . . . . .. . . . . . . . .. . . . . . . .15 6 .7 Description of LC/`42S/MS Instrument and Operating Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . .15 6 .8 Quantitation and Example Calculations . . . . .. . . .. . . . . . . . .. . . . . . . . . ... . . . . . . . . . . . . . . . . .. . . . . . . . . . . . ... . . . . .1 6 7.0 EXPERIMENTAL-DESIGN . . .. . . . .. . . . . . . . .. . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . .. . . . . . . . . . . . . . . . . . . . .. . . . . . . . .20 8 .0 RESULTS . . . . . . . .. . .. . . . . . . .. . .. . ... . ... . .. . . . ... . . . . .. . . . . . . . . . . . .. . . . . . . . .. . . . . . . .. . .. . . . . . . . . . .. . . .. . . . . . .. . . . . . . . . . . . . . . .20 9.0 CONCLUSIONS . ... . . . . . . . .. . . . . . .. . . . . . .. . . .. . . ... . . . . . . . .. . . . .. . . . . . . .. . . . . . .. . . . . . . .. . .. . . . . . .. . . .. . . . . . . . . . . . . . . .20 10.0 RETENTION OF DATA AND SAMPLES ... .... ...... .... ........... ... ............... .... .. .... .. ... 2 1 Exygen Research Page 7 of 110 p. 8 Interim Report #!23 - Analysis of Sediment Samples fizygen Study No .: P4001 133 LIST OF TABLES Pae Table I . Summary of PFBS, P511S ,and PPCaS n.i Sedimeat-Samples........... ................23 Table II. Summary of PFflS in Direct In'edtion Sedi.."nent Samples ..... .... ......... .......... 24 Table M. Mafriic Spike Recovery ofPFBS,'PFHS and PFOS in Sediment Samples .....25 Table IV.' Matrix Spike R.ecovery ofPFOS in Direct Injoction Sediment Samples .. .....26 Table V.. Total P=ent Solids in Sediment Samples .... .... ... ........................... ....... ...27 ,~,_ . . . Exygea Research Page 8 of 1 l0 p. 9 Interim Report #23 - Analysis of Sediment ,Samples Exygeri Study No.: PW1 131 LIST OF FIGURES pan Figure 1 . Typical Calibration Ct rvc for PFBS in Methanol ............................ ... ...... .....29 Figure 2. Non-Extracted Standards of PFBS i h Me~l, 4.2.bglmL and . 0.5 nghnL, Respectively . . . . . .. . .. . . . . . . . .. . ., . . .. .. .. . . . . . .. . . .. . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . .30 Figure 3 . PFBS in Reagent Blank, Q.4. ng/mI. Fortified Reagent Spk A, and 4.0 ng/mL Fortified Reagent Spk B, Respectively . .. . . .. . . . . . . . . . . . .. . . . . . . . . . . . . . .. . . .. . .31 Figure 4 . Chromatogram Representing a Sediment Sample 1RnglyZerl for PFBS (Exygen ID : C0172892, Data Set: 042 606F) . . . . . . . . ... . . . . . . . .. .. . ... . . . . . .. . . . . . .. ... . . . . . . .32 Figure 5. Typical Calibration Curve for PFHS in Meihanol ...... ... ... .... . .... .. ........ . ......... .33 Figure 6. Non-Extracted Standards of PFHS in Methanol, 0.2 ngftL and 0.5 iiglniL, Respectively ........................ I. ........... ....... ............ .......... . ... . ......... . 34 Figure 7. PFHS in Reagent Blank, 0 .4 ng tntI.. Fortified Reagent Spk A. and 4.0 nglnal., Fortified Reagent Spk B, Respectively .. . ... . . .. . .. . . . . . .. . . .. . . . ... . . . . . . . . . . .35 Figure 8. Cbromatogram Representing a Sediment Sample Analyzed for PFH S {Exyger 1D: 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 ngf mL and 0.5 ng/mL, Respectively .,........................... ................. ............... ... ................ 38 Figure 11 . PFOS in Reagent Blank, 0.4 nghnL Fortified Reagent Spk A, and 4.0 nglnlI, Fortified Reagent Spk B, Respectively ......................... .......... .. ....39 Figure 12 . Chromatogram Representing a Sediment Sa mple Analyzed for PFOS (Exysen ED: CO 172892 . Data Sec:o42806B) ..... ...... ............................. .. . .......40 Exygen Research Page 9 of 110 P. 10 Interim Repvrt #23 - Anslysis of Sediment Samples }rxygen Study No .: P0001131 LIST OF APPENDICES ~ Appendix A Study Protocol FOOOl,131 (Exygeix ,Study No . P0001131 ) with AnalyticallViethod'Vt1001 78:2: "Method of Analysis for the DetcnMinatioti :of Partluorooctanoic Acid (PFOA) in Sediment by I,C1MgIMS", and Prvtocol Amendments .. . . . . . . .. . . . 41 Exygen Research page 10 of 110 p .11 Interim Report #23 -Analysis of Sediment Samples ExygCn SiUdy No . : PQt1t} 1131 14 sum~~Y Exygen Research extracted and analyzed sediment samples for the determination of perfluorobutanesulfonate (PFBS~), p~uox?cthexaaaesu2fooatc . (PFEIS), and perfluorooctanesulfonate, (PFOS) ac~:otc~i3ig, to Zxygefl Nte'thod V 00017 92 (Appendix A) . The limit of quantitation for PFBS snd PFHS in sediment was 0 .2 ng/g. The limit of quantitation for PFOS in sediment was 2.0 ng/g . 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 . Aaatytical 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 H. The average percent recoveries standard deviations for PFBS, PFHS, PFOS in sediment samples were 85 19!e, 99 t 29i, and 93 654, respectively. Fortification recoveries for the analysis of PFBS . PFHS, and PFOS in sediment samples extracted with the original method are summarized in Table M . 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 Y. 2.0 OBJECTIVE The objective of the analytical part of this study was to determine levels of perfluorobutanesulfonate (PFBS), perfluomhexanesulfonate (PFHS), and perfluorooctaraesulfonate (PFOS) in sediment according to Protocol P0001131 (Appendix A). 3.0 nv~OnuMoN This report details the results of the analysis for the determination of PFBS, PFHS, and PFOS in sediment using the analytical methods entitled, "VU001782: Method of Analysis for the Determination of Perfluorooctanoic Acid (PFC?A) in Sediment by LGMS/ivIS ." 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, 2Q06 . Exygen Research Page 1 1 of 110 p . 12 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0001131 4.0 ANALYMCAL TEST SAMPLES Three sediment samples (Exygen ID : C0172892-C0172894) were received on wet ice on April 22, 2006 from Tim Frinak at Weston Solutions, Inc. The samples were logged in by Exygen personnel and placed in rcfrigerated 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 Bxygen Reseerch. 5.0 REFERENCE MATTItIAL 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 Exygm on January, 20, 2003 . PFOS was purchased from Fluka Corporation and was received at Exygen on April, 23, 2003 . The available infonnation for the reference materials is listed below . PFBS and PFHS were stored frozen and PFOS was stored refrigerated. Compound E, M en Inventory No . j~i .9 Purity ffo) Expiration 20 PFBS SF0005726 101 95.7. 12l04106 PFHS SPOO02401 SE036 99.6 1 0/18/06 PFOS SP0002694 430180-1 101 .2 10r31/07 ,The molecular strictures of PFBS, PFHS and PFOS are given below : PI~'BS Chemical Name: Perlluotobutancsulfozate Molecular Weight : 338 supplied as the potassium salt (CaFgS43V) Transitions Monitored : 299 ;-+ 9 9 Structure : F F F 03 E' . F F PFUS Chemical Name: Pertluorohexanesulfonat c Molecular Weight: 438 supplied as the potassium salt (C6F13S O3 'K') Transitions Monitored : 399 -3 80 Exygen Research Page 12 of 110 r p. 1 3 ~~ r Interim Report #23 - Analysis of Sediment Samples Exygen Study No. : PC001131 Structure : Y F F F F. F F . 03 F- .' . .F F PFUS Chemical Name: Pafluomoctanesulfonate Molecular Weight: 538 supplied as the potassium salt (CgF17S(}3V) Transitions Monitored: 499--a 80 Structure: , . .F~ F F F F F, ' , F F" - fl3^ F: F 6.0 DEK1UPTI0N. fJF ANALYTICAL METHOD The analytical method "VU001782 : Method of Analysis for the Deternunation of PerEluorooctanoic Acid (PFOA) in Sediment by LC/MS/MS" 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 Procerlure For . Sediment Before the samples were weighed for the eXiisction, they were mixed thoroughly by vigorously shaking the container. A 5 gram portion of sediment was weigbed into a fifty milliliter centrifuge tube for the extraction . Aita fortification of appropriate samples, 35 mI., of 1% acetic acid in water was added to the sanaples . The samples were vortexed and allowed to shake on a wrist action shaker for ~ minutes. The samples were centrifuged for -20 minutes at -3000 rpm . Thet superuatazit was then loaded onto a CI B SPE cartridge conditioned with 10 mL of methanol and 20 tnL of water. The eluate was discarded. Twenty milliliters of methanol was added to the sediment wnples 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 centri.fuged again for y20 minutes at -34(}4 rpm . The supernatant was then. loaded onto The same- Cfg ..S;P$ . 'catridge. The eluate was collected into a 500 mL Nalgene Bottle,. 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 C~B SPE cartridge conditioned with 10 mL of methanol Exygen Research Page 13 of 110 p . 14 in:n im Report #23 - Analysis of Sediment Samples Exygen Study Na : Pt)001131 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. EWb sample was analyzed by LCIIviSlMS electrospray. 6.2 Direct Inj ect Extraction Procedure For Sediment 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 mil liliters of llo acetic acid in methanol was added to each sample. The sa mples 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 LGMS%MS elect rospray. 6,3 Percent Solids Procedure For Sediment Percent solids were determined using the procedure indicated in Exygen method V0006421. Approximately 20 grams of sample was weighed into a pan. The weight of the sample plus the pan was recorded . The, samples were then dried in an oven overnight at 104 t 2C. Then the sample's were transferred to a dessicator and allowed to cool for ~15 minutes. Each sample was then weighed again, including the weight of the pan . The percent solid for each sample was then calculated . See Table V for percent solids results . 6.4 Preparation of Standards and Fortification Solutions A mixed- ` stack standard solution of-PFBS, PFHS ,' and PFOS was prepared at a concentration of 1000 ghxal, by dissolving 1Q0 mg of each ofthe stan dards (corrected for purity and salt content) in 10[) mL of methanol . From this solution, the following fortification standards were prepared : Conc. of Fort Final Final Conc. of Stock or Fort. Volume Volume Fortification Std. Solution (mi~ :) (mL) (g/mL) 1000 10 100 100 100 10 ' t 00 t(1 10 10 140 1 .0 1 .0 10 100 0.1 0.1 10 100 (}.01 t of PFBS, PFHS, and PFOS Exygen Research Page 14 of 110 p . 15 Interim Report #23 -- Analysis of Sediment Samples Exygen Study No . : P0001131 A set of non-extracted calibraEibri standards containing PFBS, PFHS, and PFOS was prepared in mefhaaol, as specified ;In Exygen method V0001 7$2 . The following concentrations were prepared : Conc . of Fort Fort Final Fitai` Ctxnc . of or Calibration Volume volume Calt`bration Sid . (Snolut)i1on (triL,) : (nglmL,) g/mL 100 1 .0 10 10 100 0 .5 '10 .5 . 0 100 0 .2 10 1 .0 J 0 2.0 10 1 .0 5 .0 1 .0 t0 0.5 2 .0 1 .0 lo 0.2 of PFBS, PITHS, and PFOS The stock standard solution 'and all fortification and calibration standard solutions were stored in a refrigerator (40 t 2C,} when not in use . Documentation of standard preparation islocated in the raw data package associated with this interim report . 6.5 Chromatography Quantification of PFBS, PFHS and PFOS was accomplished by LCIMSIMS'electrospray . The retention times of PFBS, PFHS- and PFOS were -- 0S6mins, -9.4 mins, and -1 1 .4 mins, respectively. Peaks above the L OD 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 ng1mL of PFBB, PFHS and PFOS. 6.7 Description of LCININM Instrument and Operating Conditions Instrument: API 4000 Biomolecul'sr Mass Analyzer Interface .- Turbo Ion Spray Liquid Introduction Interface Computer: DELL OptiPlex GX400 Software: Windows NT, Analyst 1 .4. 1 HPLC: Hewlett Packard (HP) Series I IQO HP Quat Pump Exygen Rescarch Page 15 of 110 p . 16 Interim Report #23 - Analysis of Sediment Saqip]es Exygen Study No . : P000113 1 HP Vacuum Degasser HP Autosampler . HHP Column Oven HPLC Column : Thermo Flunphase RP, 50 :YUn x 2 1 mm Column Temp .: 30 C Injection Vol : IS gL Mobile Phase (A) : 2 mM Ammonium Acetate in water Mobile Phase (B): Methanol U~T , ~ , %A 0/6 0 .0 65 35 1,0 65, 35 8 .0 25 75 10. 6 25 75 1 1 . 0 65 35- 18,0 65 35 Total run time . -18 min Flow Rate: {} .3 mUmin } '> ' . . . : .Ionsmitred ~Yte Approximate Mode T28iiSltlOn Rotentim Time Monito min PFBS negative 299 --*99 -0 .56 min . PFHS negative 399 --* 80 -9 .4 min. PFOS negative 499--).80 -21 .4 min . 6.8 Quaatttation and Examplc Cillcu n tion s Fifteen microliters of sample or calibration standard were injected into the L .C/MSlMS, The peak area was measured and the standard curve was generated (using 1lx fit weighted linear regression) by Analyst software using six concentrations of standards . The concentration was detertained from the following equations . Equation I calculated the amount of analyto found (in ng/mt,, based on peak area) using the standad curve (Iineyzr regression parameters) generated by the Analyst software program . Please note that the equations in this section are presented in a diff'erent order than the equations in the method (Vfl001782), but this has no effect on the final calculations . E7cygen Research Page 16 of 110 p . 17 Interim Report #23 - Analysis of Sediment Samples Exyg~n Study No . : P(>a4 1 131 uatIon l : Anatyte found (ng/tnL) = (Paak area - intercept} x DF slope Where: DF =Dilution Factor, faicto'r by which the fitiat vdhune was diluted, if necessary. For samples forti fied with known amounts of PFBS'and PFHS : prior to extraction, Equation 2 was used to convert ft amount of PFB~ and PF13S found in ughnL to *g (ppb) . & on 2 : Analyte found (ppb) = jAa lyte found (ngbD x final volume (5 mQ] sample weight (S g) Equation 3 was used to calculate the percent rccovery : Equation 3 Recovery (!o) _ (ppal e found (0b) - aDaW e in control amount added (ppb) ~~)) x ~ 00% Equation 4 was then used to calculate the arnount of PFBS and PFHS found in ppb based on dry weight. F,Wation 4 : Analyte found (ppb) dry weigbt = Anal,yte found (ppb) x f 104'/a / total solids(h)1 An example of a calculation using an . actual, 4ample follows (calculation is for PFBS only) : Sediment sample Bxygm ID: C0 172$93 . Spk F -(Set; 042 646F'), fortifi ed at 4 ngfmL with PFBS where- peak area 253819 intercept . -592 slope 42300 dilation factor ng/g PFBS added (fort level) 4 amt m correq3ondin aample (ogts) 2 .41 final volume (mL) 4 . - 5 sample weight (g) f ~ total, solids (%) 54.37 Exygen Research Page 17 of 110 p . 18 ,,. ..r.~.~. ..~ Interim Report #23 - Analysis of Sediment Samples Fxygen Study No . : P000113 1 From equation 1 : Analyte found (ngfinL) = [253819 - t-54211 x 1 42300 _ 6 .01 nS(ttti.. From equation 2-. Analyte found (ppb) = f6.01 nafrnL x 5 mLl Sg = 6.01 ppb From equntjlon 3 : lo Recovery -- (.Ol ppb - 2 .41 yRitl x 10010 4 ppb = 90!0 From equation 4 : Analyte found (ppb) dry weight 6 .01 ppb x(1 t)0ts ! 54.37%) = 11 .1 ppb NOTE: This value may be slightly different than that of the raw data due to rounding. A slightly different set of calculations was used for the direct iajsctian samples analyzed for PFUS . _ Eqpa~tion 1 : Analyte found (ng/mL) _ {F'e,ak area - intcrcant) 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 amomit of PFOS found in ng/mL to nglg (ppb) . 90ation 2 : Analyte friund("ppb) = L&nAy,te found tUgbLl x volume yCft-dcW (10 mL)1 sample weight (18) Equation 3 was used to calculate the percent recovery . Exygen Research Page 18 of 110 P . 19 Interim Report #23 - Analysis of Sediment Sampks Eaygien Study No .: PO(}Q1131 Eauatiun 3 : Recovery (anaiyte found Lr4" - analyte in control (nyl&)) x 100l0 amount added .(nStB) Equation 4 was then used to calculate the umrnmt of PFOS found in ppb based on dry weight . ,F., ~l,,n 4: . " . Analyte found (ppb) dry weight.= Analyte found (ppb) x E100% / total solidW16)j An example of a calculation using an actual sample follows : Sediment Sample Exyg en ID: C0172892 Spk D (Set: 042806B),- fortified at 400 ng(mL with PFOS when : '. .` peak area. = 1 .52371 intercept - 3720 slope 22700 dilution factor 1 00 ng/g PFOS added (fort level) _ 4000 an* in c onzspoading SDinplc{ng/g) = 2360 volume extracted (mL) 10 sample weight (g) = total solids I 66.54 From equation 1: Anatyte found (nglL) = [152371 - 37201 x 100 22700 = 654 ng1mL From equation 2 : Analyte found (ppb) _ (1 4 ng/mL x 1 0 mL) = 6540 ppb1B: From equation 3 : % Recovery = (6540 n,gtg - 2360 n8[g) x 100% 4000 ng/g = 145l0 From equation 4 : Analyte found (ppb) dry weight = 6540 ppb x (10fl'/o / 66.54%) = 9830 ppb Exygui Rcsearch Page 19 of 110 p . 20 Interim Report #23 -, Analysis of Sediment Samples ., Exygen Study No .: P000 1131 NOTE: This value may be slightly different than that of the raw data due to rounding. 7,0 EXPERIMENTAL 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 sat 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 rccoveries, 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 MUIL.TS Analytical results for the analysis of PFBS, PFIiS a nd PFOS found in sediment samples extracted with the original method are summarized in Table L 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 f 29%, and 93 6r6, respectively. Fortification recoveries for the analysis of PFBS, PFHS, and PFOS in sediment samples extracted with the original method are summarized in Table M . Fortification recoveries for the analysis of PFOS in sediment samples by direct injection am 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 V0001782 . The sediment samples were successfully extracted and analyzed for PFOS using an alternative method, which yielded acceptable QC data. Exyg~ Research Page 20 of 1 10 p . 21 Interim Report #23 - Analysis of Sediment Samples Exygen StudFNo . : Po001 1 31 10.0 RETENTION OF DATA AND SAMPLES When the final analytical report is complete, all original paper data generated by Exygen Rzscach will be shipped to the study director . This does not include facility-specific raw data such as instrument or tempcraturc Iogs. Exact 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 Rmascli archives-for the peiiodwf qiae .specified" in EPA TSCA Good Laboratory Practice Standar"r'!s 40 CFR 792. ExyBcn Research Page 21 of 110 p . 22 Interim Report #23 Analysis of Sediment Sampies Exygep Study No . : PWS 13 1 TABLE S Exygen Research Page 22 of 110 p . 23 interim Report #23 - Analysis of Sediment Samples Exygen Study 210 .: POOUI 13 1 Table I. Summary of FFBS, PFI3S and PFOS in Sediment Samples c4 suransM PF88 Cl dutonw PFHS q 3uara+Ms P" #-" Fou W AqNMd MrRM Arwwd Anal* Foue4 Aw~aW Cwt i01W WQ} Aa+ftY "b. A0 M AaounrY {FPe. ng+p AOMW'+bY C go"Pok to Dry wow* +J-'J4 +F-!1 weiRk +~L C0172E42 DA43~4WpOQ .114 40 04.3 30 NR NR can 72802 Rap DAL-8a8PP01-0a1000' 3.10 40 Od.l 30 NR NR Cot72N3 C0172003 Rap OAL-SD49MV2-0-0000 U&-SD4MzPC2-0-ODOG* 4A3 30 74.6 30 MR NR 4.84 30 61.7 30 NR NR CD1720Y4 9.87 ,f! 134 50 NR PFi 0077204 Rep OAt404PP0340000' 6 .75 30 123 50 NR NR U bonlxY Ouc4=b NR Not pOt%d do* to mtdUt mdrW tMiYt Rihxsa. bw Tabb tilw M40yiM mrUMs. Exygon Reacaroh Pap 23 of 110 p . 24 Interim Report #23 - Analysis of Sediment Samples _Etygen Study No . : P0001 13 1 Tabie If. Summary of PFOS in Direct Injection Sediment Samples Exygen ID ' -.t Client. Ie ID . CS Suttonate PFOS ~uOrCOCUMMUftrate : Anelyts Found A~ (ppb, ngf8} Accuracy Ofy W9 ht Lt/- % C0172892 DA1.-Sa-BPP01-0-(}000 3560 30 C017289;t Rep DAL-SD-BPPO'-4-t1000` - 3520 30 C0172893 DAL-SD-BPP02-0-0000 4160 30 C0172893 Rep DAt.-SC-8PP02-0-000d _ 3840 30 C0172894 pAL-SD-8PP03-0-0000 11900 30 C0172894 Rep DAL-SD-BPP03-0-0000* 12000 30 'Laboratory Dupiicats Ex'Ygen Rescarah Page 24 of 110 p . 25 Interim Report #23 - Analysis of Seditneft Samples Exygen Study Na : PQ00113 1 Table III . Matrix Spike Recovery of PFBS, PFHS aad PFUS in Sediment Samples E001 M hoOwA w hwi u w~w.1 cOf~NM~NSrfNtww aNWwoO .q .rw1M /4nt rtl - .,4Mwa MlFaa+d . ~.+ AM F4wW aww .n . in 8paptr R4tawrd ROMMV in >W" tiw w+nd RNOM, b9rap" iMeovwW rMrl wt~t ~r~lyM +MttN . ft oa4r! OALSl}EI'r01-00000 , , ~>a~uMC,aR 7~rN 4 ZAO 447 0, . . , - . . - . . OAL,$OBI~AOt-0p00 paTMM 40 0.4 1MYlo" OAL4BDiP ft 1-0-0000 p1tiM00AMCAOCM7piY 400 am' 2A9 20Y 262 06 00,1 a61 N . . .. 2070 or 06.1; 6t90 126 . HA . . NR NR OJ1l4DOWW da000 famwslr+i~.~rr ar~! QA63Pd'~'0~-0~100 90 4 40 M 00WM'nw 0 OAL4 P4 PP0Z44OO 0 MOwoaNlaMQ(DrMfIt o 241 L02 9D - . _ , 400 2.41 174 91 40.i " .. . $IS 7 0 IOQO ,2a1 3i20 06 40.3 E0Y0 126 tMl Ml VAL-4D4W*0b44UQ fCetilWNr4a~MN~r1 4 4.30 911 as, _ - DAL-$04L%*&$44= Afn~i1M OM ~-aM M>MM+! 400 439 SQY so .--64 .6 30 0I4t.-3D4IPPOb04p00 ICMqaMJ~a~S,Mapir~iNYJ 4000 4 .3 0 40 I0 121 Otl 4000 . .' . - 6E - - ?if XlNR NR NR . . !Xi AWpaf M AMYa/1K M wiNliM: NO Oow~td WrUOn: 1i rpNft%rADw IWSas a$ OwndW DWvYYrr: Ma 'frAoM wwawraMa ttt440ft tww tiN+kw+y tU +i0drowR wrwa r .av w nwwrvru. awoe a aro~Yfq WD e PbtdM~NrdatorabawMtMFMGr#r1an~DOt+102aYrDM+~+~ MVpMq (SpM "M we 7406 IV bry"OVAOSOQNReMowptlAb OL Ma1K mKS rNS aow JV"kAhftVftwdw ORAL *IL Ezygcn Research Page 25 of 110 p . 26 Interim RePort #23-- Anatysis of Sediment S"les Fxygen Suidy No . : POt}0113 1 TatblOV. Matrix Spike Recovery of-PFOS In Direct injection Sediment Samples dM.-SO 4M1-04Op p Kmtar~zaqc4NOOOpefvMtl DAL-SD4N1'PQ1-040000 lC"10 NOV4~4011 o roi sr" fP PC CO auMoaaM PFQ6 llWt WO MM Ant ~~ ~ Ant Found Affound SawQM RiGC1NIMd tram WN wk wet wt Recovery 4000 2960 86~4 105 ~0000 238p 40000 94 DAL-SD`8PP02-04000 " t2108 lit s, 4114e opbeWcN 4000 228p ~yp 92 dALSN8PP02 4400 0 lcotttua sp* M,. aeooo P1 b Op" 40000 2200 39000 89 DlLL.-Sa8RP03-04000 !M7211" tpt J, MW PPh So N dAL40-8PF09-0-0006 ICOtTI U MpA K. 400 WOO3ON 4000 $280 8770 87 41700 0 5280 41200 90 AYi/ip: 93 O IiBdild DrYUtI0f1: 8 NsnrmI Nqeotrootwirm5,.est.uanreieodrs taoeo9vpsitdnpumsvlwt oWrtpiuHwrafnttMioyn NpAspP)ifot(b0v.2e*wqulWp (*,,f,Karo,*.psMn~PopW*r nrooNry vs5,. aanrwi be oM"rree Nn1r llnor aft summary W b w%vm iwdw naWts, rewwa7 values maYw+Y s w* kO n tl valws b iM rwv dMa. Exy~ Research Page 26 of 110 p . 27 Interim Report #23 - Analysis of Sodirndnt Samples Exygen Study No . : P0001 131 Table V . Total Percent Solids in Sediment Samples mP ID DsecrtAlon Total Sows (~f.} C0172892 DAL-BD.BPP{}1 -0- 0000 C0172893 DAL-SO-8PP02-0-00 00 66. 5; .-,54.37 C0 172894 D,U.-SD-SPP'03-0-0000 44,q6 Exygm R==h Page 27of110 p . 28 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.- A400113 1 FIGURE S Exygen Research Page 28 of 1 10 p . 29 Interim Report #23 -- Analysis of Sediment Samples Exygen Study No . : P+DO4 1131 Figure I . Typical Calibration Curve for PFBS in Methano l 0 M06f 0441nanlM6 (PPBSjUMX RMr#A lonPtlk'w4 11 ANrl p2y*4.2 t4OWx+-0D2Q s Oli0Q0) 4.40 4240 . 4.W 5 3AW 3A I6 3 .4 06 3.2 66 3 .0+6 2.Y" ~ 2A~6 0 2a746 7$ 4 6 { 2A W f.6W 1.6~6 t.da6 f .2 .0 4.0~6 tl .OW eA.4 40" 20*{ 9 Z 3 4 6 0 ra~aaw4iMn, "O"IL '7 Y 0 f0 Exygen Research Page 29 of 110 p . 30 Imenm Report #23 - Analysis ofSedimcnt Semplos . Exygen Study No : PWOI 131 ~igaa~e 2, Non-Extracted Stnndn rds of PFBS in ikiethanol, 0.2 nglmL and 0.5 ng/ml,, Respectively ~ sSN!#M -MW A~wl~te~l! ~M~eselo . att,e~p, ssl~siAss A~ii~1~,1~1~r Arzsi iria oe.Atr /#!Ak Sra tN2 rpc RTr alSt<arAr 5w o,ea .oo 2W .. , +oo n 1 Z 3 1 0 b s s o io 11 12 , 880oN4dY6 i!~ (9t~r~a~3CGANQA ~su . fam,te 2~f ~ kam OqtllOAfsAt t AM- 210" eowNC i4Npht 1 .4fMptiCi cps RT : O.ff00 ale 1A60 0m 1200 a~ 'NI00 v ^. .. 1314 19 14 15 10 Yl . .. Ow . 4q0 1,87 200 0 CS' ' '(f " " T, p ' i0"' 11 ` ` 1'p 13 - ii" 10' 10 1 7 7tew . . mist Exygen Research Page 30 of 110 p . 31 itfttrim Report #l23 .- Analysis of Sediraeht Samples Exyg+m stu8y NQ. :.Pf9001131 Figure 3. PFBS In Reageat SlanI ;, 0.4 ng/amL Fortified Reagent Spk A, and 4.0 ng1mL Fortified Reagent, Spk .R, Respectively , RasllJtt Co~Mtfar - PIF~s ttA~h++w1 ~~+~ri ,a~J! i otI! ekr~ il~iiiFn.~1: ~Nt~rllt~i~ . .c' :-' -r'. ~- ~ p 13.9! dm 10A4 11 D! 13~ 06 m iA6 1 ~ A , ] ~ ! .1tlJO .T9 1a 1.1Y i~ 2 O,t/7 7~ ~ tT .47 a 4 2 ~ 4 4 6 T i 0 10 /1 Thea, mIR ~ IltiluR ipkA PISS (OC)298.6tMD mm raMNt 0 N40 from 042E0QiaWlt AMC 10i70 a+#Me MNMght 1 .090f1Q;i 0" qT:044T Ale tZ t3 14 't4 14 iT 0.40 tCLo low . fl 1 2 s ~ 4 s T a o to 11 12 iZ 14 ti. 14 IT ?in., in: ~ R.ai "t Spk 8 PfiS (QC)200AAYD anbtt santytv 10 M 49 Isom 44Z404f w111 N+a:104227 waNt FNipl~ l.i1 r.a44 s~s Ri :O.l47 ni n aae 1.00t ti000.00 0.00 2 j 4 6 Q 7 i 10 11 iZ 13 14 4 14 IT Tima. N n Exygm Rewamh Page 31 of 110 p . 32 -}-~ In*arim RMort #23 - Analysis of Sediment Samples . Exygen Study No. : PQ001131 Figure 4. Chromatogram Representing a Sediment Sample Analyzed for PFBS (Exygen ED : C4172892, Data Set: 042606F) ~ tk772pQPY'D~~l..re.i.)rl~tA~l . .i. . .~r~h t~otl!l~i.~ . .~i1iR~r ~r.~ ~ec.raa s~ ,yr~ asw+~rso . ~rn, as r .rr~r o.ey zeDo 2eoa r~oo zsoo s1M 1.pt toaa +eoo iaa o +oa o aoo eco 400- oo 0 t 2 s' 4" '~ 5" 7 U Q 10 11 12 13 14 50 Ii 9T Tlne. a+M Exygen Res=Gh Page 32 of 110 p . 33 Interim Report #23 -- Analysis of Sediment 5unplts E1cYgetf Study No. : -POOOl 13 1 FIgure 5. Typical Calibration Culve foi,PMS'taMethano l ~ OC30pOPird"indd.rd (PF4t8~"LM~rrxtRqw~irn~'11rlw+i6Mir6)cY"7AQ~ Q04x+ .1 .1~r000(r~G .Y00d) 7.3d 7.0r6 6.~y 6 A-0~0 6-Or6 6~1~6 4.Or6 = 0 es 8.4r6 3Aa6 2.6~d 2Ar6 t .M3 1Ar~ 6 .DN! 1 2 a t d 0 ' CenorMrsilrn, nsyiwt 7 i 0 10 EXY8M Reseamh Page 33 of 110 p . 34 Incenim Repoz : #23 - Analysis of Sediment 3amPlss Erygen Study No. : P4U01 131 Figure 6. hTon-Eatracted Standards of FFHS, in Methanol,, 0.2 nglmL and 0 .5 aglmLg Respectively , ssM~sli .Ar~+r~wv~~rrrarearr+r+iM~ tat.*slto~wrslcrr+F~rr ArNC tAMo1iw trlMO6 7.15"Wf2ys Mn t,l Miis a.~q too eoo u ~ ACO 9t1D 1 1M 90iD d8g` 0 1 2 3 4 6 d 7 a 0 10 Tiar . m1~ ~ ftpDV000 PINS {sfindsrO 300.WT4n saw . sampM 2 60 6 Mte 002EOOi wiw Area : 33ad3 oft** Height 11 .730063 ep kT : a .40 win 4,4 42 44 0 .40 1a W a . .. +a i4 1d 16 17 ~ ~ ~ . YA. 1 x 3' ~t t! N 7 -ab- 40 -it ix"- ii`- tA 4 16 17 TLnt, mie Rx~rgcn R+~earch Page 34 of 110 p . 35 'Tiit6im Report #23 ~-= Analysis of Sedintiedt S*Tnples Exygen Study W : POOO 113 1 Figure 7. PPH.S ln 'Reag+ent1Manic; `0,4 nertflL Fortified Reagent Spk A, and 4 .0 nghnL-*6rtiff0d Reagent Spk By Respectivel y , M Ast..tca.a.i .rt l ~Nat ot 1bsM IOi+w+w7 ~111a irMf;w*M niarefA+o~ .tir~i~ ' o .ae 1x .o . : vk A fO ~.0 3 40 o.+e ' txai s,~n =.02 '00 0,3i apY 11 . .t9 /aso .1a,Q6 1 2 3 4 6 0 7 9 0 10 1 1 12 13 14 If 16 17 Time. min , RaaoaN=piA-RFMtIOC)3DDtliOAi~r-sathpMYM40fae0M12sDi~ifF Anx 2~'2 uorptr "eight 1 11006002 aps RI : G .7C min 1000 gag Soo ae+, t 2 3 4 d 7 9 0 t0 ti na m& ~ Aaa0ant8pYH .PFNS(OC) 900 .WiDA AMU . ample l0af+16trow0~00F../! Area: 27907 awnft NaiAwt 1 .AOa * 00i epr Off : 0.40 nin 12 13 14 16 16 17 w a 1A44{ Oj P F a GAD f 2 s 4 e p 7 9 10 tt 12 q ~a 'MS 1e n Ttrna, rrhr Exygrn Research Page 35 of 110 p . 36 bnrrim Report #23 - Analysis of Sediment Sampksa- Exygen Study No .,: PUfI0113 1 Figure 8 . Chromatogram Representing a Sediment Sample Analyzed for PITHS (Exygen ID : C0172$92, Data Set : 042606F) , COMM - r+ff+s ~r.aw)sq a,Nw ... ..iti.r~ rtof.a ft,. .,arWMnr A~r: ?IC~nsvs.a r+Mip+~ tzr+Mq*a rrrr ~fYrr. ~ am zooo 1so U teoo 1400 T2W t0o0 a0o 000 AO 0 O O. Q . .. . . ~ . ~ . ~ ,~ "d ' d' T 10 1 1 12 11 14 13 16 17 Titp C IM6 Exygen Research Page 36 of 110 p . 37 Interim Report #23 - Analysis of Sediment Samples Exygltn Sttu#'y No: : PO001 l3 t Figure 9. Typical Calibration Curve for PFQS in 1tii'etban0l 04a 06Y god. Q l.Me (PFO9k "Wa+r R .puarm+(', rr wripFylrpk ~ . z .vrt044x * a .72MOD~ (t a.0046) s.e.a 2 .4~d 2 .206 2^A.a ~ .a .a t~a 3 1 .8.6 8Q { ~ 1.O .ff s.0.i o.0 .a A,0 .4 ! 2.Wi 1 2 a 4 6 O ~ i C 10 Cane.ntrrian . ~~hnl aYge" Research Pagc 37 of 110 p . 38 Interim Report #23 -- Analysis of Sediment Swnples . Exygan Study No. : P000113 1 Figure 10, Non-Extracted Standards of PFOS in Methanol, 0.2 ng/mL and 0.5 nWmL, Respectively ~ ss..f~i PF~>~ ~ ..MMi . .i.. ,.,~r~. : ar ~e i1n . ik~L,~M Aeri. t1i<3leartrlr tAMy~!l :1M+M2qpe ItI! l~IrFi ti .4Z 8G0 No 4W 7A0 'V. 1 Z 3 4 6 n 7 1 10 11 12 Tim4L mitt , 890D9 460 Pi08 (BLrd+0d)4qY .040.0 irtw sanpla 2 s}~ y~ O~LfORO .Wff Any : 1'2326 "at* Htitwk 7 .72r+002 aps RT .,11A min 13 14 16 19 17 7O o 000 CL 600 u 11!p 0 10 .63~ . 900 0 1 2 3 a 6 6 r a to 1+ 12 13 14 16 16 17 T#ma win Exygm Research Page 38 of 110 p . 39 Interim Report #23 - Analysis of Sediraai4 Samples Licygen Study NO . .-, POGO 113 1 Figure l l . PFUSin -Re~ent Blabk,' b.4 iig/mki,~ Fgrtified Reagent~ Spk A, and 4.0 ng/mL Fortffied'Rageut Spk B, 'Respectively as , ~y~e r...aw . ~os Mut.n.r?,Nu~.w~, .aw -.:~A ~ :ris n., +~ns~.~;Nr '" "'' t ," ^ AIlf~ iOW1rf Awfft Z~~w c" ".3 WIN' . . .. . .. 4 V 20 , 11.46 ~ 10 ~11 N S 0.431 0 1 ~ w 2 ~ A4AM 476 6~ 7Z0 g~ g~0.02 4 6 0 ~ i i 10 11 12 437 10 14 /1 T WA. win R eftent sihA . rOS (Ot:)4 li.Gl0.0 Anr sampl. o o#46 ltrom 042fO6g.wM Area* f00ta0 owMC MatOMk 621 H002 sps RT :11..4 rain 16A4 10 ff 000 tt,A6 i 400, 200- 1045, 0 f 2 Z 4 6 0 7 g 0 10 Tlaf e , W e 408140 9/6 Y- P0Y (0 Q 400Aq0A am . - sample 10 d 4S tmw Ot2gO6g.wR Anc Q8761 aerfdS Nrpght 6_07e4009 eq RT : 114 Me 11 12 fS 14 16 itt 17 0000 11 .44 ~OUO ~ ~ 2G00 10. 0 10 1 2 ? 4 3 6 7' 8 4 10 tf 12 ti /4 16 10 17 Time . wi n Exygen Research Page 39 of 110 p . 40 Interim RePort #23 - Analysis of Sediment Samples ExYS~n Study No . : P000113 ! Figure 12. Chromatogram Representing a Sediment Sample Analyzed for PFOS (Exygen ID: C0172892, Data Set:042806B) , p1T3N2 .R190~iT ilrtse~)AltN~.~ars-arspuArlicNSA+swi~ZNf6L~ril A~t aMtew+ttr rAryit~lar+N~tqN R9 :l7R .S~te 4W ~ ~ao 3+D W0 aoo 2eD no 20 1 tAp wo ~aD . 120 100 0040 20 Ot -9 t 2 1 q d 0: ' .x' A Y iD ti 1Z 13 14 10 10 1 7 Ttmt, Bxygen Research Page 40 of 110 p . 41 Interim Report #23 - Analysis of Sediment' Satnples Exygea Study No .: ?M1 131 APPENDIX A , Study Protocol P0001131 (Exygen Study No . P0001131) with Analytical Methods and, Protocol Amendment s Exygm Research Page 41 of 110 p . 42 Interim Raport #23 - Analysis of Sediment Samples ; E:tygen Study No . : Pfl00113 1 Exy#sa Pioroau) Nrmba: P0001131 STUDY PROTOCOL Starly Title: . , An** of Pwftor6batswW*x*W(PM), i'+erfluorohexs.uexal fta e {PFSSj, And 1'erftwrooct wesatfontt+e (PFt}S) to Water, Soli, Sedimeot, Fis#, Clams, Yeg+sitttlo.n, Small Mammal Liver and Small Mammal Serum Using I .CIMSIMS for the 3M Decatur Monitoring Program Exygen Protocol Number : P0001 131 Exygea lt"OKC11 lldldftW A. 5 atoco 3058 Ra ewch Drive Dirootdr Of Rq{ulawryAffaits St ft Colle54 PA 16801 3M Buildin X023G-t?i-B 10 Phon,e: (814) 272-1039 St Peui,14lN 55144 Phone' (651) 733-6374 " Pr~qr 1 oj 6 1 Exygen Rescamh Page 42 of 110 p . 43 Interim Report #23 - Analysis of Sediiiie6t Saniples ` P.xygen Study W.f P6001 13 1 ExyM PAarocoi Namiaae: "WI 1 7 1 r DfS3RMUTIOi"i : 1) J"mhs Kemi. Stn* Duoc3or. W4 AOa Wntim 2) Jo2ut W FWsaety, PrWipal Invatit br~ &v7'b n lmmvb 3) WwkW A. & abso. SP~ Rmpr~ve. 3M CouspS aY 4} FatyOaD.R "Ca=cb Qi?aiitY Ayun~oqe t W . , . .. _ s. _ . ..~ . ~ _ :: . . - .. ; .. , _ ~ i .i : , . . . . . .c . ' . ,,y . . . ._ ,, .. - .. . . . . / . ' . . PY~r1 oj6J F.xygen Research Page 43 of 110 p . 44 Interim Report #23 -~tlnalysis of Sediment Samplcs Exygen Study I+to . : P400113 1 Etylpq peAocol Nuofbsr . tWOS 131 PROTOCOL APPROVAL Study Td rk Analyas *fFfffiwWbWW=dftW OTBS), (PBHS), and 07OS) in Wwr, Sw, Sadtawu, Rib. Cum.. v.Snnmao, SMu MmM al Eiwxs irtia S Calt MManat Scam Ush* 1.Sh'MSIMS !br ft 3M Decaair biouftarft Y+vgmm Esnm 4u01oaol t3on6es : P40R1131 AsPxov '0 wegm soluimm . - tl D A& f .,- . y~r~.L$ Mi+eMe! A. . SpawosR*oreotatiras 3bf Compady ri u o li F7 lxrty; raW 3rvddp~ ux' ExY~aa Ra~u~dt ~ _._-.--- Riodr[d A . i, "daot. Ficft ~~ Pxy~ea .. ~ -~r- ~ DRta L Shift. Tar3no Qadity A vaul= 17ait --~~ D&W Rae ^ h .+~ Pnjr 104 b'S Exygen Reseanch Page 44 of 110 p . 45 Intzrim Report #21- Analysis of Sedimem Sardples ~ EaYgen"Stiuly Na . : P000113 1 Higs en Photoool Nmbtr. PUOp! 131 r+ - ?IUBIrE OF CO@PP8M Tii1iYA0fi . . ._ ~ __- . ..., ., .. .'-----..._._... .. .~,.. .-_. ... ... ... .. . ... . .. .-_ .._.... _. . . _t . .. . , . RtiCOQD1 ATPRCWAI _ _ . ., . ..._ _ ~ .. - .. .. . . --- .. ..- .. ._ ---- .. ._------------ TABLE .... .. . .. .. .. TBS71tAT&R]A2,S .. ... .. . .. ..... . .. .. Ofit1BCTtYY . . . _ ._ ._ . ., .__- .__. . . . . ._ __, ..... ... ...... . . .- .. . .. . . .. ._ _ ., 6 ------------. . .. .. . .. . .__.. .. . STtJDYD~8Ctti0it .- ..__ ..-... .. ._...__.. .. . ..-..._--- .- ... _...--_ _._ ._ ___ _.. .. . .. . .. .. .._ . .J S2"OR1S9R 1t~R8Sl~TA17YE...------..- . .~..,..... ....,. ..., ._;.,.._...... ...... ......_-.._-. .. . 7 PROPOSED BJQ21046NTAL START ANDTBRUR+IATlCMt DATES ._. .._. . .. .. . 7 IDENTVYCA770HA?IDAIBPiPtCATM +OFTHBTBgTSYBIFM .. .-. : ,, .,. ..,__..., . ...., ., .._ ..S SAMTLE?AOLZiRBi AMr RBC8aR'AND~TfiNTtON .. .__ . .. . . .. .. __ .. . .. . .. .. ---$ ANAtY2YCALFAOC33D[JA E YERIIRGATtON Of ANALYTICAL 9 1t@TBOPOIL CONTROL OF BTATIS7YCALM871qt~DB___ . iI.T 3TATEMBriT --__ .._ .. . ._ ~_ . . . __. . .-. . I I BAFGTYANDliRALTX .__.. . .____ . .12 AMENDMENTS TL rAQTOCDI,_. . .__r. 13 DATA RBCORD XU34 r0 . . ... .. ..._ .__ _.. .. .... ,,__.. .. . .__ .. . ._.... . .. .... _ . ..._ ..13 Qi?AI1?YASSURATiCH _ _. , .. . .. . . .._. . . .. . . .. . ..__ ... ._ ..i4 RE2'Stf1M OF DATA AND ARC}IIVRVCi . ~ .. ... ....... .-.-.-.-.-.-.-_--.-.-. .-. .-,. ........_ .. ....;..a. __ ... ... .._ .. ... .li APPS1R I. ANAl.YITGA[.3SFCfliQW_.. . .... .... ------------ _ ~. . .._... . .. ...- -___ . .,,-_-.._-_ . . IS Prgr+e/si Exygea Research Page 45 of 110 p . 46 Interim Report #23 - Analysis of Sediment Saalples Bzygen Study No. : P0001131 Ee}ypn ftoioc+d xwbtr_ P005113 1 '~ IlMODIN."lYQN Tla pupa4o of this dody is to paEfoM aulYsis for PacucsobnttuMtfonua Mu (pFTiS) and perllnomoet onewiforate (P'FM in w 0tar. soil, adwMik t *,, cluau, vegatuian,, small rnr M at ii vara and MA ==Ml ~vm ridRg Y.t`.JMSJlKS for the 3M Denua Monitociog PWF Ths A* will be aodi6at for aa aq Dauee with E?A ?SCA Good LrboraIwy Practice SSodinls 40 CM 'T92 by the QoaYty AswtAmea Unit of Exy&m Ra =dL TEST MAT6WAI. 8 1b tat tn~toridr> petlpwarob~ttittaulfaute and a s all sppliod by W. (p~) snd k PM Chamcd Now; Mokcoiar WdQGt: 338 w'ppliW ra the pot9 Wnfli tak (CaF403"IC`) Lot Ahwtbw, to ! P~aity 4b.'r35 T=UOWaar f loaiWred: 299 -r 99 8tnaotur~ F F F F F FF PPH S Chamw MrM : ParEaoaobmcrmwifoc.ua 3Wlacalw-Y 43E suppiied as the powaiiun =ft (C6B,~"IG') LO l~ktmbar : ~ 6 Purily: 4R6'!i Tmdtioes Mwtituwt 399 -s 80 Sms : F F F 5 ..+ An. s of e5 Exygen Research Page 46 of 110 p . 47 Ititerim Report #23'- Analysis of Sediment Samples' Fxygtn Sfl* No . : 'PtO0113 1 Ex" Prows; Wacker PON 1131 r. - P~OB t3>ewitai NOW Put hmoaftatf Moa.wlrr wa*w ~rx>n~-2tr $.3a.=P~ pit.a. as he pon dum,.n (cjFi,so,-x') Poft 85:9'ic TAWOM?WAOft&- 4W-*'SW SoncOua` , _ F F F F f.0f 3_ t1HJ&CTEVE ,, . The gatpwc of d~ midp is to psift aiey,y4s 16r padWombut~n3fonato tPFH3), {p'FHS) taAd tF!''OB) in WSW. iail, U&Mmt, itb, dMM vay wiaa,, pmatl n>wam w tlvus and watl mousW rr+ m for the 3M t?ooA ur 56autioaing Flopran wring the ~.,~ caameat vt rsious of *8 fiAlqwins Exygn wtlyti+caT medals: V0001?to: "MdhoQ of Andyris tbr t64t Ik orrni>rtiw of Parfluoroo manaic Aaid{ffflA) in Watorby LC1M .SW Y04t)1711 : "l~iabcQ ot .bMlydt ~ the pate~udon ad Pas~qoraaA~moic Acid0Pfkt) is Soil by tcrb43AW V0001782: "Metbod of.AaatysW for the Dd makwtion oCPattaooocunoiC Aaid.(PPOA) is Saib>!st by IJMlLNAW V440U"13: "Me14od of Aod yaa 38c the Debeeminapan of PKAwwooatanoie Add (P!K>!1) is FA mrt CUM by IR"J]d3tM3" VOR01754: "hirehod o ( Anrlyfis Or the AaGm ulaation ofPwftuoroocanoie Acid (P1oA) in ysYendoa by Id:/MSIAdS" VQ401735: "Mdbo4 of Andydr tht tpe pahnqiw>iom of Petflooeooouaoic AddMpA) it SMll MwmmLLim by LCJMt,.RtMS` Y0041 M: "'lKelbod of Andyi hr daq DoWmAu Hoa of POdbxuqogWAjoio Add (ll+oA) in Snail AM a M SWAM by LaClM3/MS" TZS1TlKc FACILITY ,,. . 30S6 ltareawh DtWe Soft ColbV,, PA 16D1 PhoaK ($ 1 4) m-1039 Pa~r bqf6t Exygen Research Page 47 of 1 IO p . 48 Interim Report #23 - Analysis of Sediment ~Samplss . Exygen Study No . : PUQ0113 1 B~.a>~oi i~ trooo>> 3, r-- -STUDY MUCTOR JdWmM ICeari PA, DER ou WOM c W*y Wart Chater, PA 19380 Phooe: (610) 701-1761 Fax: (610) 701 7401 j.kaari(~weNa~oludntu. am SPONSOR nPRICUNTAT M, *669 A. SwWx o 3M Cpqlpsnty Diroawar ot R+~datary ~ 9Yira 3M HoiAq Q236-01 4-10 Si. Pwt1, MN SS1 " Phone; (651) 733-6;374 PRWfK3'AL INY=GATDR 7oha M. Fbhuty Fxygaa .7LCSO Wh 3058 Rprasoch Drive , StatiC Colkle,, PA 14i41 Plo w, (814) 2?3-lt J39 jolm.lbtwny~Fges oom PROP+OSM 1~J4YEBIMS~NT.+~. START AND ?ERKINATION DATES IL 3g paayomd do 3hr mdyti w partiaa of this * adY be wabcDOd from tlceaber 01, It10!4 .1e D1002mba 31 . 3Q06- The ill experimeata! slut and smbudion a. w wiaree taot.Wea k the dad wpm ~ ,. Pare 7af6S Exygan Rescatch Page 48 of 110 p . 49 Iriterim Report #23 - Analysis of Scdimnt Saaiples Exygcn Study No. : PiDt70113 ] F~t}~n Ptaoeot ltiaribm: T~00 i F3 i r- IDBN'TMCATNON AND JMMCAnON OF THE TEST SYSTEM The 10111wift we aw t.c .yaam. for this amdy: . s Wa9x (Vomdw4or tmd sadace xstaj Sa4! - 5odimoot Fish - Clitmt Yo~eqtipn '.baA bf=mmW Liver smog Mammd Ss" r no umapta will be collected by Waioq $obutton . The control mrskples will be purchased and popmRat by the te W Ag Aai4qa Pme chase and prceessiag depii}s hr the control smplas xiII .be t m6ided in do final repott associated with this d dy. , - The tat tym u was chrnau to aasdtlre cmirom~ impacx of PfBS. PPHS end PPOS in the Aecaor> ALbe ns xaeg. sAMWLJ9 rROCURV49a+rr, JUIc F.Err AND RItONMN w,oumr. wit . xgmo t, n.a dam vmg emdom , mmmC momw uw and u .n mmuo W mm wnj I .hn be waived .I BxA.a auectly km Waft sot, dom The aeadr otn",re ptom m" thr this .aay .,e outlined in U 3' Mf ~work pLo~e~ar~iyt~ lat "Pb~re 2 No M Bmiroaa~nW AI ~ j ~ IN QY'R,~ ~ typo of{~ IL i~Lu ~ R!Y ~~ y . ~Y_' ~} ~ in T1h{~eP l The WWWW li~ of ~~Y~ M o i~W jM ]M Y m forayM4 . " ti11~"bf will be do. mm OOtE.d IH,1.t.-1...ftd report a.ssocia.ted with this WdOPi =4 ad 0dhoont samples will be used as waived without findi0r ptoowiog st FsyVa . Theme samples will be Owed reltiga=KeQ at 2 'G81C. Rik clmm., vemeqtift sod imWF. YAW noon W32 be P"Quod avwdbkg to sbs tqspwpriu analytical m,rftd (m Appadix t). These ,rnpi .o will he ,wo~od sea it s-ta+c. swu m.n,pw wbJ b kv t amptec will be ansrft1 in the SO a ft time of collection and the umm fraction will be used fbr the imudy. Sm.n msa m.t .orom will be stored from e s -tm The teogiPt and proapft of ffi moon will be documented in the flied .. repeal and mw data au orLtd with the sAdy. w~c.eofas Exygtn Research PaV 49 of 110 p . 50 Intenm Report #23 -Analysis of Sediment Samples Exygen Study No. : P0001 13 1 ~ SAWLE M4i' WICAiaiJ11 rsxyia+ Pn*W561 Nmnbat: P0001171 Prior to arlytdr, wAob ample witl be U iVed a itbonqory sample reference nu,ber. The rsfmbnee olttqbet will be +u,l w sin d will distinguish each hborotoiy am* that is prooewd tluoaoont the atdyticit procedtuc. Chmmitogr%Ame das< will be idemiGad by the laboratory camp3a reference nuonbur, Sample alar~o aaf~tioos wd loortionic will Be doamn~te~d l~u+otlghoat the study. ANALYTICAL PROCEDURE SUMMARY R~lereeca: Va00173p: ' McIhod of Anib*o toe the D4awin Roa of Pb,iEuotooatuaoic Mid (PPOA) in Wltlar by LGMSIAlg" VW0 1721 : "Mathad of Amtyw for the Ddiumingtion of Pestluaooctanaic Acid tPPOA) in Soil by LCJlkIBJMg- . VW017 82: "Melbod of Atratysis for the Delarmiatlion of Ped}noroocWaic ,... Acid t!R{YA) io So tdoent by LGM$!MS' Vfl001733 :: "bkthod of AMY* for the Ddarntiaopo= of Partloarooctavsoic Acid (PFA) in Nib sod Clams by LGMSlMS" V000171F4 : "blethod of Malyris for the Dahanda i tion of Perflaorooctsnoic Add (PBE)A) in Vegetation by LCUMW S "Vt)00173i: 'M@1bo8 of An{tysit for the DatmmiaiWeyi of PsrHaoroocnrwic Acid (PPQA) In Small Mammal Lfvet by LOW/MT' V0001786:" `Mo bod of ArWyEiu for the AotmvAnrtiiaa of Pa^fhmroorusoi c Mid (PFOA) ia smait 1MonaW .Sa,uaa by.tc.WSrMS^ Tf~e sbo" mattwu an u atytl w oo odit9aais capable of wprssias the isomers of PF88, PIES and PFOB. The Sroi rapoe will mcinde the isomers summed into eotal PFES, totd PFFIS . and MW PPOS famnd , VEAMCATYQPI OF JlPffJ~'.Y11[:AI.-PBDCEB[f1t8 A W malory owbW sample will be used for the props atfon of fortified canhal U nplea, The No sabsLaco Will be tatdr iaoe " tiont u per the medad. mod adUW to the m><trioe~ via s micro}dpeaa. Far wow snmplfu&, EsySao will wpply one bottle per ample coUaxM The btid,lw will be 5M mL ptaelaaed Soi/Spet Prt6ntiiar wide mouth HDPE bottles. Than bottles have base routinely used for fluoror6eimicsl ample Pqr Y a~6 3 Exygen Research Page 50 of 110 p . 51 Interim Report #23 -Analysis of Sediment Samples Exygen SuAy No . :- P.000113 1 BxyPea Peabost Wtwbex: POpDe I I I co3lxiioa at in tuning facility ad LaW,p" thaw to be A ea of PF9S . PF88 ad PM . Swoon will be added to eaft coataiar to avoltamot& 6U liae at 2U0 mL. A lfftd dapiiaro, a low Satd spike mod a hi gb EM sp" of each. am** NW be mileqad. no lpv : am ! WO lleld spn [e bottles will toe u ia PP85, PFC1$ aad PFft arwdu per&iowocMumio acid (PFOA) mod 1.2 13C p wftarcOCMaoia :aflid (!C PF'OrA?. . PFOA sod 't PFOA ara fioc adeain the t+*tf ets urea'to s pda t}ar .aEqpks. IM rawlts fbr PFOA and uC PFOA will not be, Po~ted in Ibis alady, Fxypm will supp)y one field Wank (oexrttoi vratat) mad two lkeld 6Ladc apsitet (ooateat water fo d iRaf with FP84, FFHS 4md ?F09 ztu Sow arid WO kW) ibcevory [wmuy iampiei coliaatad. At the 1 d aR Sa"tity, aaak Wnta Amos (wAWdm& Sold duplicates and $ald 4 ikaa) will be atLra ded in du~a~o and will also be * rd'lkd 11 a low mod ho meamt[rtion wi th PPBS, PPHS and PFflS sal ptocsns3 ibaooo the does ibed }too odw* to dsNm kat method "socutacy and to cbeck tior Nam. For aoIL addimmad, alanm. mod Yege4qloa, Bxygen wilt supply one 500 m L 1nec3aaed soii$pea Pniuo.W wia. mwo t31arL boal. p.t sample aon.aea or a zip"od k+a& All aoatuaaa~b~s urxt A. rwapip collection will be shipped to the mmgia tot ation. 3 empia wiU bt added to a" ooataiaer or byG in the 0" Al the Owbg Wkty. a" wmpk will be , vm=ed in &pli cate and s ffl -%M be betided at a bows caucanlntioo wGh PF'9S, PFH3 arid PFOS at botb a low mod b * "'ad p~occued t6~ the described procedure to deaasine utdtlwd aanoaoy itid to check fas bm For, amul`a m%3id firer, Bxyjieu will supply a 50 ml, polypropylaaa ar>ww toba Fatatnap Nov" unto. Egyp a witl aapply a collection kit tor nob 010400 oaataiobq OWMW aep~caaar tabes {Md soPk va09taiaM . rxee Uk holden Aid medler, trauft piAW4m =d Dob'D Wylana ujbes. A,t the ft" S anky, each 1[vdr and serMq ample will is mitrartad in duplicate and will aiio bMr"&xd6 od at it bows PM PM mad PFOS at batb ~ low mad higA taroi ied ppoporra~d ihca qJe tlsa doloabad pmra&rs eo dotixsaios maibod ae~micyaiqd tusbcck focbias Low and bid, *am' & levA fat WA mania am defined below: Maariyt I.evt2 L.evel ~V#Oer 5(~i0 AWL Sao go-maim Fi1{M LM4 1 . tft 40 40ya(z 100 nwe 100 nij, Y 10' 100 awa swan M Im ud Liver 10 100 aws &na1lM~twFSoeran' ld 100 amL i-0rse /DajdlP Exygeu Research Page 51 of 110 p . 52 Inte: im Repe+rl #23 -Analysis of Sedimcy: Samplos Exygen. Study No. : P0001 131 ftrim haeocal 1hoom I0001l3 t .~ ., Reoove* we enFScioptlod to be baavaa 7t?% and 13044 of be fowiified iaveZt; drswww, *e eotmet .pnaiqoe and accuracy 4W be dotu Wed by the ematYlis Of the qua6ity oordtnl emtlet dacrf5od above. A ataumait of ieoveaay will be 9nahaded in the BMW repoSt. MM T'tYdD FOR CONTRM OF M+l, S Conlrol of bile will be edtbtivad by takia$ mm-t wtive wb.tarap7e s fiam a b= o1paeous =MUM Of 600 Anruix &o0D Wm+aetod control Mmples, and by initytim et km Moo levels ofl6latttcirciomr. STA72MC:AL B93M~ E?jUB SttKiMtoa Will he 1f~1Ad to those fpoeilLed in th e subjat methods sad to the c~k~ ott+~rase c ovaiar, a~ ~ppficablw GL? STATEMENT All a Wtj of Via etody 4D~It be Orbrmad sad reported in compliance with EPA TSCA Good Liboratory Practice Standards 40 t'FR T92. The final wport or dpita Wkw (wpplied to the Spooeoe) " contain w wtorneut that the study rv*1 *=&wW in r,omp4feooe with cuerau and appiiqbk G[.P *wAgr& and will aadiaa any dcviap M In the #udy heist (base SWWgrdL This WRemeot Will be aigned by she Stody Dfrecm and Spoaux ~~ . R~litT A 4as1 Port will be preparod by the pdne W btveitiptqe or tbsir designa at dw coaclodoa a;'t9se Rady. iLe aeon will iuaimia.'sut will nor be Limited to, ft Follovriav The *anoe +md ~r oFd~e 3ucly Di~actor, 3ponroc Rz~maitative. and *few toetiat fiw7ity. A xWemest of GLP oMP&MOD (any miUted dowmmncion, ar,h as cb~of~a~todyreoorde,, mwt be in t9re ~wdy zeeesda) . AWtrolar Exygen Research Page 52 of 110 p . 53 Interim Report #23 - Analysis of Sedim" Smaples Exygm Study Ido . : POOO 113 1 FacyM hoWed NwmbR: Pooo1 ui s~ The aipW ad driai s4tana o by the Exy~ea Remach Quality Amamo. Uaic rsVrOaE a+tar of Aoaar m--rpdctiooe and dews findings ,rW! reposad 10 1w vkdy Meow so A dmrariptift of to =act awlytual oenditione =plolred in the atudy . It the subject waded was f4tlmired mnotty, it is aocaMry to include only a wpy ddt sNaaly" wellrod ' Any smW~ to $4 awdrod wilt be incoeponoad Into to seport. If d a method is pbolo-nadacod,, the projoct mmaber and ytga nm~tb.o.C. "mm b. e ityeluded on acb . pW ;uaai ~nd c~.'Dareip4noftu~kdga eouditiocx. AN mob ka A oob a.ipa.d . Control ad iloeMea = ple. will be ia mdrt.a .m she don abl e will Wewa., Wk .m vpbw m a ft*kmdw >.~eL . Rlprwebpittve Ckammowme the cub mlyu in e.& =av . meludins dromauMmu of k Nia A rd tmd s control *@4 lk and s c#uosnatonpa, at a l0rtUfaat3on lavel. The loaq.toa of the taslyle peaks will be clearly kWaed in an oLeoaa~to~ ~ All cnoanstanan that may .Love sOocmd t3w quality or incegrity of @)e data w91 b.e dvcvmented In d~ateporA. . i . IaoCetfoest where saw deot tnd Me MW report are to be srshlvmd. iABdW= oir wseetiarr 'b -tbe End apott t~t} be in do ferra of art aearodmeqt eip d by 16s SYrdlrileer,tor. ~s W4=dmeat eWQ clearly ideatily do pnt af le :epon tUrt is bdW shored end do rerotti fcr tba rl wvdau. The wneadtaetq wtf! be i(pad ad' deed by the Study Dkwdotart! sbe Spabeor Rgpreeanbriva AU tNpptiastbis t'qaimmenl: to rapoetiap of study eirrrultr per 40 CPR 79L1$S. SAFETY ANDHSALTB - Iabewimryrpamoirl wM pnopee good rraoititlioi and heeidl hablts. Bvwy te00o0" pwaaAioa "i7 "be Okim to prevent iwdvO cent eocpowm of. . Pon". K. idto .yavumnard qo the ma at reference ~(sI ,~ r,~. i~ ~*ks Exygtal R+oscarch Pap 53 of 110 p . 54 Interim Report #23 - Analysis of Sediment Sampks . ._ . . . . Exygen Study No. : POQ01131 sznm taao.t r7~t~bec: zpaous t r~ AM"DMMS TO Piit)30CUI. AU tiig,sd![caat changes to the lnttqlicsl protocol outlined hem will be expressed in wsidos. signed and dated by the Study Director end Sponsor )Roprosentaxivc. Amendments ttro:ily ..iU be usuod prior to talustion of study plan dmp. Hawever, vrl wn a change is required wfthout-sutl9cuttt time for the is= of i written ilqOpdAMSAj, that champ may be OffQCfDd verbally Wttb wppociift dactttuwUfoa ~ 1i~pd >Mqd , datad, by, be Study Director and followed Milk , s v~ritta . ~q0qqR at t0odt as p~dble. In this cam the eirectire dN4t of'tls4 adtiisp . toad4taw will be,the. .;ta of the documented i3MSn. Capita aP@rs s~apd asnandmicnisirill'be Weeded to all ditqnbuted study Plan oopies. The aeiSiael amendment Will be maintained with We ott&ul strd,* PAM Any devadoss item the study plan at ficom the analytical method as provided will be [iocnumod and mportrd preachy to the Sponsor Raquountstive- HATA RECORD IMVING lteooede to be maintained inch:dc do following (iu ppproptiao): s+mPl+t oticlcinS ~+tte) . SM+F1e reoeapt reaxdr~ Mct'e,ie b14aV. and doing of MKWY , Fl3Kaey s,a yrep,awdon o!'rta .xlarde (einolt, f+xui+lcetion, c.liewatsan) . Dam Wm ofaqy notiULatdone to tha metho d . Jturtaa~atmt sm :lroeta.~ tx lo~s . Auty~Cal dWi trbiee All cdroma4agraPkic sad io*vmaciat candiff" Steeple =action ad analysis dam . A coatplaee lieft of eordy Pe rsoarrsl, s4poom and initials ClKOedos CSl presentation ciao "* cam"Madsow Any other doenmartteion oecvwttty Jim the :roaonsttnetioa of the study Cdf'OC4t10gM01i- All obtomariooynnat will contain the faltowictg : Sample idaMostioc, #nfecdoe dtle, ronaw or otimr Indication of the am of bOk![f/t, and k*wdoa nmabir componding to the run. Additloodiy, i rtiHaedoot will WcJW* die eutowt of eealyta added and tie sample rttXDber of eie sample that wiu foetiffal. ~^ . Analytical standard elwonuftowas will additionally ittcnAe the aaa~or {a6 ., g7m4 Exygtn Research Page 54 of 110 p . 55 Interim Report #23 - Analysis of Sedimerlt Samples Fxygen Study I+fio . : P000 113 1 ExMa Pcoiocoi Nwabor, PM 1131 As pnt of the documanpatxi die }bUvsiag,sbaers will be, included in each nplydql act a nm 'iheeR lltft ihe penpiea to be nia in the aet, and an iaWmM"t c=WM= sheet d"dibhtg the inmtanan! M e aid 0peratiaS caaditiQm. . ~ QUALITY A$StTSA1~Ci The QA thdt of E "W ~ will' inrpeat ~ffie'ltrdy at iatervah adequate to urnrs caiwHanoe witb Gi?'.s, 'Od .wfll iepate. tb fiWhW of audib to the Study Tai wux, gxyMm Mwmpuwu~ Mod tAe Spmiior Repneaentrave. RETENTit}N OF BATA AND ARCHIVIN G All hard copy taw daui. {acladia& bat aot limited to, the animal cbmwaknpava, aadotbaW, a~oa0en~. aod tawta "D to inchMad with the daft Paela ~ submitted to the Study ~: These will be archived with the otisiOOat study pM . Kamds "m find report, and to patinas ~ inioctnatioa teorn dtia Spoc. m. oc. The tRSdiag facaitfr ahdl keep all electronic taw 4 m and aay imGUvraar+t . eqwpr=4 W Q StAIV bgs for Ow pariod at time ipasified io 40 CFR I93, Mi aadt capy of the Tnatanbt auborittod to the ~tudy diraotor will also be kept at ~.+tcyt R~airpiz L Sxyp~n vriil obtain pa:mird m tarn tlta stsidy dnceeior before dispading or manini muz Pks- , . t .;S : . ._ . - Pw !t of63 Exygen Research Page 55 of 110 p . 56 Interim Report, #23 Analysis of Sediment Sample,g Exygen Study No . : P000113 1 r~ - $z~puPm~oaltNunnDe ['040113I IX -"PLIM I ANALYnCAL METHOD S V0001760: "MAW of Aaolysis for the DftftvAbMflw Of Par![uwooctuwic Acid (PFOA) in WOK by LGNSlMS" V0001781 : "M46od of AtMlpw for the DalarminMioa of PrrAuotaoowwic Add M!) in SW by LCAS/MS" VOOOt792: "Method ot Anatyris for ii * Dperswnation of ParAaorooctanoic Add {PFQA) in Sefinwa by [.GM81lQS" V0001783: Method of Aipdy* foc the Daminmdon of Per ftuamowaoic Acid (PFOA) at Pub md Chm by LC.lM31MS" V0001784: "Mdbod of Andy* for 60 OdonmaWn of Potfluxooetanoic Add (PFOA) In Yq otdioo by LGMSIM3" V0001783 : "Idatsod of AaWpvis for the De em imlioae of Pori3uolrooctwoio AWd (PPOA) in 5=d1 Mmnoal LiT arby LCMWS" v0o017l6 : "2eWod of Amdyaia for the Dee minatiou of Porflo m ctaoic Add (PFL}A) in Small Mmmal Sams by LCAOMW Pop is oJ6S Exygen Research Page 56 of 110 p . 57 Interim Report #21- Analysis of Sediment Satnptes Exygaa Study No. : POtH} 1131 EXyVw Yfo mal Non}xr. P MJ 137 rauu.rnWALMETxoD wr~~ vanm ~lMYM~tA~+4~~rlMDMKa1~Miw K~ Aeil plO~)i Wnt r . , bLCAMAIi 9nm dU/R VA ism AW-42F r TZ"ic4 s. m~..sumn mj ..~ 4 r+ am" Uft" Aj* it eJf i Exygen Research Page 570f 110 p . 58 InterinrRcport #23 - Analysis of Sedimcat Sa.a Exygm Study No . : PO(70113 1 sxys..e~~:roooii3i i~~ irrws~.rwvoawnw uw ~rnr i >wsrBW (!!0A)In WNW" c~~ ~r Mi3aYeYtiurMw~y efw 3M t~~~ ~ rH 41 i~iwMrrw C~ro~b ~w~IN w ~ and~w etw ~D~nrcax*t W3ii lt7 M .~ r to ~ 21 .h1M'~7~tUIMNM MMIMMX}~4 21 CO0[A U qPPp~1Y! ]~~ 1!1l11i3110d1~L W CJ~I~~kt) ~t pOM~ ~7 3.! Sav o xt AcIWtMr1L~TMMNw~Mi~r~M~ u k w~rN+rawi.s+~, ..~+a .rrr~rw. 3.3 7+~1~ <Yal wOi~Nwtl +IwM p aMsw~d n~wllwMS n pnn A A mlrft mg b* &M%* 333 A~ Y~pUi e011Niit1~ w doi_ b~car!luNd Y~.3oD O=tF~ `S ai~IMWlrIerd wad ~beW d ~~ ~~~~ Mn hr t a ~i~ /~K w 3 SMN W rrr. 4 3 lV~ir-~[ C gM .9 IiMl"-@L+CF+r i.3 Aoa.rdMAiMsw - AC11u1MWQMO 4.1 PoOmmetrAw Mi/-sipr'ASMbi W ia~MOW d?~ S1 O 34" K POOP4 WP te 1 emblas sqwpw rii a wlfliY wWe Mp" d b*m*t 5-M {tL ~rwi u+t Mr01a ltw ~C iL~O NS} S3 . Aiv(ct i aY1W s iYlryrY ~MM M~+~~ i.Y A~iyV~Wreta~IN~hwiqpAl 0001 ~ !.3 l4wL~MIM~i3~b7A~l~~ Mf~a s.7 urL~r~ s.~ J~.aarwl~oli+t a.t f.1 . I11 ~t 1~fLanw~rML~Mb a st x,r.a..ws,cwsr. s~a,.r~-+~rM +rn~awawroo .r~a~eowa.wru~..+a+,r . 3as Nref~hkVMSwp~1~CL1Y"B~WM~ ry.~r+ .+. . 11 dim Ezygen R.esearch Page 58 of 110 p . 59 Interim Report #23 - Analysis of Saiimmit S&6V1es Exygasi Stctdy No . : POO4113 1 Bxypnl~otucoi 2~uaibn POOOtt3i ,+~ - . _, _~.~~s . ' ' "' ~rr.rtrwwwoeiw FP - - [rrlW~rfls A*% M-ON r+ry Jd2 ~l~w~n~~i C . ~ _AL?~r1i~MaIM~K~ir~lOrLi~biMD3'~waY700Pqr . 6.1 ~~~1Mlhr~dt (d "Mb 5eAxdK2.tas :loaia.l)+ &2 Twwwwww SK ~i ., 1~dWe 1ar1t1rreaf = AWrri2 Manr A 111 WTAMdNf1 : 1M4ni f S Oui~rlwrs AM 110 7f~ltiiiql 1id !Li a LmilU W if IS R3 1 .! is I6 0.3 ~1 2! TS 03 7pp ?f 7f 43 _ .- . a7,i R it 47 4i Iyf~dirY~irr ISMI.t~lsi~aMwtbua~slrSlN. i.7 QrN4iwc tsYckr-tioiMri~iriirtirtuna LS . >DrYtIC ~~alnlut /'b 71M ~r~~w1If11~wrrirwYd tstlw~ d rrlMuho~d it adw o ' e~Mdri)OIfip01~ 7A' tiyiNd}rs 7.1 LMMy1Mow~q1(~Mr11p1Iwo1/ MraimeM~{413-+369~. !4, iw+r S+iMlw we iiwrMd r a ! AO *d r+7 M Whwrd a bMr is ,. . W latfd d r u rr.w two Rtt - t iit,IMwO wano te wo lr 'v Rp x_ = a1~rf~arrr~b1K0a4d+^rtt. a1twM~l~sraRls Pasewl .. . . . . a . . 17 9**f 41s+ of yrxr' I'brtldojdi Fxygen Research Page 59 of 1 10 p . 60 interim Rcport *23 -~ Analysis of Sedicnent .Samp~gs : . RxYI~ Study No. : POOOI 13 1 . /^ r ^ ftypr, protneolAumbr: AOOO 1 131 ~,,~ )ara.+>+.r.r vaaernr - AM+tR UiilllfJlM yWl! 11r~iF Aei~(1+~O~a .. _!.o )~YM1air~ fi, 9ar~rt~~lMrw ti .1 Ts~awaaWknbtlorat-Joe /ylnLKflqAby+ao" 10aY atrrll~++~ ~rlri fw~+r+~ it /~} ad i{lw w ]00 mi w^ wAioi b s 13lw1. LDlEbadr. -'t.)2 AIOYiML~~INioROfROAMi~~b7Yiinyl0 sLo(tIM 100}ObL wipisa M a iri wirw of )00 riWi wArw f~s si Aot~l~~~~ 4 taa+. A ..~ia.wa~~a r13lMt tia~lMqr i.u A411~Irt~rllirrlsaorMard!lOAr~e~rNbY~ay1 0 rl.rhbLQf~L>rbtlerM+rMaltaY~stlOrwAsyr~ualr s .Yl3rail~lMfw l:Id A OM M~rt iMtMlaNrn wbYaw af7lQA h WMrrl by MiyiW l)N!b L r p a dl oMaa of I 0 rd )0 AaL as( MaM )lS 7l11~Msr1 . . ., MA rwo MMrriMtiMNfrrHNSSw lob* sbrMissnkiMrwmw qtpwdrrslplY ad Yro YiY MW s wrxirro !nd Q(6 sw') s tMV 8r d'Prl wdlw !.t SYrd~efC+ibwiMs~sirrws t=ft" yt) sa rnilii w plaarwa>1a~ tM ~rsa3s !~r lilaliulrw~i~ !31 16a lia"!rf 3s a 91+r1 ~~MiK ~rN seroatrapr aty bt 3qrd rawiit w~.v.,M ,rr*brw. rw.uwAM..wwr~sru.lrwa.rd.Woic.M.+.bww k .lar>t.4 r.~ aa MIN y :'.u,r., ftwrlanr ? u. . to a ts xa..+py ) )o . IN w it Xa .+bra )e wt o u~ xoMMryy 4 1M ~0 li0 X CONA J"1 4 . tQ4P XCIr . e 1M~l~rs ~TIr~Yirl~ r~t0i~lMfr ltillilr M av It) MI* IM Ow ' wlrrlb" 3;.MUMK4MYri0a OfYYr dsrlYlbilWt UM tro- (S1ff ~~ I~r111~lI~I~Or /lyda't .. . . . po~r iv aJ6S Exygen Research Page 60 of 110 p . 61 interim Report #23 = Analysis of SedicitCT9SabVte-s $xygen StudyNc . : Pb00113 1 gzy~ ftpWW Nm* es:l0001131 , . M~IWtr+! _ . . wrr.r ..o~wtno ~ ~YtiCAL I~RtN01 Mobil OrAW40 !rM +r Mii PO;~ Z isrby l.6J A Moa rriNd am" 4rwr MrtIV iimmmud '"r' ^a' rt .tro id m rwi ~3A tIM M400 W6 0 Mrllo~rrtllOlSrt.p *}w1tmww r rTCrs'C,s*tw*wY *j,f ~Ytyrare~~riariwiYatior~dRlril~te~ryirp~ndn AN" lQA . lrat9M t)p lAt 'tlM bri d rr6is worMd p~if 30 w Iwr? ww ir3A fr r b.90 wrt+! pWY6 flrk wiK F PLt .' Wvisr! rd ero ,mYM+ aAeeM YtlliM r Iawn aonrMiar tomb coo" WlRN to ,an1. ~N~ r~lwtt *Via" Vol 106 II Mf4 tM 1 Ptl 6" irdrV+lySWma 01~0 i* Uis ~}sL !tA _i~bIIsYrio~ . . ilA 17D L rl. ~p~y~tOD'!rr waMlM~ tds (lMft uNM. now ri0 rd 113 ~ ft Cr M awuW+ [t a 6 .t3 y P-* 10 r6 s11 Ili LOW on* G omammooddelL Dirrdalrlw aw3t , .il .ra DAY WA -S rL !0/K r WMrol t]Olr 3 st tt aWr !w O rbre .~/m~lrrarY87~ a1w G~ w~r' e W. d /^ t3ai us /vdlum.rPt++rft ir~s~ u'Aet! i! . . !.& - Ar~~rtr t2A hj%d dx lN ~ A ad iit+~iw d .ii..~~ ~b~. ~.i~i I22 !j'.W ma owd"Ol#ltOAaw~Mrla~tlworse~aa~rsiu~Mnh rtrlY YMW f arW~liwirt. A. rY~.lt of Yi01Yd M~YM rY1~rM rr! 10 YIOlOdW M IhP tyim ia{a! r Ib W of a wqta rt EsOMwt rA dr 6 . .+ k 540 WmFbL A& w ob aarrll m 16001106 r4' Y Y~awi 1i ~ b~YnK of ~s rr . f~~t by OIMMO r~rMn rMl - {+M tIMMMrW MMrft 2-t0 ~re9Ar I (ilt Coma 01l sl mo YYi rrldm** In i111r too. NIr wNi em@1Mb rYMM OM so M LM M Mllam .211 I^ _ /laarllaia~y~blYrrr,wrle~lM~i +~ ~+~' s rt Amp JO of 6S Exygen Rcseuch Page 61 of 110 p . 62 Interim Report #23 - Analysis of Sediment SampleR Exy.gen Study No, : P000113 1 r - ~. FarMaFiolocol?ittmber: P0061 1 31 ios .Mwa ww>l. .. iCaq/Nt :rrry ww+r~+riM w/n0>worusir+r4L ir~t3+a ]3 {aa~.~ .q 31S '== ir/ % t aNOni MM w1 w Ooorf li>tiY rotpGc do 1?.1 L1w~kSw~r~wv,~ter.~.Mlll.ia.1i1 ...0~ . .p.r. . id4#~ ~IIO 111~41~ ~i~AI NM~ sklMl~4~i u IB ?!pA 4kR, vlik dr . i11MMt 1w~a~rlSwM+~rr whn tfoUas riwiir. 174 lMNO/ VAN* am Mt moms FlUA a waM power ow w LOQ. ir a il sie wwdR!loAa bwY rra O a 30 a#tL, ir o we Weak wimph ~+rM M4ialr/r1 Yr w~b~Nt ~ Mn+rsrrl tlvl trwaiwaf11f~1 "M ttlaoii+iMOrtMYrtrw10.130"Kof 6 1r 1 n~. Vdw r, ra,~i. r~tr a~uid. ~h . na~ .rk wr. ~ .rn .. .r .. giMt *.Ilw be meow" A " nul1II Vibe OWIIM 16. IBM A i1 M wrYrw b do a+1Na e d- n - it sewcuwioe u rwir t 3.4 Ay eiYo aado 4 Awr1 n M 4 aMIMeY n tlw y wiy WA Rug am T+w ..r b .rsYii a.. iw ww w o. st w eWa>wi au.. 31lWMr, a 00 a1 OW .tROMIMraVbl.tl9.I/MWANk ,w .Mlw be iCpwRt il no avoid 307 it lit IIYf aAmYR of RLAtlNI tYMrOt 11,,S ~Wd n wndhdrk p1'1 Air dIhoMYa wwu poomfMO am N am {ki'i'09 m M "a_"~ w~ an aMiiY "a tloid. *0 "no be I a 0 ft ~MM wa ~I~irliwlblMtWla I .ii YWAtl W tlElr IiIAMm ardlei .*d IYoMW 41Y1 mat 16i1) Mart Yww t4xltliW~~ll~Ily~W7~ ~MOIMCMiM1IR~f~biYkilrll WIHII M 1rIp11diF~lrit~ubtryad. 14A Gliwldlr 14 1 W Is iirwiy ""no 1o qipAMr Ow awoMt r7RQA Avoid tin q+L. Mw t w~ 1t tral wiit O~ w~w4 wns A4ar swio~ ~wwrw~sf Maim d"o D! trs y .wr w. ~rrowr . wrYw, uowr~ry . lhViM ~ Exygen Research Page 62 of 110 p . 63 1 .iterirn Report #23 - Analysis of Sediment Samples Hxygt.r: Study No. : PU041131 r~ - Dow?rolocd Npnbar, NM IP0013 1 .. . ~,p.,a.~.+ . .. . . M~ihr~rwriao uar~s w WSW , ,J, 1w. .Ul w.. Yir.+. of YRw PAW r ...rpiex. w . . ,, ~'!~'r"x4*1x~iatrrrYWr~~~errrwwy . Li~i(~irtYr~Y4~LCZ -+rbM is ril in wrNO~fR~~ x I 0 0 r- . - r .ar u yas Exygcn Research Page 63 of 110 p . 64 hnterirn Report #23 - Analysis of Sedimsat San*aa Exygen Study No . : pOUt)1131 ~+ ' Bsy{et PtnmtYfl Ni mba: lM1 t3 t AIiAt'YTK.'AL 1 Q."[! OD NriW)~br NOOCl M IiiW~ .rAu~Y lw Nr ~ ifl~twlrW Ad~tlTOUi 6M b Ld~Mt~ AatMyYa17~MYi7+~MV : ~~ 3~ IiM~wir D1iw 4iNpDrON. TA 1 00 f _~~^s. _1ce~y~y~___ ta4 Qr~e/y 7ar~iw la~ LC t4 iay~r i w~rM Yiw 1~'+.o+yis~r.Ae7~a Rwwiel .i'{~yb4 Tim t~w 7piAft c 7 001k Peqs 23 of 63 Exygcn Resesrch Page 64 of 110 p . 65 Interim Report #23 - Anatysis ofSediment Saim*ks &cyygen Stndy~No .:'PO4U! 131 8x7~ts Ptolood 1i+oib~r. POOOI 13 1 /ti - p~~wwt - - iWtM.~rv~a~t+u ,. . a ~ Man" ? i S z U'l 7 1te wiMMile w Maqiqd itl iwYM1R si ~MMir ~p~rpne c pcwawbpwby va"~ 10 4 "&ha mat ~,~w>3>w'~'~ILi ta saw 3.1 Ah" NrewwrYwr+rytwWn 23 cSr~tier~4ra/{iletMbnMW7Nt~Y~~rrrop. ..A+r 3.0 lwtlisl4~rw1= ~ s.l .M wr ts a .r,waw" t . aaa~.. ss x. , ra~i~rtsn.aa.~}r R .. ._ }.3 ~Y 4~~ ioia tr. s#o .wl 10 .~itl~ol. . na,, N .~. .w. ~ 3.. Atl.~q}1. .~e~si~iyaisdw~.Mi~ .wVMlereawetle.. 3.f OwM WYaOr fMOiral wM be p udW h W w~Yatl I fM hr tatb >*~ a0 A~y~r/14Y~ 1 M~Iflc'1~fX7 1 ^" 43 Ml Pslo Aw"-Ar4X"W f3 04M &4 MaosowrioAoii - Xj erAliiaY Atl Yrfrrrit rr dqui~t $.i A IiN1 MiMu~rw i4W tlioMMm P lt apYN if /rMln{ vP 10 ] ,.r . .drt. tia.n rJu a p*w .r wOWas s-tuo 52 iMM .N Iq W_wrd A ~r ~IR r~M.~rwb4wd 4 u.W.+o.. 1.3 S.4 fO~wY~~YMtM~70~~~+ If wL~~wiiTt tl~wpyiw ahiip trbM. 133,4 Di~MlMifi~a~rlt#lblQO~i, 10~100~L} f.'t 127iI. LM wrmu4n mY raML !J IaWMr RllS4 MM1dt S! .AfYrMt PIP3.Itl A~w(tOP4000rt .~i40lOQ~,j,wi~44pMt~+ilp~. 3.11 1YM~ MRltlc Vw 1~ (k#RAJ Of w7t~r S.i~ UMir~toYi hplw~ Atjr da 01 45 Exygen Research Page 65 of 110 p . 66 interim Report #23 - Analysis of Sedfineat Sarnples . . . Exygen Study No ., BOp0113 1 &ryymt P[WOwI Nu4 Q: PUOOt 1 3 1 rqwt~r +wawrr wmixi !l1GRL~if'l7i0O ytwYoi~~3wwie oa~AW{~Ow}k6ailby LBSR~+lt . ., U4 'RNw+edr * +i w i.11 C'wMfi~~ilyd~ri~if6xLMbA~/7wMYq~1l~OOq~n Cy~axrs+Y+i~ SPUN . Q3 .t'+h~C~17~ay+1iw+1?W!x+~d~tl~q .tlxoaioxm3s 0~~l0 ! u r.~ .~. ~rc L3 Hi W Mrr W : 7 wi1 Au rwYr Aawt is WSW . . 6t .qMilMlr M : YrY d !.S Arri~ab .rs . - raw 14W Mum" %A as a* 10 3f wafto 03 !A f6 73 0.1 . . kQ 7S 7f 03 ~QU ts 75 oa . . . . . as ~ u oa ci' ~iwv.ww~ itN.~slrw+war .sa.r,.wpy. f.1 Q+rM~Nr tMRAw-+srrrlxtwldarkYnia+ar,. a{ 1tntYrt -2sxNOWL r~. Tlrie~taw/ioss ~dx a wiM Ma46+~My~d in dn w ~ir~Ye1!l,Cy~ra . - T.4 YilltS OyMID . f.l NNR ll~Mwy~ N~ptMT,iRM~ih ~M+iNdM+q .~ 3W ~ far P!0A.- _ 71w~iww A~~fIhM hol blwMda~ a~iU d pqr bsaMrM~ in wdn w . . to l~a14i6K1LMIYm i.l' lYirPlY I 1.1 !~oll ~I~Md~a ~NIIII # F wMr k y~vwd b9 fam Qt s 1 i sf ra~rflr YM~e w lWf a+t .d~. . , +M1~1~A~1~W{r1r/~'~rwl l . . .. . 11r ! N t Oak Exygen Research Pap 66 of 110 p . 67 hitterim Report #23 - Analysis of Sediment Samples F--cygeh Study No. : P0001 13 1 g=~p)tip/pCO1)~M'ibEr: F0001121 . .~r~W_.... . -,.a ._ . Iw~LfiA.vm~snl - ~ Iy iwltillw !A ' X OewdlnW aiR _ . . ?.l llWritrRrMlYdbatlerirlirr _ _ !>61- Popm *Oak MlroakWa(M~ir}ri4?r d % ~i0 1awHl+ _' Ywl~rtirl?fatLGlLbefb. '>i19 'A 40 WtrL wiUoMioa ralalqa o!!!Q~ M 9a7MaM ~Y ~^~ In 1r4 d** I00 ~y~ML Mi1MOr 1s 6 Mad vpMM ef te0 wrl ra~emN fwatflaLWClMaMr. ' AL O y01F~1 lw~i/WiMrWier rtlFOA M MMr+r bbn*do W . OLdwIO~L~YYrnprWiroAurretl0ev0AweOMWin l Iri ML LOILiOalr CIA AO.IRrst.>titMsiarwkOmaNKpAbpyrdfylrw%4 IJ ti aLKwrlAlMVL~WMp~Ik~M~MrwK100rriirrwtlwMw ~ qi wf.t37l8MW . to A Oa P#irL wUaWr rliwr K "DA ia M%W*d by MMM to OL al' Ib 4I PoiwL MeMirr 10 + tSd rMuar af I00 wd a1ralal2laS W1YtsOM CIA n680dc 016 l~YLrWa~ewwerlnrMrwrair~n0i~wra ~r YC ~d an aiiM br s rrriwiuoi ~wiri d6 ~I~r . . fir6sdMtKR~f~M rirrYirtVMMINr #41 wdbw1Yr abwk* to PiaNOi *Nqo *0 rose" 0l.Z ilMrrir o r pyieN wtryla rf11MaM rwrerWorr wr~ br ~rrl~ir+irl ~1lW hV*MCofa c"SOMMA"Or i calwam . . . ~ YK Yd0) ~ tf at ~0 30 xC m rddlY i 40 O HO XCamlrf) IM , t01 A 2f0 XMMjri4 Iw >e0, a $04 zcy. .aura '[Us~rdel!ErrrM~ MolilrirrMrOrdkrirrlwlxlsMmM 7 . ..riii0ti., w.r rwrrrrio . Kw .r.ad+wMS ~ ~0~x )oc aiurrr~wlrrrl~ w.i+.i .+. . . ao~.sa~us Exygen Rescanh Pap 67 of 110 p . 68 triterim Report #23 -Analysis of Sediment SatVla Exyg= Study No . : BQOU1131 En)'put protlcd NamErr ?004113 1 .0,.>r .n ~tcu .wi~c.r w...,Wy~,,AOen,, ONIMMINVOMMM MI VPKW A SON ' ~ ~.Z.3 A 1M0 ~MI~ ICMA MI ("Me IM bWIn MwLktjnom r1w NCt . l2.~ ~11 ~~10'W~Y1~11til~liW~1C1~#Lp01y~[OryAin h~f +t7'C+~ /'C, ~e pra~ r~ts fi! AM e1Mi t~i~rr~ ~1 are~rYriw of W~drd~ sry ispeproA o rrYd :. B" b17F IQI b4 Y~i d ammllm W mad folK+r!' 70 or W4 KIM foaWdc r 1ra asfmiMM somRI OrrMrillirt wiy S wiLat~Mrr11 art two w~pr 4$OWM eraYroNS 0* SNOW opcAy r reny *0110106 IOi U '~wr1e tw MM rrwr iphqr ad +P" +lt kJPOaM . 3~bqrlly~fipe~j+r. /~ il! 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An a" nt of wM Mi aY1Miw rrird mm" ar ;rWa r rr bw%m* id a ft ad 0t i moo !f. momed Gobi" a" AI iir4sw hwrw~yf-14a VasA~arb4r~rr~rR d _ .. . v Pop I7ofd3 Exygen Research Page 68 of 1 10 p . 69 Interim Report #23 - Analysis of Sediment 5aiMlcs Facygvn Shidy Ne .: POQ01131 ,.~ - . s~. . rtuooa~ ruanne: rooau3l "~ ~+wd~+ ~i _ ul~ts~e 1 . s~1er ir.w It *WNW wftnro. o .e m + . w.o~.a ...r s ~o ..~w Q+w~.wr'r a wiwt M +twn.er! rrlyd.l b dir carr. .suaew , . . 4`~ . 1~iM~~lYtM4Mlpt IYMi Irt 1~10iMt 611 wApb Ni. 11~ . v tJ.etWil ar1Ai w.+w far "..iMba LOW .qW liM Gne an ~ ")w~MIMlk arwW.b4wrnv ies oft u,cwAOft eto+.& .wa alieYw W WW n O.a4'Mim oft waML.yas 3.3 4at ehiMwn a .d+ w"qwg 113 tr.~it 1rtINIW isi/ ad d Aiwi W wNVNAM A ! owV W *w _ aMw~ .Unlti w~M dr.Y is EnThrdl4ud .r1 r..n .iY+~1 . . . . . . .a 413Alj^..TWw CYtAlk v, ` 11.1 qiwirilr.~lwR iv.' N~t N. MI*IM 3.u a 3p aw im . rrwM of 413 aa Ti. <Y! Wr P 1.t 000046 Y Ib !!OA Id74 rpiN M , .. 13.3 Fn1h{ ~MiM~irNre ~Ot NNIOW MA lt kvvk M~ MN It IM LOQ . if a WWRArYin'R1KM R Iwd1 ywliriLOl6 iylL .. MMY a .w bi aqM "M M .1rY. d rMtM wrw " =rnM rta MMt 133 FnwM r .f OW" !pW ai Mruls #f1a. NM I. Dw.uM ?I ;- i)9+c of tluirll..~.a ~i.a Y . .a~lni qir ia wridr t6w as.q rlir soft ALt . ; G Ib Ad ii KNOW iwIY he sakaMd. Aq aAfta q it* awaN A. 170M ft* be " wd by f. w1Nc e MeeNs if 1040moa 1 . 13/ AV a .NW .s .b@W 1)wd as be a Moil" Nt)<.r by wiy flr 1ia p 7iwr M w M aairdd Iw 0~ ~YM~a d do aNkww awe. lHrw~, ta UY r~ir t aA~rt dieair Mri~lr tlre wat !e d.1.i s.d am am" ]a Ord* %W ft.*w 8( ieirr, 11l- ' Ifr wiwiMir ...NAM p1 tre WAN" wiM 1 MMM ru be KM 0 s2lt 4 r .er. . u ..r r w *di. e w win, ,nm wpopim OP Ao M pMM q sQIM 1ruM mMC qwOM al Iht 19,f 1lYwft ft" Mta1~ ArM k ad ;wFM.~s~t a~it dia ~ urn a{!i MY1~1~Y~.lrr. 7l~M~ipAdJtpeM~~.lirh*M~m . O~ al~ b11.1M 1~1#M iH qI~lU1j7~. . ,~ ., hrar['f flpjs7d O/4S Exygcn Resemb Page 69 of 110 p . 70 Interim Report #23 - Analysis of Sediment Samples Exygen Study No .: P0001131 ~. _ ~,. Sryyaa hdoaol tvwmEw: POD0113 1 :w.,.a...r ,,a,, M Loae.r~ ~.~ . .~~ ...~~ , . x.r Rlw rr t~++iy~ s~www to oMpMl. C~ . ra~awtotr! QA Mww t a~+tYrd po/t sW *ft +M Sw4t or" piwrr mvwwkw prwrwvc) i~+~brialYr LS~x ~M-ar Pe ~ ~ p-llMw b~M rrt wMwr w+ItW . Xawwiwrir it2 I s 11,11,11M bNti~l rMt Iqv~+ rwnwtM~ d 170A pinr is aieu+iwt w d r bMwit sum"* odrMM}wpr ,"tooto o arl~aditlA/Q~ w ctir r. rde .r e "p+It ("i "aA s .tbA)- w+~+~ts~ 14A t~r ir riarV~{ .~rdw ~s .~Y .rra ~ . ....e ef rro,~ tow~a : yp lw/r bvW^ ma aoww W>tr www -nwwa W" J iaoxR,r uwus) PAW Oja i Facygen Research Page 70 of 110 p . 71 interim Report #23 - Analysis of Sedimerit Samples Exygen Study No . . PU(I4113 1 ~rr.~oea~ t+~+la~ eooo~ t~ t ,ix;u.YMA s. MWnsop ww~w . .., voa~m Ml1~1~~FAM1AMArrr~~~ 4PQINMWct+rk ACM RVCW M Aw q*d ItiMiylYeiYra i~IrC~~lA t6qt , A})wvwl ~I At nM IF r 4ft4+i .2MM a,w+ todl~c , Exygen Rcswch Page 71 of 110 p . 72 Interim Report #23 - Analysis of Sediment Samples. 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A~a~Mli~lrw~1M~t~wlMKSO.ooooi ~ tA lOatli~M~ry+ .M~r1~111r .1r s! li~c.M~.~w.>MlypqSl. .rl~.w Si Dii~r~LMwiwy}*4ti~iqt,t4P .lp~1 .1 !.7 ~~rL[~Iiww~~eriYMBra ~ Z ~ ~ )dL 304 1re1i/aM{IIFI00I L wt 116t00MU. arfMiWpoaMqa W L S.Tt Aa1 mfAtatWri 8 t (3#) ICifREsr3irw M2 IITd wtarr raiM . . . . . _ _ . .. . ~+V7it 1 Pbp Jt o/'6S ExYBen Research Pagc 72 of 110 p . 73 interim Report #23 - Analysis of Sediftlent-Sarnysle5 Exygea=StudY No : : P[l00113 1 Bxyam Proload Nmo6ar. P000 1171 r ~ - ~~,,M! *r.i~rrrorna ,is Yw~ . ;c,d1A, 1)h M W lwrlrb& )X'11i10 KAU (riwJ+ ty iG . Q~MM~~ tt J~ICda~cllr~M~w3C4KqMn~td~d~b2)w~x70an~ .)y rw pq~ ~ [I -?wPafaw C W ilYOltwr(Ay : itliA=od=Awrs)oNru p WOOMW i f O~Yre"i~a Plow Rw ~Mlot 3 Y 12I 03 )a ti! 7! 03 u 03 ~ u n w 72us 83 3s cu [u blow= UN~ t6rt(ra)wYarradrrrd a SorLl i r p.P(rMft twr AM -nwaw Wr+d oriiM .wp .~n. . . i:! L.1iws u .i~ra Tlrww~nMr.. .err .+rr .pMl . .ep.ywae~~e ;eww io .pr.t .r .Wcvr.: 1A 1O+1Qi~M 7.1 ! iWU rYO OW1Mlh 1a7I aoir. ~i vt)3 -.360 .z for }IOA. TL~ia+M~Mdir w i~rrW r a*iM a1 er~rA~dwipd'o Rbr a qY~JM ~~ r1M~ a i3 l~eftpiqr~ i .) iiMblaw t.t.) 34 wMwMiw Mww Y w wSr Ffi)h' rflto3 RI3a Y .t . ~wuMloltqOaL~f~M u Exygcn gcs=b Page 73 of 110 p . 74 Interim Report #23 - Analysis of Sediment Sainples Exygen Study No . : P0001 13 1 l~ hmloao! tiuaabir p0001 t31 Lvr..lr..~A wr lrrr w~elxx ApaY1GYZlCAL11~fLOa s~.~i~!)cf Na~i - ,~mGr' ~dfir a~o ) M bs I.tY~AtlI ,_ = ii LY~ LiMiw t.T.1 IX Wit ~d ir 7MIS i11KMrM 1Y M~ni W 4l Of ieA! /W b laoo>.~.r .+r. A~r ..i .. .v+.ra..a 1s ~clri.Nqwd~ r `iti :! `flyr~ s neNc 1rMrfM d+iOG ~bL it i7W Iqr weip~u~ ~J w0 . . .. .drIT~Y111 FAM i~MMMr Ao fwMl! 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KOilOd ~y~, MdIwIMRMIltMr. l.U 7fr ilqelrlK it+11ow 0 ii0300 did" nwasusiou ay be .elr~t.4. va .r Dwr tiYr.iw+u. . . - 10M 10 ! 10D S 100 ! .0 M10 3 ~m SA it 10 i00 I A a 1a is a ~0 1w ea __ , . .,---.., . .r. .---_ Pap 97 of U Exygen Rmarch Page 74 of 110 p . 75 Interim Report #23- Analysis of Sadimen(Seinples F.xygcn Study Na .: P600 113 1 r- .... LxN,e* bowel Nmbw. P0001 131 "Mew, qddMwir~'Oan9a ~ ' - tS~tHq fi3 ~wn~lii~..~r~ylwt37- ml.illiCarso "arn boo" r1~CwiC.~wdswai li lYwlrt~aYrrWrwrri~dirtlrd~eylrp~Mr sMUi 10L iVIiLK~ 1 61 irk iMiY sl'+i.lr +duWi pP wDf 20 K MM) no irly* K Mp /rt VOW m tlwYri M meb letl6w it ]w.~ Mr~drs Or "a d #wA *TwM111 "66mm * w- 5 ><* tle hteA. 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Ca" 9i NArw ad W i w Y 11.W 4w13m s +wwiCsN'i1s4wo Olti 4aw efI-'NiOai . -b+d MiM~rtDyilrl.iCillLCvlMt(-2i~/wt} paMNt~oMirsw~~dry 11, it AY io frArd 0 -10 wi. st.rs id iW a ft iwoM ao "m+a s~.eiwWt. 17. 33- so *i1F5 Mi, 104f1 e20maol Calla i sL of "N iwo mrsomd IiaRNhP+l7~~~M~w W~1oW e' f ad.) . 11. 1 3 N~1/r^iwri4~o?ICYT~S s.~ e r+ Aa~r 3+ olas Exygen Rtsearch Page 75 of 110 p . 76 Interim Report #23 - Analysis of Sociimm* Sann1es F.xygen Study No . : PM1 13 1 r~ - . $ayj0a Partied Wiamba : P0001131 y~.rr,,, Ir.rw.r ..vm.lxr a~u, >la~t~ou Ada crrcA ~ r 12l i~e ~ fr~ irr arrrlldwM AMA" auyM Id Old" wa*L aro>M , tSAqRi~rr~ ~r. A aalbWra 1Wd wart pwea6r W faeaw all ~at~}pA.Qa~aMflriLrrar give .mu .awwonw.ua .re+.b ~rs.sYeMSd M w r~4~Mni M. lu1 +y. OWN M d .w.lw .aMlk. Now" am bs ;nab" . tac . . : NOW* d aft ~i ef s p1~N M4 LIeWM am be hlup+nM Ml "M wM'!' 8-10 wMb& N M aMw I00, rr Miw rM a[ aliMnwm Am" way be WwMd a M MOWN{ Of a wt bMOwM Irv adi0rrb+ I~~aY iryMraM w~ry SdQ +elOw I.s w awa IN a NOW la at IMpIWI~ id ddrt Wre. n1lo lies *am" a M a Or Am ad Law r~Wlala+ra>a a ~ 17 .4 1M Saw OWNS urvw Ox lweabodw Lirar Mwdri ana re ' ~ri11YMi~irr!1!l1Alb~r~~t7h+Ai~li~ai~Ikao ~fsr aaYds wr~ot eerrbri~t I~illt AlrN.~aR ).3 (a ~quWWi+t ~ hr ~~~~ 6191rlrini ~ 1i.~ Aee~nwCMre~ ly,f fbmiew arw inriana Pwicafiir o lari n at3Namafm a "Ma elNU am na il l aie pn rt aaaawwY b to MCA aeiar. rYe of M {7p>~ nlrwaw~ Mis afasM~Mo11tM. 139 ~b4ds>.rta 0400ia IlOAatMNY ~ fMa MWQ. Mai 11M * NOW" TlQA st b"U iarW 9 m 93 +rNi.. ON a war Idol; r I Atses -aaYuinl 4 1 Ar aie w4 Nert Mwarlwd i13 rrrwdr Kard I~r a I No 4 a" art be l ettrw 10-IAA of beibowr ruMrr. wa Itrlwtqb "Nramo tlr w1~1~IM Ipniwr. N . . ailr aM aR rM1~iM MM~i 1M ww~wqK Aq rrb ~ilu aariie le. 13 * *UK M .wr vit N. wl} * a Mmim" if Irx" M. is IM Aar M011 MIIN n &ll[i M1 Or b s aYliaa a10i or bY riy tw MW Saw ? A MI be adLinl !we, Or dwiYlm of ft diMalioo swK . N . a1M rwlw at oeoa Ni aaNnli: alydm at N . nald 6 ai~orir . .W ..t mMa 10lY r ri . au Now of w.aMM mw.a~ aS 7f wrlrr. ..iewr w r we1. w ea .,.. ~. ..wa wwl be aaM aP iasW uwr~lt /.Oft *n W alr *AMP MAN, UM *kip No Owbe his amom boom" p I N . eiw oWrM w +M ._. _ ++. .~ . . f'~r3Sof65 Farygen Research Page 76 of 110 p . 77 Interim Report #21- Analysis of Sediment Saasples ExygenStudy Na . :- P00113 1 ~^- - exywa raroool NneebR: PM) 131 y~,~._ . _ . ~. ' wr,++ww~~oa .~u. ua~mnn f~ 6 a+r"a *11i Mii:i. .rrrr et Moto rwe .w arta .m u .. . :y a . . . . .t 4l4~iw.a~ ~..broal ~,.. 1fal~liwu..,w .e.d . r . r.n .~a~io : ..aifliw M r 0 wae mm.br .dYrd. t44 4~MM+Wf.n v. r~+wr~i{+4~+~~w+r,M ...we .crrwlra,aww~~lw e~i ~.~c +~rV+~ ~ wdud ow" (OW wfww w+~en+ pow ~rrw~ .4~ .a~ ~r+ d 7lCNMrIpW~t?Qlltlu~ 1v10l1~P F ~ 142 P* nj }! bim11 mal fow{ m0lib 0r ltQA 0[iw b ovate*. is ~~(Ipili~~Ylio~Mt~id~lerr~wwlvwsrir7 1MIns1(%~- . . ~ ~ dlM~1~l~L,2' ~MJ~b~Mbao qr y~ {yrd.~ y1~0 w~l~adiri(aytaW 41 .ar~dqQAlrreia~t r 4 " y~$~bM~~~~~nArr !ldAh wiiNM- ~N~*rlKOi1 14-4 t!~ M lifwin w~1 w of ~7y -mlortw or ~aro *("OA , ~ri~~ilwiaar7~ }KK 0++r1rywt* .tloAtamt 00latlo0'% I w l nkiI(Mi) . . .. . - ~sKv Pop 16 rj6S Exygen Research Page 77 of 110 p . 78 interim Report #23 -_ArWysis of Sediment Samples, Ex,ygm Study No . : P000113 1 8,ryp. P+olocd Muker. taool I31 uMOrncAu . MWFW u rtOOtrlYr. vpool'tD Mad dAMMk ilYr 6 Y wmY190w rtNe/Mnw "60 AM 4'rtiN A iW A~yprdi~MUMf~4 : ,70 M* PtWr ipN{kiMt !A IpOi ~ Vioslhwidw, C~eM wt Rx7lM DM A4**r . . TMYlyc ~ PW97 af 63 Exygen Research Page 78 of 110 p . 79 Interim Report #23 - Analysis of Sedini~f'Samples Hzygtn-Stad} No,' .- P0001 13 I S~eu r .o~oeoi xns~ar: poao~ ls I ~ _ . ._ _ itrwrl~_ . u.r.r+r.rwri~a AM4YIICAi. V )la ~ -A Cluatb~SC1~1! ~ li! ~ONIl~` . ~ , YYh auk i Yir MyMyrl (w do WOW" NW vewft"Mmm am b WM rahmam GqN QwirMPIrYY No01Y r a am" "to smormalods Doman il mmm ia ii mdi+t,ea - .. . ' .r t . to Lb 27 en.it Y~ .~.ACr.3t~01t 6Aws Y~ .s w~aiat Rr aava aby %M* *.~.~ ' 34 M Mrt76 K/Ma~lrwtaaqos 3Y : i~1~slr~war~/MMw itMafs 1b. w 5~.w ~M w . ~ioliIl~+~ei~.ric~wlYMMw .Y>tfyio . rrrra+.~DMalioe.w.~n IgJad OW a* ~fa *ANN WNW ..~d Won at 33 s>w~tb .www. MewW eo wrl M RrafW r iM. weqibs r+r ro.,hi. 4.4s MiAS-WAIAp1a A. ..Iw.-lis.c ..as 43 c.w076100n.+a-AwwwpiM &i N$6rY-!Pl.C "1 ~ $u W j .aXo .* go* .. cy Room Pub 43 l .aw -N1LC p+. 0 I.AMrw ww-1ay .t S d. 61! AA IApiddoRilr-byNt gnB u 1 Taim - Name" pub M 2 AwrailMAa~r-AC/ ><rr~tOwds 613 P a I Asi!-lf~a~Ai/dr4 3 0 I aYO~rat><0} =ir SJ A LI* !wft~ kAd aLowYvqY aMbls of 1 w p % W n 2 wi.wr~ ~ ~!M aaM~W wM~r h~wMr e~Y1e af i~s s iou rl.wrrdbaere~Zl~rtrrYw~rO G~OM1li1 U AialwrwlM.c~.rirfrprtiaY~daWqnWrNr 3 3 ArlrintlYre~MqWadrw+tl~MaC~mi ~ PM~{v 3d nJ 63 Exygen Research Pagc 79 of 110 p . 80 IriterimReport .#23 :- Analysis of Sediment Samplas : . , Exygcn Study No .: P000113 1 E"$strumeot %mhr: Pooo 1 131 ~ _. on Aft"MCALUM . Fisk ta s~fw~pa~ s i.! Ti~rlYw ~ ~1 . aid7ii~~Mi~Yt i; u .cOOMM POWIPO -*'swab- $3, xN 0"48sw8c4uux+s.N.w ..{.M.r."rOdac,.M L uo04 s~ii ~peNmo ;srruaa .U,.;+y..ra .,r~ ?.lt i~laiwt~){~~xa.tl!!lCt7 > 6.1f` illitraiwridMt. s.~~ a.r~Or.~~NWatyi~arSioa~i ~wa~ir~t~OMOevo 6A " . ~!ww 0.1 IIJII~i{~ (51i~ 7lMMYM x} pyy~ ~M~lill10 .1 IM x SO vJn. ~V - " (Mtt GCf~li721i1 42 't ' WC 6. 3 1i"Alir W : ~1~11~rr~oxirnrte~q t~waut 44 MiWMAVM : WM11Y0) 63 GqWWO? a 10~ ~~"' Pbw iw 3 MOoYi 7LA !ii MAW QO f6 b 03 u,o LO ti ri 03 LO s 73 w as w sts ss ss w . . fi Y~r6+YY~s ts~J.t~~irwrMn~rrekrS! L> V (}w dbircl~lcAw-aYxrtsrrlu~wl3~rausaawc fJ IWeTB~ -itwinra . " , " . . 'AtilO~MitINF71N1Mrddrapiirxod~yb~olr~rtinodaw . yO~IHItAr A~C$rrs _ ._ _ . . ._ __ _ . _ .. _ . . . . . .. . . .. . . . .. hr)d1 !n'` tW 30 vJb! Exygcn Research Pagc 80 of 110 p . 81 Interim Report #23'- Analysis of Sediment Samples FAygtn Study No . : P0001 13 1 r~ - 8ry~aa T.o~eooi N,a~i~a: Pooa113 t ie ua 7A I{iMSFjMS ' %l Waft 3> wvWp' 1IIMWMR11l1Nd4wo" iV 4t a r)6f avi kt PPOA 7riaMwswMiw rt iaMNadaF a MIM aet ary M aY.~i ia oar m _ . a~driYtrlWf{q~r iI PY V, >ZNr rw. LLI ! W awriar awYN Y wMr ir r4nr by a61<rI 0.134 SO awAWMawlaM Y tqD Ml. d+iNR, U ieYrift iWB w t31 ifYa naib .tlaaar.att PaPta0rr WABeh M s{4tre .Poic "MIN UDwLKaNlnrt. L$.}" ~01L 0" F~ teYra fa P~ b' Mr/ia{ ~ w~. Qfd~idiMil~+ti a ari rol~or ot 1! wl i0t+dliwa AMYw~wY~rsa~Mle~ L !.1 ~rd~ip~riirtlrlMW s ~ct ~ M.fti Yw~rw'twi 1bireft) Md 4 fi o f e M ML' + h% sw.w 1. utOS u1l7t tnri. l.L7 A1Adfki. 1 11 1 w1MMwefT/OAiaAwr vA lryL.inrii t ~4di~ 19f nYr. wll/iM p s 5111 trNaati of 190'ri16 m4nol L~ 1~! rWt!!#a~it 0.13 `A A1 ~ML JitrdlMlW mLWft Ofp1 QA 11 pwpYt Yy 4iN 10 albi M 1901aLoYrm r - bY veMti of t10 Wn . awo in . . 4i9S ~b LGit1~M1~ 11A Q t01 r,~i1t, Ytl~ ae>tlYo~ atlf0~ ia rr~rtl ly Yf~ 10 aal. id 9r 01 p&%L ask*m p a firl yda~s of 1 00 +dt w Awd iR a qf aL t3118LIM f.13 an MA r Irwandw wlriwa v lo be oared in a nltSWaar a OC ad a* k hr a easLae ywird afb mood* foe~~reiNy~to,Ml pop en Pb~r 19 oJd1 ExySm Research Pagc 81 of I 10 p . 82 Iaterilr. Report #23 - Analysis of Sediment Samples Exygen Study No .: P0001 13 1 8t"en Pmlox ol N=bec 1'000113 I >~ . . .. ~,.,r.~. >M..,.~+..,..~~ cia y t~ClrctAC 1 r .A+ s.7. i~i~iCyMk.desiwiar w sxAMMSas~l.r.ta~~w}wtr~t3~s~an.~Ih,dlWa ;~a. +.t rM~. aa+b..~oo .wria ~.112 . as bi..d.~ i t#iw araNa ar/IWw .er.lnt3eu .v M ~rR~r MMd _ .. _ . vow rt>~eYrwr VOW OWN * " . . ~~. u LA uo r.ql 1) 1,! no O11 am Na o" JIM N Xo kmiS UI N 1N 6.OP1 . . tYl~ 1 a~ew~moalh la/a _ ' R2"C~NC.~qfo~asaaEr. . ' l.7.< AMIMIM teMMNI Md OIEOMIO~119~ otsd+ds ~sY b~ plyaw0 a . trN~ L :A4 fnWibM q 19J W 3R~ da m ir "maw ftkRSy a a is* mm Mlodr R low 40 O MwMit am" ad to fq1" f1~tA bnilYt s pwn w~o~alliA W M"d M VNfMPNMwN AM+wy MIM bob , ID2 tNbo RY inlw ad 606111110 WvNt wIM M qM Sq i .u. ~riky rrerr~Ua Iir Rr t~iw~. itt ~ -12 of f~wo 1rw X wi, pinp~yN ft a+r iAyo too : t~MR.P aOm*K vwm-m i Uk mlp. 113 . AotaRwtd~wr.MrO~ .rrRo.m .+niswr.r.Mtar-ilmi.w U4 rw~~rww4~trwrik-tMrr. ,ll.t, rat .larrlwwwrSrlnbwnaRY ft ew}w p YWq.a Aoki, -tls [at IM 16 iVi a bm i n w pow wie 7 ; OaiM, 2 & milw V b 2 wra,.r iLt'rl~, CwMMr 11r Iww .;a m> .{. of mrrow, tlr~ i~ Nt otRa~W)t D1rN W rWa no aac Yloo as MNnM ~. . 21.6 ROmIK to i73 ai. Jomi"W bib by rwivg il` tL 30% ~wi~iiow~r Y MM ~w ~e1MY~, ltlr~e dM xNY ioiw awe Ills 1186" 1&0 Ms/iwy biAn w% ~rd~pY~ i~1lr+ rMwru~~~kl .. . . . ._ . ._ . -_ _ . _ . Aa ftp 41 of E3 Ecygen Researc6 F`agc 82 of 110 p . 83 interim Report #23 = Analysis of Sedirimt Samples Exygen SU* No . : PC00113 1 r~ - Furyyenrroeoodtd~ loao1l31 ._ . . a.~.~.. . ~ 01 wM .r.~e.neo ANAAMAIRTWD 60 OftiNc> IMO..MbyscOcNnanOOftiaak AvW MMOA) in FiA OW It? -061kop 1ho 74 ML )of!lop~Mr sub" "soft moos s -ZWD qm . .- , ls,t-jDwa MMwqatalw .amOSwri71ler11w fUdieridrweMiat /rPa11y11 NIdL COW Or *am in In 133 N, niMNSid Par'O W AM 10 ML of a.pYdl. TA Ow y.p e w 50 ML ..sclye Whit iMwl~iMar~err>titllw~tatl~emrilx ~{l+MOna+wriw~ ilullwrlYwMM-14ai+P~ irs MrW ixia 7f"1 .tr Mitaar-10 .r.rr. . .ewcd . 'taw . 11 .11 liMf~M4i~s8~sle-tlwrw a i1 .Ji QrYIlIp 4 11 ML l7RlP1 Ww --inks +moh r-2C00 me atir-1~~IrN a 11 .u oMl.c so mum am ft .. . alls .lyne. CAW r . *MAN ame oi r+r4mW iwc .r uaw .M s. .Moir e. . w WW .l~.de. 11.14 14.Mw{,afaa.l~Ytasiwo +rllf .alm ,o1 . .,0'w A. *-ft ir tlr rrr$i~i Ork 11 .13 Add 34 610 of teMrtiW b 1w OM 4 Y Wad r~ ilbe+iiuw~irYl~~lr> w~w~p (rs~OC~ ti .lf ~w~a 3fi t. &W,*. by aid{W 2 M. st2AG riabit rW i. rsad 6@t . MN M1*Mwdd w WhpMwoM a lt .it 11ariMtisMUSww1{Mt,C .1MY wOyir, 1Lt $ 0 t2A an .rr16,11* 17 WM~ . ..areat .aM .rr~*~pt .,.afwrsra~ksead. .1 LCW qMaa A wiiaer MWoM aMt pyW at MW IN Y~/ IIIIMIIa 132 i~ilKl~lriAMSMq11M1q M1t r/fwrra wsenumm Iwh wMN tricWd il1 Yi1rb1 Y M. lss /a .~. wt ~we.iie.aoinr awc Me in.l.+~l rt,r M ooft old w do Ni Ka 4*M w. llydrr wiwl M Mrf~W lrwa wrr s i 0 yMMis Asa irf.w r wdr w d aliatlw rnYnh ar 6r 1N1ow1'* M lNoris nt 6 on b ftrM by OtliYwON *ueaw ~ iflw~Nw~tw~er3de~i1s11~aaewe#aMe~MawatiwMuri to sow w" w64~ 0=6e6 at M to En WA IM Yyeebw is a owPkK MA -EYF'Nwt Mriii aw St qmmYtYeawb 1Jn11wMWbp Wiwi re ++ e~iw~i~l~ONr~~srwa~~irY~ lf~rt,Ts i i {er~ip~R~l " . - YOllr~yll0 hrr~xf ~ Aft. - pa~t Il aJ6J 'ExYBen Rcmtth Page 83 of 110 p . 84 Interim Report #23 - Analysis of Sediment SasrVles Exygen Study No . : P000113 1 Eacy~eu Profoool Mvs~ber Pt~W i 191 r- .a ..~rw~ xu~.N~r.+~aonp ar~reec~ arreruwta a .e~x'S'G~a .e a Now am am" mom" cwwo. ANY *Nwa ,ex ~r.ad =qar. iaid III llaOw +dM k ..a r ..waa ~u Acoy.rncara. .114 - ly~~ am aMw a D" do +IN*Yr loo 0304M *so a pawss ~tat# ra 1>te 4iu Mw NNO mYrmir r Oa p1wDA wow +YWr Is a~Mrr fw(~1liry a1+~aa~ ~~ otaAOadA~ie r tXt Y~i. t Yi~it wt ~N ~rlri?!OA ~t Iwde ~rwt MNa IM Lt~p- j r . IIMOt wO lb T/OA Ylwra =or W 1/1~ 6w s oav block ewq N wt N~Mwat M~a wdw 13 t><Nw~iw a(mwt Ma W M 16i giw art to IMnw ?0-170% at lMlIM! ~~IM. Yi ~MMi1i ~ 11~ 01tr~ tw p0a/~Nt ){ftlR ~i ~a ~ il~ IiIA!f O 111MII1~a ~I. 13A ANY a INWIaa rrYwi had to V a Aids" wa'ir by rieR the Nvys Awr TO, aw M auala0ad AM Is dbidm at sm wlbcwbe am AwwM Is ow loci e at aciftwMi 1M161M am caw b. waYdd ar~ so ami IQK d7MMMt mobar afMrYma iqo ri. 13.5 7r YdW aO aM Nalatl M 61 piilMwOR 11/M ~IMtalai/ OW be i4lli Ge iAl13} V NpRyNa mob Y OW" tYrs feia. 6e. +vM 460 MP as be err u "a Orrr~.ot oamiea. as Is srbra ti awmm ,w qf awaiw Awit M combat 1I.4 ROOM dwu YMwM wrMrfi Ad =ON MW eat Afii WAn Is. 3~71sIWaitlMllRklts IteMIMC~M~4adnpaMNMii ti~licr~lMiw .r1" 7. .0. 60 ad A" be {NYyw 1MO GUiwMaia.a l<i (1sMtlwL~a~Ml~larlrYM'wtarMtdlPUAYoY[byrol . l+llMll D~'pk i{'M~ 11~71~ i{II 1111r1M1 oMrf7 (/YUr {~i0p /~aRMpy ~r!!7'blt~taasMa/e~a: , 142 1bON/owir qta~a~ to aowwt 1M rioo[d!! O A lard ir t~1at. p u/yy16} ]fQA~WaIj (1! GI~Ae41~*ii~FYdrd+eM~aariM~l it~nr~y. J4w 410163 Exygcn Research Page 84 of 110 p . 85 Interim Report #23"= Analysis of Sediment 3arnplcs Ea,y*m Sbidy No: : P00p113 I r-~ - sxyl ra rroO oaW TlwALar Poool 13 1 ,. . w.t~.r+. . . . wwrwr . ~rownu .rncu. e ws 60HMir qWos IDOAUN**s poem ~reNry1N+1' ~ ~~oMaMiMi~dfaY1T ~M~i6sasarttw+atl , tOD ., . . . . . ... . ~'ii0'd~ID r.MSr P~S 1~ oJQ3 Exygtn Research Page 85 -of 110 p . 86 Interim Report #23 - Analysis of Sedimeaf Samples . Exygen Study No . : P000113 1 r. . Number P0001 131 0Unimp ANALYIIC.AL MBSi)OD MAW-r..b troo0t?W lGiW .f Ar6o+ lr f. aw.arafr. .t kFAWS.n.He Aw Rrotis r . ' Yq~YW~1D'LCJ1f~1M~ MAO" Taft$ >4dR 3~M DiM lMCaOlp,lA Sinl C- a. x.~.wtrr.i.aaac, a~n~.rw ~iwdW or.ata ft f yqi. Reab M r,wr.~ t 00-Farp sJ of td Exygen Research Page 86 .of 110 p . 87 Interim Report #23 = Analysis of Sadirri<art: Samples Eaygcl, Study No . : PCDQ1 13 1 r+~+ Ae- 1DcyyanPnloxoi Nmaliac P0001 131 +nw~+ wi.r n ..~ Mon ne ANALIMCAL ~ 1 f~ q~uhw tR ~ ~ " hkMMYiY 1rM+~6i~~rMboWlwY~i~rr~.d~ Ural madaw Haw 20 iNYqr 7.I Alr~~bww~AYtlwMnY/~~ 22 C1ri do 40priplrs iODt 6dw iraCtq my chow" for Peper wqx Y IIKrKrM. 3A h~>, R~Drro ' ' ~ 3.1 bMisi l~l!~yrr,~~ ttw#w0oi t 12_ ir a srrdr .Flew Sw ime ample a NMA ism , l101 in amp ~~d~1 M a1w /s tiba dwide wl PIw IM wispls in 11 a a! wr goo tirs o! alio~ 3.7 S"kiMlu "wai rr witl Mop"ai in is rsyfls yYs fie, tYb 4 .0 U*Sw&4Aft4* 41 Rt-1p3CPftp 6 r 42 Awmaleib- 43 CubwtU4406~rwoft-ILwpmyM 44 FiM AMN-IZRC Vale 41 lrYa (d0iq~r1)- Kr~r. iYb l141~ ) P"M 47 tM~tRupnf+e+ 4/ I .ONn~-1a1JCpM 41 LJ1w~Yisrii-><wrtMd~ 4100 DIwMIpi~MlraiYn-rlw 41 1 iMMmi->ficav t rnis 412 AsoYirAMYY .ACI.1bMrCeb a.I* 1f a arrieAdi-#~rAYi~Y !.~ Y~w~rsaraf~rr Lt A Y~ Prvrr" _ ~wplk at Prli~i ~ b 2 PL-- "ek"AMM"Sposimas w 7.2 AMlwiewMR~.iYYN /wtMMqErraMlwpwrbs SJ A~T~iwlld~ar4ibdw~r00000 ~ I+Itf 7 Exygen Research Page 87 of 110 p . 88 'ritcrirr. R.epart #23 - Analysis of Sednner"t S;~mples Exy$en Study No . : PM 113 1 J^` - Exypa pfOaool Number FW01331 byy~l~ tNrl fMiM/14~Iw t400l7k ' ~ Rl~N Yi7GA1 .1fLTNOD ~Aw~b :~n w~ gpwftwwomm Md i m YyrW+a IryI.ClA1SAO 3 OWr 33 231 0t p~i1l~dYa u sa .~r~r+rr~rr~~~ ~ 1e N4Mar1l13~~~ ~~wo+ta s ctiCDliwr 16 .! ti3ilYerIO .wLC i.11Y raa4 7.Tt DI~lr~ !Ii' ~Kl13(~OQINOilLa1i14~0011ta .tdll~MMi~ti~ l13, ~"t~LIrd41WOM~ataaHllS7tt1). iH 1MNr&rYliYn. !.u Cwrii~+~1M d~in~4sle wLrM~rY~ rMs~e 3mo ~n Li t:1~41~Ik~lql i E : ~cay11r1L11l~li+~i~f p(~]w~~J2.1m~lOmw!' AqL ~I7fi Cti SbqiraMe 7rC 43 1p1A t!~ t N* i wM Awwo~ Aew b wrs L 4 35tXLltC3 (% : !{MMM 1.5 tt~N~[ w~~ Imm" IA ao n? 2" ~ X 83 13 25 a Ilw. Rrr ~ i V ~3 0.3 n aa n a3 33 0. 3 it WpMf" wMrr! 1eNI {+rf~w~wawreMw.r3orw i,9 Q~1#iM~ Trt .1w~-s~rrfwdrda+lfYstk~a:ra ii an7Perr -T3~rr~ 7irYr~sro~ilile~w Y~wd~d r a~ii~ ~t uef le aMyN ir odlsl~ 'ifir~i~ItttC+s~ is MMO tp*r t.l I~MOk EW~~q I1M11lM /Qli InOM iroMelYy ~t3 -+ 3AYb+i ~t MKkL P~f7qf63 Exygen Reswch pop 88 of 110 p . 89 Interim Report #121- - .Analysis of Witt=i S=ples EXygcb5tudy No . : P0001 13 1 r-, - .4..~...w _.._ ,_ _ . . ,~ ...~..~.t~.,~. l 1~0Mw MMdld r & rl&IIYI MWtyldrli b MrR b ~bii~ 1A11ta~. i1' iiililYw LM IN" w.wr w r~ .rr r a+1r++ b~+u a ~sa e er ~n~iww+o~~o1010idwrr. R2 laliiwiaa 7F1MIeiN ta.1 216~ww~rMiYaMYd s1~1~+lr7~oi2lofas~Yie ~fAi lQQa4aftlWrl L2~ ]Y!i L~d~1 Y NM~o~ 1s M~ by b"A" ] Kt. si~pdMrNa~tlr~ M alr1 ~aYrr vt i0at ri~ rYwN . ,. . 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Mnwltb auu .f,ynd, 1M C1dwYWi s til SMM~eaft soon Y+wlorrY as aoomtatlKlA ft tl(taMAO L . 1M/ q a OrY .a* "iy b AN"l w" tir.r r~rir FM+*ru.1 iiMMN b~. JIr L~m r/.rrt O.opw: l!O fl.- tftMti -MMLjM&jW eMA sops Wp w Aaa .le~. DO i .MAYMiit IM frl ydM. ~ ttMrW. Krormy. A~,IMt YMr~ 1 0 _ . . . . . .__ _ . . ~qr.rv Pop 57 #f65 Exygen Research Page 98 of 110 P . 99 Interim Report #23,- Analysis of Sediment Samples Exygcn Study No . : P{100113 1 ExMW imfocoi Nanrbw. P000, 1 3 1 w~ Ifik f" U lt+~wusbu~Ml~ti 4 1'oN) lf t 1dr~sdii~i >Mllr AMowu rheanb of 1!'OM prkr a now" we . . . ., UMklM~di~itws1sL11 . ~~aNNt~I~J Yll0 .' 11.3 Undo, w~ loan r Mrwc 68 am= oftlfCM i~ai Y iyAd, tr y+!'tll kY r~ ~i rw+r ~ attt~r~s~x t>rrar ULs " .~ , , .. . t .. : . . - r .., .. .~ ~'~ .. PlYf M 0/6f Exygen Rcsearch Pagc 99 of 110 p . 100 Interim Repa-t #73 -- Analysis of Sedimxnt ;samplees Ezygan Study No . : P000113 1 r. - sa9.e rmmW rammbw. PM) 131 MAt.Y3'WA04tTO00 ue"+a..rr vooerrsa +rr,rtw~~t1are~txs .sm sria+.) IN u. s ,wt~w 1~rrir~ ~~rat . ~aw~ukarw s+rr W wr,, PA MM MM++K s ~ ri~~+acaU'lQ,a~la~rd~ ~ Dr. Pqs ss afes Exygon Research Pap 100 of 110 p . 101 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0001131 r-~ - a<,~ ..rl~e~a :~ rooo3 ~ .,..a~.,..~ - - - .~...w. ..~w~~. ,~ .wi.. ricna~cs aid by M# Fw* .r .ar t *W Crw . .~ anpra is a aaam w~. ~n~A t~tsarit+~ W >~ wWdm. 14 lsa.~w Ak p .r.warirrrwrrOw.+a 12 CwUtbM - W1i3L1fMliw~iYo{a~lyaWieaerp~ra~Y~r~ ~A t~Y~prrw: Ii- AtN~t1 NlMS~r~r~~iw u ~e ~rrw~M eww ~r ~.r. .% + a a.r.,w ae ws~w ara .uarw~~ ee~t~4~tr~w ~ro~.a wrr..w~. rra. rr. u moo k +rwao waaa . wow w.em.d ~1 w .+o~r r~ r~r rrk 44 R.ti .r..a*wwr ai ~r~ie-lOf~fi~rpr'- 42 k 1.3 ArMW l-lM fw M A~wo~iwAawr-A+~i>Z~~ct1uM E.s 1~b~warria eail- llip AY~i~ so I ru+rnsSw 20*w++ zt A W~ f.irwrr b"i Mraw~ynM +w~ at r~+t ~r a i wlwMw~t ~ a+rWU wivr iljwer e1N6Y et i~jaetlwy S.UO N.earwrlsEtmM~lWri~uew~ p~tA 'iA A~IMlI~U~MIMaw~~'lUR~IM~IM/QwWlMlbw. i) Aa~i~itrildroampoY/rfar ftn0A9M !a ~K~Mb~~Rw~1a IA DYMrtiM~Yro/MK{f6NA~L .140W00~L} i~ 1~~1 .1~ lSawa~ulw~WllMlw L 31 DM/ilwYryi~MK ~I s~a A.r~t~r .(lasioas~t :riasaar~.i.r~rprr~ru~a s.lt 115~/irliYn6ar(>A1~Cti~lltarrNM w an t~t .wrrw.nrf s-la v.n..r. . Awl Ay~ ~rd' d6i Exygen Reseaneh Page 101 OHIOl0 p . 102 Interim Roport #23 . - Analysis of Sediment Samples Exygen Study No . : P0{}0113 1 F.xyyen Pnol0eol Nup#br: p0Q01131 iyM~rrd 1(rW~f1~M~171 ~'~11 . IIMV~ Lns i~r I.C/IOM S ilit7~iMiNprpii~af~iMil~SOad .P~71~YM~~M~OW~p~. ~ .~;1 :F,~~ ~IVir~IWt1Yr~lJ~iw~pQ~lr#draitc>,tiwwrl4w~r~fN Qqt ~16~it1311 ~ . M~wr~rc wC i3> MiiUllfU) : ZrltAs srY M ArYYW'Aorr 34 " 1t11Ml.~oft ilMllrt if : Qyiir3~f~ nolow %A 12 OVA" x r: to .# I" tif 3S W 23 73 OJ as 73 063 S~J a M 03 " . i.i INoMiowYYM~c t! L(MaMkO~MMtirrand~r3bYL) L7 QW MYYW Ta~kANR-MMH1YOfW M~~llbawttw. . 3J1 1ta.7Inlc..rt7riulY~s. ""+ iL~la~ ra NMrrsi~ImMd ra 1+~~ rd +urY brAwM M i~ w0~r r ' +Mi!~iir~I1Ql.C ~i+Y n 7.0 yllTAqf)o w 7.1 aklK lrrwa~r~l M g ei.. MM wda+awiM .hr 4# 3 -.3 0 on wr l40x. Do MW SW /WW W inrid r a *MU 00 OW M aMiyd 'c mtr m i.! lu~r~Mw~~!'Mi+irt IL1 IO tiOalrew ~tta 3r.tr a.a.rr. r.r . IN .rw I. awrnr s waft a i " 1, at rrrisr,r.~s 1oMwa . .t+nar. :.r~rr~s~wuawri~ ~+wt . . , - . " - -- r+wastr ~. r,~a~ofes Exygen Research Page 102 of 110 p . 103 Interim Report #23 -Analysis of Sedirl"liedt-Sgripteg 1 ? ExYgraStuO Nb : : PO00213 1 . . .. . $cn n rYO,oCOt AOmbsr: Poool 131 '. . . wtw~wr+n~ar~w ADt~14 Koko ~ _ ' ~t~w1~1 awa brLCJM~IS o !0 . ~Wlbd?n~wion ' !.1 ~rri~ilrelsA~atlle~drastw e IL .1 In~w s/INkw Miurt *f -100 yhnL sr>!10A lq .doYK 10 mg sf IrllJrfli rYwAvt (i01Nt~ld Atb/witYl wl *Los w 100 mL rI H . . , MWItMa}ZS.M$LDlF.Ia ` 9.I.~ A 1 .9 ~rYi 1MiMr/w N1doa ~f ROA Ia ~t~we0lry YnaYy n~ - - ~t.di1A~MN~wlriwbalrtralrrMtDOwGb .+rA~oi - Ya11ltiLLOl11MMr. l.t3 AAtrMt.lVilsYarWbaof!lOAu , a~wityidapW l v r 1iCot>ri.OAaYM.wMM4ooafaYoYetott00n!iikwiwmia s7lSaLLD!'lYMIL 4.IA t1aMMkMitAll~OYl~a~i~l~~nlnMaloMdiaawf'i/MMwr ' ,~~al~ 4'C ai an ai~Yis !Ir a o~ ~ sC6 woniM l~Mir~t~a~~a ' !.i QYMM~/QIINMliiMJallfUr !it lCR1~~iWulii>i~aspea~alNlatMWYvL~MwiOn adlr.0i ><r~1~t.latlMoMr wYwYar. 042 !ha lOlr** } a pNUY be 6id*09 40014064d" my be . ~a~raiwwaMt ~.. , - , .. . ,f14.1~arYr r.Y~r DMaYir O~u.MUW . 1 MR . . L to 2.~ 7ML~ am 1.9 sa . H ta u} 11 !f 1110 !3 11 A IOo i iYpMnN 17S" LSWR w u vo.wsrhYcttlw .., .IM2'Ct~f'C, .MMliwal~~L a,i1 AYaata i~Yara ad sawwr W fMt atxrMrr mq Y. pnprM aa an" tao srtr>tieUrr :. )a~ 4R Y+dY .t+~s~+wYr,wnr+l~iWq 30 of Yr! s4c iw~ ~ Yrs +r wrrr1 mod ad tws +www i aMOY Y1tlaC a um wraarr4rGY~+~rrri piM1 r .wi b rt+~a+wat ~w.. .rr ~+r Y.e Wril+rwlh Rall OW ltieiw+y **awn am will by ApKir,ai is r.yiruq a .a.o.pi o a aM Ow* L _ . .~ ._ . ,y. 4 .1? ,... 1qr 61 ~lE1 Exygen Restarch Pagc 103 of 110 p . 104 Interim Rqporc #23 - Analysis of Sediment Sampies . Exygen Study No.: P(140113 1 67w PlOIOtW Naoiur P00111 131 /~ . , . [thY>iM~l/i fiY~NrWrYtMO17N 1/w,i I~nw k!' LSYI~ AUi 11A SMlloit {tMNN~ . ttri . Maw 1 a11.qlsompb bb a!0 Al. pYyparyMr MM[aiow 4!n UwUy w an" aq Yw Y N! W woo, tdw fix alMnw rdrs d Mftr lsawnUM+tfta SryrayM do wmbMU fm w. 7L2 AM~InIrie3frrMlriRallri~olrseK7DSi. CNrtyWy .. , 3d3 YMl~4~~1o4iY - ._. ILA sop*' "- ai *t M o oMr %44 a fowAb wmt 6r a l3 Al. . ~lM~~1Mtd11Mi~il tl.i, dii3~4atwlodrir/abir>it-O~wfASraoow+irFw6owMrec 11A t7ol0lt/rMr 00 144 M4qw ft -4aiM " . . .t (~,' GM w 16r+ p11 sRrC trs a f0 ai . 4YgW " il I tattt w am 11 ".4 wwm ItA c+rMrw+W Co Ift *4 (%&f .t.T vjavft to s.w ..o1 IOMMbb+tfltt,C.~rwt~2 i.plrrl lsrt is rar~ w dy tr* Ir~Acwyirwa~dCpQl~r4idM p4aolil .wa. :LIO RAW vAR -4 Wi. K aH iwi^ CatYS 2 al, etrkr be* a va* rrl I 1-11 LAwi1waw/Irwl o siNwyiqtCAW)ML ~.` . . 4'.P a r1Y 9~(~fow ~ria KarY aM~~ aaapia~ 4r[3LL~ +na at tXAI'iiiilr Y~~7Mra . ~ A wl~Wor iwMti ~aaw Inw~is Aid IMMw &tl i2.S ~ dllfN Mww~wi~ o r 1~wt Anvr aaweamorKrrin krd~ . iwaxlsinWalifanril,~dwl+t tv $III w tfskYfqlNwtlw mp/1ldtwYlli e Aid" tlln Mw ios a" at dES a&! rf sarVir as. 'ierMed arc Mt iaNipwrd bwrNw r+wy S io aar*lw As W ~Ya Irq r WAN me of a, llorNios Manawr may be **"A- 49 do Mw twUr g at a wt l - s~w , be aanadw rawiYr irtr~rn! wcp}14wyMstti aawew t owe" otra8cil. M 4dow am tJ~1Mim An dltit xwa be dlt d'N M1 An i{)MYeD is > o t%Cz 42A An limper Mrrd tinr ir qrudptlM^ tirr awrY arvw m sr~d 1r1b asyr b iw e~ rq~ vw ~wpqy w!~ aw .rr~ saMinltaa rrW! mr~rK4~a ~ie~ lti~t.lr+s Yf t~r oO~i+siar) . w~sr^~~+14a.. . 1~5 L's1s .rruw rrW up arwt NwIN a~rrwi. ANY q M1M+ wq a .r tndW1 wWol iw +MrlO i,s hots Yb wd Aid wr41w. 'lit, .'.' rrW ai4'aa Exygen Research Pap 104 of 110 p . 105 Intrr4rn Report #23,- Analysis of Sediment Sarripk9 'Exygon Study No . : PO00113 1 lxnm rn. wai N .mbw. rooet t 3l ~ v 7w .tr~u FAMMOnommm* A" MFOA) Is &=I YYr .r awe y [siwsw LU tirmpr W;pyh . .r c l?.t - p~tie rw r?rtat~ ~ayrr rw r~ rrr ~ f w .~ ~ .._ _ #~ rt 7L N3 ~w ~w1 o~wl~ark lo Yr MwPA norn wayM uw 133` YMiI1~1Md aiR~iMt a~iMii " OA plow *M tli LOQ. tt a . . YYSk as~Y~iS17lRU s NwN fIM !r 10 ~1rL, qw a aa YMt ~ . : _p1~MMtMpWIlMlasif~oMIDMtMilb~aql d - Jb3 ~tMatlsa K p~Ni/Iiw M~Mhcl~ aast ! Mtswr 70 .tiyN sE IYrlrlYi~w V/si& Nswsid qASitisWiMttwwa?lYliria, * e rWi M M> w Ir *=WIN n a,YalM. +V4'+arfs ~ie arsitle /M1 v, i7tlf fMiil fav "aMt by so wiWt is OwtYt it Mitmtton Y vrwirL" l3 t y44aY~wM sfrird % q1 r M a MNUiwi aw0w y rws iYS Mw IMt hi0 ww by swam We W aNriris at am adiedea esc*a llmwal Y bri an" K eOaY a a m"* I" to" bg "OWN us tYsr.tat ws wuMw?.O4K0+a0f4M,asHwrl mI.sobw*rvY[wmr.N. iss.is.inyaIm W ..rr aWa be auwQ O' muss u owAu .s NNW rr as" 66" h :,.. r. "opiMe s p wr be wcm r .4rw s.iY+ . ma "a.o,w ,.u ft irrWMaW sMnus of~lo AM M mw1fM m* 144nIM am Vwl waft* d IN w w aw 4~I1 aw Mu -. . .3~1(~(~fYSYNYbYd+w~ NnwadSawrsOEtWSSitiqlioi~ .idY, lP nMtll*wlwnAnlwMwAbwwl~pi. . . ~'t0 . ~i~lYfOY! ~- - ltF . , , Y~1 +i1 P* Ulr) Ube 11 YOiMt~ .. ~YIM1iYlYlMt.poaoisass0sspawc "00NI04 ppratMSI . _ . tlOYY~rIi$SAaL~~~y1t~Ml. :til=atl~setlLmr _ . . AF~i1Mr y~Y0Y11riiari~asJlYrdYaloNW} . ~IM~t~l~s.~p a tt?' !Y +rNr arYW .MY swa wrrr sr ?Nn t~a m usrsaiac is. rr i~rlsa ~~ f.aYslr d es+wr wwsr jY~wt.nh+~Yrr~r6~t t ... ~. _ - -Tp~t 4lal4f Exygen Research Page 105 of 110 p . 106 Interim Report#Z3 -Analysis of Sediment Samples Exygtu Study No . : PWI13 1 ' Bx~tl. nwoee~ r~ Paooi ~ }~ .~;` _ ani i._. _ .. .~ .r.,~.~+u r.w.i~.ra w~n~ WON of A04" are* R~ a ~ terwrti~~nn Iq st~ti~y~ .. . ~ ~ . . s.is yrilw+oMwr~t .ri~J1 . r ...w~ w. r,arcarero~ +sw o+~ac. u~ . _ .. ~. , : ;tltlllwi{~?. _ . _ .. _ . . . . .w . .4rn.irs . ._ . . . _ ._ __.____ __. ._ , . . _ . . . :~ 1 . . . . ' . .. . . 4_ .. . Y .. . . _ . ~. 1~ ' .. . . . ~ . t^ ,. . . . . .. . .. . . .. . . . ... . . _. . .. . .. . . ~f ~ ,t _ .. ~ ' .. ., . y .. . _ . . , .. . . .. ,. .. . . . . /~A/I ~ ~~ Exygen Research Page 106 of 110 p . 107 Interim Report #23 - Analysis of ScdimentSamplet -Exygm Study No . : P()40113 1 Exgen' 30sa ReseW%h DOW Ptaw: $14-M-1039 State Colare, PA IOM F&%.91+231-15M pwrocamw EM" M,ay tbrillfer'~,~ OW sa+dj Nun+Wr:__hMDL_ 1) Arwb*W Prc~o~lur~ 3~mwy 1tQdQ17aacSer~kx, 9 t 2) Ya(llCatlon of Ar A y kal F'raw4tre !) Add W S*t don 9.1 : 8a~ck n VA Alamele weloMs d~rrxlerds may b e uMQ to O OP INS aksrt NO be M teaitr'aYrx o C( sbCk Pok+rM a necassary. NEwnMb1 iwds of fnt UNCONon wiullaM may abo !re ppp - end. 2) LOW and rdph spl " b ak a to arWyw for each mwbc ntiry be shared deperdkg an arrn~ir six. a valah ie tar -tr~oaae arxibr !Q oowr ae~yl. aonarM~stiar ~+c+.d tnu, . ..nvi.s. 1) ~~~ d sMnartiw need b be p~.pw in arwr ta .plio~1d. a~rr~pi. 2) The slrmft go Owi{snM a s,nA ma rw* Ow ana .o un was nnawr a m I a+ " d. 8PAbV at ft pr40errnt~d bob In the prr,looot pws to spMced eanar~wMon ~ow.r b~t f~r d.tidan iNt Ara ~ ai~t)At NNek kt ~r pra~na w~ wnpb, aitl ~padsd 1a Pe~ly px~sd ri~ pe~ .d~qlte11i~1 apAcdnQ Uv+rie KsOrd h the Prol~~cd rWMi1 tto fwNs h rir wn~iM pb w moved ~ spAdft WAls. a n sQSVwY nwwwy wMo arrwt bo e *AAWa ! ier #* QC ms pM, f Mpl w rpift bwir in fN hoWs YA aoreNF * srwtyh,COrloeAlrw oa 1o~d In to wMsr s~t ip MMs JUPAff The LOO is 1 Do n" tar . Q.1 9 .004 i. of saa1 nrm~1 War and is laao rphni. fora 0.01 eN. swob d and m anW *sun can be used. of sai~fio br 1Ar wNe~ ~pNs w!i aur. wM n~a. ac haow~Y ara ~. . . ~~ uewuer ic: wMrissj : . - A Lk AS fto n c K U R ev iew J V nLLdr . NcwwmnvE POW Exygen Research Page 107 of 110 p . 108 Interim Report #23 Analysis of Saiiment SwVles Exygeri Study No . : P000113 1 RE5EARC H 3OS3Raimch DrIw Maw 01+272-1039 UM Callepe. PA 1E8Q1 F1nC 814231-15l0 Anlendmalrt Number. atecrN+s o.te E*pnftudy MWmbw ' PROTOXX7t, AME7dDAAENT -' 2- PrpO 1 d 1 PM i31 ._. CNW8t* Ntprbnr; None 1) EiRpo papr 11 dfif 2) Taq Mf1eAI {>wpt 8 d 8 6~ PF'88 buwtron mq0wrod 400 OR t) IrM1~.Q~tonRDnMl~pprt,hNrtn~nppbiNRE~irturd ' Z PPaB trM~itlOrf ~nCMCr~d r1~p s~D M~ s~0. BUM & 1) ON a t,. saOeriM c fNr dtM wb, Waft ieporb we be taw rd b alc,w to a,t io r~w s!~ ~, i~a.~.r ~rr~w~ ~*.~v ~~lba~ 2) The Awaoac LC u M 4~ inns dud j,. 4v*z-eo PFoa t mw+ww g a w tl `ihs al,nt wltpr aE~ir ta ~N. wxtlM~rw IN~ dxa ~e+oc~ q~idi~r. i) .Tt s 460 .a 80 t Mor~ an be dejj~ with prvw iRkll~r, riwv1a., Vm p b.arrd,ron~MaPa~fg~. ' ari k 4r ~ Now" . .~ .-t'o_,- os < AL Ew,,qa cvw RrN .w " ~ ,: . now#OrrnNnWFaw Exygen Research Page 108 of 110 p . 109 hderim Report #23 - Analysis of SedihawSamplas ExYgen Sh*-No : : ,i'OOOl 13 1 n4 RESEARCH 3058 Rr.seanctt Diiva : t'Phorw: 814272-1039 Rite COik$G, PA 1 6841 Fax: 81423 1 -f580 DEVIATION FORM ~ -. x Arajsct specNio psWdtbn _ fat~ity~ Exygen .Ptq W 0 : P7b8tPM 1 31 Cosnt Pn j sCt C NA t7~a uro~a,rreru:.: 01128108 DQWatiGn 0 : 5 PMa mact # : a8.076 X GiiiP GLP ClKiar Na+n . , .. Qvkft Tvoa ` flntA ds V# fur waatpds svad X, ,P vioad, M00 4M1 . W NA Matsbooh niaanaa ; NA _ ) SOP Login* - Lb : s z~ of mime : The three sedi~rrrt sqm~ea h L~i$1. (cDf ~28~,~ CQ1~xBR4)arsne a~~ ~ ustng the se~l+asrd rneit~ad.'~D01l3.782, Paclr ihcc~ltieK wKl+~ abtsfnad laFP!1k3 a4 and PFt}A, BVsuss ot`1riia,tha A* ipaisoi reau+~d'~hi ua~ ts'a o sRs~iM axtrm;6on for these oo~mparxJs, es ~otiows : tNract InJaatic~s MstFwd :,BMab 1ha seunpinw~ets rvsiqhwd for fhe sz vMn. they were rMxad tbwo u00y 4y vipowurtY *i ft the oonisbier A antqtam pation of adh " vat weighed iMO a 154m MK ca *NuQr tube for the eztraclinn. TO mHlqlers bt 1'X acetic acid in melhend was added IO"AmMufnp L The swYoiw wars Mon r( w k61i br.r111W. wft%cd. and ldtllcalad for 11iiny fTfilflutBa. The simpins irbre than aPn6'ruprd for -10 m hAis`yt 300CT ipm. Each sample wss ertetyteQ by LC/MSI AS its0$'0iPuip. 4 Using Oft mNtioQ acaspfibio daft wee obtairrrl.tor PFM EiiAffia rsoowstbs for PFOA and ft PF DA w~ :sW paot. AeroOWOWPOve tri MW was men used for PFOA aAdtC PFOA, as blows: ilf6Nntqw on meow. The sampM that were prep red in t',K at 6k mw for the dtect injsotlon nw01 od wrers used for 1nY axtractloz. -P1wTn11W1 ers of aach srsrnpl k waa alkpuolsd Woe 50qnt. prrlyptopytaiN asrtmps 4jbe a r4 the waYxne wm td m b 40 mL w%h vrstet. The samples were teen +ce,wt(upid tot,-I0'mipu4es at-3Q00 ". The supwatYrM wat own', Wo d ont o a Cis SPE cartriQpa oonraBono '! wb 1D mt ol mifMrwl and S ent ot rwdK . ?ha ewats was dlsqrded. l p~@"hv rMN bm d nieihei'roi was added b Vie i wtiidg e. FAe mWi Mxs of s1 m a was oakeeW Woe yradtusbd 15 mL potyprapylrnts wMrUtiqa hbs. Each umPN' wa s anetyzad by LCawtS!lA.S aNecOrot~raY- Csusa: Preperstkr _. Analysis Insuurnak C ft tt R.quNt X Other has& Mon usable data was abcsb+ad . LBRARY Mt V0000404 ADMNWRATFVE FORM h:xygen Research t'agc lug 01 1 1 U p . 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P000113 1 CFtEM EHait 236 18 651 733 1958 05101 '06 13 :46 N0 .106 03/03 WN-Uu man 1vw#wm=jff1w P.M= r-111 ;,`t. :%' ' WS ~~i~ ~ ~ C~ ~t~ ~Y + ~~,, ~ .~~//`'~ '"~++,1,r~ i~~'r . % TdiX ~~ifr ,rt~t r~~ ~ iwr'n ~er~recte. ..,.~!'il~'i~L .~ f ~ri-fr~N'"~r , * ~ ~v : ,~ mitit .~ w+wl ~i s ~OUI~ + /~~1` ~ .wi~jiir,,~y~T; { . . . . , A.r{ +r ,, ~'r~y~ ~rS '~ ,'}.. rr , } .. . . , , , . .j ~~.i"~ sa S:i'~ . . }~ '.r ~ . . . ~~~.r\'~~~~~ f , .Y J . iiF ~ ~ ~~, r, ' Yt ` . Y1~4!l~4w+~ '.'l7~ AYrF t ~ _ '7} A~ ~ ~ ~`~i~~,~+w~ s l '4 . . ,. ~` , , . . ' . ~~ . ~ . . . + ` 7.` !F"~IV ~,,Y'Y . . tl . '' ' . /J , r : ;~r .4 q{1~"~ . 'ti ; '" . . _ ~ .~ ~e~'N+ ;^ Y . ' , "~ M ~, 's t ~~ll J ' .~ y. . .~ `~ _, I . : ~`t " ti' , t. . '~ . t+~ :r~ :. : .j~a'r IY j . . . '!. t1 ''t ~ I. ' " . tY'Y . ~ . , ' . ' ' ''~ ;~~ 'r ' . . M-~ . - ~ .f~ . ~ '7~~iM~~.~ .~ Y Mp . ~ t r ' , ; ' ""~ ~};,; . +~{: .', . ` % ' . . = ' h_ r~ . .+ ~ ' ~'t ,7w, , ~ ~ `+ ' i ` Y ' ',i~ i: '~ ~ " ~ . . . . . . 7 v r. - . + ' . < r ~ ' . , Y , . ~ . . ` + w J,'rY,IN s + ! ~i . ' . S ' , . .r ~ ~~ ~T~ ~Yt~ ~i4 r4~ .~ 'I , M . ` .. ' ~ ~ . , . ~~ . , ,M,~1y~~ i ~~ . ~. . ,'! . + 'T ~~Y; '+SJ . ; . t Y . . ' . ,r , _ '~ .'~A'?~NrI. '~ :A, . ,1t ~ . , . #~, s+ 7 +1r ~wMwAY7 ' t . . . . . W'r . . '~~ h~ . Exygen Rcscsrch Page 110 of 1 10