Document 2NqNyDoYV6JVoDp6NoRq7kLnp

Northwes Bioaalyieat ARRREL _ [21] Study No. reporivo NWBS00.05 NwaRor a0, Quantitative Determination of PFOS and Related Compounds in Human Serum by LC/MS/MS Sample Analysis Report for Protocol EPIL-0011 Northwest Bioanalytical (NWB) A Division of NWT Inc. 1121 East 3900 South Salt Lake City, UT 84124 g 2 a =z 30 Sn z= s PREPARED FOR: 3M Company Corporate Occupational Medicine, Medical Department 220-3W-05 St. Paul, MN 55144 Connie OSuhnuitll AUTHOR: Connie O. Sakashita, B.S., NWB Project Manager APPROVED FOR RELEASE BY: Rodger L. Foltz, Ph.D, N' Technical Director DATE: _/1:dp-01 DATE: _//-30-0/ ~maraint NO CRI Page1 050339 Northwest Bioanalytical RSeptourdty No. No. NNWWBBRSO0L0..000815 QUALITY ASSURANCE STATEMENT LABORATORY: : ANorDitvhiwseisotnBoifoaNnWalTytiIcnacl. (NWB) Sa1l1t21LaEkasetCi3t9y0,0USTo8ut4h124 SPONSOR: 3M Company 2`C2o0r-p3orWa-t0e5Occupational Medicine, Medical Department St.Paul, MN 55144 COMPOUNDS): PFOS and Related Compounds NWB STUDY NUMBER: NWBS00-088 SPONSOR STUDY NUMBER: ~~ EPL0OI 1 NWB STUDY TITLE: `QCuaonmtpiotuantidvseiDneHteurmmainnatSieornuomfbPyFLOCS/aMnSd/RMeSlated grTuehigeduelclalitineneidscanolofnscttlhuiedniyUc.daSel.sscFtruDidbAye.dGHionoowtdheivLsearrbe,oproNarottroitrhymwPoertsaitcntBciilcoeuadnReaedlgyuwtliiatcthaiilonnctsohnefdodurecfNtiosnnicatllilionsnitocuadfilaesLGawLbioPtrhaitnorthye SJStatupuddaiineeesssoe(nTMittHlheeW2S1aGfCeoFtoyRdofLPDaarbrtour3ga8st),o(rtOyhrePdriOanEcatnCiccDee NPSroti.annc2di1ap,rldePsAOorBfdGiNonoatoindfciecLaaftobiroorNnaoNtnooc.rliyn4Pi2r4ca.ac)ltiLTcahebeoarnfadotltolhroeywing inspections were performed by the NWB QAU per SOP. Inspection and Reporting Statement. DateofInspection Phaseof Study 2126:O2c5tS2e0p020000 2070-2153 ONcotv22000010 0237DNeocv22000011 ASnaamlpyltiecaRlecPeliapnt RSeapmoprlteDArnaaflyVsRiasw Data F2i%nRalepRoerpotrtDrafvRaw Data "Reports to NWB Management are issued monthly. Date Report Sento NWBProjectManager 2156 OScetp 22000000 2154 ONcotv22000010 0237 DNeocv22000011 Date Report Sent to NWB Management* 3219 0Scetp 22000000 3310 0Ncotv22000010 3310DNeocv 22000011 iAnscocrapnorraetaesdonianbtolythbies efsitnaalblriesphoerdt,atchceurmaettehloydrsefalnecdtptrhoecreaduwrdeastad.escribed and the results A HD y Lynn Chain, B.A. /2-03-21 Date NWB Quality Assurance Compliance Auditor Page2 50340 Northwest Biosalyticat ReSptourdtyNNoo.. NNWWEERSO0L0..000818 COMPLIANCE STATEMENT cr`oTehgneudlucalctiteneiddcnaloinnscatlcuicdnoiycrdadelasnscctreuidbwyei.dthHinothwteheivgsuerired,peolfriotnteihssoenfobtetshitenocfUl.uoSd.uerdFkwDnioAtwhliGenodtoghede,LdtaehfbiiosnripatrtiooojrneycotPfrawaacsGt.LicPe tRheegumleatthioodnss afonrdNpornoccleindiucraels dLeasbcorriabteodrywiStthuidnietshi(sTirteploert2.1 CInFaRddPiatriton5,8)thaensdtaucdcyofrodlilnogwteod the guidelinesofthe OECD Principles of Good Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safetyof Drugs (Ordinance No. 21, PAB Notification No. 424, ) Any known iinnccilduednetds itnhatthimsaryepohratv.eTahfifsecrteepdortthereqpuraelsiteyntosrainntaecgcruirtaytofetrheceorpdroojfetctheorrraewpodrattead data is Connie Aukaotll N`CoWnniePrOo.jeScatkaMsahniatag,erB.S. fer. Foltz, PRD. NWB Technical Director 1-30-01 Date Batye -3a-4) Page 030341 Northwest Biourslytical TABLE OF CONTENTS ReSptourdtyNNoo.. NNWWBORSO0LD-.000818 SIGNATURE PAGE wrens QUALITY ASSURANCE STATEMENT -------- i ------------------------. LIST OF TABLES ..c.coccssossssssssmsmsmsessos esos LIST OF FIGURES ccs, 1 INTRODUCTION worsens 4. RESULTS AND DISCUSSION. ..c.cocvrrmrrrerresrnes EE SS-- LIST OF TABLES Table 1. Calibration Curve SUMMAIY Or PROS....covcvcsemveessssssromosomessessse cers 18 Table 2. Calibration Curve SWmmALy for PFOA .cccrcvvsrrrrsosorensenosnn1n9 Table 3. Calibration Curve SUmmMALy for PFHS ccc 20 Table 4. Calibration Curve Summary for PROSAA ...c..cccveverrrmeesesesssssess eres 2 | Table 5. Calibration Curve Summary for PFOSA ....coccvvvrmerre torreon, nseered2 Table 6. Calibration Curve Summary for MSS6............... E ---- x Table 7. Calibration Curve Summary for MS70.........covvmmsersrrssesn esssssssnsssssnsnsnasasnssssnnnnnn 2 `Table 8. Back-Calculated ConcentrationsofCalibration Standards for PFOS .....c.ccvunrnnn2S Pages 050342 Northwest Bioanalytical ReSptourdtyNNoo.. NNWWBBRSO0L0..000818 Table 9. Back-Calculated Concenteations of Calibration Standacds for PFOA.................... 27 Table 10. Back-Calculated Concentrations ofCalibration Standards for PFE ..............20 Table 11. Back-Caleulated Concentrationsof Calibration Standards for PFOSAA.............. 31 Table 12. Back-Calculated ConcentrationsofCalibration Standards for PFOSA .............33 Table 13. Back-Calculated ConcentrofaCatliibroatniosn Standardsfor M556...................35 Table 14. Back-Calculated Concentrations ofCalibration Standards for M570 ..............37 Table 15. Analytical QC SUMMALYfOr POS v.39 Table 16. Analytical QC SumMATY fr PFOA... 41 Table 17. Analytical QC SUmMAY FOF PFHS vcr 3 `Table 18. Analytical QC Summary for PFOSAA.....cvcrrcnrsmsssmmssss dS `Table 19." Analytical QC Summary Fr PFOSA ccc] Table 20. Analytical QC SUmMArY for MSS6 wcrc 49 Table 21. Analytical QC SUmMAY FOF MST0 corte S1 `Table 22. Study SAMPLE CONCENTBHONS cv. 53 Table 23. Repeat Analysis Table for POS veins 92 Table 24. Repeat Analysis Table for PHS wcrc 92 LIST OF FIGURES Figure 1. Representative Calibration CUrVe for POS... Figure 2. Representative Calibration Curve f0r PFOA... 93 mms 93 Figure 3. Representative Calibration Curve fOr PFHS .........ccuneonnsmmrsmsnnn 94 Figure 4. Representative Calibration Curve fOr PROSAA..c.covvvinrmsmrssssnn 94 Figure 5. Representative Calibration Curve fr PFOSA wc. 9 Figure 6. Representative Calibration CUrVe fOr MSS6 cvs 9 Pages 090343 Northwest Bioanalytical ReSptourdtyNNoo.. NNWWBBRSO0I0..000813 Figure 7. Representative Calibration Curve fOr MST0 wiser 96, Figue8e.Human Serum Bankfor PFOS woven ss 97 Figur9e.Human Serum Blankfor PFOA worrisome omens 8 Figure 10. Human Serum BIank for PFHS cvs 99 Figure 11. Human Serum Blankfor PROSAA ccc 100 Figure 12. Human Serum Blank or PROSA wc. 101 Figure 13. Human Serum BIank fOrMSG... 102 Figure 14. Human Serum BIank for M570... 103 Figure 15. Human Serum Blank with Intemal Standard (QO) for PFOS rere104 Figure 16. Human Serum Blank with Internal Standard (QC0) for PFOA... 105 Figure 17. Human Serum Blank with Internal Standard (QC0)for FHS... 106 Figure 18. Human Serum Blank with Intemal Standard (QC0) for PFOSAA .........oooor 107 ! Figure 19. Human Serum Blank with Internal Standard (QC0)for PFOSA ...........over 108 Figure 20. Human Serum Blank with Intemal Standard (QC0)for M5S6..........nrs 109 Figure 21. Human Serum Blank with Internal Standard (QC0) for M70... 110 Figure 22. Low Standard (3.94 ppb) for PFOS.....cccccrrssmmssssss1n1 Figure23. Low Standard (1.92 ppb) fr PFOA crane12 Figure 24. Low Standard (36 ppb) or PFHS cco nl13 Figure 25. Low Standard (1.60 ppb)for PROSAA cero 118 Figure 26. Low Stan(1d.a00prpdb)for PROSA ccs 15 Figure27. Low Standard (2.50 ppb) fOr MSG. 116 Figure 28. Low Standard (1.00 ppb) fOr MSTO....ccrcsssnrssmmssnn1e7 Figure29.High Stan(d41a4prpbd) fOr POS... 18 ont 050344 Northwest Bioanalytical ReSptourdty NNoo.. NNWWBBRSO0L0-.000813 Figure 30. High Standard (481 ppb) fOr PFOA rcs 19) Figure31. High Standard (523 ppb) fOr PHS ..corcaracrnnrrons nnn 120 Figure 32. High Standard (S01 ppb) for PFOSAA wcrc 121 Figure 33. High Standard (S00 pp) fOr PFOSA verre 122, Figure 34. High Standard (500 ppb) 08 MSS6 ...crcrcssmrsssmssen123 Figure 35. High Standard (S00 ppb) 08 M570... 124 roger 050345 Northwest Bioanalytical ReSptourdty NNoo.. NNWWBBSR0O0L.O0O8T5 Quantitative Determination of PFOS and Related Compounds in Human Serum by LC/MS/MS Sample Analysis Report for Protocol EPI-0011 1 INTRODUCTION `This report summarizes the analytical results from the quantoifPtFaOSt,PiFoOAn, PFHS, PFOSAA, PFOSA, M56, and M570 in human serum samples for 3M Company in supportof Protocol EPI-0011 (5.1]. The LC/MS/MS method for `a quadratic response for the following LLOQ and ULOQ values: _-- Analyte PFOS PFOA PFHS PFOSAA PFOSA LLOQ 3.94 ppb 1.92 ppb 1.36 ppb 1.60 ppb 1.00 ppb. M556 -- M570 2.50 ppb t1.p 00 pps b the analytes ULOQ 4l4ppb 481 ppb 523 ppb 501 ppb 500 ppb 500ppb. 5O00pppb. exhibited `The testing facility was 3M Company (Corporate Occupational Medicine, Medical Department, 220-3W-05, St. Paul, MN 55144), and the Study Director was Jeffrey H. Mandel, M.D., M.P.H. James K. Lundberg served as the technical contact at 3M. The following isa list of NWB supervisory personnel involved in the completionofthis work: Connie O. Sakashita, B.S. (NWB Project Manager); Patrick Bennett, M.S., M.B.A. (NWB Laboratory Director); Rodger L. Foltz, Ph.D. (NWB TechnicalDirector). Laboratory personnel involved in the completion ofthis study included Suzanne Newman, B.S. (NWB Research Scientist); Emily Yardimei, B.S. (NWB Scientist). NWB SOPs and guidelines were used in the conduct of this study and were available to study personnel in electronic and/or hard copy formats. Pages 050345 Northwest Bioanalytical ReSptourdty No. No. NWBS00.088 NWBROL.001 Date Study Initiated: 22-Sep-2000 Date Analyses Completed: _ 25-Mar-2001 However, Northwest Bioanalytical conducts all studies within the guidelines of the U.S. FDA Good Laboratory Practice Regulations for Nonelinical Laboratory Studies (Title 21 CFR Part 58), the OECD PrinciplesofGood Laboratory Practice and the Japanese MEW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the SafetyofDrugs (Ordinance No. 21, PAB Notification No. 424). Any changes to or deviations from the original protocol (Analytical Plan) were documented through approved protocol amendments or deviation memos and are retained within the raw data. 2. METHODOLOGY `The assay used for this study is reportedin Northwest Bioanalytical reports NWBR0O108 (5.2] and NWBRO0-122 [5.3]. Chinese human plasma was used for the calibration curves and quality control samples. Serum sample results obtained using plasma curves are discussed in NWBR00-122. : `Samples for this study were received at NWB on the following dates: ------ Receipt Date NumberofSamples Received Storage Condition --_-- f 21-5e p-2c 000 epdu52i 6 gan(excl ept d2u ur0ingCl analysy is) 22-Sep-2000 7 20C -_-- 21-Feb-2001 e6e2 , 20' C ) es 030347 Northwest Bioanalytical RSeptourdty NNoo,. NNWWBESR0O0I.000819 Reference Material Analyte PFOS PFOA PFHS PFOSAA PFOSA M556 M570 THPFOS Lot Number 193 245 SE-036 Purity Expiration Date 100% 31-Dec2010 100% 31Dec20l0 100% 01-Jan-2010 617 53.8% 31-Dec-2010 214 100% 31-Dec-2010 NB113047-8D 99.89% 31-Dec-2010 11850626 99.75% 31-Dec-2010 59909 90% 31-Dec-2010 "Stored dy Source 3M 3M 3M 3M Mm 3M 3M 3M Storage Conditions Room temperature Room temperature 20C Room temperature Room temperature Room temperature: Room temperature Room temperature. `The reference material purity for PFOS, PFOSA, PFHS, and PFOA was not available prior to the conductofthis study. Therefore, the reference: `material purity was assumed to be 100%. : 3M contracted with Centre Analytical Laboratories, Inc. in State College, Pennsylvania to determine the absolute concentration of PFOS, PFOA, and PFHS in NWB stock solutions used to prepare the analytical standards and controls used for this studies. All `amangements for purity determinations and the transfer of NWB solutions to Centre. Analytical Laboratories, Inc., were performed by 3M. Based on Centre Analytical Laboratories" results, the concentrationsofplasma calibrator and quality control samples `were corrected using the following factors: Analyte PFOS PFOA PFHS Correction Factor 0.821 0.961 1.043 Eight or more calibration standards were prepared on the dayofeach run by adding 100 kLofblank human Chinese plasma and 400 KLof 50 mM ammonium acetate in J 090348 Northwest Bioanalytical Study Report No. No. NWDS00.085 NWBRO1-001 water (unadjusted pH ~6.9) to 13 x 100 mm polypropylene tubes. After abrief vortex mixing, 10.0 iL of the appropriate spiking solution wasadded.The final calibration standard concentrations in human Chinese plasma for each analyte are listed below: Analyte Calibration Standard Concentrations* PFOS 3.94,5.17,113,23.6, 44.2, 85.4, 209, 332, and 414 ppb PFOA 192,336,106, 25.0, 49.0, 97.1, 241, 385, and 481 ppb PFHS 136,292, 10.7, 26.5, 52.6, 104, 262, 418, and 523 ppb PFOSAA 1.60, 3.10,10.6,25.6, 50.6, 101, 251, 40an1d 5,01 ppb PFOSA 1.00,2.50, 10.0, 25.0, 50.0, 100, 250, 400, and 500 ppb Mss6 2.50, 10.0, 25.0, 50.0, 100, 250, 400, and 500 ppb *--T_h--eMt5ar7ge0t calibeation curve1r.a0n0g,2e2s.0510.,0071p0p.0b0,t5o205S.0,007,p05p00b.,(0e,1xc01e0p00t,,fo22r55M00S,,34460000w,h,iaacnnhddhS5a00s800LppLppObbQ of2.50 hPuPm).anECahcihneasnealpylteashmaas uasdeidf.frent final curve range based upon the persistent fvels ofthe analyte in he In addition, blank plasma samples, both with and without internal standard (designated as QC0s and Blanks, respectively), were assayed in each analytical run. Analytical QCs were prepared in human Chinese plasma on October 6, 2000, October 11, 2000, and October 27, 2000'and stored in a -20 C freezer. For each run, analytical QC levels were assayed in duplicate. In addition, for each dilution level, dilution QCs were run in triplicate in any analytical run that contained diluted subject samples. The QC concentration levels are shown in the following table. _-- QC Concentrations -- Analyte Tg oLow owv AlMlMceaMonedcr dedniiteauutmnimonsar eHxpHrieisggsehhde s pbH. HiigghhD,DFF==22 PFOS 6.40 126 332 335 PFOA 481 14s 385 386 PFHS 448 156 a7 a8 PFOSAA 4.60 151 401 401 PFOSA 400 150 400 400 Mss6 400 150 400 400 _-- M570 P4.F00 11500 d40e0 a4e 00 Page 11 650. 549 Northwest Bioanalytical ReSptourdtyNNoo.. NNWWDBRSO0L0-.000815 The intemal standard (THPFOS) was added to all plasma and serum samples (except Blanks) foar final concentrationof approximately 200 ppb. The analytical method consisted oaf liquid:liquid extraction procedure followed by evaporation and reconstitution ofthe extract residue with 20 mM ammonium acetate in `water: 20 mM ammonium acetate in methanol (30:70 Viv). The samples were analyzed by liquid chromatography/tandem mass spectrometry using a PE Sciex API 3000. The instrument was operated in the multiple reaction monitoring (MRM) mode under optimized conditions for PFOS, PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 detectionofthe negative ions formed by TurbolonSprayTM ionization. 3. SAMPLE ANALYSIS PFOS, PFOA, PFHS, PFOSAA, PFOSA, M556, M570, and THPFOS chromatographic peaks were integrated using the PE Sciex MacQuan software (version 1.6) with a smooth facotfooner. Quantitation was based upon quadratic regression analysis of weighted (Ux?) calibration curves using area ratio vs. concentration utilizing Watson DMLIMS software (version 6.1.1.04). The samples were injected in asystematic order. 3.1. Acceptance Criteria For an analytical run to be accepted, it must have met the acceptance criteria listed below which are consistent with regulatory and industry recommendations. Calibration Curve `Each run will include in duplicate calibration standards at six or more concentrations covering the lower to upper limit ofquantitation. For all analytes except PFOSA and PFOSAA, at least three-fourths ofthe calibration standards back-calculated concentrations must be within 15% (x 20% for LLOQ) oftheir individualtarget concentrations. For PFOSA and PFOSAA, at least three-fourthsof the calibration Page 12 030350 Northwest Bioanalytical ReSptourdtyNNoo.. NNWWDBSR0O0.L00803 standard's back-calculated concentrations must be within 20% (+ 25% for LLOQ) of their individual target concentrations. A calibration standard will be considered an outlier ifit is greater than two times the acceptance criteria for that standard. Lower Limit of Quantitation `The back-calculated concentrationsof at least oneofthe duplicate lowest points in the calibration curve must be within 25%ofthe target concentration for PFOSA and PFOSAA to qualify as the LLOQ and within + 20%ofthe target concentration to qualify as the LLOQ for all other analytes. If this criterion is not met, the next level is subjected to the same test and the LLOQ raised accordingly. Quality Control Samples Each analytical run will include low, medium and high QC samples in duplicate. The `measured concentrationsofat least two-thirdsofal analytical QCs must be within 20% of their target concentrations (+ 25%for PFOSA and PFOSAA), and no two QCs at the same concentration can be outside the limit. If study samples require dilution, a dilution QC will be analyzed in triplicate for each dilution level (except for PFOSA and PFOSAA which should not be diluted with control matrix). At least two dilution QCs at each level must be within + 20% of ts target concentrationsinorder to accept diluted study samples at that level. The dilution QC acceptance is independentofthe undiluted analytical QC acceptance. 4. RESULTS AND DISCUSSION Serum sample results obtained using plasma curves for PFOA, PFHS, PFOSAA, PFOSA, M56, and M570 did not meet NWB SOP requirements for validation. Results nay vary on average up to 26% from results obtained using human serum calibration curves at some concentration levels for PFOA, PFHS, PFOSAA, M556, and M570. For PFOSA, results may vary on average up to 43% from results obtained using human serum 050351 Page 13 Norwest Bioanalytical ReSptourdty No. No. NWBS00.083 NWBRO1.001 calibration curves. However, in order to obtain the lower limitof quantitation less than 5 ppb required by the Sponsor, it was necessary to use plasma curves. Each accepted run met the acoeptance criteria set for the calibration curve points, for the lowerlimit of quantitation (LLOQ) and for the analytical quality control (QC) samples. RunlD PFOS PFOA PFHS PFOSAA Comments Result Result Result Result T Rejected Rejected Rejected Rejected All analytes rejected due to sample preparation error 2 Accepted Accepted Accepted Accepted 3 Accepted Accepted Accepted Accepted 4 Accepted Accepted Accepted Accepted 5 Accepted Accepted Accepted Accepted 6 Accepted Accepted Accepted Accepted 7 Accepted Accepted Accepted+ Accepted 8 Accepted Accepted Accepted Accepted 9 Accepted Accepted Accepted Accepted 10 Accepted Accepted Accepted Accepted LU Accepred Accepted Accepted Accepted 12 Accepied Accepted Accepted Accepted LLOQ raised for PFOS 13 Accepied Accepted Accepted Accepted 14 Accepted Accepted Accepied Rejected Low Qs failed for PFOSAA. is NA NA NA NA 16 NA NA NA Accepted 17 Accepted Accepted Accepted Accepted NIA = not analyzed RunlD PFOSA M556 M570 Comments Result Result Result 1 Rejected Rejected Rejected All analytes rejected du to sample preparation error 2 Accepted Accepted Accepted 3 Accepted Accepted Accepted 4 Accepted Acoepted Accepted 5 Accepted Accepted Accepted 050352 Page 14 Northwest Bisanalyical RunlD PFOSA Result 6 Accepied 7 Acceped 8 Accepted 9 Accepied 10 Accepied Ul Rejected 12 Acepied 13 Accepred 16 Accepted 15 Rejected 16 NA 17 Accepied ReSptourdty NNoo..NNWWBBRSO010-.000813 M556 Result RMe5s7ul0t Accepied| Assepied Accepted Accepted Accepted Accepted Accepied Accepted Accepied Accepted Accepted Accepted Accepted Accepted Accepted NA NA Accepted Accepted Accepted Rejected N/A Accepted Accepted Comments -- SRetiannjdeacrtdiocnurovfeRufanile1d1 ffoorrPPFFOOSSA.AA only. Low QCs failed for M570 Standard curve failed for PFOSA NIA = not analyzed Becauseofthe limited sample volume available, several samples in this study were ( analyzed atadilution factor of2. High QC samples, diluted atafactorof2, were also analyzed in triplicate. METHO0040 did not meet the validation acceptance criteria for analysisofQC samples. containing PFOSA or PFOSAA at concentrations above the ULOQ (analyzed after dilution). Samples containing PFOSA or PFOSAA at concentrations less than the ULOQ and analyzed after diluting with control matrix were not evaluated for accuracy and precision during method validation. PFOSA and PFOSAA accuracy and precision for the diluted high QC samples from 3 separate runs was determined to assess the validity of diluting samples with Chinese plasma when samples have PFOSA or PFOSAA concentrations less than the ULOQ. (Refer to PFOSAA results in Runs 12, 13, and 16 and PFOSA results in Runs 12, 13, and 14) Both intra- and inter-assay precision were <15% and intra- and inter-assay accuracy deviated <15% from target (data not shows). Therefore, the accuracy and precision wt obtained after diluting samples with Chinese plasma when samples have PFOSA or repett 050353 Northwest Bioanalytical ReSptourdtyNNoo.. NNWWBBRSO0L0-.000318 PFOSAA concentrations less than the ULOQ is acceptable and PFOSA and PFOSAA results from diluted samples will be reported. `The lackofdilution data prior to analysis of dilutedofhigh QC samples did not affect the quality ofthe assay or integrity of the PFOSA and PFOSAA data. Sample 230 was analyzed on Run 1 which had to be rejected for all analytes due to sample preparation error. There is insufficient sample for reanalysis. SOP Deviations `Samples 2193 to 2363 and 2366 to 2500 were analyzed for PFOSA in Run 11 and Run 15. The standard curves did not meet the acceptance criteria in eitrhuneanrd therefore, PFOSA results were rejected. There was insufficient sample to reanalyze. Since the runs failed, no standard or QC data from the runs is included in this report. All subject PFOSA sample results obtainedinRuns 11 and 15 were less thanthe LLOQ. ` `The standard curve failed due to scatter and less than three-fourthsofthe standards were: `within the acceptance criteria. However, the meanofthe low QC results in the two runs ranged from 109.8 to 114.3%oftarget and the LLOQ samplesfor run 15 deviated less than + 5% oftarget. Since there is insufficient sample volume to repeat the analyses, the client has requested that the <LLOQ results be reported as conditional information. `The criteria specified in the analytical plan for rejectionofcalibration standards was not followed for the M570 curveinrun 12. Standard 1, replicate 1 was deactivated as an outlier even though the %deviation from target was less than 2 times the acceptance criteria for that standard prior to deactivation. As a general practice, both LLOQs are deactivatedifboth LLOQ results are outside of the specified acceptance criteria. For this run, when both LLOQs were deactivated, the calculated concentrationof Std 1, replicate 1, deviated 61% from target and replicate 2 was 11% from target. This indicated that Std 1, repl 1 wasatrue outlier and Std1, repl 2 : was originally not fitting the curve because Std 1, repl | was skewing the curve, When fm 650354 Northwest Bioanalytcs! ReSptourdty NNoo.. NNWWBDRSO0L0-0.0018 Std 1, repl 2 is reactivated, it has a deviation of 2% from target. Therefore, the regression will be accepted with only Sid 1, rep! | deactivatedas an outlier. Since the tegression is scientifically sound and acceptance criteria for the run are met, this deviation does not effect the qualityofthe data or integrity of the study. 5. REFERENCES 5.1. 3M Company Protocol EPI-0011. "Identificationof Fluorochemicals in Sera of Children in the United States." March 16, 2000. 52. C.Sakashita. "Quantitative Determination ofPFOS, PFOSA, PFOSAA, POAA, PFHS, M556 and M570 in Human Serum by LC/MS/MS." Assay Revalidation Report. NWB Study NWBS00-040. NWB Report NWBR00-108. January 24, 2001. 53. C.Sakashita. "Quantitative Determination of PFOS, PFOSA, PFOSAA, POAA, 'PFHS, M556 and M570 in Human Serum by LC/MS/MS." Assay Revalidation `Addendum Report. NWB Study NWBS00-040. NWB Report NWBR00-122. November 20, 2001. 6. DATA RETENTION `The raw data and final report for this study will be stored intheNWB Archives, 1121 East 3900 South, Salt Lake City, UT 84124 per regulations and contract agreement. `After submissionofthe final report to the Sponsor, remaining study samples will be stored under required conditions until confirmationofSample Disposition/Retum Authorization is received from the Sponsor. 3M Company will be notified concerning final dispositionofrecords at completion of contract obligations. Page 17 050355 [T------ ReSptourdty NNoo.. NNWWBBRSOULD--000315 Table 1. Calibration Curve Summary for PFOS Quadratic weighted Ui. All concentrations are expressed spp. [oro imme | ~ | |]Fra og) ee 31002000| 2 |-0.000005| 0.027791 [0010509| 0.9956 |3.|9414 4| 01-Nov-2000]3 |-0.000005 [0.027419|0.006602| 0.9990 |39 [44 14| 04-Nov|-24000| -0.000007| 0.030558| 0.012087| 09961 ooNovaooo]50000017|0.03395 00tsens| 09953|39|ai%e| 08-N|ov6-2|0-000000011| 0.035306|0.007489| 0.9960 |39 |414 4| 09-N|ov7-2|0-0.00000010| 0.039703 [0010533| 0.9894 10-N|ov8-2|0-0.00000008 [0.035218 [0.033595| 05921 |3.|94144| 1123N-oNvo-v2-020000|0 9 | 0.000003 0[00.20920965151|| 00.00z2z0s4s7s3||0oma9 is ||9 33941 9 ||a4t2 % 1e4|| 14-Nov-2000 0.000005| 0.026248 09791 |3.|9414 4| 15:No|v210200| -0.000005| 0.041499| 0.007161 | 0.9829 ` 16-N|ov13-2|0-0.00000003[ 0.036442| 0.026638| 0.9520 18-N|ov14-2|0-000000006| 0.034381 [0.024135 | 09970 |3.|9414 4| 25-Mar-2000 | 17 |-0.000001| 0.008025|0.004145| 0.9969 |3.|94144| [Mean] [0000006 0.030833 [oot60i6| 07 ||| 0 CE CC [sp]| oooocos [0.008779|0008935| 00063 ||| CoTwlwlwlwl [ |] A,B, 0dCace coefficients usedto detfhecialibnrateion curve, Page 1s 030358 Northwest iasnalyical ReSptourdty NNoo.. NNWWBDRSO010-.000815 Table 2. Calibration Curve Summary for PFOA Quadratic weighted Ui. All concentrations see expressaesd pb. Run a Number C [R-Squarea[LLOQ 31-0ct-2000 0000001 [0018750[0.001244| 09967 |19 | 42 s1| O1Nov-20300|| 0.000002 |0.018998| 0.000186| 0.9980 |19 | a2 si| 04-Nov|-24000| 0.000001 | 0.014032| 0.001606| 09945 06-Nov|-25000| 0.000000 [0.014340|0.002050| 0.9941 |1.|94812| 08-Nov-2000]6 |-0000001 [0.014866 [0.000095| 0.9971 |19 |as2 i| 09-Nov-2000 7 |-0.000002 [0.014932 [ 0.002985| 0.9961 |19 | 482 1 | 10-Nov-2000| 8 | 0.000001|0.015103| 0.009536| 0.9941 12-Nov-2000[9| 0.000001| 0.010333| 0.003017| 09961 |19 | e2 sl| 13-Nov-2000[10 | 0.000001 | 0.015660[0.002794| 0.9936 |19 | 42 81 | 14-Nov-2000 [11 | 0.000008 [0.013586|0.006940| 0.9842 |1.|9 as2 i| 15-Nov-2000 000002|0.015457] 0005125| 09903 16No | v132|0-00 .0000001|0.017638|0.007935| 0.9922 |1.|9482 1| T5Nov2000 000000 | 0020192| 0010441|09|9 1522| 1 81| 25-Mar|-210701| 0.000000 [0.006597| 0.002091 | 09921 |1.|9482 1| I -- [Mea| oo0000l [0015056 [0004003 | wo09937 ||| A,B,3nd Cae coefficient usd to detfhcialibnratieon curve. Page 19 050357 Table 3. Calibration Curve Summary for PFHS Quadratic weighted 1/x'. All concentratioanres expressed as ppb. T [v|aoe E iows [owm n[ome o T |oe|1s 36 55| Number [[o6v5N%eva0tt8o[|5|[oaotso [eve 500] -onaors [[oomsaro[oorsns||osososes ||11336|553 [oarsoso | ovr|336 | || | Tolmer [[1F02%Novat3m0o ssa-o cosoo[[som omrr|m oowosn|o113366|n 553|] [[13 136% | 5 [somos0 [[oomseons [aao0 rzosn |ovseoro||s 115366||555|| [[1i6%rcaratomeo[|zisosoomo [[oometrs[[waoz s|oosoor||115566|55|| [1500|e someon [ose[omar|owe|136 |52| I [swoe TTomsoms[[wommmon[s [wowrs|owom|||] Te wlw wl1] 050358 Norwest Bioanalytical ReSptourdtyNNoo.. NNWWBDRSO0L0-.000813 Table 4. Calibration Curve Summary for PFOSAA Quadratic weighted 1s'. All concentrations are expressed ss pb. [o>Tote| ~[]or] oe ree 31-0ct2000| 2 |-0.000001 | 0023946| -0.003099| 09952 |1.|6so0 r| 04-Nov|-24000| 0.000000 [0.016980| 0.005491 | 09840 |1.|6so0 i| 06-Nov-2000 0.000000| 0.016621|0.003312| 09827 |1.|6s010| 08-Nov|-26000| 0.000000| 0.018859| 0.003795| 09939 |1.|6 soi0| 09-Nov-2000 0.000002 [0.014599| 0.003438|0.9 |1.960|0so1 r| 12-Nov-2000 9 |0.000001 [0.011371[ 0.000468| 0.9982 |16 |s0 ol| 13-Nov-2000 |10| 0.000004 [0019123[ 0007920| 0.9937 |16 | S0 01| [14-Nov-210100| 0.000016 [0.014974 [ 0.016220| 0802 |16 |so0 l| 15-Nov|-210200| 0.000004| 0.012533| 0.009564| 0.9810 ! 16-Nov-2000 0.014478| 0010593| 0.985 |1.|6so0 i| 20-Nov-2000| 16 | 0000003 [0.020670| 0.021239| 09927 |16 |s0 o | 25-Mar-2001 0.000001| 0.005029 | 0.010607| 09928 |16 |so0 i| [ Meam| |ooo0003 [0016328] 0008540 | 0990 ||| [sb] [oooooos [0004833 [0007974| 0002 ||| LoTw[www TT | ALB,and Caecoefiientsusedtodefine thecalibration curve. Page21 050359 Northwest Bioanalytical ReSptourdtyNNoo.. NNWWOBSR0O0L.000818 Table 5. Calibration Curve Summary for PFOSA Quadratic weighted 1, All concentrations ae expresas ppb. [oo 31-0ct-2000 me|0.0=000[ 13| 02 .05281 59| 0 .003517|e 0.99o 49 |1s.|0e50e0 0| 01-Nov-2000 5.000003| 0.046250 | 0.010476| 09961 |1.|05000_| 04-Nov-2000 4 | -0000012 [0054175 [0011593| 05918 EEN 06-Nov-2000 5.000018| 0.069706| 0019030|09|9 1.006 | 54 00_| 08Nov-2000| 6 | -0000015 0060806[0009414| 0.958[100[500| 09-Nov-2000 0000013| 0072938| 0.011198|09|9 1002 |51 00| 10-Nov-2000| 8 |-0.000011| 0.067435| 0.045288| 09914 [Too[00| 12Nov2000| 9 | -0.000007[ 0.036833[0013009| 0930 [1|0s00 0| 13-Nov-2000|10 |-0.000005 | 0.051854 | 0.018661| 0911 [10 |s0 00| 15-Nov-2000 0.077880| 0.003529| 0.9855 16-Nov-2000 0.000007| 0.065240 | 0.029141| 09812 |10 |500 0| 18-Nov-2000|14| -0.000010 | 0.064050 | 0.019102| 09945[100[500| 25-Mar-2001 0.000000 | 0015780 | 0.005386| 09945 |1.|0500 0 | C e so o ToJw vomows[Im[osns [w[coenserl ][e owmee |_[s _||| ALB, and C ae cosfiients usd tdefine the calibration curve. tt 050560 Northwest Bioanalytical RSeptourdtyNNoo.. NNWWBDRSO0I0-.000815 Table 6. Calibration Curve Summary for M556 Quadratic weighted Uc. All concentrations ae expressed as ppb. RunDate | Run A Number C [RSquarea|LLOQ| ULOQ 31-0ct-2000 0.000001[ 0.018373[ 0.001923| 0.9972 01-Nov-2000 0.000002 | 0.017583| 0.005331 04-Nov-2000 | 4 | 0.000002| 0.007944| 0.003887[09|9 2500 |s3 00| 06-Nov-2000 | 5 | 0.000001 | 0.007717 | 0.004452| 0.9822 08-Nov-2000 | 6 | 0.000002| 0.009283 [0.002596| 09949 09-Nov-2000 0.000002 [0.007610| 0.002860| 0.9985 |2.|5s000| 10-Nov-2000| | 0.000002 [ 0.008464 05975 12-Nov2000[ 9 | 0.000002 [0.006106|0.003591| 0.9968 |25 |500 0| 13-Nov-2000|10| 0.000005 | 0.008526 | 0.004733| 09%2 |25 | 500 0| 14-Nov-2000 0.000007 | 0.007051| 0.006423| 0.9867 15-Nov-201200]| 0.000003 [0.006747 [0.0|0039901219| 250| 500 ! 16-Nov-2000|13| 0.000002| 0.006485|0.002510| 0.9936 18-Nov-2000 25-Mar-2001 0.000002| 0.008566| 0.004178| 0.9942 |2.|5s00 0_| 0.000001 | 0.002650 [ 0.001081 |0.9 |29 50|5505 0| [ Mem|| ooo0002 [0008793 [0003647] 09937 ||| vo Two[wo[wn[65 ||] A,B 2ndCaecoeMicients usetdo define the calibration curve, Page23 050361 Northwest Bioanalytical RSeptourdty NNoo.. NNWWBBRSO0I0--000813 Table 7. Calibration Curve Summary for M570 Quadratic weighted V'. All concentrations sre expres5spepbd. oo 31-0ct-2000 me *[1 Fo hoses ~0,000006 | 0.038561 | 0.012040|09|9 1.002 |54 00| OlNo | 3 v20 |-0.00000 001 | 0.036248|0.019154| 0952[too[500| 04No| v4-2|0-000000002| 0.027976 | 0.012726| 05860 |100|s00| 06-Nov-2000 0.000002 | 0.026862 |0.016535| 0.9908 |1.|0500 0| 08Nov-20600|| 0000000| 0030532 | 0.016991| 091 [100 |soo| 09Nov|-_2_7000| 0000001 [0024223|0.014409| 05863[100|s00| 10Nov20080|| 0.000002 [0.028172| 0.063424| 09950[100|s00| 12Nov920|0-0.0000|002 [ 0.018677[ 0009480| 0.9951[100[s00| 13-Nov-2000| 10 |0.000002 0.030589 [0027413[ 0.9938 [10 |so0 o| 14-N|ov11-2|00.00000020 [0.025065 0030430| 0.9807[100|Ts00| 15-Nov-201200]| 0.000003|0.021180 [0014447 09847 |100|s00 | I6Nov201030|| 0.000006 [0.022590| 0.034515| 0.9802 |100[soo| 20Nov-201060|| 0000000 [0033466|0.044312] 09914 |100[soo| 25-Mar-2001 0.002606| 0.003896| 09929 |10 |50 00| Sima ovowor [oust[wom ow ||| Cwlwlwlwl TT | ALB. andC are coefiieas used to deinth calibration curve. Pages 050362 Table 8. Back-Calculated Concentrationsof Calibration Standards for PFOS Quadratic weighted 1/x'. All concentrations are expressed as ppb. [rI oma | Nu+mber| vael[E on E 5a] a Esa]E wr] [oma| 5Twatoo [[5o2w3l[wiai[mmr] 67[wwss]mooo[[oowl[a2]] [Sev ||Twore[ooow[oes[[mao]oieo[Joosr] [[o3s]] [C Severn|5T[owor [[slormT ss5]7]w5r[wwal 0[Jeolaoo]] [T orev ||sw[[e5]lw vi1 msaelloess[[wmol]7weT[3*00m5]] [C overs |71 [ase l3s5al25 w[1m07l]sowor [[wsm0 ] m[[m3h]] [eT verson|| asr[eaww|1sT 5Jmoasslwo0[Jasi]7w[soooa]] [vera[5T[ososr[3 [w[5m1]ov[[oim]w0[molomo]] ova | 0[[esess[aev[1as[mmao]]me1[Jossls m5[oaom]] [eT verson|r| ase [[37e[w1T sm[10l5] osoe7 [[ownsl=oss[smem]| [svar ||Twyas [eswe[o08w[1w59o]woos[lsaees]zmww[wrwe]] [C erioT r| T[saor[[eases]0i3[[wmos]]omes[[r7oi]mw0e[[o5l5]] CTTo[salwlm wn ml wle] LLOQ failed 050363 Rtgs `Table 8. Back-Calculated Concentrations of Calibration Standards for PFOS(Continued) [l iver] | sa[d 56[td l oo mi]wae[wo]we[wm] T [TE eoe JJ[aaern[wn J[smwo]llwwarsrn [f[noonaoeo l]]mawsnr[[[owow]w[eo0]]] e I [sws Jo]ws[wo] 5[ew] e so] [osv sJ[vowii[fooom[lise2w0e [J5w]]a05[[waallaang] ww {os[3a[o3oE5]EaTaEs] Ewo [EaaeEsY] 030364 "Table 9. Back-Calculated Concentrations of Calibration Standards for PFOA Quadratic weighted 1x'. All concentrationsare expressaesd ppb. [FreromemJ|a3 mar v2or[[3526[o0w4[[s2o8o0]]orna[Twoaa] aoo[Jooeor] [rom]5T[uvew [osoe[[oonr[[sao]wsuaa[[wooa]] wv TLoasia[onm] [T oem] +[ams [ooawr[[o5T s9[[aaa]rora maa]asaosJ[oews[oe) [ooI o]5TTous[oois[oal[mssso ra [[sewo]sme[[wewa] CT E EEEe EEA ws[EmlEse [CmlEeN|EIJw) I [o[[vm oims[[oT wr [osnwa ]wsa[[ssro]] or oar [[aowm[[osnr]] [ovoI vam] + T[u37r[o27ns [oosm[zmoer loosn[[sssoo]]os[[ooww[[aorr]] [vI om]>TTToreessi[o5m [[ouaoln[mmaso]lwsusa[ [[mseasl|]aen [Jwaerlfow]]) [EI vo] [T7omm[oooo[[oanl[msean oanz[[vsao]] 0a[[wao[n1a]] [evra |tTa ow[onor ooms[waova[omes[owrws[[eona[l|] (vTe e[moir s [oore[m3a s oeso[fon ws|wa[[o e0s]] eC varT ] [Tvwe[ooa[wtose[[wooroo]]soios[[owesr]]a0[[0a][ama]] CE Pagerr 050365 Northwest Bioanalytical RSeptourdty NNoo.. NNWWBDRSOOI0..000818 Table 9. Back-Calculated Concentrationsof Calibration Standards for PFOA(Continued) Quadratic weighted I/x*.All concentrations are expressed as ppb. [[oRnmb ]Rwonain]r132[[53334 oioon3[m0r][o5w7[3o6r5a]320J[oa[i]] [Emo] 7T[iees[[eown[utosa[mrei]] weorw[Jos]s]m0e[m[sa[eot]] [T [suso [mo] wos[peaw ]oa[aus] [el Vor re eft en] uo [320[04 [356]so [sea]aweJot[4m] [sol [ev Toi [omoa]io[247[sor] 509 [196 157] Tor[(ea[ei[55]a9[5a]5 [042] [wml i[eas[ae 29[a9] 1a [is [an] Lo T=(=[a [aa ] ] zss] nn ' 650368 `Table 10. Back-Calculated Concentrations of Calibration Standards for PFHS Quadratic weighted 1/x'. All concentrations are expressed as ppb. [RC Serveeo J|R+ oe memio r i[JToare[1wa7a[3me6o5]] 6fiorr]5 [aowm] fw we] [[Ooroomoo]]+5 [Ts swa[aolmn[[owwwaeT[[vwssm]]owan[ffoewees]]]sswnow f[e5l0ov]]] [C T oem]5 ow anJw a[|wowfawemse ] tm swffowriw]sr e]foan]]| [[oC Svoerra]|7 o e asJTr aae[wuasJ[somoros ]]waeefffoooes[|]a2ao wef|0aeo]]] (om v [rs[eaiJlfaew[[wwwooTwwse]s5o1[fT0w]]neaeeffnw]5a5]7]] [(Boorram] T{ vo [|lwotaJ[waams[[[wwwooonsT[aswawa]] wa5f[fovwers]|]esaeee fooenn[r5]]5] (oT C rm | [ve a ar[[[1www 0es7[[vwaow]oasoen el|faf][weoen[eeenl]]| [Emo] TJeslaee[wvaa wmsa]]asst[[eoon]]aoe[olarn]] IT Tw alwlm se wl fal] 030367 Table 10. Back-Calculated Concentrationsof Calibration Standards for PFHS (Continued) `Quadratic weighted U/s. All concentrations are expressed as ppb. ([f"euNsoevzioo]nisoamer||1a5a2J| 1[|o0i7[[5a5]] s2o0s[[oorea]]770|[oes]| T [Eve[m awa |wwT o ss[wweor ] oosef[| o0r] 37 7J[wev onm]] T1w e TTw T[wTm] =w 1[1wm]] e so] [own[vmoowT wm]a]zr[fww] wa[[meomla]] = ew] I [BeNr[EwLs EaeY]EoiOTEaEo]RoEvN[EmEaEsE]N Co Tslulalalolsl=o]=] Page 30 050368 nr me `Table 11. Back-Calculated Concentrations of Calibration Standards for PFOSAA Quadratic weighted 1/x'. All concentrationsareexpressaesd ppb. " [p[Seeeem[Toun7Sembr|] 1t6a0 T[a5i5o[Tiwora msoewsi[wwoar]3oeor[[7sr] [ors5oTr|eaam[[ a1]] ww wl [w ow] [ovo] + | vsJsha[ssrto[asawas 0[T2wL[ea]] [oeveram| 5|aow [J7w7[[wwootm35oso3[worss]]wzms[3 Tove]] [Pm]--cT|wa[[ase[[oonslemlseasloero2we[] =2[5]] [sC ora]w[eos lu[mas[twoen]i[30[m9l[e40] [sera]5Toton[pa0a[sulmeu[srll]m3e[ww0el]] [omI ]5]Teaa[l50m[orw[a(s[was[wie]ww0e w3iw[m4]] [Soro]ot e[u5a [uamlaowsa]wm]e75[[wmarr]] [ieSeram| T| tes[[5wl[oursl[mms wwaewss[rwo e1w] [SC ora] a [tw T[oww [lT roer[lm5mwlewwsw70[w[o5]] [ieSeram| 5T|wonJ[w[lwow[av(asmo[loee]zlw anol]oemr] [Eom] [|o1w[oau [[oowmaes[waiweilon[oowo[oos]] C SpewcI tmewrlw[w[ow] Paget 650369 Norwest Bioanalytical ReSptourdtyNNoo.. NNWWBBRSO0I0--000313 (Continued) Table 11. Back-Calculated Concentrations of Calibration Standards for PFOSAA `Quadratic weighted /x. All concenteations are expressed as ppb. [[vRoamne [ ||s ter |20n [16a[a 52u s [1|535s [on|r] CT Ton[es[ws [aor[ws] 0 [emfar) [[ vel [so T1aT [oT w[wT s] T[oTs wTo|31 [01] [ow [oss ios[asi]ss[awo[0]5] [wv] [wor[wsJwos]er[eof es|53 [7a]ss] [ew | i3 [3as]eeoa]io]52 |15]az] LA Tw als[s]als]x]|z]a=] Pag3e2 050370 Table 12. Back-Calculated ConcentrationsofCalibration Standards for PFOSA `Quadratic weighted I/x'. All concentrations are expressaesd pp. 3 (reamoE |=s[Rwlo|7a[vs[7] oEr aoE[on[55] [[ orem]5T Towss[[ea2as0[Dwi ooowne[[mn1rilm[saxe][ww1o m3 [[[oowao[ro]]r] [[oosxom]| 5TT[oioswmo[[25a[[ut5osi[[[siaeoo[[wosrrtlowrr[a22 0[[vsoew[[o1r]] C[ E NC CT Y[Eza Doo [EmoaEw dEE mE]Em] [Nimo]7T[ovmss[[aerr[5o0s[[mwoo[wss[som]|ms1 [oa 5a1) [NC ei]3TTomww[[ooaswsso[wI 10un7[[aewosoosaowus|am3s9Toaeo a)r) [[NeEvNa ]|stoo Tw|wnvoie[[[aaosrosr [touoewrl[[zmasse[osxessfwoorsa3tsoom[oo7sr]] [Nome] a [Tommaot[saon|ovm[[mzoonl[asrn]ve|v26[em1] [Teor]5JJeorm[[ssaealov[[saeaoswelsu|me [3m[ao]n [N[ amo] isT T[aowas |m0 ooow vww[ssloosewamvsno [z3mwe0mmww[a))v ime rp 0350371 Table 12. Back-Calculated Concentrationsof Calibration Standards for PFOSA (Continued) Quadratic weighted 1/x*. All concentrations are expressed as ppb. [[ERsosamro J|ean7nieT]o3m0[[25310|[1005[[500[0005]oorr 05fo[50]] r TeTmTw r Tm TT a m]w II [oo[C1[Eow[EmTeElXo EX[E9E] w e [[oas[[a oT oso[[aw[owena[oxweoTaa]e] CfTwlwlulsslalsls x] 0650372 Table 13. Back-Calculated Concentrations of Calibration Standards for M556 Quadratic weighted Ux'. All concentrations ae expressaesd ppb [SeowToonSem 358ToTso] oaTw5 [om] [e ovSoraio| 5l Tese s[oue s[s mo]553|pTaa|lre zmai oTre] [[[ o6oSoSrzm]o|5 7T TTaamsesToar[[e raar]se5o2J[[eoooa]]e w5 saeots5n]]] [T [ oome ] T l Ta Tll wm[e (zomre iao3[[[omwur salw 5rm]es +loTeoer]]] [[SC Foorrzoe]] [TTeeessoriT[[o5onm[[[T 77m]]sorssa[[[oossm]]7maToTooorTtoomr]]] [[ S1 om]5 TTTeeeaaerl[loooa[[[I mwwar]oows[[oaw]mw55 [5wailmoev]] [ora [Soramo o T[eeasan[T[1oo0w5s[[[ma5oa]]]ws7ae3ss[|sooesss][]soourTooeoTToosvet]] [SC [ ermo]TTae sele oos[1 s mo]565Js asl3mw[a 5oeTTv]]] [[S[ Soorroo1 ]] 5TT[eesmhT|ooo0r0l[[m5ma]lwmoas[Jeoas]]lzim[aose T]sor] CTTpe sr t e are t rowmne[nolwml] Hers 050373 Table 13. Back-Calculated Concentrations of Calibration Standards for M556 (Continued) Quadratic weighted IA. All concenatce rexparetssiedo3snppsb. : [[REoxrecsT]swunaan220[o10t 3o5s0]5003 J1or][730[J0a]] [ TT n TeT e l[owee [w30]T ]ws oov[[o1l 755t a[[1o5f]a] [swoel {[uwms[wow[n]i5]sv[[owwl]15[ms0m]] w Ialslao l[roe[[on=| lwv[ws 5l]1v2[i35s]2]0) 650374 Table 14. Back-Calculated Concentrations of Calibration Standards for M570 `Quadratic weighted U/<". All concentrations are expressed as ppb. E[EseEomeeJNhEon v0[7R5E50NTEwoE] T0] 5 ao [C oom] 5T[ovomr|asmw boT Doma[alamashleo[ir wweo]]mae[[e3a] 5r]] [Soro] [ooo] 5TTTooemm][|aeaomsr[ [[oorss21ml o7 oessmoorea]]wa2s ew|0ei] a]]] [o[ rm] Tav ssl| easno[[owsst[l3wsole mmleo] wm[]ao5]] [oT rm] TJwossa|saos[Cow wowsoll[mwaosrlfaesmss[lfswwue]]]aer[|[ww][we5]]] ([ooI rroo] v L| iiTn[E 065P[orsE[2H0Eeno[IowDs]Ea0S]EaA]E Jame|50[om[1]rs oer as|v[a] (T BoaooJuss[os[l foorw[lmalsosswvo]] efaera7]] [e[ mo] T Twvio|[aemn[[[w vowmnollwmairofl5ev7r0[wrwsoao ][lves[fwaoarla]]] [Emo] [Norm] a 5T[[vmwise|]a3tovT( 7sm weo at][5733m [oo| ae r[|ewn rr]e]] [[ EerIo] iw T[waT o|[swsu[Towonow[lawiwlaemw os[wsrm]osm0sa[f0or]meoo]]] pert mon enn Page 37 650375 Noss Bantyi CSotaptsNNoo.NWOSROD 00818 Table 14. Back-Calculated Concentrations ofCalibration Standards for M570(Continued) `Quadratic weighted U/<'. All concentrations sre expressed as ppb. [Ru pete [2vecao0 [Run amber]50 [7503 |230[100]350[soa 0| |195[os[moa[102 | 250 232 Jov Je 0] 8] L [T1 [w ieTT woT leo sT seT303] s 2m [1 a]ws [en [sol Towmoer[[e2so0s[[1o5amn[[ae|79to2r|123s[[asne[a28r5] [ev] [wes T2w0e[407[[asel]etsa[] 5taao]]230|[e2s0ss] [= o>[a[mlan]x]n]a] ` Pages 050378 Table IS. AnalyticQaCl Summary for PFOS |[oe RE 640ppb| 126ppb | 332ppb| 335ppb [oTmT ] 7T|ewna |[w os Tw a] DF=2 [C oer TT 5| em |e w Tww w |] [oT everaT mo]T | es e orT [sm ww |] [T oerT]I 5 | em |m orT| mwm i|] [oTSamT o][ a[am |o wr|Twem |] [eT raT7T|me|lwTwser|] [vCamI ]TToe|m [oowe|] [oC ramoI]T 5[an |o or[oeww w |]] C [amT o]Teenm|eT|oow |a] ] [T ieee] [e 5| me [e owmm |] C [mo1 ] &T| ew w[o wr[[5w|w]| CT 1 1T Tw] Page 39 6503%7 Northwest Bioanalytical RSeptourdty NNoo.. NNWWBBRSO0I0--000818 Table 15. Analytical QC Summary for PFOS (Continued) All concentrations are expressed as ob. | ER Ee Number| 640ppb| 126ppb | 332ppb | 335ppb DF=2 [ioNovaoco] 13 |66s | 16 [| wr| sor | [1[s ws |so]] su | [TTTT Ts] [1 Tew [ ws| a6 | se | [TTT 13 ] [T[s ws| see | ss| [TT Te] T 1T TT 7 | ew] [ew[ wv |om[365| [so]Ta1m [21|l as | [ wo] | e | m8[ eo| 1a| [Weill | 913 |124|967|10| [we 22[e 20 [|d a3T] 50 ] LdT= =s |x7J wo | 050378 Pag4e0 NorthwestBioanalytical RSeptourdty NNoo.. NNWWBDRSO0I0-.0008L8 Table 16. Analytical QC Summary for PFOA All concentrations ae express5esd gob. oR RE 481ppb| 145ppb | 385ppb | 386 ppb DF=2 [2] = = [1 [orNovaoo0|73 | ens [ee [6|] [J|e ww [ass [ 1] [oeNovaooo| a | set [we [aw [0] [|Tso[ ww[wm [ | [ooNovao0| 5 ass[wo | se |] [[Ts wo [ow []] [osNovaoo| 6Test[se |es[0] [[ T xem T 7[oe me w wwe [osw wwe [lJ I vomn] 5C [o0 o |w3m |] [eC amT ]5 s an[w wm wwme [| I orem]F [6|w C OEw |] [C omT] T[eeev[ [w w[n m | ve1 m]Twwo|w w ww w | w]w] [1 | [oNovao0] 13[ass | ww |a0| ows | [1Te wws Ta |] =m |] CT 1 1| rath 050379 Table 16. Analytical QC Summary for PFOA (Continued) |[oe ER 4.81 ppb 145 ppb. 385 ppb 386 ppb [eva]w[oorw |w mw e [wD| Fe=2 [T Ewa] 7[aw w |ww ] ] rT [w TwT [wTew]] e -- T T mT w|e| wseo][ [om[m ww |amw e||ews]] [meimoe] w33w | oot |woae |w] r| CT Ts[s a] wv] Pagesz 050380 Table 17. Analytical QC Summary for PFHS RE Number| 4.48ppb | 156ppb | 417ppb | 418ppb fC emaTl 7T[ ew m w | ww w |]DF=2| [oI rseramol 5 C as | C | ww | [C oomT] +T|o w w |w ww []| EC CE T[ EA IE e CC [Ioww [| EE C CE TTe E Tww [eC rmT ]7Teaem|m me | w || [eCrmT ] 5[| 5w %|www T | wsw|]| [C imoT]T 5[5m| mw Teww| C [amT o]T 0| wm |e on T| oww m | [C ierT] T|oawm|w e oww |] [TmoT ] |w ew |w www w wr | [T esr] 5 | se |T w1 e| wr|e TT1 [w1w1w Tw o] ] Page d3 050381 `Table 17. Analytical QC Summary for PFHS (Continued) | | Number| 448ppb| 156ppb | 417ppb| 418 ppb [vCerT a] wT w |5e|w|[wwow DF=2 | [amT | 7| 55T |mw Twwo]]| I TTE TT CTw] I r EC CT AIC sweo] T[wwm|w sow |woe|m] 0| | [im mme] | oe s| wosv|[os r ||oao1]] I 050382 "Table 18. Analytical QC Summary for PFOSAA |oe2 PR PE Number| 4.60ppb| 151ppb | 401 ppb| 401 ppb [rowmn|7T|w w6|w w |w wm |] DF=2 [C orem 5T|wwwm [ T mw o|w | oC om] =T|e[ ew T m we| [ooo] 5T|eswm[|wem Twse|] [C ossovamo] T|som[w T we |o w ] || [oC m]7T|wsw w w T ww |] [oC va =T|e osw |T wse |ee|] ] C [ovals 5 | ars |m ww w|e ] [oC vamol T| ssmw |T ws wes|] [wC al Teownw |w T ew |] ] [aC ml 7Twoo[ w T wooow] ] exT o]w Tw owTww] n] r C Tes1 w T T 1 e[[aow] r-- 050383 Table 18. Analytical QC Summary for PFOSAA (Continued) oS RE Number| 4.60 ppb 151 ppb 401 ppb 401 ppb [vC am] T|esme T|w T wwe |e DmF=i2 ] [var ra TawT ||Twwo] w] Tr TT TT a T = T]e=]] r elT TT e T Te1 w |ow ] e sol Tee w [Twes s we[wern]] [Feri] Te557 T|eTooss[ | tow r| w v7] 0 ~ 050583 Sm Table 19. Analytical QC Summary for PFOSA ATR TR Number| 4.00ppb | 150ppb | 400ppb | 400 ppb [[rooomm]]5=T[[w womnT[ w m |m wmw w DF=2 [T oversI] +I[wso ise T|w w a w eoe || [[rC oeeveT mamlsaT[soe an T||w w w[m oew ]| [T BeaT m 7T Tw wwmT|T we[w | ow |] ] ] [[sT Eovmeo]] 55[|wo osw ||ee|T|w mwe| | [T EerIoT Tw | w an |o m TT www m |] [er va] T|T ew w |ooiT wew|e a]r] [eT T am 5|T o ws |w 1 TT w oTe [wwwom]]] C------ GS05385 i os `Table 19. Analytical QC Summary for PFOSA (Continued) ER[ER Number| 4.00 ppb 150 ppb. 400 ppb. 400 ppb. [vT eranTo] T @| aom Tw |ww]weD] F]=2 [vT nwT owT |w Tw Tewr]] T r TT T oeT w w e ee] e r so Toa w [TwT mew [e we w [| [Fiwme] T| Twoe [twoeo||Teur|wwse] I owo re--o --1 75] i 050388 Table 20. Analytical QC Summary for M556 [P roma]=R | we [ ETw[w | Number| 4.00 ppb 150 ppb. 400 ppb 400 ppb DF=2 [Oromo]3Ts a[ w ww [w | [oorI] =T[eewe[o 5| e || [oC eoramT mo]T 3| 3o 5[ wTw ol m|m e ] [NE era]&[aE n |mT w |] [C oemI ]T 7 | se [ e Tm aw [e | [Nam] 3T[eesn|e ww w [| [Eom 5T[e3s%[ ww w wm |w ] [NI ea] 0[tCoC | tw [NaC |] [eerI ] [Tswe[ wm Te w w [NC ovaT]T [e w |oeww s |] TTT eme T ow w] ] [eNT om] 5|w ww| oweww] r] Cr a1 rea1 in t=] Page 49 050387 Table 20. Analytical QC Summary for M556 (Continued) SR ER Number| 4.00 ppb | 150 ppb 400 ppb 400 ppb. [NC oonT]w Teo w |o ww w aD] ] F=2 [EvT an TwwT |wT w] ew] T CTTew e ew [r Se Tw r w] w wo] a I)TC m R en nw [m Fens] | oa s|ewer |T aoess 7 | o] rs] TF a =--= un] i 050388 Table 21. Analytical QC Summary for M570 |]RE Number| 4.00ppb | 150ppb | 400ppb | 400 ppb C rowT7T[weo | wwee [weme DF=2 [CoroT]5[Ternes| wwmm T |ee | [C omeT r] +T|esee |w wr[aw || [oC ssoraT mol 5T|weoT| wwm [oaw || [C oomI]I [ow |s wm |we wem [C osoT ]7 s |ws|e|we | [C oorT ] 5T[owr|w ew Twa| [C soaT] 5T[esoe[ w mw |w [oCvaT l[| ew n |m es oww |w ] oComI ][ ewo wTwww m | C --T rTrseTT TeTw e ew C TeoraT mol 5T[3e8T [www ww w| CT eam 1T Te reget 030389 ns emma Table 21. 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Piiyy 13143 ag 5 2 28 E5 EES $f is i 8ilzlzialzlalzlzlal52i]za5 la E2E52 i Pie - 47 E23 ZiZ2 HE PE :EOE LEE gels | |e B5212E(85]%)3|3|2(%(2(2)31837)1355|538|7|2|23? ilslzlzlzlzl Jal | lelzlzlzl | lle HEERFEIrR)gFn5 gnngFb9i3i9za gg 37 2 3 PHEEHH EE EE HEHEHE EEFE?E|F FEFE|7E7E5R7 EEEEE EEE : is EPSz i : 3 EE. = g2E 23 3B8EEIl5|zE(5)2||2E|35||5R]2|3al0nl03a 0 0 5g50la|a3|sg5l 52 ]lEf 8 328 &% (58 7 7 Jf ff % 23 3 3:4 EFEl.2 "2 H : E2Et 5 |Eilzla|z|z]2(2]a HEE 58: 2 2 33 g2i3s% gBl8m(3z|]|%ee= s 5(2|3|3|5)4 f2ifiis 3(88 aBlEa|EEE4E3R5T8 F857% 3|3|3[R[2 2c if 25 Ez FREER IEEE Fifi EE | eles ae eee e eel H i 3 3 s $s E S 3 7T :z B|Ets1l1z553l38z]5|l21z/8E|58s/Il12s|8l521s15l|5)s(%l25z11l5152e|)l)588a11l1Ia855l18a525le)a2lk2ee5|1ekt5E8se1]le 5(eE] 1251E iii Fk8 iz $s SFITIFFRFFFFIFFIFFIFEE58 ] 28 Fil, HEN gf: a elssf f:dx gE gz 2 lg =% igii 3$i: 2 i: fi3i.# i Li 2 2 E: a3 %F 83 S 3 fr ld Pics i% Ss zlalala ales 33%135:2 ANEEREL 3 2|g(3|3 $5 2|3|% flied: iE F2 iEZfi e3 TEE Es i1 33|[33|[33|[2R||z5||22||23 2? P1h:r4i0t 3 2 2 - 5%3E CEE gz iEH i g2E: slg 5 8E8lhs Isg giz gE/g3 2 E: n3 227 37 3 IF Ez 5 am la oo a FI g E77 5]7 7 3 i3 EERE re a a sf EE TO [H 3EE IIEEI FEI EREREN cFAzIFAF5E AE F5UI 5elE R PYeFcEO EBS SHEHHHHEHHHEEEHREEERE i3 g HEE FE EI EI EI EIE FIVIFF)]9 if iid 30588 |. SLIELL IEE Pid EERIE 3 1 12 ZEE3R|E5% 2 = 37 35 iid i iil : 5i8it1 EER} f i d EgfE2[5|5(5|(3)8 HEifB32iE35s53RtH:3 5 RAR 2 z < 3 alalal3al3-|3 wo elols g 3 32 8 Es 2: s2FsEl|2l3z|]Rzl|aRl|zRlR2RlzRlelsRR IleEl \lslBal|sR|a5|l5|l 2E 322|s %8E 2] 2i)5F i3: 2 gi3la|lal[sZg s axa g|312\8)2 2 AREgA 33g)2 &. FE zz 53 EH : 7 Eg | SF [FF FF FF i3 EL ELE ERP REPREPE 35 3_T |FH35$ E(E2II1 (Z385 1I81E1|8E2]E5 |51181 2511I5 3E51E1 311a25 551E501I1553E5 5/0212( 1555E5 0))I88|1 505EE0|05 15230]E1 230)0)5 83232 e3 d8si $&EsE SEF FRIFRIF 7 RR RIR 331305] 1 [I diE ERP HEN 32525 g gf 5% 218|213|3|212(8lal5| 5 & Si gv v 7 v v5 FE) 3s [E5358 2 |. giz HERIRRERI2EE |3|2(53 5 F$2838$3= 23] fi 5s 3 g gE ES EH 2" a=5 e(8 NEHEAE EEEsEL3 Rlgla| 2353 3 z3 tii 3 FFIEHRHREEHFAEHHRERAENRERREAARAEREARNENEF 1E5RL 3E5 i BLf2)i3)2g|7 2) z2zZ i E E 7 F3 gll25jzE||z)|zg)] i 33 2#1733]3 3|5]33 HE2 i FgiRzPREgR8E 3 g 2|2|8 3 5 gE 1 77 HE : S SIFIFIFIFIF[F|F|7|7)7]7|7]|7 [777 IE P1EE5 tf E2E$E:R1E5.:E4g 3 &3 S3 $gfi S: TIB2lsPl3E12RFESRlaElf 1I5: : fig aAlSs|Rz|EzlRs ERRaEls) 3ffifif 2SLEE880 Hg(Hs(H8|Hz(Es BEiEeE IERRE BzRlEs EHEEI BE 1z 5s3 sBlzElzlRalRsl 13885052 1i 2z1l8a(l3s g= 2s(l2|g2l|2s|l3|g5l|5z|lelsEl3aR&lEz5]]3 8|8 E8F EL iL:I2 REEERAEERREHEHHHSEE EEE gl|el]|:E g] |1E 5g)|55]|3z s2 8 = HE JIFRF JF] |7)3)7 ge #H5H a2tl.a 1|z5lz1lz8]|1512.|1.0. SIERglE EEE 1s312l18s). clsER B51E5E12E) E i: 2 HS RIERE RARER 33 EEIEIEIEid: Cn |EiR8IE E I515/5|IE5 EIE EEIgE|EE%|R5E/EE5/HE5/3B/E E5E/5E1E5E ]815E ]) R g:d% 3 SFFFFFFFIRIRFRFFFEEEsy 28 PoE 14 S5t:es |=2|8 FEEil:. E E5 |RgiEls 5 2 - & oHfHHEEEAENH i g 83g 35 gl SHEE J HEgf i 21IiPz:3,oFgs sls s sgl2 iFiE:; EsElE3lzlsER]NsR 77 gEEE 3 B EAE CH E E 4 YY id EES _ 35355 gag 22 H8 EHEHE HHEEREE RL 7 Fy is ici gE i 8% ps 1223  2 FF > J 77 3 [37 Ex ig BSH EEgRlFgEEcEisReREEElF| EEFe EFRBlREz :Tg . FA fEIG OE[eFEHHEFSBPREHIRiFRBIeRRHIeRREIEc5EFa1FE5f3FE1eI5RsF)5Ie)HR3iEF1s5lFHe5(lE35e1H7l5z]1EE55|3&i 2i gEE8t] $E31E (55slslel Is] |g] Isls|e] Is] |s|e :fsi fii:d: sEEL l2Il5l8R i5l5E 5]:1N 5]c E8]Es $2 TSIFIFISL FF RIRIR| EHHeElEEEfRoERs, S| FIR) |B Ef & if EE LiE B iifE a 5f(2k8|s(alSg|iSg]alS5lels|Slo|2S3||2z)S||3E]lal]HE8 2tii a Z iE ]3 333)3 Jl EE] EE a 5ElelxSzls]elelslalelZglxls] 5|=(3(8)3|3)2 S&F (53 sv : slel F521324i18 SRli3 gF Feit 1 ggiss FalIzRlEs sFlzRlsElalEzlRz) 20808 s52 1 - ii :: 2al2s 3H3H2H BslEslEalFz| 53808i32 2 3zz 3% aE EE St 25217151717 EF IF )J3)R8I1FF2IF1IR8| 151F|12F1|2F5]12F)22F iz i2g ai2<|fgf8| E|E8/8E|2/|25|51|58 5g/g0/g|52/8200|85E|08|E88. 3 5EF1)2781[5F1I8F)8S)F83)35 5E551E 7 E[3|3E]3]E5]R5&] 3 : 33 FEEREREER EHEEEEREE EEE5E5E5EEEe dg sioizs $7 7 RIFIRIR|F(F)F ls 3%: 5E3l |ailz|olelals]= Szl1z5lz2|]2 [els] iLisfd & (77 > 88 39 i 2 HEE 2| |z|g 2|5|z(5(5|s|z|2|5]a]o) 3 ify 2 2 2 BE - wi 3 2 33 2%: 52 tii i: dgF2F3 sZF EH HEEEHHEE HEHEI iz iz i % EIS) > RRR RI] 1331513713 is is i5|zi5|2|2)25|]2l|es5s|l2s] [5 2i1E1351|551(828185(51815 |52 (55]511551/85185/58155115815g8z1 i :y $HEEIEEIRIE EEE EET EE iiEI 3 - 513151212122 215 3080818 8128 08 ILE is SIFFIFIFIRFIF F7 [5|57 )3]3[57 3]3| &i osigi 5HHEEiLIEPERH[F8| REE57]z REH1|5EF0EH850E)5HE05E0 REH5 E5 EREH5s E5EE 7 33 28 Fi aagS3Esta%tF: I= sd 5" 1.12. A 3g 37 552 RE 5HHEfE f1ii1z:i HEE I [ i: :iSit SfErE i il Hig Pid EL EFF Firs 5 2z 2F 53 I$s5134i8z zlalslz| 8252 | Ege ie i: 52 5ol35el5e 5e5e ea eesEER 28E 32 ii:z 2312I1F81%/2F3R1R8(28B2R|5E(8F|5 3R/88RS318 2 f2z i= BEE EIR[FF|F|F EsggEae 3350313055 5 5 805 oTolzilclsE1e2jz|z|EslsElslzE(EelsE [slsE le ReleEes IH EE EEEE HEE Sg EFSF FRR RR51535)3|5)3 315 31 3 F(5%lele|8(lsg|lSs Po E8e|5lEi HEHE EEE SE5CI7E8E]TI3IF3F)F3 tFii E ER EE R gSlieg) |(gS] | ISsllss 3 79 33 5 7S7 ioe g2 3s 33 3 7 =3f 3 g3gv| 1 Ii2 3 7 F 2 dfe TE253g zLI iF iI 1i:2%= PI ooEii" : Ffeiti sPaig :82 F231g4s E 3E 3zE7 232%58 53 g : 223 2|2|8|5]|2 $< 5 cE 15 2g3z 3 22 3FEs Z5aZ5s ZHE5z 22 & i gs 3gPI45%% |HiSsTglz g5 S 3 2 [8.8 2CEE|3<5(- g2 s[i82 i2 zz :|Z & E5EE8 5g 18[896 ||2 c3 E |s ; I 2 3 i 2 a H 2 : E5S3 iE$E3e & ig i F5e2i) g PFYIiEalRa E |Z 5:[5.3= 2 |383 ez | il i3 Bi2] 2 T[I%SE|g gZ |(581 [[83 <g |S |25 Ea | I & J 23 i 3 3 8@ 3 1z 2: E ogf%: 8232 gs i 3 C223E2H 22S EzeM i FH a25 gs Northwest Bioanalytical ReSptourdtyNNoo., NNWWBBSR0O0L.000815 Figure L. Representative Calibration Curve for PFOS NSon e Co ans 158? ms i | . - - E ---- = wo Figure 2. Representative Calibration Curve for PFOA aEEE pChhoarn]ereeskdr1 y i | + | | Neco ts Poge93 050431 Norhvs Bin . StyoNogAlwSiInnrgS a ne t Figure 3. Representative Calibration Curve for PFHS : " oo ri " Figure 4. Representative Calibration Curve for PFOSAA TT re rss 0350432 Northwest Bioanalytical ReSptourdtyNNoo.. NNWWBBSR0O0L.000815 Figure 5. Representative Calibration Curve for PFOSA idE tndOY CbS e 05gs IN ooo Nortre ty Figure 6. Representative Calibration Curve for M556 RR RS ee || | i Newcoty Pages 050433 Northwest Bioanalytical Study Report No. No. NWBSU0.083 NWBROI.001 Figure 7. Representative Calibration Curve for M570 Rr i reere tl | 7 [-- . Page 96 050434 Norwest Bioanalytical Figure 8. Human Serum Blank for PFOS RSeptourdtyNNoo.. NNWWBBRSO0I0..000815 m m EE y ae e a -- en w " w mme t ea 82 a a -- ee = ef ir--t----a ] -- Er f re --w --] -- CE GA He Fh fh Br E E E w--e-- y m nape m Conta msfme rnrr mae CS e --_-- wmy 8 SP J PL " EEEE -- -- orE --r aa in | E Es --r | Ve # ma Fe Bh mh Page 57 050435 --_--Figure 9. Human Serum Blank for PFOA --= i mm R a B mrn E] Lo Li -- Gea SE n am a - F WP BOO Rew -- J Tee aEETEEElERE) em m-- f y E EE B Ees E S a E" H = aa ies BE Be We Wo HE Er 050438 Northwest Bioanalytical Figure 10. Human Serum Blank for PFES ReSptourdtyNNoo.. NNWWBORSO0I0-.000813 wmrre Presta ten SJ m ave as"3 w mwSam a m ed4S CE= eE -- 3 Ef -- ir -- a Ea] Coes SE 2) Pa I. Bs We Bs Oh TR wmman S= eabya 0 esa a m m wE m a -- S str12 ot CORG_s oC rn CE= -- E -- or r r " RT E-- E E E rr . CEE SE # aan | Fe Te OR mr 50437 Page 99 [-- RSeptourdty NNoo.. NNWWBBSROO0L.0003I3 Figure 11. Human Serum Blank for PFOSAA CEEe -- Emg a) [= ON a Lo% ferumrsioeggison o miiimmm 2Y E--_--E ---- seems , E|e= E C-- -- ormea. Ef S a CRE SE |" " V Te To Ho 8, Thor E-- E -- gr--E ---- EY moen EeER ron SwAmEa 2J J er ms " mon-- t]me + ro E= e E-- = e Ea--r arlI:sl|" E-- e ---- REE Gl o:l #1 amo EE Page100 030438 Northwest Bosal Figure 12. Human SerumBlankfor PFOSA ReSptourtyNNoo,. NNWWBBROSL0.000018 GE E rmm e m me Ee Er SIRE e e f_-- e e r mvow n[E2r -- 0] 2n or EE= E E E -- ro e--E m --e--.L "| Le a Ee ------ BT Be BW mr ---- m esmvamemEee eE wn SIRE JE Te ---- E=-- s I o-- E E -- eir-- a El r. E EmE meE ] " wan Ge fh Bh mr Page 101 050433 Northwest Bosal RSetpudoyNNoo,. NNWWOsROO0L.0G80,3 Figure 13. Human Serum Blank for Mss6 -- rbmmyaa r = E m mae mn i ="2 Easel --_-- Teremamlsm] 3% aren artosar om oo EE E -- E e mmm e ] e I" os ws CEE el | EET PE =o m a _-- m gE rher e FR -- e -- on w SSSEmCy E 23 Emme oe E= e -- E a = e p e . .l|" Hama feeeneO]E = EEE Page 102 650440 Northwest Bioanalytical Figure 14. Human Serum Blank for M570 ReSptourdty NNoo.. NNWWBBRSO010..000315 or gp [ee-- aer pe-- em e(ft SdT sm ETE mee --_-- SS el i EE = -- o -- t fE f amr e i] ] em 7 = EERE C emiE Jm oeE [m ie] Te won --_-- w seh g eel TS ren EE E -- i o -- E rol Eer-- " | w Ee oe --e Goo=ge ni #7 ao Ve Pe BSH mar Page 103 030441 Northwest Bioanalytical Study Report No. No. NWBS00-083 NWBRO1.001 Figure 15. Human Serum Blank with Internal Standard (QCO) for PFOS. a Ee L anee s ss = amaTo Cin[2H] 1 sCoonmunrr nTasnk faiermne5 [n3 )14s --_ wrmeen-- n] 50 d f= e f e re m w [E-- meserme --i23] 7 | [Erm----r| GREE 20 We Tho TO T[ esEr Snr ont _-- Ee S wveane 5n8"] )ne rfoam] ent ed Bmp [n[ fme r ------i m ta--n ] |w [L= [eimaornirtor--eseussT]]t|] EEE Ol | eB BS wr Page 104 050442 wo Figure 16. Human Serum Blank with Internal Standard (QCO) for PFOA _-- Cm mm 5 a m= a EEEE BEEreE--= r E rms re a o -- EEE E EEE EmS=TEEmEeEE EE=eG Ik = E E e E Eae m e e u [empAameEnrieEs 3.S0E6] EERE mr e105 050443 Notthwest Bioanalytical Study No. NWBS00.08 Report No. NWDR01.001 Figure 17. Human Serum Blank with Internal Standard (QCO) for PHS [j-- e r o e-- s m = Fe re 5 p-- re. wwm iee= 2e3 _-- =e pm meme ome I cE= -- -- oo-- -- --rn e =-- a y -- | =w Ye PP fh Bom m [ -- e e i y mm%m _ Conant e ms mw e ay a mm ne 2 SR a Eo= -- f Es s [E-- E =r-- E | E CoE el EEE Page106 050444 [---- ReSpuordt NNoo, NNWWBBSR0O0L.000513 Figure 18. Human Serum Blank with Internal Standard (QC0) for PFOSAA Em aa) Em oweToes.(TEE, Sleeern S mR = wEeEEl T --_-- em Th il ii E B-- a e--r -- ---- l Emma, vx Hl AA . EEE T _-- ehm i' es frame "TTL ees eb E= = e -- e e-- = a a -- -- ] l .TM a] Ea = EEE EEN Page 107 050445 Northwest Bioanalytical : ReSptourdty NNoo.. NNWWBBSR0O0L-000818 Figure 19. Human Serum Blank with Internal Standard (QC0) for PFOSA e-- Ee m r _-- r op a To-- ns I= S ------ Conan a _ T wm aEe nsw em s E BE y P EE E e m -- e o rl, aw wn I OE k Rf,aNow E EEEEE = J re ae Pp wane JE al a Arwe3n) m0 = oE E -- E o ar e . f= a GRE Gl Rf Oh wr Page 108 050446 Northwest Bioanalytical Study No. NWBS00.088 Report No. NWBRO1.001 Figure 20. Human Serum Blank with Internal Standard (QC0) for Mss6 e =Emm LE e en EEE f --_-- w aegone]d ve me mm rr = = E rr ---- r2 EE-- f ro -- r m ea | Tr Be Te To 8 Ww [ m meeC my E ame -- on an e msml eam n y m 2 mm -- em = EE E -- aEr--i m t. m fm CE EB] =o EEE Page109 050447 Notte: Biosnlytst RSeptourdtyNNoo.. NNWWBBRS001000018 Figure 21. Human Serum Blank with Internal Standard (QCO0) for M570 e-- s _------ n no s aim nnmv, 255130 Sa T --S_it e ew a]s y E o= E E E e-- e a E e l s " es a > w= - TURP fh Bohr _---- EE Lcm-- err ww = = SSmAebEdk ] e2d -- te omaena iE8 s = EE E -- p E m -- i e rTM| f ieas ] Gi = To Th 5 Tr Page 0 050448 Tr -- RSeptourdtyNNoo,. NNWWBBRSOOLD..0005,5 Figure 22. Low Standard (3.94 ppb) for PFOS Ba --E -- m-- mraeme 2 Pe-- mimie e=mss = E E Ee -- E m l =-- EE ol EEE p en som naerewa (C5r R51 Jae ron S= SE --_-- mrs om mess tecaren re, al EE E l i fmm a Boc=g- na Te fh Sh Fm Paget 050443 Northwest Bounslyisat ReSptourttyNNoo.. NNWWBBSR0O0L.000815 Figure 23. Low Standard (1.92 ppb) for PFOA _ = o-- r rn m-- i = E A -- --l: e-- ie------ Beco fh Be fh Mor meEE oy te Tora,[RE ebor [ Cont -- o w--mi--P Emr 2e -- E = E B-- e ae -- l m Boca ny [MEE a a a [am 050459 Northwest Bioanalytical ReSptourdtyNNoo.. NNWWBBSR0O0L.000815 Figure 24. Low Standard (1.36 ppb) for PFHS e E r i-- in e ii m hEe 3 am _-- e PrmSel tE Ee = f E E E E a a a a y r| | a EE] | BT ta Bh Bm m E e--E --F r man e ns oer wn SsUmRdE 2 --_-- =e 0 feE -- E f oe l E mTM| C= E = | Te Th fh Fh Ber Page 13 050451 Northwest Bioanalytical RSeptourdtyNNoo.. NNWWBBRSO0I0--000318 Figure 25.Low Standard (1.60 ppb) for PFOSAA E e m e yEe m frEoovaerT y E Ssplvo]et mee 2 --_-- eld 3 e-- -- i = m -- fE [e Ea ms itw Bf a HE wr [e-- e a ----E = Conran fov rre=m == ---- eld h Ef i E -- -- -- t a i [ema] TES 2) | Be Te MST wr Page 114 050452 -- ESetdyvogeurstiteisys Figure 26. Low Standard (1.00 ppb) for PFOSA m mEO oreeer r. S= EBESEEEEEEEEe ER %C3E8 E=H 5 = a E = E = E" e :| Eoc=--F We Be We OE my E E -- mmEaEzBEeSoEEREeEP RYEe SET4 aI-- PET =EeE E EE E EsE E sl m: EE ol 7) Se BREE mr sis 050453 Northwest iosalytical RSeptourdtyNNoo.. NNWWBBSRUO0L.000815 Figure 27. Low Standard (2.50 ppb) for M556 --a E r --E--la e m) ntETnbE,E E dRnt2 [ "ose -- ArwE en[ -- smm= -- = E E EE E s. E = Emr e m. ea GA = EER Re mr E Ee H EE e) m = min mm e _ --_-- 1 wmseaumteme 2 ol ) " EE f -- E o m l a . o-- = = o m-- ] (te BA EEE NEE Page 16 050454 Northwest Bioanalytical ReSptourdty NNoo.. NNWWBBSR0O0L.000815 Figure 28. Low Standard (1.00 ppb) for M570 @e -- -- e ---- e ---- m ovTerhvsm a5e y5750 anme --_-- T wsmere eanessds }2 J -- en = = EE[-- E eeeatsa ---- -- sr 3--r l ] %] EEE SE | BE 6 er [.e .._.--mom-- p= mrmae _ -- wmeaE iaemms enes 2 Eo SE -- = E E p [mE a s aw l|l a Gime 6 | Te Te fh Th Ho wr petty 050455 Norwest Dianalyal ReSptourdtyNNoo.. NNWWBESROODL.O008!8 Figure 29. High Standard (414 ppb) for PFOS vE mmrmee = mem sar von.[ETT a] S aatmime--wm a. meneb ndxsYi. 3nS-- . -- ETT. ween f= E f o m mm pTMt] Ef e m -- m Goole n iy Fe To a Oh Th tr _---- me wEom Cr n = m aTmhn m ees --- -- wawnesl sn E mm m. sTM CEi E -- oS am -- ----a CeGH To Fo fh Oh Thr nurs 050436 Northwest Bioanalytical RSeptourdtyNNoo.. NNWWOBRSO0L0..000815 Figure 30. High Standard (481 ppb) for PFOA [---- = Sem fm] fE e --r -- = r -- er] fae Sl 7) | EEE AE } er = J myeo oan en wa ah rE eea 2 3 wm Er ee -- = E E rs E m] m E= a -- r r]te EEE Eo Page 119 050457 Nortwes Bioanal ReSpaonrdtyNNoo.. NNWWBBRSO010..000815 Figure 31. High Standard (523 ppb) for PFHS [T..E r o..s n s m -- me -_ = m = maEamnrsbaE f ] 2d= weed [ E fm em m ) s "| C -- E ae---- E -- c= TEESE wr [ E-- e] = = ooridsJ 3 -- omeseleedI 2 me ee p -- f a -- oooc=e -m ) m nly| . LE Page 120 050458 Northwest Bioanalytical ReSptourdtyNNoo.. NNWWBBRSO0L0..000818 Figure 32. High Standard (501 ppb) for PFOSAA. Frnred i J wh) e 8 a nree wmreeteees B or-- A w-- ------ ---- = E-- e a = 4 Er E -- -- ncn | EEE ---- torr a8 J = meEs om ro ne = m a oEE -- m Ee ] r EJ LE EL mu a Eis S|) | To Te fa Th Ba fr Page 121 050459 Northwest Bioanalytical RSetpuodryt NNoo.. NNWWBBSR0O0L.000818 Figure 33. High Standard (S00 ppb) for PFOSA fi rEEyes respnie Gaaewmnne3a]l 33 wanE a 5 fE E e a m rr L Eo o rm ag ea GE | WP WO WoErR [ ECr ete --a ras wm a enE v --8] oe osB E E m r eb ] e Et c Eo n GREE > | EEE 2 0550044660 Norwest Bioanalyics RepSoarytNNoo.. NNWWBBRSOOL0000818 Figure 34. High Standard (500 ppb) for M556 fa e e r oe = e T abYe e + =, wmmabEra = oE E E r-- mm e elI [o EEinees 2G0 al | Ye Te BO NRT =) = Ee -- EEE r -- Io -- mrr r r ] r= eGosc=rTa-renlylg | EEE eage 13 050461 Northwest Bioanalytical RSeptourdtyNNoo., NNWWBBRSO0L0..000815 Figure 35. High Standard (500 ppb) for M570 pEmrBeay rae poraneitTyo Se aomnE d8H333 w sasvwm n nn E= E E r tE e EEE r m -- r m m EEE SE 7) We Pe Ws Oh RRR m a E E awnhn E e orn Aamwanl rt] EF-- or -- EE a m ro a ag Eo | EEE Page 126 050462