Document YVNVvpEMeQq0gEDemw9Ld9eE

ee----e--e-- e ------------------ AR236-150 STUDYTITLE ExtractionoYfoPloktafosrsAinuamlyPseirsflUusoironogcHiaPnLeCs-uEllfoencartoesfprroamy/EMgagssMeSmpbercatrnoem,etArlybumen, and DRAETQAUIREMENTS Analytical Method Requirements STUDY DIRECTOR Sean Gallagher STUDYCOMPLETEDON : September 06, 2001 SE EERFORMINGLABORATORY/TESTING FACILITY Centre Analy3t0i4ca8lRLeasbeoarartcohriDersi,veInc. (Centre) - StPahtoenCeo:ll8e1g4e-,2P31A-810638201 STUDYSPONSOR 3M EnvironmentaBluiTledcihnngo2l3ogEy-0a9nd Safety Services St.PauPlO,MBoNx 5353133331-3331 EROJECT CentCreentPrreotSotcuodlyNNuummbbeerr::0002P3--002633-063 "Total Pages: 102 000243 Con SyNo:23.063 FPLCBlciorprayMssSpactromety"condscied fo SH Evista Tochaonny Cento Study Troon Number 023063, eotitkd `Bxinction tn B03 Meximne Abner, su Yok of Potassium Go Ansys Ving 4ndSafetyServices, wasperformedincompliancewithUSEPATSCAGoodLaboratory Practice Standards (40 CFRPart 792) by Centre Analytical Laboratories, Incwith the followingexceptions. 1. $i7c92e.6f3o.rMheabieandbtessaannideeCalni0bectsteieocnraocf eo hoof Equipment.NoequipmentSOP ha in Ee-- CentreAnalytical Laboratories, Inc. safe -- SemAarnrne - Dupe Alief Shadyit ntmations,Lud Dua | PE retain | || 000244 _--_--mmm--------,----e CentreStudyNo:023-063 M0`C2ee3mn-bt0rr6ea3nA,nea,leynttiAictllabeldu,mLaebn"o,Erxattroaarncidteiso'nYQoulaoklfitPyfooArtsassuAsrniaaunlmycseiPsUenrifltUusroirenovgoicetwaHenPedLsCuCel-fnEotlnreaetcetS.truodsfyprroNamuymMbEaegssrg apASpnplaeilcycttraiobcmlaeeltGrLoya"ob.odrLaAatlbolroireeasxt'aomrSiytnPaerndadcaptrhidacseOSeptsearwnadetarirendgsr.ePvrioAeclwelfediudnredfsio,rngctsohwneedruScettruedapycocrPotrreodtdionctogolt,thoeaCSntedundtayrlel Diranedtocmantageomenrt. hase 1ProcolReview 2 FBoxrtaicfticoanti,on 3 RawDuaReview 4DRraafwtDRuempaorntd Review 5. FRienvaileRweport Due DateRCeepnotrretedto StDuadtyeDRierpeocrttoordantod. lopected Management SponsorManagement 33001 a1 EL an001 sn EL) 45901 41801 EL 4171801 42601 EL) aas01 srs srso1 Q`Anugeafkli) MAossrugraannce Alditor Upon Date `CeatreAnalyticalLaboratories, nc. Page30f 102 000245 ComStyNe: 30 CERTIFIOFCAUATHTENTIICOITNY D Smita v n Ge CJFom onrt eAenstamonLv, Thisreport, forCentreStadyNumber023-063,is trusandcomplaterepresentationof PrincipalInvestigator, Centre: Luton Emi Scientist Con Any abortion FstMtge a ABbaidd4. gos~ CentreAnalyticalLaboratories, Inc. alll s9-lpus5B-- -0o/ r StudyDirector Ll/ R nde Soxn Gallagher `WildlifeInternational, Lid. EN Eo a Rodale Wonid CoeA abt ali o Due. spss eretrz 000246 Centre Study No.: 023-063 STUDYIDENTIFICATION "Extraction`oYoflPkoftoarsAsniaulmysPiesrfUlsuionrgooHcPtLaCn-eEsullefcotnraotsepfrraoym/MEagsgsMSepemcbtrraonmeet,rAy,l"bumen, and CENTRE PROTOCOL NUMBER: 00P-023-063 CENTRESTUDY NUMBER: 023-063 TYPEOFSTUDY: Analytical SAMPLE MATRIX: MaYlollkardandQuailEggMembrane, Albumen, and `TEST SUBSTANCE: Perfluorooctanesulfonate (PFOS) SPONSOR: 3BMuiElndvinigro2n-m3e8n-0t9al Technoanld Soafgetyy Services PO Box 33331 St. Paul, MN 55133-3331 STUDY DIRECTOR: WSieladnliGfaellIantgehrenrational, Ltd. E8a5s9t8oCn,omMmDer2c1e6D0r1ive `TESTING FACILITY: 3C0en4t8reReAsneaalryctihcDarlivLea:boratories, Inc. State College, PA 16301 TIAMNEATLYATBILCEA:L PHASE `ESxtpuedryiImneinttiaatlioSntaDratteD:ate: `ESxtpuedryiCmoemnptlaletTieornmiDnaatte:ion Date: 03/26/01 0326/01 04/02/01 09/06/01 `Centre AnalyticalLaboratories,Inc. Page Sof 102 000247 CentreStudy No: 023.063 PROJECTPERSONNEL T`Thhee fSotluldoywiDnigrepcetrosronfnoerltfhirsomprCoejnetctrewAansalSyetiacnalGaLlabloargahteorriaets,WiIlndc.l,ifweerIentaersnsaotciioantaeld, wLiitdh. `various phasesofthe study: Name EmilyDecker Dave Bell Mitra Arjmand Ling Ling Lin Yu Qiong Tan XisomingZhu Lawrence Ord Rickey Keller `Shawn Robb. Title Scientist Scientist Technician Technician Technician Technician Sample Custodian `Sample Custodian `Sample Custodian `Centre Analytical Laboratories, Ine. Page 6of 102 000248 Cente Study No. 023-063 TAOFB COL NTEE NTS TQGIUOLAOBLDPILTAYAGBEAOSRo SAUTROARNYCEPRSATn CTAICTEECMOMEPNLs ITA.NC.E.STAe TEMENT n rr Pa3ge CSTEUDRY ITDEINTIFFIOICFATCAIUOTANH.E.TN.TIICIOTYN... PROJECTPERSONNEL... LT LISTIOOA FFOFTS FAICB BGOLTNEUTSRL Ec ENTSSE .....co cecscs nomsmmm smnsso nooos s LIST OFAPPENDICES... 1113 3200 OINBTJROEDCUCTTIIOVNEc ... ss 19 13 5600RDEFEERES NCECMAOTFREARNIIAALLYPTvIcC.TA..LI METOHoODNo..n. 1143 666432IPCrNIeSpOaUrMRatEMiDoOnoSGfEESSEtPVHaIYYn.ac .ndd.Faocrt.iro fci.cdactisoon nsSsosls sumtminoensss.e.s.oenssss: 1156 6:5 DescrofiInpstrtumienotanndOperating Conditions... 1176 7BO0 90 ERXCEPSOEUNRLCITMLSEU.N.ST.IALODNESSIGw N...ome sn ms ssss2019 10.0 RETOFEDATNAAT NDSAIMPLEO S...N .......c..ooooo 2201 CentreAnalyticalLaboratories,Inc. Page70f 102 000249 - `CentreStyNo. 023.063 LI OFTSABLTES Table Table. SummaryofPFOS in Resgent BINS... Page 23 Summaryof PFOS in Mallard Membrane BIanks.........c......... 24 Table IIL. Table IV. SummaryofPROS in Mallard AIDUImen BISnkS.......v oe... 24 SummoafPrROyS in Mallard Yolk BIsIkS vc... 24 Table V. SummaryofPROS Recoveries in Mallard Metsbrae................ 25 Table VL. SummaryofPROS Recoveries in Mallard AIDUmen.................... 25 Table Table VIL VIL Summoaf PrFOyS Summary of PFOS Recoveries for Week | in Mallard Yolk... Mallard Membrane Control Samples....... 26 26 Table IX. 2SumBmaryB ofBROSform Week 1 Malo lard Membrr ane Samplese at 21 Table X. SummaryofPROS for Week 1 Mallard Membrane Samples at Table XI. Summary of PROS for Week 1 Mallard Albumen Control Samples.........28 TaTabblleeXXIIIL..SSuummmooaffmPPrRFOOyaSSffoorrrWWeeyeekk 11MMaallllaarrddAAllbbuummeennSSaammpplleessaatt 61.72.p6pppmmia.i...2298 `Table XIV. SummoafPrROySforWeek 1 Mallard Yolk Control Sampls.............. 20 TTaabbllee XXYV.L SSuummmmaarryyooffPPRROOSS ffoorrWWeeeekk 11 MMaallllaarrdd YYoollkk SSaammpplleessaatt 61.72.6ppppmmaaii...... 3300 `TTaabbllee XXVVIIILLSSuummmmaarryyooffPPFFOOSS ffoorrWWeeeekk66MMaallllaarrddMMeemmbbrraanneeCSoanmtprollesSaamtples.......31 `Table XIX. Summary of PFOS for Week 6 Mallard Membrane Samples at `Table XX. Summary of PROS for Week 6 Mallard Albumen Control Samples......... 32 "Table XX. SummaryofPFOS for Week 6 Mallard Albumen Samples at 6.2 ppm i... 33 `TTaabblleeXXOXXIILI. SummSaurmymoafryPoFfOPSfFoOrSWfeoerkWe6eMakl6laMradlAllarbduYmoelnkSContarolamSa1mp7p.6lplepsm.e.ai..s3343 Table XXIV. SummaryofPFOS for Week 6 Mallard Yolk Samples at 6.2 ppm ai . 34. CentreAnalyticalLaboratories, oc. Pagoef1s02 000250 -_-- `Centre Study No: 023.063 TableXXV. - SummoafPrROySforWe6eMallkard Yolk Samplesat 17.6 ppam ..35 TTaabblleeXXXXVVILL SumSmuamrmyaorfyoPfFOPSFOiSn QiuniQluaAiIlbMUeMmEbNrBanIeTKBSlaks......c...o................3355 `Table XXVIIL SummaryofPFOS in Quail Yolk BISTKS cv... 36. ``TTaabbllee XXXXIXX..SSumumamrymoofafPPFrFOOySSRReeccoovveerriieessininQQuuaaiillAMIebtUaIbEtNa.g.e...................o.r.............3376 ``TTaabbllee XXOX(XX1I.L.SSuummmmaarryyooffPPFFOOSSfRoercoWveereikes1iQnuQauialilMeYmObrKan.e.C.o.n.t.ro.l.Soaomwplosr.s..r.........3387 "TableXXXII. SummaryofPROS for Week 1 QuailMembraneSamplesat `TableXXXIV.TSuTmmBaBrMyoB fPFOSforWes ek 1QuailMemn brane Samples sat 39 `Table XOCXY. SummaryofPFOS for Week 1 Quail Albumen Control Samples ........39 ``TTaabblleeXXXXXXVVILL.SSuummmarmyooaffPrPRFOOySSfofroWr eWeeekk|1QQuuaaiillAAllbbuummeennSSaammpplleessaat6.2ppmsi...40 TPP sss 4) `Table XOOKVIL. SummaryofPFOS for Week 1 Quail Yolk Control Sampls.........4.1 `Table XXXIX. SummoafPrFOySforWeek | Qual Yolk Samples st 6.2 ppm ai ......41 Table XL. SummaryofPFOSforWeek 1 Quail Yolk Samples at 17.6 ppm ai......... 42 "`TTaabbllee XXLLILL SSumumamrymoofafPPFrROOySSffoorrWWeee6k6eQQuuaakiillMMeemmbbrraanneeCSoanmtprloelsSaam6p.le2sp..p.m..a.i.......4432 `TableXLIL SummoafPrFOySforWe6eQuakil Membrane Samples at 17.6ppm a..43 `Table XLIV. Summaryof BFOS for Week 6 Quail Albumen Control Samples..........44 `Table XLV. SummaryofPFOS for Week 6 Quail Albumen Samples at 6.2 ppm ai.....44 `Table XLVI. Summaryof PFOS for Week 6 Quail Albumen Samples at 17.6 ppm ai. 45 `Table XLVIL SummaryofPFOSforWeek 6 Quail Yolk Control Samples ............. 45 `Table XLVI. Summary of POS for Week 6 Quail Yolk Samples at 6.2 ppm i ....... 46 Table IL. SummaryofPFOS for Week 6 Quail Yolk Samples at 17.6 ppm si.......... 46 Table L. Summary of Moisture Determinations for Mallard Membrane Samples..... 47 Table LL SummaryofMoisture DeterminationsforMallard Albumen Samples....... 48 CentreAnalyticalLaboratories, nc. Page9of 102 000251 Centre Study No: 023.063 Table Table LIL LI. SummofMaoirstuyre DeterminationsforMalla Yolk Sampic......... 49 SummaryofMoisture Determinations orQuail Membrane Samples... 50 "Tebl Table LIV. LV. Summary of Moisture SummaryofMoisture DeterminationsforQuail Determinations for Qusil Albumen Samples....... Yolk Samples........... 51 52 CentreAnalyticalLaboratories,Inc. Page 1007 102 000252 [I CentreStudy No. 023.063 Figure 1. Figure 2. Figure 3. Figured. Figure 5. Figure 6. Figur7e. LI OFFS IGUT RES Base Typical Calibration CURVE fOr PROS... 54 Chromatogram Representing a 0.1 ng/L. standard for PFOS ccc 55 Chromalogram Representinga 1.0 1g. standard for PROS... 56 (CChernotmraetIoDgRreaamgReenptrBelsaennktAi,nagSeRte:a0ge3n2t6Bl0a1nkAfo)r.P.FO.S.cvvsrsmsss ST CIDh:ro0m0a0t3o8g0r2aBmlaRenpkrAe,seSnetti:n0g3C2on6tr0o1l)Ma.llard Membrane for PFOS (Centre88 CphprboomfaPtFoOgrSa,m(RCeepnrterseeInDt:in0g00C3o8n0t2roSlpMkalAlaDrudp.MeImnjb,rSaent:e0Fo3r2ti6f0ie1d)wi.th 10 59 C4h1r6o.m2aptpomgraaim(REeDp1r-e0s2e6n3t-i2n08gM2a5)ll(aCrendtMreemIbD:ra0n1e03S0a9m2p,lSeeft:r0o3m2W6e0e1k0)1... 60 CentreAnalytical Laboratoriensc,. Page lot 102 000253 - Centre Stady No. 023-063 LAISPTPOFENDICES Page AppendiAx Study Protocol 00P-023-063 (Centre Study No. 023-063) and CentreAnalyticalLaboratories, lnc. Page 1207102 000254 Centre Study No: 023.063 1.0 SUMMARY `aClebnutrmeenAnaalnydticyaollkLasbaormaptloersiefso,rIntch.e(dCeentterrem)ineaxttiroanctoefd mpaerlfllaurodroaoncdtaqnueasiullfeogngatmee.m(bPrFaOnSe), according to protocol 00P-023-063 (Appendix A). Thelimitofquantitfaotricaocnhmatrix was 10ppb.TheLOQ forcachmatrix was determined in a method validation study performed at Centre (Centre Study: 023-027). POS ranged from non-quantifisble (where nor-quantifiable is defined as less than the `mcaolnlcaerndtramteimonborfatnhcesalmopwleesst,caflriobmratnioonn-qsutaanntdiafridab(l0e.1lenvgel/sm(L0) 3l5e5ve0lsngt/og4i3n4 tnhge/gmailnlatrhde albumen samples, and from non-quantifiable levels to 63,500 ng/g in the mallard yolk msaemmpblresa.ne PsaRmOpSlesr,anfgreodm fnroon-mqunaonnt-iqfuiaanbtliefialbelvee.lslteovel9s3.t9o n2g/0g90i0n tnhge/gquiainltahelbquumaeinl o`fsatmhpelseesr,easnuldtfsraroemrneopno-rqtueadnotinfiaawbeletwleevieglhsttba6s5s,.500 ng/g in the quail yolk samples. All Tahlbeumaevne,raagnedpyeorlckenstamrpecloevsewreierse9+1s%tanda6r%d,de9v1ia%tion1s6%fo,r aPnFdO9S3%in+ma1l3l%a,rdremsepemcbtriavenley,. The average percent recoverics + standard deviations for PFOS in quail membrane, albumen, and yolk sampleswere 102% 119%, 85%+ 5%, and 96+7%%, respectively. 20 OBJECTIVE "Theobjectiveofthisanalytical phaseofthestudywastodeterminelevelsof paelrbfulmueonr,oaocntdaynoesluklufsoinantget(hPeFaOnSal)yitnicsal mpetheodoctfimeiadl,l"maDredteaernmdniqnuasatiilonegogf membrane, Perfluorooctanesulfonate in Egg Membrane, Ablumen and Yolk by LC/MS/MS". 3I0NTRODUCTION ThisreportdetailstheresultsoftheanalyssforthedeterminationofPFOS inmallard and qual cgg membrane, albumen, and yolk using the analytical method entitled, "Determination of Perfluorooctanesulfonate in Egg Membrane, Ablumen and Yolk by LCMSMS". d`Tihriesctaonralsyitginceadl Cpoernttiroenporfottohceolstnuudmybwears00iPni-t0i2a3te-d06o3n. MTahrechex2p6e,ri2m0e0n1t,alwhsteanrttdhaetestWuadsy March 26, 2001, and the experimental termindaatteiwoans April 2, 2001. CentreAnalyticalLaboratories, nc. Pa13gof1e02 000255 Centre Stdy No:023.063 4.0 TESTSYSTEM `Thecontrolmallardandquail eggmembrane,albumen,andyolkusedforthematrix blanks and matrix fortifications were received on May 18, 2000 from Wildlife Iwnetreermatiosnasl Ltiiodt.,gheEdanisftfoeenr,ednMtDmatarnidcesst:ored frozen at Centre. The following Centre ID's MallaMradtMiemxbrane Ca00r0e380I2D MallardAlbumen 0003800 MallardYolk 0003799 Q`uQauialilMAelmbburmaenne 00000033779986 Qual Yolk 0003795 OnFebruary23,2001, 308quaileggsampleswerereceived. Thesamwperlesetorsed frfroozzeenn.unOtinltFheey wberre2ul4o,ag2g0re0d1yi,n1b9y4CmeanltrleadpeergsgosnnaemlploensFewberruearreyce2i6v,e2d0.0T1haensdasmtpolreesd wsetroreesdtofrroezdefnr.ozBaecnuhngigltshaemypwleerreecleoigvegdedwainsbdyivCiednedtienpteormseomnbnrelaonen,Maalrbcumhe1n,,y20o0k1,aanndd shell. Each componentofthe egg was given a unique Centre ID at the time of log-in. Althoughalloftheeggsampleswere receivedatCentre,onlythosedesignatedby the sponsorwereextraandcantalyezedd. `Samplelog-in andchainofcustodyinformationcanbefoundinthe rawdatapackage assowcitihathitssteuddy. StoragerecordswilbekeptatCentreAnalyticalLaboratories, Tanscs.ocainadtedawtirtuhetchiospsytuodfy.thestoragerecordscanbefoundintheraw datapackage 5.0 REFERENCEMATERIAL TEhnveiarnoanlmyetnitcaallsTteacnhdnaorldogPyaFnOdSSweraviscrees.ceivedatCentreon June3, 2000from 3M tSthaebicleirttyiwfaiscnaotofet aansasleysssiesd(ifnrtohziesns)taunddybwuatstuhseerdperfieorerntcoemeaxtpeirraitailowna.s Tshtoersedoalcucobridolifnitgtthyeo rrefeerencfemmaeatteerrriiaalieswlaissntednocbtelreoewle.vant to this study. The available information for the CPoFmpOoSund Cont0re0C0o3n.y0o2lNo. TCTRCORONIoT.4~S~ Pur9i7ty9() Expi0n8t3i1o0nD1ate CentreAnalyticalLaboratories nc. Page140f 102 000256 Centre Study No: 023.063 `The molecular structureofPROS is given below. PChReOmSical Name ~~ = Molecularweight = Perfluorooctancsulfonate 499 (CiFinSO5) cFuz--o 1 Noobtien:edT,heisnpeoattraaslsimuomlepceurlfleuaonrodoscttaanndeasrudlffornoatmew[hCiacFhirtSheOsPKF]O,Smo(laenciuolna)risweight 538. 6.0 DESCOR FAI NALP YTITCAI LMEO THN OD `AMnaelmybtriacnael, AmbeltuhmoednaenndtiYtoleldkb"yDLeterCmina/tionMwaosSfusPe/edrffloMrutohrioSosscttau"ndeys.ulfonate in Egg 61 Extraction Procedure Egg membrane A0.1 gsamplewasusedforthe extractionprocedure.Onemilloifmletihantolewars addedtothesample alongwiththre stainlesssteelbeads.Thesawmastphenlplaeced o`n mabeiadnbeaitear-tse~ct2a0te0po0nsirtptimofnior7~ffo2rumSimngiuntueetse.sE.aTchhesasmapmlpelweawsafsilttheernecdaenndtanrailfyzueogdnebady LC/MS/MS electrospray. Egg albumen and yolk A 10 g sample was used for the extraction procedure. Twenty-five milliliters of `methanol were addedtothe sample. The sample was placed on awrist-actionshakerfor 15minutesandthencentrifugedat ~2000 rpm for ~ 10minutes. Afivemilliliteraliquot oafltlhoweesdatmopilte.wEaascthaskaemnpalnedw0a.5s fgilotefrced aand rawnaablyszaeodddbenyd.LTC/hMeSs/MSaelemwctarsosspphraakyl.entehen 62 Preparation of Standards and Fortification Solutions SLatbaonrdaatrodriseosl"utpiroontsocwoelr0e0Pp-r0e2p3a-re0d27o.n AMnaricnhdiv1i4d,ua2l00s1tocaks sstpaencdiafridedsoilnutCieonntorfPAFnaOlSytiwcaasl preparedat aconcentration of 100 g/mLbydissolving 10mgofthe standard (corrected for purity and salt content) in methanol. From this solution, a 1.0 pg/mL fortification s1t0a0nmdaLrdwsiotlhutmieotnhawnaosl,prepared by taking 1mL of the stock and bringing the volume up to CentreAnalyticalLaboratories,lnc. Pa15gof1e02 : 000257 -_ Centre Sudy No: 023.063 fTorhteif0i.c1atipogn/smtLa.nfdoartridfaicnadtibornisntgainndgartdhwevaoslpurempeaurpedbtoyt1a0k0minLg w1i0m th moeL ftthahneol1.0 Apg0/0m1L 1g0/0mmLLstwaintdhamredtwhaasnpol.repbayrtaekidng10mLofthe0.1 pg/mL standardandbringingto gAs/emtLofssotlauntidoanrsidsnctohnetafionlilnogwiPnRgOmSannwears.preparedbydilutionofthe0.1 pg/mLand 0.01 TitelCone, (ug/ml) [o3l o0o1 o0o01 ofPROS Volume(wl) 5 2 51 2 1 DilutotGeuld) 110000 110000 110000 Final Co0n.e0.05(ug/ml) 00000012 0000000025 00001 `The stock standard solution and all fortification and calibration standard solutions were. psrteopraerdatiionnacarnefbreigfeoruatnodri(n4thCer+aw2daCt)aawshseocniantoetdwiinthutshe.isreDpoocrutmentation of standard 63 Chromatography tiQumaenotiffiPcFatOiSon woafsP~F4O.4Smwians, PaeccaokmspwliesrheeddetbeyctLeCdi/nMtSh/eMcoSnterleocltmraotsrpriacye.scoTrhreespreotnednitnigo.n iottehtehaenarlesyutletrseitnesnetvieornatliomfe,tbheurtetchoveearmioesunrtespodretteedctneddtwheerreesotnwleyrseiglneisfictahnnttehneoluogwhetsot calibration standard (0.0001 pg/mL). 64 Instrument Sensitivity Tchoenscmaelnltesrotasftt0a.in0do0a0nr1dgamo/uontfmPFiLnOjSe.cted during the chromatographicrunhad a Centre Analytical Laboratories, nc. Page 1601102 000258 -------- ee ---------- CeatreStudy No: 023.063 65 Description of Instrumeandt Operating Conditions Instrument: PE SCIEX API 3000 Biomolecular Mass Analyzer Interface: SCIEXTurbolon Spray Liquid Introduction Interface Computer: Dell UlraScan P1110 Software: HPLC: WPiEnSdcoiewxsANnaTl,ysvtervseirosni4on 1.1 HewlettPackard(HP)Series 1100 HHPP VQuaactuPuummDpegasser HHPP ACuotlousmanmpOlveern HPLC Column:Genesis Cs (Tones Chromatography), 2.1 mm x 50 mim,4 Columa Temp: 35C MoInbjieclteionPhVaosle.:(1A0):uL2mMAmmAceo tatein nASTiMtyu peIwm ater Mobile Phase (B): Methanal Flow Rate: 0.3 mL/min. Tio me e%A %4B 0 0 10 0 0 10 n75o 00 440 Tons monitored: AnPalRyOtSe neMgoadtieve Transi4ti9o9nM5o9n9itored Retention4T4i0me(min) `TPuanerFialemeters 1SC-oTnotsrporlasy 'DFP-PD-eFcolcuusstienrginPgotPeontetnitailal ECPE-CEonltlriasnicoenPoEtneenrtigayl CXP-Colision Cel Exit Potential CentreAnalytical LaboratoriIensc,. 42s0a00 2531000 1E0D0 EK Page 1701102 000259 _-- Centre Study No.: 023-063 DF-Deflector 3000 CEM-Channel Electron Multiplier 28000 GasFlows Sat Nebulizer Gas, 12 Curtain Gas 14 Collision Gas 4 TIS Temperature: 350C 6.6Quantitationand Example Calculation Ten microfosalmplieotrcaelibrratison stawnerdeianjerctded intotheLC/MS/MS. The `peakareawasmeasuredand thestandardcurvewas generated (using 1/x weightedlinar regression) by Analyst software using at least five concentrations of standards. The concentrations for mallard and quail egg membrane, albumen, and yolk (ng/g) were determined from the equations below. `Equation 1calculatedthe amountofanalytefound(inng/mL,basedonpeakarea)using `tphreogsrtaamn.dTahrdencEuqrvueati(loinnea2cralrcegurleastseidotnhepaa ramem terosf)oangaelu nyetreaftnoedunbt dyinthneg/Ag.nalyst software `Equati1o:n Analyte found (ng/mL) =(Peak area -intercept) slope Equatio2n: Analyte found (ng/g) =anal.foundsa(mnpgl/emwlt).x(gF)V(mL)x DE Where: FV = Final Volume DF = Dilution Factor. For samples fortified with known amounts of PFOS prior to extraction, Equation 3 calculated the percent recovery. `Equati3on: Recovery (%)= (anal.Found (ng/g)- avg.anal. inctrl (ng/g) x 100 `amount added (ng/g) An example of a calculation using an actual sample follows: Mallard albumen sample Centre ID 0003800 Spk A (Set: 0326014), fortified at 10 `pbb with PFOS, where: CentreAnalyticalLaboratories,Inc. Pa18ogf1e02 000260 -_ CentrStady No: 023.063 pmeearkcaerpeat. slope =So 3369 a dilution factor = 1 ng/gad(d forte levd el) = avg. amt in controls. = 10 ng/g. 0 (Not quantifiable) fsianmapl lveolwueimgeht =S 2l5omoLsg Note: Not quanitfisb is define as les than the concentration of the lowest standard (0.1 ng/mL). From equation 1: Analyte found (ng/mL) From equation 2: = Analyte found (g/g) = = [3369-9711 6700 036ngmL (Q31060n38gm)Lx25mL1x) `Fromeq%uRaetcioonve3r:y = 897ngmL = (89170nngglelex-0ngip1)0x0 Note: Thisexamplecalculation=wa9sd0o%neusingrounded numbers,andthereforemaybe slightly different from the values shown in the RAW DATA. 7.0 EXPERIMENTALDESIGN fBoartcifhiseedtoatfksnamopwlnecscoonnsicsteednoftonarenradea~tg2ein0tosalnmapnslke,,so.nEeamcalhrsiaxmbplalnek,wtswoemxattirxabculsatniekndsg tbhleasnpkprwoapsrainsatleymzeetd.hodandthen analyzeidn duplicate. Also, ineachset,aTyp1 ieO Centre AnsyticalLaboratories,Ic. Page 1900102 000261 eeeeeeee------------ Centre Study No: 023.063 8.0 RESULTS P`OmeSmbfraonuen,dailbnutmheen,reaangdeynotlbklablnaknskasraereligsitveedn iinn TTaabblleesII-TIVh.e TPhFeOSPFOinSthinetmhaelqluaarld d`meembtraenienc,steavleebruadmleonf,tahnedcoynotlrkolblmaantkrsicaerse,hgoiwveenveinr TfaebwlweesreXsXViIgXXnVIiIefnLoiuPgcRhtOaoSanlwtatesr the recoveries reparted. IndividualrecoveriesforPFOS in themallardmembrane, albumen, and yolksamplesare detailed in Tables V-VIL. The average percent recoveries + standard deviations for PFOS in mallard membrane, albumen, and yolk samples were 91% + 6%, 91% + 16%, aalnbdu9me3n%, +an1d3%yo,lkresspaemcptliveeslya.reInddeitvaiildeudalinreTcoavbelreiesXXfIorX-PXFXOXSI.in Tthheequaavielramgeembperracneen,t recoveries standard deviations for PFOS in quail membrane, albumen, and yolk samples were 102% + 11%, 85% + 5%, and 96% 7%, respectively. PcoFnOceSntrraantgieond froofm ntohne-qualnotwiefsiatbleca(lwihberrateionnon-qsutaanndtairfdiabl(0i.s1defnigne/dmLas) leslsevtehlasn thteo 434 ng/g in the mallard membrane samples, from non-quantifiable leveltso 3550 ng/g in the mallard albumen samples, and from non-quantifiable levels to 63,500 ng/g in the malyollkasamrpleds. `Theseresultsarereportedon a wetweightbasis. Individual results are listed in Tables VIII-XXV. Someofthe high levels of PFOS reported for some of the mallard egg membrane and egg albumen samples could be from possible contamination from the egg yolk of outer shell fPrFoOmSnroann-qgueadntfirfoimsbnioen-lqeuvaenltsiftioa9b3le.9lenvge/lgs 1i0n2t0h,e9q0u0anilg/aglibnutmheenqsuaaimlplmeesm,barnadnefrsoammpnloens., qauwaenttiwfeiaibglhetlbeavseilss.0In6d5i,v5i0d0uanlgr/egsiunltshaerqulaiisltyeodliknTsaambplleess.XXTXhIeIs-eIrLes.ultSs aro eorfeptmohretheeidgohn lceovuelldsobfePfFrOoSmrpeopsosritbleedfcoornstaommienaotfitonhefqroumaltheegeggmgemybolrkanoreaonutdeergsghealll.bum`TehnesSapmopnlseosr. Representative also informed Centre that the quail outer shells were not washed prior to separation of the intemal components. `Theaveragepercentmoistures forthemallardandquail eggmembrane,albumen,and `yolk samples are given in Tables L-LV. 90 CONCLUSIONS `The mallard and quail egg membrane, albumen, and yolk samples were successfully extracted and analyzed according to protocol 00P-023-063. (CentreAnalyticalLaboratories,Inc. Page200 102 000262 CentreStudy No. 023-063 10.0 RETE OF DN ATATANI DSAO MPLN ES `Whenthefinalreport is complete,alloriginal paperdatagenerated byCentreAnalytical Laboratories, Inc. will be shippedtothe sponsor. This does not include facility-specific raw data such as instrument logs, however exact copies of temperature logs will be `submitted. Exactcopies ofall raw data, as wellas asignedcopyofthefinalanalytical report and all original facility-specific raw data, will be retained in the Centre Analytical LaboratoriIencs., archifovrethse periodoftime specified in40CFR Part 792. Retained `samplesofreferencesubstancesarearchived bythe sponsor. Centre AnalyticalLaboratories, Inc. Pa21gof1e02 000263 - OOOO . TABLES Snir srs 000264 --_-- CentreStudy No:023-063 Tablel. Suom fPFOm Sin a Reager nt Bly anks -- SpooworD RegCeu"_ a3Btrie kA _ NeNuOmSm0bbtIe_ eAr BDaGt_ Dru6aetc0eeton _ WAD6Dmuu2iiMsesI_ FFoomAummiM_ idQygipeh mm RReegpuuBBllkkAA 0026600A ReguBakAt O20B Ws6o0l1 M3e27200m 32600 2700 NNog No mmo RRaeppnaBBulkkAAt O02200ICC a3sa8o0 33220000 uw RegaBkA 020M domi 32w00 NNoo No TMTM m RReepguuBBllkkAAt O022008 RepmBukA O20 zmo1 30 w32m80l0 vm0 NNGo NG nnmm RReagpeoBBukkkAAr o0ZOcC 330010 030990000 NNoo Bnmm RReegpmuBBllkkAAt OOIRAR 3320310 335000000 Bm RegBmxA 020 m0 3001 NNoo No nMmm RReepgwuBuBkkAAt O02N0SA 3W2930010 33300000 NNoo mmo RReegpemaBBllkkAAt 0O2S0BA 33950010 W35A10I0 NNQo mwm RReeggwwBBlluakkAA' 0ONOBOIA 333900001 3441010 NNoG nm RReaggeowBlBolkkAA OODBOOR 33000011 44210011 NNoo mm RReegpwwBBulkkAAt OO%0BIC 3300000 4422000 NNoo = +Duplicate jRcteiognmBekA noc STwAoNDoAlRDDEV4AIVAETRmIAOGNE:: NNNgGO NQ = NotQuantifiable (lessthan the concentration of the lowest standard (0.1 ng/mL) LOQ= 10 ppb I CentreAnalyticalLaborsoris nc. Page B3of102 000265 ee -- `Cente Study No. 023-063 TableIl. Sponsor n mm Mm SummaryofPFOS in MallardMembraneBlanks Centre n OCBC2BBkAA* OoOmEaRBBlkasAkCA Se Nomber Exinction Date Asabds Date Amaiyte Found (ppb) 0O2E0IICC 2601 360 3zml 3200 No No O0RW0OIC Ol 3701 VL 39% No NQ STANDARDDEAVVIEARTAIGOEN:: ~~ NNQQ TableIII. `Sponsor D Mm m m TM Mm Summaryof PFOSinMallardAlbumenBlanks Centre D COOJOBBlWmEkAA* OOGXB0OBBUlskkAA* 0O0ONM00BBInmkkAAt Se Number Exactin Date Asay Date Amie Found ppb) OOIRMAIA e32660011 3w2e52i0l1 NNQQ 0072008B 3201 3201 3282901 IML NQ NQ OOIC OBC 3001 M001 42L 4am 603 659 AVERAGE: 294 STANDARDDEVIATION: 262 Table IV. `Sponser D ry wm m mm SummaryofPFOSinMallardYolk Blanks Centre D OCOMOMOBlMmkAA OMONOBBnA kAr St Number Extraction Date Anais Amayte Date __ Found (ppb) 00N26I0IBB 23620601l 332z0LM NNoQ OOOWI0IAA W201 327m 3281 wor 957 90 AVERAGE: S48 STANDARDDEVIATION: 487 *Duplicate injection 'NQ=NotQuantifiable (less than the concentration of the lowest standard (0.1 ng/mL) LOQ= 10 ppb FwoarsruesseidduteoscraelccoulradteedtahseNaQve,rahaglefoafntdhsetacnodnacredntdreavtiiatoinoonf. the lowest standard (1.25 ppb) `CentreAnalyticalLaboratories, Inc. Page 240f102 000266 - Centre Study No: 023.063 TablVe. Sponsor IY m mwmm Mm mm m mM m Summary of PFOSRecoveries in Mallard Membrane Centre D Set Number Extraction Date Aualyss Date Amt Added (ppb) cCOOmDmMR2SSpEKEAA 0200IC 0260IC 3ae0l 32601 2700 32700 0 10 OOONSMRRSSKKBBe GORBGGIICC 3322660011 332270010 11000 GOONBm2RSHSKpAAT GR2OIC GR0IC 3701 3701 3900 32901 10 10 oOoNoBmoQsSpXkBBe GR0IC owoic 20 mol 32901 nomi Ed 9 STANDARDDEAVVIEARTAIGOEN:: RELATIVE STANDARD DEVIATION: * Recovery 5 o aa 0 0 9s 9% 91 76 TableVI. SummaryofPFOSRecoveriesinMallardAlbumen `Sponsor D Ceatee D Set Extraction Analyse Number _ Date Date Amt Added (ppb) ms on OONOOOSMPOSKPAAT GR60IA ORGIA 32601 32601 326210 326271 0 0 wm Mm GOODOBNOOOSSKpKKBBT ONOIA OGOIA 3260 32601 3262701 3262701 9 % mMm OODOSNOSOOSSpPKKAA GORR2070IIBB 3322770011 33228822990001 0 10 mm nm OOONIOOSSKKBXB* GRI0IB GRO 32701 V20l 3282901 3282901 9 9 mTM COOODMOOOSSKKAA ODOOINCC 333000011 44220000 1100 Mm nm OO0NSJO0OSSpKKBBe (XOIC aoc 33001 dAomi 4200 4201 one ours AVERAGE: RELATIVESSTTAANNDDAARRDD DDEEVVIIAATTIIOONN:: * Duplicate Injection L0Q=10ppb % Recovery o1 ot 1207 105 to %5 6 % % 91 16 17 `CentreAnalyticalLaboratories, Inc. Pa25gof1e02 000267 - Centre Study No.023.063 Table VIL SummaryofPFOSRecoveriesin Mallard Yolk Spomor CeInDtre NuSmuber ExDmactsin ADmuiss AddeAdm(pb) Res*owsy NNao CGOMSWSSKEAA 0022606i0B 636001 3320000 T1o0 T1o4r NNoo OO0NSUOSSKKBBe o0Rn60eB ssuull a2m0oln 55% % NNee GOOmMmOOSSRKAAT O000I1AA 2l0L1 3302880000 0 n NNo ooCOWsOSeKB OoRm0IaA Wdoe 3o2w0e0 95 58 STANDARDDEAVVIEARTAIGOEN:: 9133 RELATIVESTANDARDDEVIATION: 16 TableVIL SummaryofPFOS for Week 1 MallardMembraneControl Samples Sponmsor Centre NuSmtber EEollmeeaone oOWOE0 | 00200IICC BBolLmOesOaoMse OolEs O0RIeICC EELLossoze0s8ese oOmse 0OR6eIICC EElGmeeaaomswee oONiE oGR0AiICC EElLmMa oOldiIes OO0IR6CIC +Duplicate jection EDxaitmscn ADmaites FoAumdi(toept) Mweeue 3samn NNoo e3so0L 3m0L Nnee We60101d3L NNoo awesoul vmaol nNeo saswoi 3a0mn0L NNeo STANDARDDEAVVIEARTAIGOEN:: ~~ NNQQ 'NLQ 0= N1Qo0tQp=upabntifiable essthan theconcentrationofthe loweststandard (0.1 ng/mL)) CentreAnalyticalLaboraoris, Inc. . Page260102 000268 - Centre Study No: 023.063 TableIX.SummaryofPFOS for Week 1MallardMembrane Samples at 6.2 ppm ai Sponsor Centre m TBolcmaeeaameess o00o BEOlLOe62u0Me6 OOBIEG B EOLL 26I0O8R OO3BI00 EEOOLLOC3Sa00MMT7T OOBBIIS EEOlLm6eS2a0uMEs oOBwIsE NuSmeber ExDtaratcetion ADmatei FoAunsdiaept) 0ORIOICC J3aaeso0ll vwaaml tTeeses OORIEICC ew deol 3am 3m 6s 62 OORIGICC dseooll 3aol 7212 OORRGGOIICC 3s6o0l 3371m 3219 oORnGeOiIcC adessou 3a7m0 s5s4 STANDARD DEAVVIEARTAIGOEN:: 141021 TableX. Sum ofPmOSa forrWeey k 1MallardMembrane Samples at 17.6 ppm ai Spossor o Centre St Number ETooLlOmseza0ilsSes OORlIeG | O0RRORIICC EELls;a0eme0sr OoBlIaS OORRMOCIC EElmLeE rs oOmZo OoRa6oIiCc EEOLO23L208]51 OOINONSS6 GORRe6O0IICC EEllsmes ooomme o0RnRiIcC Bxncin Amis Date Dats __ ndeesool 3wm0l 63s00L 3371m dwaeeonl wwem 330610 moLl meeom wwmml AVERAGE: STANDARDDEVIATION: Amite Found ep) 226000s0 22556 709 amm0e 0s021 2S3211 + Duplicate jection 10Q= 10ppb R+epProessseinbtlaetciveorequnesttwerabeynyomotlukisoerdontuotceaalschutellatleciothmepoaovnenernatgoefasnd sa tandaam nrddadsepvpieartl iSopno.nesor CentreAnalyticalLaboratories nc. Page2701102 0600269 - Centre Sdy No: 023.063 TableXI. SummaryofPOSforWeek 1Mallard AlbumenControl Samples Sponsor I E01-0263-20852. EEB01m-i02e6G3n-o20e8o5e2% EBmeiosGse EBlimmeeoaswr Boma Boer Centre 0103201 0OO1oo03mm20ss1 OoEnD OOmNeG oowesess NoSmbter 0326014 0mG32uR60aA14 GGORAA GORHGINAA mpeAin ExDuoen ADmaited__FouAsmdipepb) 32601 3262701 NQ sS6o00l11 we26e2rz70o1 NNNQQO M3Se0o1 W36622001 NNGO nSeOoL M3662M0L NNGO swoeln Wsemzool NNQg AVERAGE NQ STANDARDDEVIATION: Ne TableXII. Summaryof PFOS for Week 1Mallard AlbumenSamples at6.2 ppm ai Spomor Cen"t3re NuSmber BDaumscon ADmuies FoAwmdiipeh) r Tomese On URI as01 ezidl 24 EElpmeeasss OONWTT omnAe oSs0o1 dWasszaomll 71580 EEollmmaesnee Oo0o1 EDEN OIS mOeReiInA GIA eSOwL ssazm We0l W62m SS6m7 S76 | BEolmLeiaMows OOOoNNSNs RO2OOIAA MMee0nl WW662O1L SS9S8 | Eolmeous owns oma wen eAVrERAmGE: 564 | | STANDARDDEVIATION: 130 Duplcte Tjction 'LN0QQ==N1o0tpQpuabntifiable (less thantheconcentrationofthe lowest standard (0.1 ng/mL) CentreAnalyticalLaboratories nc. Page2801102 000270 --- Centre Study No: 023.063 `TableXIII. SummaryofPFOS for Week 1Mallard AlbumenSamples at 17.6 ppm ai Sponsor Centre NuSmeber EDxaitnscin ADmuiiss FoAunmdi(eopt) ETolr;oweesaamoesses OOWlRoDm GORR0MIIDD G326U01 wdaaasawri wasosmo BEOLOO2L308DS6 001002321177 OoBx0oIiCc soon IOI aol 4200 13850 136m EEoOLLO6sI3200M8SS66 OOI0RRTDDwp OGGIOICC 3336000011 442200 Taiesee ElGa060 Elmeaes OINISH OJI3 ORMIA ONIA G3D60Ll a3assmii B24S7 EEOOLLOO62362320068SS77 0O1l003s222211 oolAa oseoml e dasmzm 8B3s EEOLLCEIR2a00sSl1 O010N31S97 OooIlA a6001 e el l @T7O EBnoolcmzioaeessst oOlloXwaaSs oORnGOsIA nIe60oI wdepie 11997s STANDARDDEVAIVAETRIAOGNE:: 222250 Table XIV. SummaryofPFOS for Week 1 Mallard YolkControl Samples Sponsor Centre EToLoo220a82e OODIEE EEOoLlOcGsaIo0e8sSsI OooRm; EEoOLL26eII220086SS4e OOlI00RS0066 EEl;le2e0s OOINONSSS EBlmomomesrsoomne + Duplicate jection sa Number GOReBl oOnNGeOIsB OORRE6OOIIBB OGRR60IBB o2eBm Estacion Due Amys Dats Analyte Fousd Gp) wdae6s0wL aILm NNoo 63ae0on 3d2a7m0m1 Nxoo 33aasso0ll aomll NNoQ 33660010 332m0 NNoo eeeon omll NNoo STANDARDDEVAVIEARTAIGOEN:: ~~ NNQQ 'NQ = Not Quantifsble less thantheconcentration of the lowest standard (0.1 ng/mL) LOQ= 10ppb R+e+pProessseinbtlaeticvoentraeqmuiensattiwoenrebynoytoluksoerd tooutcearlcsuhlealtlectohmepaovneernatgeofansdamsptlaendaanrdddaesvpieatriSopn.onsor CentreAnalyticalLaboratories oc Page29.1 102 000271 ---- Centre Study No: 023.063 TableXV. SummaryofPFOS for Week 1Mallard YolkSamplesat6.2 ppmai SponDsor caTrDe NSem BDnucein ADmuei ouAnsdiaep) ETloelamomasne OoNN GOM2GO0ID wWa6e001r I32mraasmdl 22457800 EEllmeemsaiwse oOlTae O0NOGDD a6u0l1 3371as2e0l 1122510000 EBllmoeeer ooluouss 0O0RDD 3ee0l r37a28s00 0100 EBlomleesr oOlIoEs O0NRGIDD asbull 3amassell 110150000 EEllm6eaMmss OoiRe RpAeInDd 6s0e1v 3o2sse 1122110000 STANDARDDEAVVIEARTAIGOEN:: ~~ 4344500 TableXVI.SummaryofPFOSfor Week 1Mallard YolkSamples at 17.6 ppmal SponDsor CentDre BToLrcQae@ssamee| OOoRulMs EEOLLO;GSGZS0Z805S0T OO3O0S EEDLl232m08s57 OolWowSis EBoLicIasAaoSs oOleIs Elsa Ow NSeum BxrDmuceton 00R%66IIDD wpa0e1 OORRGAOODD 6Ie0bl OONREeOIDD sWoalo oORnGIoD wasoo Gu6ND sul ADmuiee 3w17a2a0o0n Irraamei 3r1a2sao0ln n21a28e00 3zashl FoAunsdioept) 330030000 "0a0n0o Ss6ma600 5p10y0 si00 STANDARDDEAVVIEARTAIGOEN:: 4182500000 Duplicate recon . 10Q=10ppb CentreAnalyticalLaboratories, loc. Page 300102 000272 - Centre Study No: 023.063 Table XVII. Summaryof PFOSfor We6Meallkard Membrane Control Samples SpIo"or Contre BE omaE ss E0) 10364 BBoLwOeGs O010l37e68 EElmwess 0o1l0s3 EEllmemrss oolsken EBLoOlE2e9s7 _ oO0li00s5T7E800 NumSbter oaozoo aaomco owzzooicc oownoioc oGrmocce EDxaitmecon ADmaiten FoAwmdiGep) vzoemn vaesll NNoo vvoomm wwmmll NNoe vvozm wwnmt NNeo wwzzm wvmm NNoo swmm nwoomm NNoo STANDARDDEVAIVAETRIAOGNE: ~~ NNCQ. TableXVIIL Summary of PFOS for Week 6MallardMembrane Samples at 6.2 ppm ai Spomor Centre m B BOLL;O O0l100s3T7O0s8 BElLLesO2i0G0 0011003379966 EEoLloesmaoease O0L100sT5A7s BmLiRmSAeSsI 0o0l36e7s6 EE0l3m0s9 0011003374488 *Duplicate njction NumSbeer owmoic mozoocc aaoocc Gamoo oawoocc EDxaitmeco ADmaites FoAwmdi(pepb) vsmmn awml 0085 mwomm v3mm 555533 wamee ovomm 558577 vaommo waem 1m6e0mee vvoomm wwomm m582 STANDARDDEAVVIEARTAIGOEN:: 7117.03 '1N0QQ==N1o0tpQpuabntifisble (lessthantheconcentration ofthe loweststandard (0.1 ng/mL) R+e*prPeossesnitbalteicvoenrteaqmuiensattwieornebynoytoulskeodrtuotcearlschuelllactthoemapvoenreangteoafnsdasmtpalnedaarndddaesvipaetriSonp.onsor CentreAnalyticalLaboratories nc. Pa31gof1e02 000273 J ---- Centre StudyNo. 023.063 `TableXIX.Summaryof PFOSfor Week 6MallardMembraneSamples at17.6 ppm ai SpIo"ns)or Contre ETondoass 0ol00s3Ts6e mmiiawmsoe 0o05s82 EBLomsas0n OO0000 BELslsmzis0e olonlssesoose EoELoolamesss20lo000s 0o0w3s8s0o8s NuSmtber Tmzioccso wazzooccoo oomzooccoo oozoocoo oozoocno EcDukeo ADmues wwmol snonm vwoon 3s9o0m1 vvaamm 33990001 vvaamm 330000 evnm 3s0a90v0 STANDARDDEAVVIEARTAIGOEN:: FoAwmdieey) oaos 2065 330 0a6 220 63102 TableXX. Summaryof PFOS for Week 6MallardAlbumenControl Samples Sponsor Emaam E01-0263-20993% Centre n 006s 0103765 MeStmb wom 0327018 EDnuec ADmuisk FeuAmdipeh) Al wss0l Ne Ec 328-2901 Ne E01-0263-20094. E0E1-o0l26m3-s2a09m94s* Emiomness EElnmeeras _Enocowwr ---- 0103769 0o10w37s69 001003793 o0lss ows 032701 0oo32zo70oo18 Goanoon ozo owls 3m 328-2901 No E vzL zm 3ms28-s2m9m01 NNNoee wamme mmaaem NNeO azo aman NO vmoy smAVsEwRAoGlE: NNOo. STANDARDDEVIATION: NO 'NQ =NotQuanifsbl essthantheconcentrationofthe loweststandard(0.1 ng/mL) LOQ = 10 ppb Centre Analytical Laboratris, nc. Page 201102 nNN0274 Centre Study No 023.063 `TableXXI. SummaryofPFOS for Week 6MallardAlbumenSamples at 6.2 ppm ai Spomor Cenmtre EEol6as9ao9n o0I0SsTOD EElLmeSr 0011008379917 E EOLOLGSZ0E988 0O1l00S3TasS BBoolweenn 0001%07% sEDoLOl620o98s9 Ooloonna NeSmbee ExDiumcsion ADmuien FoAumdi(pey) GGroois smainn smasle 568 2 oozzoosB oomn mmaaem 1s%o oazzoo osnm mmsee 66 6 aomozs onoen mmaaem 1es ooooln somm soasem ssnn STANDARDDEAVVIEATRIAOGNE: 0751897 `TableXXIISummary of PFOSfor Week 6Mallard Albumen Samples at 17.6 ppm ai Spoor Gennre EBOLoOaG2o0L 0O1l0088T7SSTT EBoomlasd0ar oolloss EBOLoOGlZIgO0 o0ll038l0L EEoLLOmeGs2a0I0s0 0o1l0os3k0o5s BoLoeszion olsun Eom 008 otosan * Duplication NoSmebe ExDmuceim ADmuei FoAusmdinpeh) Goozlos swzmimln wssmdel 2u8o3 cazmooms mson asmseo aulr oooolm vmoL wssmzem 119974 oomwosm zwom asswme 224s0 oom oon omomn sssszwm 1192a STANDARDDEAVVIEARTAIGOEN:: 421023 L0Q=10ppb CentreAnalytical LaboratorieInsc,. Page330 102 000275 . --_-------- Cone Study No: 023063 `Table XXIIL Summaryof PFOSfor Week 6 Mallard Yolk Control Samples --D ConDte Brlgmeaame oonvaa BBmww oovvee BBiimaeasmes momoom BBilwaeasrss oommee Emimnmuem ooormn MeSmtber BuDuer.n AmDiunre sAemmiie) owoom meel avmeel MNae wowooiA eell mvemle NNae oowowiA uemle aammel NNee mowooaA eell uvmaem NNoe owwean umel ummeel Nnee STANDARDDEVAIVAETRIAOGNE: NNao `Table XXIV. Summaryof PFOSfor Week 6 MallardYolk Samples at 6.2 ppm ai E `SpoDnsor. CenI Dtre MSeembter Due Extraction Dur Analysis SoAnmaliytre) Bmleasmoe oolwoew GGraouiabb mamml suemle 1ow5e0 Diimmees ooowme Gcaobooalml daemle lookwo BSlemeaaenm oowveas Gow;oOiAaD> dvomm oeoe lieo EBGimmaemaiwe oomoewne GGwomolAAD> damoll doeel mloeee I game ou moon wml AoVERoAGE: s161o00 [E-- STANDARD DEVIATION: 6330 ! '1N0QG==No1t0Qumantifiable esthanthconcentrationoftheloweststandard(0.1 ng/mL) CentreAnsyial Laboratories, loc. Page of102 02786 EE -- CentreStudy No. 023-063 TableXV. SummaryofPFOS for Week 6Mallard YolkSamplesat 17.6 ppmai `Sponsor Centre EBoLmOeaL91e oOll0o3sTsSsA EELlOmG2e9r0 0011003377500 EELOlG2mI0s02 o0l1o0s3m9s8 EE2l6m2s0 oomie EE0OLLUOEGSI21Z0I00660 00110033880066 NSuemtber oTOoAdD oowooluD> oooopp oooopp o oood EDxtartacetion AnDauliyssis woolm wweeel zwolm vweeml zzoon dweell ooll wwemll seoly nOoLm STANDARD DEAVVIEARTAIGOEN:: `Table XXVL SummaryofPFOS in Quail Membrane Blanks FoAunnadlyptpet) a4m0 essoow ssmsoo deein adsewoeo $80877000 Sponsor CenotDre NSumebter ExtDraatcteion AnDaluyesis FoAunnadlyptepb) Wo COLTSBMEA| GIOIA 301 36101 No mTMo CNOITSSSEBBkKAAC OONZOSOIBAR 3300010 340210000 nNeo nm ooovosBmkAt oneBR 3001 AVoERoArGE: No NQ STANDARDDEVIATION: ~~ NQ `Table XXVII.SummaryofPFOSin Quail AlbumenBlanks `Sponsor CentDre. NuSmebter ExtDraucetion AmDluyess FoAunnadlyoteod) wmo OOOONSBGaBEkAA| OO0MIBB 33220810 330000001 Nnee mwm oOooNsSmeGbBimkkAAr OoNsGoInAa 3s6e0m0 4aiAmI nNeo * Duplicate jection STANDARDDEVAVIEARTAIGOEN:: ~~ NNQo LNOQQ==No1t0 Qpupabntifiable (lessthantheconcentraotfitohneloweststandard(0.1 ng/mL)) Centre Analytical Laboratories, Ic. Page 3sof 102 000277 EE CentreStNuo:0d23.y063 TableXXVIILSummaryof PFOS inQuailYolkBlanks Sponsor Centre Su Euros Amis Amie Ir) Number Dae Due Found gph) Wwwo oCmOTTSSBBuAkkAA| GOZMOIIAA 332288000 3305000011 NNoo mwwm oOwMmIsSBSBuumkAAr o0mSSeOB 3o9mm WmaMnOo NNDp STANDARDDEAVVIEARTAIGOEN,: ~~ NNQQ `TableXXIX.Summary ofPFOSRecoveriesinQuailMembrane SpoIn)sor CeInDtre NSetm ExDucel ADmuiss AddeAdm(op) Reco%very mwoo OGHSTEASSAETA OONS00IIAA VSO1L WBAILOLL m1o0 0104 mwom cClTISBESSNKDBe 0O0I1AA S9O0L O33L01 o8n6s r5y wmoo oCmOSWEESSEMAA OONBOOIIBBRR 33330000 44220000 110 1h1m6 wnmm eomessmsksBne oonoon 3v0i0o 4a2o0n1 5%8 110018 STANDARDDEVAIVAETRIAOGNE:: 11012 RELATIVESTANDARD DEVIATION: 11 *DuplicateIfecion 'NNDQ == NNootpQeuaakndteitfescbtled.(lessthanthe concentrationofthe loweststandard(0.1ng/mL) L0Q=10ppd CentreAnalyticalLaboatoris, oc. Page 36.1 102 000278 -------------------------------------- ere StyNos023-063 `TableXXX. Summaryof PFOSRecoveriesinQuailAlbumen Spnoor CIoDe NeSuwb BeDiumcsim ADmuiiss AddAeimGpd) mw GGTeSSSKA GGOmB 3os8o0i 3305000011 T1o na 0003796SpkB 032801 32801 35001 9963 -Mm 00C03M7M96SSpEkAB 0O3N28D01AB 332080001 354010011 19963 nmnmwm 0o0o0oO3m7m9m6eeSpsSkpBAe* om0m3o3m0i0n1AA 3do/3o0m/o01 auwolur 10 STANDARDDEAVVIEATRIAOGNE: RELATIVESTANDARDDEVIATION. Hea"rs TM 0 =) 5a8t8 55 & `Table XXXI. SummaryofPFOS RecoveriesinQuail Yolk Sponmor CIeDe NaSmwber RaDcuein ADmuisk AbdAedmop) Re*sor nmno coms 0003795SpkA 0o3w2m80i1aA o32w80e1 y3o0u0l1 1100 110024 nannm 0c0Co0O3o7mS9s5SsSEkpkmABe oo0um32so8i0B1aA 3ou2w80me1 olw30o0e1 9s60a2s3 09n%1 nwmm oOXwweessSSKkABY COmmoeBD mmonl aalnoanm owlon n54 nm coomsswpe owsop doom wim AoVwERsAGE: % RELATIVESSTTAANNDDAARRDDDDEEVVIIAATTIIOONN:: 77 +Duplin L0Q=10ppb Centre AnalyticalLaboratories, Ic. Page 370f 102 000279 Ceatre Study Noi: 023-063 Table XXXII SummaryofPFOS for Week 1 Quail Membrane Control Samples `Sponsor D Centre D set Nomber Extraction Aubpsis Amlyte Date Date Found(pb) EOL0255.20506 0101987 E0L0259-20506% 0101987 omsola ool wool vel 3600 38 S20m se E0LO2S920507 EDLO253.2007% 0101991 0101991 oma sol BIO onsolA sol BIOL Ng No EOLOSO-0520 E0LO259-205200 0102043 0102043 omsolA onsolA ase se BIOL 3601 NQ No EOLOS20S2 0102047 EDLO2s00s21% 0102047 ool mola vol sw sol 38M ~Q No E0LO259:20509 E0L02S920509 0101999 0101999 sonosloal swomn 33BnUwOoL NNQO AVERAGE: NQ STANDARDDEVIATION: NQ Table XXXIIL Summaryof PFOS for Week 1Quail Membrane Sponsor Samples at 6.2 ppm ai Ceatre Set Extraction Amalysls Aualyte D D E0L0259-20526 0102067 Number osoD Date wenn Date Found (ppb) anal 18800% E0LO25920526" EOLO2SO0S14 0102067 0102019 onsoD omsolA sel sel 4n0l BIOL 170 E0L0259.20514% 0102019 BOLO) 0102071 omsolA ool wvoL oo BIL BW El m EOLO2S9-20527% EOLO250:20515 0102071 0102023 oso omsol aso sel BIOL 300 116 m EEoOLLOo2Ss9s20s5l28s 00110022002T3S momsoolpA oseIl a3noBn 1m1S E0LO2S520528" 0102075 OonoOID neon AaVaERpAGE: li14s0o | STANDARD DEVIATION: 253 * Duplicate Injection 'NQ = Not Quantifisble (less than the concentration of the lowest standard (0.1 ng/mL) L0Q= 10 ppb += Possible contaprmiionrattoiosnepbayraytoiloknoorfoiuntteerrnsahlelclomcpoomnpeonntesn.tAofspseamrpSlpeonsisnocre outer shell - Centre Study No.: 023-063 `Table XXXIV. SummaryofPFOS for Week 1 Quail Membrane Samples at 17.6 ppm ai Sponsor Centre D D EEO0L1O022S5S92.200552299% 0102079 0102079 EE0OLL2O8S92200553311 0102087 0102087 EED0LL20SZ9S292005533220 00110022009911 EOLO259-20518 E0LO2S9205180 0102035 0102035 EOL0259:20533 E0L02S9205330 0102085 0102095 set Number oso nso nso oso oonssooD oso oso onsoID oo Extraction Auslys Date Date sol nani W901 wow anal 4n2nl wow sol 1200 ann op ase anal nan ase anann ws woe 41200 nam STANDARDDEVAIVAETRIAOGNE:: Analyte Found ppb) 20900 2000 11000 11100 16300 1390 12500 12600 23 69% 13100 4730 `Table XXXV. SummaryofPFOSfor Week 1 Quail Albumen Control `Samples Sponsor Centre 'y n EEOOLL0O225595-:202500066% 00110011998888 EOL29:20507 EOLOS920507% 0101992 0101992 EE0OLL205S992200552200% 0102044 0102044 EOLs50s21 EOLOSS20S21 0102048 0102048 EOLO255:2009 E0L0259.205090 0102000 0102000 set Number opm oso ops 0B oz0B oonssoisB oossB oop Extraction Avalyss Date Date esol awol 30000 36000 mmooll 3385000000 wel 36001 womwooll s36o00n1 msooll 3365000010 wer soo AVERAGE: STANDARDDEVIATION: Analyte Found (pb) No NQ NNQQ No NNao NQ NQ NO NQ ~~ NQ *DuplicateIjction INQ = Not Quentifiable (less then the concentration of the lowest standard (0.1 ng/mL)) L0Q= 10 ppb CentreAnalyticalLaboratories, Inc. Page39.0f 102 -_ Ceatre Study No. 023-063 `TableXXXVI. SummaryofPFOSfor Week 1 QuailAlbumenSamples at 6.2 ppmai `Sponsor Centre D D EEODLIO022S9O.22005522660 00110022006688 EEDDLL0O22sS9O--2200551144% 00110022002200 EEOOLLO02ZSS9O220055777 00110022007722 EOLO2S9-20515 0102024 EEOOLLO2S5O0:22005512S8* 0102024 0102076 = E0L0250.20528" 0102076 sel Nomber os0B Ons oonsnolsB omsB oonsm0B osiB ou0B oso Extraction Amlpls Date Date 3201 wel 3360003310010 30l 3as01 336600331I0011 3n801 mol 3300033110001 wel 3003101 wel awoL 33031010 031 amo 3n03uol AVERAGE: STANDARD DEVIATION: Asaiyte Found (ppb) 603 54 20 2m 204 53841 608 99 gare 438 1.61 Table XXXVILSummaryof PFOSfor Week 1 QuailAlbumen Samples at 17.6 ppm ai `Sponsor Centre D D EOI0259-20529 E0LOZSO20529 0102080 0102080 EOLO2SS0531 EOLO2S9-20531% 0102088 0102088 EOEOLL20s2Ss902055302 0102092 0102052 EOLMSS0S18 EDLOSSSIE 0102036 0102036 EE0OL0L2OS0S-O200533330 00110022009966 -- ~ *Duplicate njection sot Number ORB oomss0iBB o;sB onsIB oOsnsE oRsIB ORME opp Exmcion Date Amis Date 3280L wel 3503101 3803100 30s0L 30801 3603101 3503101 sol 3003101 2aem0oLr 3363003310001 3mOL wel 33060033110010 ower 3n0suol AVERAGE: STANDARDDEVIATION: Awbte Found (ppb) 9 3 997 105 107 2130 316 907 101 160 892 L0Q=10ppb CentreAnalytical LaboratorieIsn,. Page 400f102 000282 ee---------- Centre Study No. 023-063 `Table XXXVIIL SummaryofPFfoOrWeSek 1 Quail Yolk Control `Samples `Sponsor. Torsone E0BB 1-0i259-L s205s06* BBiisHa iElmss EBLvsoez0ss0 Centre. oles 01001010101919898589 oollss o0lo2s0ss ootio0iisseerT MSemebter moa 0oo32uu8oo0li1AA4 ommooll oozoAl oonpssa Due Extraction awl Duc Analysis 35001 FoAunadlypteh) No 0 a28w0n1 33330000000010 NNNooo mmoorr 3300mm Nxoo namwoor a3n0o0l0 xxo wwwmeww 3n0o0o0n oNo STANDARDDEAVVIEARTAIGOEN:: ~~ NNOQ `TableXXXIX.SummaryofPFOS for Week 1 QuailYolk Sampalte6.s2 ppm al `Sponsor D Centre. BBoicsats OOlWe EBLmiSSs0sSu OoHoVn EB LsSLTe OoIoGd EEiLmsoSsiIs oOlpmm EEmwonws OoAoDm + Duplcste Ifction NSumebter UGROMIDAD OORHM0OIAADD GoHMOOAADD oOmRoAIaADD GomRoAaDp Due Extraction AnDaulyissis FouAnnadlytpeh) mw0o U01L0 1177500 awo0n W3oML B#I0D wdaoto mMmI L12a0i0 aMmool dAuOoL a1m3e0 mweLe MoOLoo Lo STANDARD DEAVVIEARTAIGOEN:: 132165000 'NQ =NotQuantifiable(lessthantheconcentrationoftheloweststandard (0.1ng/mL) } LOQ= 10 ppb Cente AnalyticalLaboratories, Inc. Page dof 102 000283 _--------ee------------------ Centre Study No.; 023-063. Table XL. SummaryofPFOS for Week 1 Quail YolkSamplesat 17.6 ppm ai `SIpo"nsor D Centre. Bolsa 0102077 EBollmssa oolsasn EEoLlssmasse oolmse E Emn monss oolms BEoonLasssa0ssins oolooamss Elms oon MSeemtb.er ToB0IAD GGuooaAdD GGuaooAADD GGuaosAoDl GGuomso0AADD omsoAD ExtDraucetion AnDaluyesis FouAnnadlyGtpe ) BOL 36IOL 42500 wmweorr wamonn a00 wmeoll aanooll u3e0 swwoo r lmno 33si00 wnesOlL uOmLl 4000 moi sum ais STANDARDDEAVVIEARTAIGOEN:: 346173000 TaXLLb.Sulmmaeryof PFOS for We6eQuakil Membrane Control Samples `Sponsor Toros E0B1-o0L25m9-s20m73s5* BEoLLosSoa0T6e BELimmHamn0 EmoiLomsso2a0nn0sr ELT +Duplicate econ ICen)tre 00 001012990073 0o10l29i07 o002i86) 0o10i28s43 otomis NSumebter soos 0o33m0o0o1m8 oonoooms 0O0B8 ooowmn osm ExtDraucetion sooo AnDaalytseis aur 35o0o0n1 4anaon1 aeoonn aaamn 3a0o0l 4a2p0m1 3w0o0m aaaann wom AVwERmAGE: STANDARDDEVIATION: FoAunnadlypthe ) No oNsQs aassee ulsaen Aesee eNsQo NG NQ = NotQuantif(ieisstbhaentheconcentration oftheloweststandard(0.1 ng/mL) LOQ=10ppb ** Possible contaminationbyyolkoroutershellcompoonfseamnpltesinceoutershell `Rweapsrensoetnwtaatsihveedrpeqruiesottrotsheepearvaatliuoenosfweirnetenmoatlucsoemdptoonceanltcsu.latAesthpeeravSeproangseoarnd standard deviation. CenteAnalyticalLaboratories, nc. Page201102 000284 000285 I-- Centre Stady No 023.063 Table XLIV. Summaryof PFOS for Week 6 Quail Albumen Control Samples Sponnsor CatDes BBoLroosSsAzonrSs lOosmoos BEooLsrssomts 0011002990088 mBioisosasmr oowwsisz EBiousssamsor oollzessss oELoplspasmsee_oi0o0sin6s NaSmebee EmDuien ADmuiisk FouAnmdipeb) wmoaa 30000 mwmnl No xo mmuooan cceeno aanoonn xxoo oowxoeAn aceoo aanoonn x no ooxxeon cooooor aannoonn xxoo ooxxeon ewona aon Nxoo STANDARDDEAVIVAETRIAOGNE: ~~ NNQQ Table XLV. SummaryofPFOS for Week 6 Quail Albumen Samples at 62 ppmal SponDsor CatDre BToLssTa 0o0l BBlolossssaomem 0o0l2e9s BBiLmSsaTmUs o01s02o90 ELoLseSrTs oOlo0Sm BEoLooswsTeis 0o10s24e8 *Duplcat necion NoSmaber BmDcuskn ADmaitek FouAnmdiiep) Goooam aanonni waimr S5334 mmoolna e0n aannnn 6as1t9 oGxxeonA oaono samnnn osnn cGmHoAn a30m0 mainn Ssi2s6 GN A aT 0 am 3a536 STANDARDDEAVIVAETRIAOGNE: 518122 NQ = Not Quantifible (less tha the concentrationofthe lowest standard (0.1 ng/mL) LOQ= 10 ppb Centre AnalyticalLaboratories, Inc. Pa 44g of1e 02. 000286 Centre Study Nos 023-063 TableXLVI SummoafPrFOyS forWeek 17.6 ppmai Sponsor Centre su m IY Number BEoLO02s5L207T47 00110022995522 0ox00iA oELOsLs2aS0o2n0aMgSe 00110022995566 ooxxoollaa EOELDLOSO02704M9s 00110022996600 oomnao EEOOLLO22SS9S220077SS00 00110022996644 oopowoliA EEDOLLOs299220m7SSL1 00110022996688 oonnao 6 Quail AlbumenSamples at Extracto Amipds Date Daic swaooonr uawoonr woowo aaiioo owoowl waoirm wwooowl awomn wwoern waoun STANDARDDEVAIVAETRIAOGNE:: Amite Found (ppb) 9o8s1 11321 11426 116637 i1s5s6 21343 `TableXLVIL Summaryof PFOSfor Week 6 Quail YolkControl Samples Sponsor m Centre set Number Ecracion Date Amaipds Amiyie Date Found (ppt) EEOOLLO22ss2520077535e 00110022990011 oonoon wwomml aalwan NNeQ EELOLOS2SS0207766 00110022990055 oowusosB wwomm laaawnl NNQo EBOLOO2SLS07TSIe 00110022990099 oosooo o9mm IImaanwmmLn isisee EOL2020 0102861 EOLO2SS0I0 0l0284L ooo caso wml aml a Iaam NNQo EELO2Ls22o00mT88 00110022991133 ccouuis wnmolm a iamm NNpD * Duplicate nection STANDARDDEVAIVAETRIAOGNE:: NQ NO INDN=Q=NNootpQeaukadenteictefd(ilessstbhalntheconcentrationofthe loweststandard(0.1 ng/mL) L0Q= 10 ppb `+w+aPsohsesdibprlieocrotnotasmeipanraattiioonn bofyionutteemraslheclolmcpoonemntsp.oAonsfspeaemrnpSlpteonssionrceRoeuptreersesnhtealltiwvaes not request these. values were not used to calculate the average and standard deviation. `CentreAnalytical Laboratories, Ic. Pagedsof 102 000287 ---- ee ---- -- -------------- ---------- Centre Study No: 023.063 Table XLVIIL Summary of PFOS for Week 6 Quail Yolk Samples at 62 ppm ai Spoor Cenmtre B EOLoL s920S702 oOlIsE EEOlLOmNOa0MrS oolloessn BEoLomsloaamasse 0ol0o2993s7 EEoOLLmOsNsOa2m0eAsSe o0lioassel EEolLOm2sSOa2o0uM6se __oowln02soeess NomSbeer ExDruceton ADuubee FoAunsdipeh) oomsOoD waoomr aunnaomne s0o,r oomoonp wweee wwomm i 30g oooop wwomm wwoamn 22s0 ooowp wwomm wmoamm sooo oGoopD wuowm wwoomm oosewo.r STANDARD DEAVVIEARTAIGOEN:: 373611000 Table IL. Summary of PFOS for Week 6 Quail Yolk Samples at 17.6 ppm ai SponDsor BBOLomSaO2oAT BEOoLOmSS2a0UrS EOLONO20US EBOLoOSlO20a74s9% BEOOLLDOSSOO22S00ST EoLos9amste *Duplicate jection Care 001020945 0o1l02s95)3 olomssT o01w0a2s9s5t7 01l002295661S _ onoasss NugSbter oooupi oowooD owoD wosno oooop ops ExiDruceion ADmuiee wwmmll wwnnanan wwomm wwaann wm wom meomm aanamm wwomm wwoaon wom AsVEiRaAnGE: STANDARD DEVIATION: FoAunmdipteh) sswceo, eosos' so, 4e6e50,0 sso e 5s65o00 6510 NQ = Not Quantifiable (less than the concentrationofthe lowest standard (0.1 ng/mL)) CentreAnalyticalLaboratories nc. Pagesot 102 0600288 -------- ee ---- -------------- -- Centre Study No.: 023-063 TableL. SummaryofMoisture DeterminationsforMallard Membrane Samples Sponsor Eo0L100226633.2200885523 EEooLaas63220088842 EEooLLa622s3028082053 EF0Lo0r26m3s:22008m462 EEooLL00226633.2200884478 EEooLL2a62s332.028085506 EEo0L1a6s32200885571 EE001102G6a3s:s20089598 EEO011..00226633..2200009945 EOB1oLL00226633..2200907957 EE00LL0022863:32210090719 EE0011..00226633::2200997818 EB0o1.r0a26s3:2200909819 EEoLoar2a6s3s.2210009002 EEoorraa2zss3s2211000034 Cennte [ourosrans o0w103e208 oowsoisns ooaris ooiossisss oaiooss2i1s6z oai0omsz9z60 oouoomsss olo03o7m68 oouos 0o1l003779068 oolo0s7earss oollooresse 0o1i0o3sr8s0z0 oouwosassooes MAvoelrsnugres s#s000 70500 0100 71500 a@s0o 7s5000 51500 715500 14 0s0o 07500 0750 00 71500 1500 sso CenteAnalyticalLaboratories, Inc. Page70f102 --_me --mmm Centre Study No.: 023-063 Table LL. Summary of Moisture Determinations for Mallard Albumen Samples Spoor maEoLssse208r53 Eo0r1c2a8s3220085842 BBoL0c2ass3s2200884235 EEOo10n28s3.220008426 EE0o1L0a226633..2200886478 E0ELo0v2a623s:32200885560. EBooLaraa6s3200885571 EOEO0L100226633..2200895983 EE001L02266332.02909959 EEooLL2286332200099775 BEoorL2sss32210000719 EB0o1l 285332200097818 E0ELo02c6a3s:s2200908019 EE00LL00226633.2210000920 EBool s83211000080 Centre I") mm olosns ooluosine 0ou00ma16ms parseit oowsss oowusi ouolsazsias1n ooul0osszezss ooisem oowuossess oousso oolwseesn oprleed ou01s0s3705r3 poeaeses Aversgs % Mobture %0800 -- 8050 2#00 11600 00 885500 5u0o 88500 155500 2s0o usoo 8o0o 8040 B86o0 m2o0 CentreAnalyticalLaboratories nc Page48of102 0600290 EE Centre Study No: 023.063 `Table LIL. SSaummpmlaersyofMoisture Determinations for Mallard Yolk Sponsor TT E0E1r263o.208s53 E0EL0100623823020084524 EE0oL0L2m6e3:y2200804235 Eo01r6s322008m425 EB0010128633.2200884487 EE00L10.2026633..2200885560 EOE1o.0v226633.2200888571 BEooLL226633220089538 EBooLv2e63y2200099954 EE0011 0228633.220000797 E0BoLLaa226s332201000719 EBoOtL.00226s3.32200097818 EEoorL02a66332200909819 EBOLo02n63s.2201909002 E0BLo26v3e2211000030 CenDtre ow003s202 o010s32s06 ooucna0em ooanrss ooassiss ofornen oowsss oowmne oowesso olossesn ootaasse7s0s oowwnsers oowtaonsss 0o1u0o3s75s0s ooltosss0s MAovtersatguers wsoo -- awsoo 00 a00 wao0 s000 w0o 050 w0o 060 5s0o wsoo sss000 2S100 uuos Centre Analytical Laboratories, oc. Page avr 102 000291 _--_-- Centre Study No.: 023-063 `Table LIL Summary Samples of Moisture Determinations for Quail Membrane --_--Spomnnsor oCamnre e%AMMvoeolrsstgwueree EB001100225599:-2200%50070 o[wesn 5ss0o E0ELo0r2e5s9p2200753286 oloains swoo EBoOLa022s53s2.0270425 porlea 50 --EnoEEosoLaazosspos2a007e4s80 ooowuommnsesss e3ms0 `tThheerepewracsenntotmoeinsotuugrhe wsaamspdleeteavramiilnaebdleffoorrcitghhetootuhterosfatmhpel3es0.samples received because CentreAnalyticalLaboratories nc. Page500f102 000292 _--_-- Cente Stady No: 023.06 Table LIV. Summaryof Samples Moisture Determinations for Quail Albumen --_-- Sponnsor oCenmtnre sMMAovelesratwgueree Eo0L10022559-.2200550067 Goilooiissessz 00 EEoorr2sspn0250201 oooamses 0880 EE0oL10025295-52200552069 0o10z20s00 1#20 . EoE0L10225535.2200551247 ooul0natzn s8s50o EEooLLaa2zssoo0015258 ooamres 0oo EEoorrasaass2a005s2n19 oouuozzoosss0 100 BBoorLcasssp 00s5t2 oou0oanmas 1100 BE0oL0L2s5o5.22o05m3s3 ooll00az0sn0ss 581500 EEooLLaaassoo2200m767 olosiozn 1n5o0 EEooLraasaos2ao0mms0 auozzssis 58200 oBorrass 0740 oowess s 21600 BBoo11cc22ss55..2200774445 oooszees 1no0 EBoOv01o0a2s5s5..2200774475 oouoazmessz 1060 EE00L100225555:.2200774489 ooiiazesss 88500 --E01B 258.205u 0 mooles ws s omws #o0 i CentreAnalyticalLaboratories, nc. Page S1of 102 600293 _ m -- mm Centre Study No.: 123.063 Table LV. SummaryofMoisture Determinations for Quail Yolk Samples `Sponsor Centre Average -- ED1-02D5920506 _ 010DB1D985--M5l eM8olw0stusrs EO1.0259.20507 E01-0259-20520 ol0198 0102061 a0 40 E01.0259-20521 E01-0259-20509 ot0204s 0101997 450 450 E01.0259.2026 EDL0259.20514 o102065 oi02017 0 0 E010259.20527 E01.0259.20515 0102068 0102021 0 540 E01-0259.20528 E01-0259-20529 0102073 ot0zo7 a0 a0 E01-0259-20531 `E01-0259-20532 oi0208s o102089 40 0 E01-0255-20518 E01025920533 0102033 0102003 45000 BO1.0259:20735 E01-0259.20736 0102901 otoases a0 460 E01-0259-20737 E0L0255.20720 0102909 o102841 a0 410 E01-0259-20738 E01-0259-20742 oiz913 0102929 50 "0 EO1-0259.20743 EO1-0259.20744 0102933 0102937 40 450 EO1.0259-20745 E01-0259-20746 0102941 0102945 50 460 E01.0259.20747 EO1-0259-20748 ot0294s 0102953 a0 460 E01-0259-20749 E010259.20750 0102957 0102961 40 40 E01.0259-20751 ot0296s a0 `Centre Analytical Laboratories, Inc. Page S20f 102 000294 eeemr-------------------------- ca FIGURES ---- -- 000295 -_--_-- CooteStudyNo:023.063 figure 1. `Ivolcal CalibrationCurve for FKUS a - =.- a a\ `ve= aa \ \ 2 a \ a \ Io to a \ IN a \ 2 \ ` I = \ ta a \ u \ i lo a \ a # \ NY a \ reg \ 13s = \ wa! \ [a 5 \ Vo 5 \ = g \ = = \ = 5 = \ wo "- te a = \ In \' a ve ) a --_-- ly MIT asaatasectacaggago i - } 000296 -_ ams om Figur2e. Chro Repm resea ntint g a0o .1ngg /mLsr tana dardm for PFOS RESO. | Fea Centre AnalyticalLaboratories, Inc. Pa 55gof1e02 " 000297 - nnn Centre Study No.: 023-063 Figure3. Chromatogram Representinag 1.0ng/mL standard for PFOS aa | BEEF | EN ! rita nstct in 000298 -_ CoS es2308 Figure 4. Chromatogram Representing a Reagent Blank for PFOS (Centre ID Reagent Blank A, Set:0326014) EERE | | | | on Astron. Pri, 000299 --_-- ca sartacamon Figure 5. Chromatogram Representing ControlMallard Membrane forPFOS(CentreID: 0003802 BlanAk, Set:032601C) B= arid | Centre AnalyticalLaboratories,Inc. Page58of 102 000300 - como Figure6. ChromatogramRepresentingControlMallardMembrane Forwit th1i0pf pbi ofe PFOd S, (CentreID:0003802 Spk ADup. Inj., Set:032601C) EE, | SEEEREHy| || PT ro | CentreAnalytical Laboratories, Inc. Page 59 of 102 000301 --- Figure 7. ! Centre Study No.: 023-063 Chromatogram Representing Mallard MembraneSample from Week 1at6.2ppmai(E01-0263-20825) (Centre ID: 0103092, Set:032601C) SEEEHE ,[I | | ConteAnyi Librosbo Pcs 000302 ee Centre Study No.: 023-063 Study Protocol 00P-023-063 (Centre Study No. 023-063) and Amendments and Deviations entreAnyaLabortores, sc. : Pageotot 102 000303 000304 000305 000306 000307 - CenteStNouv: d023.y063 GePrmpt zs63 Faanyrsonoffwriliebodmsaaoisem0tpovpirdec oafccsiicnnovfelprnogdaurco.n tLahentigeohneesrchngcoee,vsuebshtnceketweiilFlnboe.fsopfpdSiepdTioe0ftshr,eideesitngnnediaomnpclnesoyvia5gd8 = hengielecileyriytbe.edelinveseeedfodevnidnsftharscdievdisnlFosr wcilhl TheEpeectgtisereiislh ieoxbecid.srForcachamaeic,hc1ncslesspllbi Cioee weildbnemdoviend i105Cpfloarsw12h14 btho.Plicion rmpfor 11. 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Page6700102 000308 -_ eran `CentreStudyNo:023.063 ConePt No.0R2e 3.053 45&.ADosensmacmieipodeocfnasseybacmls,eobedn isefsscoheimoeothsod ASeDmepleehxcoi motdsmdasoimspdespcoiofiicons: 11051.Ahcyroomtnpgellrogdilcsirnpsageconssarioyodfnoopferresersceoldn,ysgcvocamissoepnoosnfdnehdeciendys Alhromvsillcocaghze omlivsia: +b.SeAeedmdprdlo,enMlenytd,iffifocoucniioSnm,cdaaistso,nwcssi.oowfpxeoontebdeeoitinfedniorcnaigt.biocnaotfietoveenal oaoff wAoamrcieeelans(u4m.edofchoLmaoFgns.wil)l aiionly ocude he ExpS ihna,n speo s,ilncomnenm mioeb onfor p tce e , mtpfet ,occor.r oThxechChdoeiyrn per I. QUALITYASSURANCE CGoormdamereQtssAaiUeomsne(taw.ciCilluniiogwOrAtvhUesiirnwoi0tlods,fassaoctetthhpees)dfdyo caconnederrnssUnadtetghleilssGyLP Prairnecomepasspsnt,oGCLePse's,MatnodagielmlerpidhtheeSSauidagDsiroecfiorh,eauc to he 14. DATAANDREPORT 1 AalbaowTeehdyintdeaonbdoei,csagltyhs)igspnaeodnpodrlrascmelwnioldepsrme,paisptriniona,doslfndltehevcohdni,yn onf ytooybesrossp,o pldewseepkesahcees,,cRahwraoctmvootw,dcafialionscaeves8, The tyeTherionfoexlsionwil bedosent. 2 Ap egoeSwpiolulsseReeddpbyts eeinb,sdprfoivceeide1dnntdfioxebidsbyothneS0yEPDAi.cTthe 2TOAeirttvs innddproceelemdethodsavhied goes. ConveAnaly Lbs, Pera Centre AnalyticalLaboratoriIessc,. Page6Bol 102 0600309 FE : -- . ConsStyNo 73.053 Comrienc Retecutseit yd =P r igE riayo-- riR ent ---- ie = ieo obein cnt fCri omneiosekt ce pforfkdoeprtittpse tcihwiimSotnhy Dse=e ivech ipvmdis Sd dd eecy dC pi: ot nTa o sOAD toT rswerof18 Anycomcons or tions totefil, port hlbefnte formofan FE -- ere oEe ee mvoaa tet.os Copy: CentreArchives. FR a SD e ty i tu e emitRp ohrinme 5iid ore0dsr toyopei:s DA m i opea sar Po `characterizationdatasodanyshippingrecordsshallberecsined. oy newh i ly bites em Pe---- | UE S. imme PoinAAP pes STrteSraCe nne Acn tTCH. 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PROToOCmOLeDEVrIATION Duta: TOL,yum Coes Nore:3063 Coertenter: mazes 1 Aric Mand 4441 TEN amieee 113 i es ci 2bfe4cAonoccenirnaieon,swere greterthen tha ooffth8ei%ghest1st8adCinnSe 0326t0e1OR3 AOtde 12Prt ionmt e Cm e remo Due ALfe of iby 1 Nop pu bc SETTER rswe <5rshoh, 2 ompiyeieencteer.gr cpteis odmle pct So 5 Yolo ip olule ee StodyDirector Signatare Due' ae = ReCteseOarnst, cu usnerL AB tll N ry Centre AnalyticalLaboratories, loc. Pago 10201102 000343