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Report 01-1256 PFOS: A Reproduction Study with the Mallard Study Title PFOS: A RANEAPLRYOTDIUCCATLIPOHNASSTEURDEYPWOIRTTH FTOHRE MALLARD. FIDFaRAtSaubdRiveisqioun iE,rSeecmtieonn7t1-4 (OECD Guideline 206 Author LisaA. Stevenson Analytical Phase Initiation Date February 19, 2002 Analytical Phase Completion Date At Signing PerfoIMrEmnivonmgentLaaLabboroatroray tory 9B35utuinngv2e3r5.v0e0 Stan S5108 Project Identification 3M EnviWriolndimfeentIanlteLmaabtoiroantaolrLyicS:t4ud5y4-#10E901-1256 Total Number of Pages 28 3M Environmental Laboratory Page 1 anh Report EOI-1256 eponsor 158 PROS: A Reproduction Study withthe Mallard 705: AReprkcion Shy in poets GLP COMPLIANCE STATEMENT Stuy Tie: Anant Prase Report for FOS: A Reproduction Sidy wih ihe Malar Study dontfcaon Number. E01-1256 TGhoiosdanLalaybtiocarleprhaPsreacwicss (cGoLndPu)cStteadnidnacrdosmwpiahncheewxichepTioocnsSuibtsetdanbceelsowControl Act (TSCA) Exceptions GLP compliance: AuCtoonmsiadtereedd d5atnaecoolncgtnolnrsaywstdeamtsa are not vaiate. Tre hardcopy printouts ara ++ TNhoteaslaabtaigoefntenreatseadmpwleees hraesconrodtedbedeirnecdteltyeormpinreodmpt,o ited nd.dad on date Great gFols/aA SAtevensSone,vPerinncsipal Anayica vestiaor oD1a/tzalos dAe Sesh GlLong --------G22/23 IM Enironmental Laboratory Page? CALSHG `QUALITY ASSURANCE STATEMENT I [o --|m or enn ] _ he 18203 -- re Cn? Report 01-1256 Repon E0r1256 PFOS: AReproduction Study withtheMallard PFOS: AReproSttyuwicn hieaorns TABLE OF CONTENTS GLPCOMPHANGSSIAOMENL....... -- QualityAssurance Statement m------ 5 LisOF TAGS. wo sm---- 5 EC ------------ ssm-------- SPERECCEIDTaN eSIOTn8GO asm Method Summary. ------------------ sony PHODERONY MONOD... A--- `SampleReceipt, PreparanadAtnailyossn...... nmol Analytical Method... - sm-------- AnalyticalResults. B------------------ wt DB SUR sumone smmm----------h Statement of Conclusion smm-- 2 Statistical Method.s - smd StatementofData Quality. ----rl RESUS sms -------- sms Lis OfARGEIIGNS......c.coor anol Signature Page . sss `AtAacnhmoaefnFAlit:uoEyrxotcrsahcetimiiocnsaalnCd AonalmyticpalfoMreotumhBoindo,lodgETiScs-a6l:23M1a.t1r,ic"eSs"olid PhaseeEvxtnramctmionn sanodnsnh Atachmen8t: Data Summary Tables.................... ston AttachmenCt: Sample Chromatograms, Cafraion Information, and Instrument Information.....55 AttachmenDt: Sample Preparation Sheets... 144 Attachment E: Study Protocal, Protocol Amendments, and Deviations . " 178 AttachmenFt: Example Calculations - ssa 3M EnvironmentalLaa boratrory-- pace aiz16 Paged GALLERY Report EOI-1256 Reponon1256 PFOS: A Reproduction Study with the Mallard PFS: AReproSdtyuwcthtreiaotonrs LisT OF TABLES Table 1.Summery Table, CyF/SO; Concentration in Sera and Liver... rn Table 2.Summary Table, CyF,SO5" Concentration in Sera and Liver wih Outlers Removed .....8 Tobie3. Ref00CE SUBSIZNGOS.......c.r I Table4. SPE Extraction Summary .......... -- SY Table 5. Sample AaySs........ so 1D Table 6. Serum QC Summary Table. BE I Table 7. Sorum Marx Splke Summary Tabl....... min 1S Table 8. Liver QC Summery Tab . -- BE 1 Table 9 Liver Matix Sike Summary Tabe......... BE 13 Table 10. GyF/S0;" Data Summary, Female Mallrd Sera (Adult and OFSPHNG)........rve 14 Table 11. GyF,sSO5 Dota Summary, Male Malrd Sera (Adult and OHSpG).......... 16 Table 12. Gy SOs Data Summary, Female Malrd Liver(AQutand OSpring................. 18 Table 13. CyFSO5 Data Summary, Male Marc Liver (AQUl an OFSprNg cv 20 Table 14. Summary Table, oF1SO5'Concentration 1 Sera and LET.............. 2 Table 15. Summary Table, CsF1SOy Concentration inSera andLiverwith Outliers Removed.....23 3M EnvironmeanmtaElnoLanbmoernastoarvyostoy Pognsazis Pages COLLARD Report EOI-1256 Reponon1288 PFOS: A Reproduction Study with the Mallard PFS: A Repaducton Sywi ho Mots STUDY INFORMATION Study Director WSeiafneP. iGtaelmlaagthoenrsl Lia E8a5s9t8onC,oMmamreyrlcanedDr2i1v6e01 Sponsor 3aMM EEnnvviiroonnmmeennttaall LTaebcohrnaotloorgyy and Safety Services SBtu.ilPdaiunlg, 2M-N35.5059106 SusanA. Beach, Sponsor Representative Ansyticl Choisy Laboratory ' 3IMM EEnnvviirroonnmmeennttaall LTaebcohrnaotloorgyy(a3nMdLSoabf)ety Services (ETSSS) 9Bu3i5ldBiunsgh2.A9v6e.n0u9e LSits.aPaSutle,veMnNson5,5P1r0i6ncipalAnalytical Investigator . Stay Personnel SJoeaannn.B.GBaelalavgehresr,, WWiildeeIInntieommaattiioonnaallLLTTDD,,LaSbteurdaylDoirryeMctaonragement WSiulsiaanmAK. BRoeaacghe,nS,pIonMsEonrviRreoprnemseennttaaltLiavbeoratory Management LHiasraolAd S.ivJeohnnssoonn,,PrIi,ncOirpiaglinAanlaPlryitnicciapaIlAnnvaolsyitgiactaolr Investigator KOegnrtioRn.kLainKdrsuptlraormi,n,SeAnniaolrytRiecsaelaCrhcehmiCshtemist Marlene Heying. Anayical Chomist Experimental Ones SSaemmppllee AAnnaalyyssiiss CIonimipalieotni:on1:9 1F1ebArpurairy20200202 Archivos ALlaboorrgailnoarlyraacwcoarldai,ngp0rot4oc0olC.FaRndPaarnal7y5t2i.calThreepoarntalhytaivcealbreeefneraernccheivsetdanadtatrhder3eMserEvnevisraomnmpeenst,alas wEenlvliarosntmheentsaalmpLlaebosrpaetrotrayinaicncgoroditnhge taona4l0ytGicFalRpPhoarste79o2f.tis stucy, are arched af 1 14 3M EnvironmeEntralmLaabonratorryas Pacesazie Page6 C1590 Report E01-1256 Repmcorzse PFOS: A Reproduction Study with the Mallard PROS. Aeprocucion Sty wttaMotors -- e-- S ------ smee -- SUMMARY tcCTaoahbnFelt1eos7cloSsnOgcu;remKonm'tua)rprawtiaaiznosedn dtaoehfte1et0rChm9e,ipFCnm,e,SdFdOo,i;nsSeOtdch,eonglacrineovineurotpnraafntordifoomsnpeseWrrafifolodufuionfradeodouifclnetteatdnmhieaenlglsIauvslretfdrousndaaayntned7d,4s5tpe4hoer-tia1ra0oso9sf.fissuptmrTuihdsnyeagltsfinao(mlbPopoFwltOiheSns,ga pcEuxartltrbyarcaatineoddnmhacluerrivpxeotfaoPsrFsCiOyuSFm,,c`SosOntsra.nbduatrCidoosnnceatnrototrhaeutsimoeandssso1of0fChoyseFtyaPbSRiOsOshSartrheeef.erreHepnPocrLetaCsd.ufbEslStraMncScoMenSectinoenmfmorennot cTearbtlaein1rseusmumsarhiazeshaavlesbteuedyn staamtpilsecdaala.deTtaebmlien2edsu1mmbaoroizuers sstuwdiyidzantgatahfetDr smeonvGiTnogst. Table 1. Summary Table, CsF17SOy" Concentration in Sera and Liver jCooat ENosSaaC enros||EGArveursaoc,e | Roweolmmais | formaeely| GPruesso, | Rannge;eeof waar com earn || |v| femme) [em|| |=] `FameControl =| I <aoongm. soz) emma] |em| = | vem |x| mom| omauson | own | semiesmonon "oe | moon| essere | | oso | nso ] | | cwmman !I ControlGroup | * erosm Ore | : { w=o | y 10w3ngeimt i.e(10n/3) | by --shondod 1 M " seomer w - " ars LH --, me-- | 3M Environmental Laboratory Page? nanan Report EO1-1256 Report 01.1256 PFOS: A Reproduction Study with the Mallard POS: A Repraducton Study wi th Matra Table 2. Summary Table, CsF17SOs Concentration in Sera and Liver with Outliers Removed E E Noop n |sAvL insce E Lan" |r craso, r | ane Cro Pr MoleContGrowp| 16 [ Foremeica|Ty0 |v . w| =] loreoriCat| [0[0 +rrn]] moemem |=| |] Woeorrs |. n B om | Geman | | | Weotwe | |. FmasooOnpery|| 7 : anRdGActaucrmoTnetosr Fo VEGHGSo e TORT TrTe Far T " 1. '7 | Bi Aae lo SE Te TTS PURPOSE `bTahteh pcuonrtproosleaonfdtdhoesaendalmytailcaalrdpshaasnedionftthhiesisotfufdspyriisngto quantiy CaFSOs in th liver and sera of REFERENCE SUBSTANCES Table 3, Reference Substances REFERENCE SUBSTANCE PFOS PFOA |ExproatwoneDale |__|___osc3ev2m00s8 | OstwoTod2P1ro2cc0s, ie StorageConditions | Fro20Cz+e-10nC _| Fro20z+e10nC_| 3M Laboratory Who CosinePowder| Whi Said so wo fPorFrOoiAsonnuadmecaalaorrodeec4a0ndcni io,5 3Parer afndur oo3f0Q6u,daonfteol ca0dacendsclyfiomacnor 3M Environmental Laboratory Page8 caLnan Report E01-1256 Rupr ot PFOS: A Reproduction Study with the Mallard 2708: AReproduction Sty wit osars. A `SPECIMEN RECEIPT AND STORAGE , 2Mca0olndlcalsruedsnitosnetroouf3mtMahenEdnnvvireoernmpsehanamispaellefsLawtbehoerraesttoourbdytyafi(onr4e4da5n4fa-lry1os0mi9s)t.hocoTsnahdceurcifstipecdeecooiftmetWhniosditwfeesetreiannrtieomcmaealitsvieodun.psos,nt LOtihWse ofEnvEiOr1o-n1m3e6n7t)a,laLnadbowrearteorsy.oraesdsiagtn2e0dCl+a1b.or1a0toCryurnaickpirnegpa(rLeIdSfo)rnaunamlbyesre(E01-1256, Eo1-1326, METHOD SUMMARY T3FihMueoErdnoevctihererommniimcneaanlitCoanolmoLpfaobCuo4nrf.ad,tsSoOrfyyl"ommceBotinhocloeodngtircEaaTtlSiM.oan0t-ri2ni3ct1ehs1e",Iv"eSrcaindPshearcaewEaxstapceirfoonrmanddaAccnoarndisnig o0f wT1ha2et0esre(aro0a.asa1m/T1ph0leerslaeworeprsreiaomprprtleoepashrowemdoegrbeenyipzmrieenapgsa.urreidnFigbvyea mmveio.alsouufmreaicnoogfosaniewrueimiegawhnadofiaIudvdieerndgn1dw1itd0iwamnlogrofwihniena ipwaetsreseedhdse{onoacueognrth1ri.af0umcg.eodnoffdotoen1e0hdommisoongleednss;plhaaisoeef isevuxeprreaamcanttdoanwnat(sSwPsaEhs)akdoeslncaafnnotr.a2d0 imAnfiteocr4s0y,iinLTghoefiseewasclaoempmal,neds 2an0almyzedofomreCthFanSolO,waUssipnagssHePdLCt.hEroSuMghSMthSe,column fo sus he analyte. The samples were PREPARATORY METHOD + fbEirTooSlom8g.iB2cia3lo1l.moa1griic"caSeloslm,iadsturPicchheaass.se"seErTxahtiarsancdmteietorhn,odaunsddiensgcArnsiaobleiysspitshhaesoeefxetFxrltrauatocortnoiconhofe(mStiPaEcr)ag.ll Caonmapeosneontms Sere samples wsRoaemmropogleeGnsiiuzwteeeddr.ewiuAlth 1eK.da0n1md1y0s,oanapop(rcooofxmitmmheaetraGcliiyatl1egb3ooft6laveedor)r waNanotdmeorogre1n2ao0fl.eKabonfedileyoorhiowXworasetceetrxo,nsa.encdiLdtheborny aSudpdeirnngat5a.n0tm.vaosf arcaentsnfierriree,d s{h0a-akincglefaon t2u0bem,iltuetse,dawnidhc4a0ntmuigonfgKfarnd1y0onmiitweaste.r, Tahneg faSinplatelecryeizdoetmdhernobyuyg(hHahPicLgoh-ndEitSpieMornSfeoNdrSmCa)1n8ce(SPuEi)dc.oluemno.malAonoatlyatpehsy-wselreecetloustpedraoyff thteancdoelummn,meatnsd Tabsilce 4. SPE Extraction Summary pr-- 7| WDoisseursoorva (o72m0 oafsnrsvorwi0hwpiohrtnfer [E 5Oaacocrotrd)iSohT foaf30mksheasacaonimoS0o od mTogSsGr.eoTAGnN.Soikase aiod s [ [55]| Foooorsasnuspleomraorutgwhinco40ndmoicnhewdaStPeEr GT si. 7Eu rstanysFomPecour ih 20m mlb (0H) 3M Environm0entEamlesLoambeonrsatLoar"byraton Paomsazieoennan1sdH Report E01-1256 PFOS: A Reproduction Study with the Mallard vLenLiE rA LTLT EirvTsTa--a-- SAMPLE RECEIPT, PREPARATION AND ANALYSIS a ST En pr err or reer `Table 5. Sample Analysis {|Ea |af m i rEa = R i pFEa -- =a fi oergEeE iT-- E ------ r T -- || -- wr | 12 | AnaofDlayy 3ses rasi amplses =13 | Preparationofmethodblanksandspkes,andserasamples, r E r rm E =E E mE r =! m||e--Lr_n--hi-- or shreceahnOe | ses -- CALsdE ReporE01 1256 Sonn PROS: A Reproducion Study with the Malad 405Aaccionapne ss Bol hers E Cr op n etne e S300 Oo h | | P samploes) ns eaisp . enwopi reo eva Tpmeerer 5 Tosserss |7 |Aral ofGC eran serasams `Analysisof dilutedserasamples. a caE 6 z_-- ~ Tr TA,202 11 Ap,2002 ANALYTICAL METHOD + SoCT amgLpeEsaoSwee,rrermaaetateadacusTinnHgnHePLsCdavEeSnesSiIemsNrSr,oaGyei5r0va,oecccoenocaaa TnworeAS adteaLroeem nnoedssd iSNonmacacotonat,eubetdwooecos awoade(POaA mwssorodoi boPth aLEmCoCn pponeefoore5:2 + oa oThPepHkPeLreCvounesaoSsfcorahBn,EstSudeysw0hasiG1e5HsoWPwpLlaPSaaecamebridcl1H1c0oE0o.resTh isyiteemaactdo,snsatiesoTsfts oarmc esaepuJgOoCwciocaonaan enpeses. S5 1t. omen oma Io C --T ----=-- TT %= [=oTw= + clTrooooosnesimtansTosRfaG2svo5cka(aomieatro5asu8edeiafdoaohtCwotisvthyeinwSeSaoeslcoaheoMsepieayreapsoecehaUosslnipln,aeeddThreersseatslesem or mem bh crass on 90 FRG. Stans oA eon brent 3M Environmental Laboratory -- Page 11 ALhD; Report EO1-1256 Rapa 01-1255 PFOS: A Reproduction Study with the Mallard PFOS: AReproStusdyuwitchtie ootna fMeotmhamniez, w=as51m3aintotaminzeda=t2a9p9reswsausremoofniatoprperdo.ximTehleyc3ol.i0sxi1on0,gmaas,r95% Argon / 5% _-- ANALYTICAL RESULTS DmExeatltr,aaceqtuxiaoclneiptatynodabsjAencantloiytvseeidss oaoufntdlFiundoeirdsocciunhsetsmheiedc3ablMelCEoonwmvpi(rosouenonmdeAnsttiafalrcohLmmaebBinoortlaotAgo.ircyaElTmMSea-tt8hr-oi2cd3es1a"n1ad, npd"rSoAottlotcdaolcPhhwmaeesrneet E. Study Protocol, Protocol Amendments, and Deviations), + Rseagmrpelsesdiaotan.s.EaQcuhadcraaltbircatciuornvceurflv,ewheaidghatceodef1iXc,enwtasof adpeptleiremdintaotiCoanlobfra>tion0.6s6t5.andards and + u0Csa2il0nig1br0mata1il0oi0nx0-SentxgatrnCadca,trfeddSsO.sstaTInmndsLatrrdmusemterhnaatnngorilen,sgpcoionnrsrceeosnwpcaoesnndiciranlagilb0ornataiendcotdnhaceielnyftiprnraaitriSootnlovoesfnat6m.pe0xl0ter1aacnt4a0lf1yi6so0im.s fnaocgucirumtrLeaecnoyf mosafetrreaiaxocerhxt4rl.ae0vc0etleldowas2st0a0n8edv0aarlndusgatgebdr.Iavcekr.eAtniynTghleeaveclwalibodrueatlsiicodonencce7nu5tr%rvae-t1ia2onn6a%loyfzoefsdnnaciooymntiesn.iasltedwTahosef ndnooomamciiinniaavlla.treedIqnuwiisrloehmmteehnetc,eaxswceaespstihionencolfluotdwehedestwlhocewoennsctecnoctnursraivtreiuocpntoiicnntgu,rtvwheheipecahailninb,ereaatdlielodhnotucogurhmveeoe,uttbs7uit0d%eft-tw1ha3es03%n0oo%lf uceuxsrtevrdecotmeeddeestttieanrngmdiatnrhedesth3ues0im%nigtnLooGmfiMqnuSaalIniMlraSetqiuioinnrs.etmreuTnmhetn,etaItmiDiouneo,ftqthoueacntaihteiactuqisuoatnderdwatacioscnciehrneetsnrpeaoxtn!isoepn.ooiofnfthoimgnahletrrhx:e tdlheeveteelqrumsaitdnarneaddtaircbcyseqwtuhaaetsiohonif.gtheensTtdheectaealrbcmrciaenlpaitonentd,suttpahpnaedrairsdcaonmscaieennttigrnagtreisotunhletrca7on5ug%led-f1no2ort5s%bteuadccyacluscraualmacptyleedcsruiswoiarn.ag wAinlhsetanrnuabmlaeycnitkcaclalcrueisautesd t0htahtearoergirneaplorctoendcenatrreatwioinnspithkee aicnctetphleedexcraalciibreadtimonariansgteandoafrdtsh.o + StmhiyecsHetenevdemloSfuuineteaaxcbthirlaiactntayleySdtaicmcaapllliebrrsuan.t.ioSnPryissottraen(md0atsruhdiesacbawileiitrbyerawtaianosanlycdzueermdvo.ensatnTrdhateaefdpterpartikhorear1laesatthsperaemsctpialrseti,oantndarneadet rpieemtaeekntwiaaorsnesteiqpmureaelcpir0seicooinrsiweoanssswaieqnsuaanmlo2nt.io6to%orReldSoDas,t htmheaeentbie5ng.gi0n%tnihRngSstDaantadenddednatdlhaeofqprtuehaceilrsiuoonvnsjeoepfceirhvaeeteslry1e.6leontTiwhoen + ChoantttihneuiinnsgtrCumaelnitbartaitoinonwaVserpirfoivciadtiinognsu(iCaCbVl)e. resAultmsitdherovueglhoumtateraixchcaonlablryattiicoanl scehqeucekncweas adenvailaytzieodn `Samples boerfvatechrkyetteatrdegnebtyscaoomnnpeclenoetrsrmatooirroenlsef.sasnOfgnolCymCodn'aitstaowrberraicenksretertauenmdeanbltyyazlpeadscsriin,g wCiChV'as wienirte orfepo$r2t6ed% + (WL0ii9hm/ii6tn) toahfnedQ7ui0an-nst1ei3rt0ua%tmin(oonnmgii(nmLaLOl)Q)c3.rsietrThienaelaonlwdoeswwtietahlcciaentptaoanfballqyeuteeenxttpireaaatckitoerndec(aaLlLiabtOrQea)taisowtnac2sutrdivemefeispnoehidnetihbnlaiatvnekirs Tacrceeputpapbelre cluirmivteopfoiqnutaunstieadtoionca(lUiLbOraQ)thwearsespdeofnisneedofatshetihnestcrounmecnetn.lration of the highest + {Bhlaonukgsh. thMeetehnotdreblsaanmkpsle(puprrecphaarsaetdionKanadnidyohainaldyrsiinskinpgrowcaetsesr), background contamination. pserrosv,ideadndlaormIevaesrurteokeonf + emQxautalrliaixcttyesdpCioaknnetdrsoaalnmap(llQyeCzs)edaatanndtdhMecaotlnrosiwixesstStepdicokonefcsee.nteOrantleieovsneeltswoeofrfenainpnareleyQptaeCriensdaUmrwippillhceastee.ancheAdaedcxihttiromanacattlirloiynx,wsweaots Resuls are as follows: 3M Environm1entEanloLaambeonrtataorbyot P1a200700 Page 12 ainds Report E01-1256 oor 250 PFOS: A Reproduction Study with the Mallard P08 ARopetcion Say we ost Table 6. Serum QC Summary Table a aii [IE J Deviation QC-25ppb ac-250m0 1004 ng/mL. 10040 ngimL. 145%" oon 1| 9.8% aw acaopom | 160800 mgmt wn | em Er me. "TheseSampleswerespied Using 1.0 nywoop on akuot ofspiking soon.NI 5pKesDopared on 3sare dey UsingSO of 3 Table 7. Serum Matrix Spike Summary Table FouMaixspkes | 1004ngmL 114% [FrHor| mamos onrng. | 2-- rr EE r ---- Table 8. Liver QC Summary Table iver OC Sample Diluted Liver [re par aaacc c-2zS5spi ee0e| os wrT4em9oa7etnoneggnlgs0ss ti |Lonowohawsn D ssa] "Thesesampleswee spikedusing 21.0ul iquotofspikingsok/son.MatixspkespreparedonfesamedayUSgS0U ofa Table 9. Liver Matrix Spike Summary Table Er PLC JPW, [ronnie 457 rol iw Four Hain Sphes - Tem "Sone RR oRTR Duplicates A 497 oR nglg A Aor + TDSohekeieispmrattgeoescotofssranetelskspteh1rtmbitetheeouatceicrvespplrnoTctooeecorolavbnegtaerefsdo7n5re-v1l2e6rT%eobftuslormnaskGeososralloywaSnceerspifortta SGorehtonovocenteohne1s atL2hOovGlAslGnSceasyshangSaaLlOlyG.e.sDalyat0wesraempnlelsDoayom0ersphoewsSoafyasneisvenoSgarneoaomny saps 3M Environmental Laboratory A Page 13 nino Report E01-1256 Roper or259 PFOS: A Reproduction Study with the Mallard PFOS: A Reproduction StihhueVayllrd Abcsoomlpaurtieng Rtehecorveersiuess.of thTeheexrsabcstoeldulqeuarletcyocveornytolofspthhkeesQqCuanstaimaplleedsveirssudsetaenrmeixntreadctbedy tmhaarnxwhceurnveusainngd oa msaollvreinxt-ecxurravce.tedTchuerves.eraTshpeikleoswqsupainkteisataerePi1gh1e.r1%ushiingghear,sotlhveenmtedcuirovme osfpiktehse 8r.e3%ehilgohveer,s aonfd sthpekehsighussipnigkes@ 6s.o3l%vehnitghecru.rveThVeer9s.u5s% aanvereaxgaecthiegdhermaqturainxticatuioen odbesmeornvseidrafloersIvheartsaitmpilsesa.pproTphreiaetxetroctuesdevmearlrmxalerxitxraccuirveedssatraend1a2rd.s2.5 hiTghheer,sa7m.e8%rheingdheri,s daenmdon5s.t6r%athiingghetrharets'psecatpipverloyprfiortethfeo uloswe,mmaeldrxi-uomxraancdiehdigshtasnpdiakredssof the fer mal, again + PinFtDeAmawlaSstanontdaursde:dfTorhqeuainntiearntailosnt,anbduatrwda(sPuFsDeAd)towemsonaidtodredfortogralolsssaimnpslreusmeanntdfsatraend.ards. In(ussPtiFrnOguSm)tehtenhtactonRwceaessntparodanjtsuiosenteCodaffloirtbhpreautrCiytoFyn,.arnSHdOP,iLhaCen-ipEoonSt/aosfMsSpi/euMrmlSuiocinrnoscotorcntuirmaienbneuttsiruoelnsfpo0onanttsheee,' mwpaoatssasscsaoifliuPbmrFasOtaelSdt euxsperdestsoedpraespaareperscteocnktagsoeluotfiodnist.aryAinnyakfuelumruestcaalcduljautisohntes droesqeuidrianmgoucnontcse6nt5rwateilons 10 be DATA SUMMARY pTraebsleenste1d0 itnhArlouagchhm1e3ntsuCm.maTrhiezetailnedidviidsupallayssaCmapFleSdOatya.conRceepnrteasteintoantsifvoer icnhdrivoimdautalognreacmtisonasr.e cAallidbarattaioanrecucrovrerected for purity of the PFOS reference substance used for the extracted matix Table 10. CoF17SOy Data Summary, Female ] Mallard Sera (Adult and ]Offspring5) Mi ss FO Nee . no ; GrEOe I | | | > or s5ean Eo125620663 _|454-10P6PM.F3o2ne1.6p,d0t |05 | 1 | 0 01-125526665 _[454-10PP6M-,F3e2ma2,0A,ct0. 01-125520667 [454-100.322,0 PPM. Fema, At 05 T <0 05 i [E0or1--112255662260666700 4(5145-4-1100PP09PPMM0-,,FF-3eamm22aall22eo,64Apdu,,unt |[o0s5 |1 1 | =o | eorrzseaser2Ju5-100:3228,0 PPMFam os | | wee| eE0011--1122556.6226866774_[4544-51040:31290,08PP:PPM3,,2FFa3mma2,,,AAud0tu 0055 <20 | coorr--11225586206867700 [Jas116054.3-2041,0P0pMP0w,,-FFae5mma2al,e9Apd,dut0 | "0o5s |1|eiw o || co1-1250.2091 [454-106P.P3,2F0o,al0,Act. 05 v 00 [EEoo1r--t12255662288666835 [sa5544--110056PP3.PPM2M3,4FF2ee00mma,a2ll0ee.,0ppott | |0055| | 1 1 ||<i0 o || [Eoorr--11225506.2208060897 4[5s45140-9130264:03020PP4ow,M,0 FFoemmaalloe,ppoott | | 0055| | 11 | <<0i0 || eorass ssn jessunsassopm ramos | 0s | 1 oe or-125620653 [454-10PP0M,-F2am5a0,Au0n |05| 1 <i0 eorr2s620665 [usa-1003252,0pPM, Fomaiepdt | 05 1 Tse 3M EnvironmaentEanlvtLoambeorrsatLoarboyrato Pron te ct216 Page 14 0n159y Report E01-1256 RaperEot1258 PFOS: A Reproduction Study with the Mallard PF0S:A Reproduction Swu htheMd atar sus ER a] al rt [1 [<0 i| [JFeoonr122s566228677001 les45a4.-1100003:225508,,t1o0PPoouv,, FFeammaal.e pAddut |A 05 |1| o2e0m [JEEoott--11225566.2266770075 45544-110008-33226642., 1100 PPPPM., FFeamamle,, AAddiitt 0s [Twon re)| ceoorn112255562200771010 1J4a5s4t-11110000PP0PY6V.--FFo3a3mmo2a2n,,6AA6dd,,iitt o0ss | 1 |emm 0 || Jeo 125628712 [454.110P0P8M,.Fo3o2l.7Ac0t os 0 arao0n [E[oE0r1i-z1s25e6228877151745[44150042-7,111000PP6PPML:,FF3earn2mala7e,,AA2ddui,ltt 00s5 |1 w|w7m JE01o--112255662206772116 [4541-1050-3+2761.11000PP8oPv,.:FF3eemma2lae,.7AAdc,itt o0ss | 0v | a500 [Joot--112255662200772235 |5[11501115000PP:5PoM..33FFoo22omtal88,AoAd02ditt | o0s2 0i wa 0000n| ot-12s620727 _[usi110p0e0,:Fe3ma2le6ha4n 105 1 ssn | [E01-1256.28729 454-1100P9P-M,F3om2al8e,6Ad, 0s 01-1256.26731 454-1100P0PM-.Fo3ma2to,8Au5t. 0s [cEo0r1-112255562206773353 445544--111100000PP3PY-M-.3FFo3o2man2l9,o,90AAct,,it | 055 | 1 1T6o0i0000 [eor25026737 la5-10031200PP8V,.Fema, Act 05 | [Eor-1256-28730 454-108:3296. 10PEM. Female. An | _05 | _1 [E0T1256.28740 _[454-1P0PM6,F:or9ma5l,8Of5sp,in0g. ors JEt0-11-21255662206776472 454105PM:.9Fo5mo8l.2Oft.spr0ng | 0022 E 45410E 0Po.,F5o3t8o.s0 | 01" 3 "roo [Eov125626767 5+100610.0PPM,Fam, Oring 1 <i [E1o 2562[6457+105000129. 10Pow. Fem, Ogg | 01 I [E01-1256.28752_|1105P4PM-,1Fo0m6al.o9,O6fi3sp3in,g |0 __ 1| __ 1 3420 E[co0Er1-0t1s215s-62218677255559 62_467|55444_5_1441050p-4PP0oPP-uMI1t1,9FFF0oe0omm56naae0le.,e4.O9,fO.Oi6fs8ss4pp9rro5ii1nn6.gsg 3||4,0o051r2 0|| 1 6w76m0 sino] 01125620750 4510010P4o.6Fo5al, Orn | 01 3 ee] [01.1256.26750 454-1100PP9M,-Fe9mal6e,5Off6spr.ing | 0.1 1 ineTrhvels,efo vatlhueesrewjeecrteiornejoefctoeudtebrassed on the resuls of the Dixon's Q-Test, 0% confidence 0Emicoments Laboratory 3M Environmental Laboratory pace t5ot218 GRLGPAagDe 15 Report EO1-1256 ReportEo. 1256 PFOS: A Reproduction Study with the Mallard PFS: A Reproduction Sywin haNotas Table 11. CeFnSO5 Data Summary, Male Mallard Sera (Adult and Offspring) y SAMPLE DESCRIPTION Sein0en | OTL | CES, pi [Eor-1256.20652 _1454-10P0PM:,3Ma2l1o,7A,i0t lE01-1256.28664 [454-100PP0M-,M3le2,A1du9lt Tos Tr 05 T i aw| ----Th -- 05 1 <1 ee [Eot-125520675 [454-100-5229.0PPM,Mate,Ad os| 1 <i co1-125626675 [54-100:3291.0PP,MaloAdu 05 v "10 [0E10-11-1225566.2208668770 ___||445544--1010PP00EP8.WM,,-3MMa32atl23eo,,37AAdd3.uul,0t [o 03 s [v1 <<1000. eor-126620652 (154-1PP0M,M0ae-,A3dw2t 39, |05 1 <0 [o1E-01215-6122056865.28[06445_4|-45140-0PP1P0:PM9,3,-M2Ma3at4l2eo,45,A1A.dd,u0l0t 00s5 |1 |eo| eot-125628080 [u5-105P.ov3,2Mo4ke5.A,c0t TI 01-125028500 [usc105.P3ow2,a7e,,c0or Tos | we| [For-12s6zm0z_asa-tooszss,orm MaeAan | 05 | 1| wom | [Eoorri122s5e52280069004 Ja4s5+et1o0o382.s3to70pP5p3r.MealeAdt |T o05r |e1w | ] io | or125520090 Tusctopsewav2e5.5Ac.t os| 1 1 ow | [Eo267r00145241055.56257 0Pw, Mol,lt 5 mn [Eor-1256-28702 454-105-3250, 10PPM Mal,Act. oz 0 so| JE11256.28704 454.109.3261, 10PPMMale,Ad | 05 | 10 | eero0 | |EEoO1t-1-2516:22567006.__2[84574-01065-_312643,5114001PPP0AM0,,:MMaa3lle2,.6AAdc5u, o0z06 0 ceoo2r5205a.2771102_Taaosa-0512007011300pwp2r 5eo0.nmnp ||9 05 5 | 101 || o0 eroeso || [E[0E1o-r1-2i52s662288771146 [4[5485140180:0130:PP23PPIM72,M73ia1l.oe,AA1dd0ut [Coo sT ro |o wm0. | EJEo0r1--1122566.0226871762_0_ [445544-:110098-3:237257,,1100PPPoM,,MMaalle,,AAduiltt [os05 | [0 [e | oas 0 0| or-125620772 [454100527910 PPM,Mil, Act 0 To00 [oEr01--2152566.2266772255 4[5445-410-01-03118200P8P-oP33wM,,,2ii8ee5,,AAdudlut 0JE1011-21525662-626775320 _45|44-51046--13112000PP99OP9MM:,,.M3Mea2llee,8AA7dcu.lt [E026173-4 1[4542-1050-35291 10PP, Me,At [os| 03 03 | | reo [Eon125628758 ast1095296, topeu Maepst | 05Tio | "sero | 3MEnvironmaeMntEaml LoabnorsatLoabroyratory Pape 1601216 Page 16 ------ Report E01-1256 [I PFOS: A Reproduction Study with the Mallard PROS: A eprcuction Shc wn ar ShTs SWPCOEP SCRN TION | jSeavi 0P0E0P | Gis Eoor111225566220774450 5[41048.5557.10 pO0PPo5M0aol.,8Otf0sis6og |0on 2 | ER) ow] eorzss derso [i005625 10Pr Nk,Cte ST So eeoorvia2a5s6e2v7r5ss [lasss01089863,610EP4PotL.t2oke,.1Ofgio0isr, | 0.1 teTvhao.sefovatlhuesrwecetrioenjeofctuedtras.ed onthe resus of te Drs Tes, 90% confidence IM EnvironmentEalmLaiborratory f-- Page 17 nnn Report E01-1256 Reoncor 1258 PFOS: AReproduction Study with the Mallard 708: ARepriin notts. Table 12. CsF1,SO5 Data Summary, Female Mallard Liver (Adult and Offspring) " ee Eo113252062 0 gpmoi S28 F no, aut Renna | 10005 vig Bh sey wGi00F Lats) T= [[0E1E0-011-11332126632-2920665082139[6l0o01o9ppoppmmma.a...i.333 2222422FF2 LLLiievv0 eerrr,., asaduutltt 1 1.0944 3 <50 t1o0m5s | Tso| [e01o 132n 629s 6lho5op7pmm erss2z6rFLovmeraangust 0115262053 0 ppm 1.5230 ivr: aut || ttLooouisen| | 1| |Twms o0 ||| eeE0oo1rn-1133322266.522929677601021000 ppppoommmaa1a.1..35325224FF30LLoiv20eowr,vaadecuolntt |1110203000 ||1| em] 0e0111.51322062.626776455 00ppmoam1. 2.33FFiL28ri,4eau0nt m0 | T=] ecoo1r115022602266778515 0oppmp 011..39FF22iLn4e4rr2, aasttt SToozer1 T 1 wSo [JEErt052r62-91633l5op2gpmp6am253%2244066 L1i7e FaLivter,atdut | 1L1o2r4e | 1+ | <=0 | Jeo 152075850 gor a.30FLomrsaut|e|1 | 0 | [Eor152629671 opma 3252 F veraun | viorour | 13 | w<o0 | 1.0660 : 50 [Ecoor1-11532260229992556 1100ppommai1.35228506FnLvreraagta | 00s |1| e70m0 [cEo0r11-15322062-200506601 [1100ppommai1..352264F6LLirv2e,r, aatc.t 10 | 10 [E|0E0111-91232063-0209919680110mppmaa.i1. 532288F6LLihve6err,,aasduultt v1.i04z87 | 11 | s5m38o0 | [Eo-225300% hopema 5270 versa | tarsi10 | wen | 0|oE101r1-521232266:5-3330000005276_08_ 1100 ppppmm aai.. 35227742 FFLnivert.aadc.uulnt 10 pom ai. 52F i7vra8dit | e11..01s625280 1 01 [0 3580000 or 32830108 10 pom ai.5278 F Lr act FE [FEo0r1r-1o322053:300114224 1100 ppppmma. 3225802FLniveerrsosut 1o0a6r0s0 | 1 |zee| 01-1326.30160 [E01-1326:30178 110 [10 ppma.i. ppm a. 3284 3286 F F Liveadrul,t Livearcu, 11.00961557 [E011526501109p5pm .. 2288 Liver, acu oeorr-r22s50a2%n2 10 pomm ea. s202e F vee s |_tosse 110 6330 | T 1 o | e an]| Endonnan Lavras 3M Environmental Laboratory Fretsatzis Page 18 GAL Report 01-1256 f---- PFOS: AReproduction Study with the Mallard -- ooh azo 0210 ppm, ee P Len gun R eor-13751T 507 ppm Jor136751515 Topp T 1 050502 rvT eerratevgeyn ITtEiow)s Tr: a e= oorr1137675371531256 olopgepmm eitoo se vvees rrcatmrnyg | L11i5o5r0 Eor1367:31357 0pom 1.F5Li6vero1fsp0rng T0217 [ooEr0v11-e3136r6733a1133436_r{80 o1p01p0mma0ia.gp6725300FoFnLheimerno:tafriperleongs| vTTiooesroze |1:1 | F2r0soy0 | oeto1v-5167753113584 1 10pm0al 6so5ps4sFLvm ve:r of.ieerss TTiaess i eeym eor106751305 eor106731404 o0gpmmaati o6s5oFFiLhheesroottipprgg || i tomo2 | 6 || ss1 sawo || eorervto Jiapomasosorimecotipwg | vos |1 | sw | 3MEnvironmentalLaboratory Page 19 ond i Report -- 01-1256 ---- PFOS: A Reproduction Study with the Mallard Table 13. CF1;SO;" Data Summary, Male Mallard Liver (Adult and Offspring) gen ENTLY (er -- mle = froma pasate Loom LE] [Eor-132620574Toppmai 3210Mier,saat | tear [1] mnfotaimee a [Eor132629646 0ppmai3227Muver,oat | toss|v| eo | 01-132629662 0 ppm 1.32ML5iv1er, acut__|__ 10165 1 <0 Te] Eot-1326.25718 Joppm as 326 MUver sat 1 |tos| 1 <0 wo | E01-1326-29736 0 ppm a.i. 52M3Liv7er, adut 1.167 [I [01-1326-29754 lo ppm a.i. 32M3Liv9er. adult 1.1493 [Eor132620772 0ppma.3241MLiver,act|tobteTv[0 [oris2629J6o4p4om. sasomiver ag | toms | 1| = | E01-132629916_|10 ose 13 jos | | | ppm a. 3267MLver,aou | 108s | v0 [720| Eo1-1326.20052 [soppmai3261Miner, | 130 | to| roo | [eor132620670 10ppmai.az63Muverao | tra0s |v0| wesoe0 | JJEoO1-1n326a-30s007|10 ppr m a. 326T 7 MLver.adun |106|2100| = [[EE010-1131263-23060[[31810100pp0opm4ma5a1i. 532712MMev7err,,aa3dcu |10|113 0 | 63000 10 54200 [E[0E101--113322663.030061715_1[100pppommaai..332727MM7ULiivv0eer,raadduutt | | 1002 | to | sw0 | 10660 20, [E[OET011-51256236500115619 10pom 10 pom a. 3263M Liver acu a..32M6v5er, acon | | 10985 | test | 10 | to | ero seem | | [E01-1326:30187 [10 ppm a.. 32M6Liv7er, adult [E01-132630205 [10 pom a.32MLi6 ver,a0gun__|10251| [E0r132630223 [10pomai.5201MLver gun | 1081| 10 E) GAL Report EO1-1256 Report E01.1256 PFOS: A Reproduction Study with the Mallard PFOS: A RpreStdudyuwichhie otanrd hod ST Se ; Eo0t1-.11996677:3511330311 lJoo ppopmm aai. 09650916 MMUUvveerr,,ootttssppriinngg | | _t1i0o4t1e1 | | 1 1 | | |Ect-106751548 lopora g578 ver,otsprng| toutsTv so | 0| 0| 0o1r-1193667739113932661[100 ppppm moai.996462M9Livv6eer,, ootsspprrinngg|| _111326572| | 1 1 T | e 20o|| STATEMENT OF CONCLUSION CSaeFraSOrexsultisn 1f4roomf t1h8emmaalllaerdcson(tr<o1l00gnrgo/umpL)poartnidonquoafntihiiasbslteudcyonscehnotwreatdionnos doeftCeyctFabSlOe slevienls4 ooff qh1ui8asn(tfisaftniuagdbeyle1s0ch7o-on1cwe4en0dt0rnangto/imoLnd,setToefacbtCalybeFl.e14,)S.lOevsTelhisen o2SfeorfCay1rF7e,s(SruOasyngferion1m616t5h-e17off2enmg1a/7lmeLb,ciornTdtsarbol(le<g11r05o)0.unpgipAmnoaLrlt)yitoiancnaodlf s8ree7rs3au0l0ssanmgfpo/rlmeLesigCfhyrtFoemSenOthssee1ra(0rpaspnamgmepdlo6es8se7d0f0rf-oe1mm0a8tl0hoo0g0r1no0gu/ppmpLsm,hodTwoasebedldeanm15a)a.lveerAganrgaoleuyptoficS1ahl6o6rwe0esd0ulnasmnfLoarCvaenfrianSegteOeeonf (range 6350-42800ng/mL. Table 15). soSfeerr3aa brrieesdsusullt(ss<ff1rr0oo0mmngttihhmeeLmf)aelmaeanldoefaosfpqfrusiapnnrtgiincfgoinactborlnoetlrcogolrnogcureporuisprhaoptowornetdiionnno1ofdoaftth3eiscl(sa1tb0ul3deynlgesviheomlsw.eoTfdaCbnyloeFdy1eS4t)Oe.cytaTibnhle2e 3sle6av7me0pl-sl5eo4sf5f0Cr0yogFm/ymt,LhS,eOyT1a0bipnlpe7m14od)f.os7oAdbniamrldaystliec(a<olf1f0rs0epnsrgiun/lgmsLgf,roroTuaspbelvseehno1w4s)ee.draaAsnnaaamlvyptelirecasaglefrrooefmsu4tt4hs1e0f1nor0giptmpLms(drosasenergdae female ofspring group showed an average of 4960ng/mL. range 3420-6760ng/mL Tabi 14). bLiivredrs r(e<sSu0lntsglfgr,omTatbhleem1a4l).e coTnhtreolligvrerourpessulhtoswefrdomnothdeetfeceimaablles cloenvterloslofgrCoyuFpyalOso sinho2w0eodf n2o0 (Idveretarencgsteaab2ml4pe2l0el0se-ve1fl2rs5o0omf00tCnhyeg/F0gS,pOT5mabnledo210s4)e.odf 2Am0anlabeliyrgdcsraol(uf<p5e0ssnuhglo/sgw,efodTraawblneerat1v4ye).rIavegAranasloayftmiGpc0laBel0srOefNsoGuIlmtgsCtfhaoerF1trw0SepOnptsmy d1o4)sed fomale group showed an averaga of 10800ng/g CeFSOs (range 2480-30700ng, Table clLeoivnvelelrrsolroefgsCruyolsuFp-fyrpSooOrm5titiohnneoomffalt3hoisboifrsfdtssupdr(iy<n5gs0nhcgoo/nwgte,rodTlanbgolreodu1ep4t)e.pcotrTatbhiloeen iolvfeevrtehlrisessousfltsuCdfayFos'mhSotOhwseedfienmna7oledoefotfe7fcstbpairbrildnesg o(f<f5s0prnigngg, gTraobulpes1h4o)w. edAnaanlytaivcearlagreesoufs31f7or0ntgh/rgee(rIavnegres2a2m0p0l-e4s64f0rno/m9t,heTa1bl0epp1m4). doAsneadlytmiaclael orfe3s6u2s0nfo5r/sge(vreanngIeve2r24s0a-mp5l9e3s0nf/rgo,m Ttahbol1e01p4)p.m dosed femals offspring group showed an average SM Enon Labcrairy 3M Environmental Laboratory Page z1cr2te Page 21 Ga vy Report E01-1256 PFOS: A Reproduction Study with the Mallard Table 14. Summary Table, CF1;SO; Concentration in Sera and Liver bs Ei SAMPLES | Conc. LIVER bi PI T moms - - Group i ad | 166.2680ngim.range(5f20) oy wooo.| mono| vi a`Control Gowp. s " FemaleOffspring. 7 NA mE`MaleOfispeng | EE Fersaoas| 7 | 1002100000. sosvareonomt me Lr [me me 103nomi(1043) m= e a = Bmt i 7 | sworss | 2ewrmooron | morn | 20cm 3 | me 7| | i Er o1e08 Report 01-1256 rman PFOS: A Reproduction Study with the Mallard JE ------ Table 15. Summary Table, CsF1,SOy" Concentration in Sera and Liver with Outliers Removed summation | a Nowe|| oAvreraacle | | Rangoon | [aownr| GBEaiySe0sr | Srl' I i ml Pe Ceo o | 7| wm |wromr amean| moon] Tn] wom | :| ; |- mmame |v en wwe |T= | T] nn Foaecmnes |v| ------ | | T -- | TT rsl| ; ll TEETo ROT TT SR TT FE STATISTICAL METHODS O SSatsetcte matshsa .iansclvuides csacilsrlonegsomoaemnmsio,hnOosetwtsann0darcoNdElsHeaGdv.Se.anTAso1eC,slfoeocrsnsocTSefoeosafiohmfuavierrmedganahfoeiortsm,thene Eetme n npsA rsewtoaossrawlevlasssfc.oCnoAfitcoaA nlce mOarol.o ideobrGmainleed afssgree-- atoenr haenu1m0ber of m`T SeTAonTlEy MmEeNoe TsuOrFmeDnAtkTsAnwseQaUa1nA7uo5Ls3.It:TccwYohintovprbaendcyhomena,aimsoepsskessparecs5,us.ExpArrcecasusnreadrcey2(.dhoepvoarbeseneraovfewd1a0s aan Sa oan ang om O77 0 1575. 3 Ensirommral Laboraors TU pgens 1807 Report EOI-1256 ReponE011258 POS: A Reproduction Study with the Mallard PFOS: AReproSdtuduywcihtteiMootanrd REFERENCES 1. WMaildare" Intemational, Ltd. Protocol No. 454-108 `PFO: A Reproduction Study wih the 2. WLiabdoirfaetorIyntPermoajteicotnNalu,mbLeird. U2P7r2o3t)oc"olPFONSo:. A4R5e4p/ro1d2u0c7t0io0nMRSItuSdUyBAwSi4h th(e3MMallEanrvdi"ronmental 3. C"EexnttrraectiAonnaloyfticPaoltaLsasbiourmatoPreiersf,uoIrnoc.octSatnuedsyuo0n2a3t-e044o,r O"tVahleirdatFilounoroofcheAmniaclaylicaClomMpeotuhnoddss. PFortoamssSieurmumPefrofrluAonraoloycstiasneUssuiinfgonHatPeLCor EOltehcetriosFplruaoyrloMcahsesmiScpaelctCroommeptoruyn"dasndFr"EoxmtraLcitvieorn foofr Analysis Using HPLC ElectrosprayiMass Spectrometry in Quail Serum and Liver." 4. 3ExMtraEcntviiornoannmdeAnntaallysLiasboorfatFolruyoroScthaenmdiacradl OCpoemrpaoliunngdsPrfoocremdBuiroelogEiTcSa-l8M:a2t3r1i.ce1s,"."Solid Phase LIST OF ATTACHMENTS + AttachmenAt: Exiraction and Analytical Method + AtAttatcahchmmeenntt CB:: DSeatmaplSeumCmhraormyatToabglreasms, Calibration Information, and Instrument + PAtatraacmhemteenrts D: Sample Preparation Sheets Attachment E: Study Protocol, Protocol Amendments, and Deviations + AttachmenFt: Example Calculations. 3M EnvironmWentEanlsoLoamebnotraattLoabroyrsiors Pace2401216 Page 24 01808 Report E01-1256 Repont01-1258 PFOS: A Reproduction Study with the Mallard PROS: AReproStuddyuwhchieMootanrd SIGNATURE PAGE We certiy hat this reports a rue and complete representation of the data for his study: (hn A Sten Lisa A Stevenson Principal Analytical Investigator olfdals Date SZ Witla K. Reagen Laboratory Management o/h 3 Date IM EnveonmentaLaboratory 3M Environmental Laboratory Page2501216 Page 25 31609 Report EO1-1256 Roper E011258 PFOS: A Reproduction Study with the Mallard PROS: A ReproStduuywcittteiMootanrd ATTACHMENT A: EXTRACTION AND ANALYTICAL METHOD, ETS-8-231.1, "SOLID PHASE EXTRACTION AND ANALYSIS OF FLUOROCHEMICAL COMPOUNDS FROM BIOLOGICAL MATRICES" 3M EnvironmSehnEtnavlioLamaobnoiraaltLoarbyo.rato Pron or Page 26 01610 Report E01-1256 Reponon1zs6 PFOS: A Reproduction Study with the Mallard PROS:AReproStcykwichbto oatonrs 3M Environmental Laboratory Wem Soll PhaseExtraction andAnaoflFivyoroscheimicsal Compounds fromBiologicalMatrices . Method Number:ETS3231.1 Adoption Date: 301 Revision Date: 2//5/e2. EfectoDat: 3/11/2. Ap: Sd LiWbiolrltaonryK MRaensaegner 7s 5/02 Tae MEnearmansl Laborary 3M Environmental Laboratory Sd haCeormineoaisSappiFeiec! netetis Pagerot2t6 Page 27 Ce1611 Report EO1-1256 ResonEo 1266 PFOS: A Reproduction Study withtheMallard PROS: AReproduction Swa i th y akan 1_ Scope and Application TCihistmx hea ddi ex n (bVeEc.aThsisomghrmay slicbcod m fh. 0vcssB.ogmaoneivcsraprdovmidesehewing iyces eet. 2 Method Summary 08 hutntofi aoerg mnerivdete nrcby bhyebret..wibrnerg iagseddpideswnd essAn ogehnqioefubattea Cnacoownhtoad sshpikevd ishchetprlop0e sruorig.eThtAeemnodap. Acaen,e (NCR)io2ec0idg53s0 Ci eoiroo nemdhesCiyqarc SPtyEc.io T.h5Fpo heeurco,tmp heaabiefnsedroefedc1r0 sskcasnhdcdFdm(1PwLiSCPwEEcSaMraSrMaSed)eadsdaBsodgigfrh 3 Definitions 34 Dilution Cehsianercvapersed.15oc Unena. | mfsinge +3m ofBnfo 10 of6miscombi 3.2 SPE cartridge 5cGeoigeedctosrein0pseanposurnttssof rmrttcnnecrdsaandneJokhedwciobionnesdasodsceehrms dbeeroebrer, A SeSppishhi tnsacon hiervedacompoundscanbeeve om uhbiog ces sod ntooed 0 33 Reagent grade water. Weervith decconcn beastmis. 3.4 Quality control sample fSeattnepreitlae eccofee smisheand vr hecidacc fe id 4_ Warnings and Cautions 4:1 Health and Safety Warnings ayswe prosegoes, ever. nd dingshe woking wiser send rqee eUsseconvhelple fe the pe. When crs, cpg ole poss 000 42 Cautions TCakoencicrsotplslowntelSPEc1or1m 1ad1 dees ahcfeSPmE acroleafnoddwnrsashes. Afr sing Soi Phase ExcEtsrnsdisAarosniynisofForchenicl Compounds rom Blogs Mates Parco MEnionmertlLasoatoy 3M Environmental Laboratory Page 2001216 Page 28 01612 Report E01-1256 Rope Eor-1258 PFOS: A Reproduction Study with the Mallard PROS:AReproSduduywcihthoiMaolanrd Do0rpoe FpPeLCilsleesshtoveecdaocmy.of400a(50ps) ackprs. sb:back presse exceeds 400 Dot nan sohcnt patno ygesss. 5 Interferences TCoomtimhievearireeor,xTe.k hdonbed rsp re eyprof namenion ha ons in 6 Instrumentation, Supplies, and Materials hienfnlowain,g npmplentainodnm, rplsc, an erd plcseoarfe hvoeed ehide pean is meted. Equi 61 Instrumentation Vorex ise,VW. Vortex Geri 2 Vir TuronT25teboogie Vac Pp SPE Exction Mio Canoge Msta 100 EC Sue, Bcchor VWR Bole (010008) Miron. Qoa Ulin iegplMs Seco sped witness sionste: POD Agpeo betpings,she ese.colina,ssi 6.2 Supplies and Materials Epppeostnepidcestlsocprs Disco pls Plyptes coabpobyolinegSOn.| lee) Volume leks,gs pe A P----" Fasc mou v. Wha, 6m (ocherspp sae) Conb.n polgos 15nd SkO Labs redpeesps Syringes,caseofmessiSnL1g 000M. BoteTopDspever apeof dpiSlofan) SPE cationcvs, |. ctCon Wark) 75 sampleceri acerspp iz Crcia mops anndiops. Soi PhaCsaenEpouxntEcs rrtsosnmdiaABalsooiinissoMfaFltoiocrchenicl Page dofi WM EnonmertalLaboratory 3M Environmental Laboratory page2901216 Page 29 C01613 Report EO1-1256 Repo E01-1258 PFOS: A Reproduction Study with the Mallard PROS: AReproSdtuduywcihtheiMaolanr Green. HPLC wie clan,secs te decriedby he steddcmetdin w di 7_ Reagents and Standards Renner, MI" NasoporIeoqa Acer, HPLCpdeq Metool, HPLCgradercaer moronces, edeoe r ven . Solsesg , roa nromwr ppis 74 Reagents preparation 2o0lmeMsacommmeos ncoiratioRhaop: aWeigwhopepr.ocielllyl03k00hGamsm,o sce.1vPouotoRl2e200ae 0pmi awr, Sst rote. Nnodte:Wohpeenpaempidnerenntvoltume ohnoge.sein is reersionrsasesodden, 7.2 Target analyte standard preparation Praelplowingurg3e0 sxna escaynakd)mfyohf esyoabdpcavee.pMeooralaridcpvoeesmuan.gdsoreoscepinle, The: Weighrdtpbrooxikuicclyer10p0mgpofutneesovneno 100ml.ome fk ndrecedects!weighin Bingovohamewith iol or schscarfpsc1000pi). Dcrleitnhe:so0c0k0sogionnxwSih0t0h. =foO+wgorkingsander |slainof provi 50 om.Example cDoieuenengsamdxn1IMwiLthmen~oSOjrgoc.he +workingsanded 2slo ofson $0pm. Exar cDioe nchinSgsagndxrL 1 withmOenoM00SpprA opclh.e oki snd 3soloof peo. 050po.Exaile 7.3 Surrogate standard preparation Srempiredcpoeopsos.ore. Th ling 30 creolyad ey my otbe ppep forollsrogne Weigh spin0y10mofrogaine sd condech igh. Brig vukrewir for pte dndsockofpcsialy 0-100 pn Fremrererecmdaaundkgsaannsdrieroonvevosanswiahabt o.STolnsegswperhoivimeeysre|dmoiflo9e0f-1a(rpopsmh.eosRneocdorad ccki03o1ha0r5e 7.4 Internal standard preparation Psreenpiare peeranttsoannd.Te llowin 1xp aly and my may kb ppg fo ol ed Weighspp 0-1 101m ofrlsnd 310D. mec lk econ ech ih. Soli Phase ExctiEosrnndssAaansofForochemicl `Compouns rom Blogs Matis Pacsorts 0 Envionmental Laboratory 3M Environmental Laboratory Page et216 Page 30 51614 Report E01-1256 Repo 011256 PFARO eproSduct:ionStudywiththe Mallard PROS: AReproductionStdwih he Malar Brin olewith fo nr sndsockof spprovinacly 0 005. oPmererredfeaapandd rdigcoenesnosemmoenssah.oeSnaTstroee3swkpgoOdnotyarF|o.Of oEfTrpsl.nsReshoecskce0 v1odl0umke 8 Sample Handling Aspe ied cnand stbeke rn cainis eons owsrgistha to oom erp:roetoexci. Tppeds Gha nrlist shadia wepreore wihcchass. Exencidsb adsees be sed a Fyatscewheidelsrc elsrdts cnodnsbepcOyT.b lid ppl C nef 3_Quality Control 9.1 Blanks 9.1.1 Solvent Blank Asqooftnld ve bak.Sve aksrkxine. 912 Method Bank Cs riedisodfa1g 0umd.on fwwirc,oohrostelsowpsphsPoou a(vsa3rSmpiokedd iahks.arFaemetdhofdbnas7okrc kel) 913 MatixBlank VAposeiepo L.im 10BgfrmaiGpeeeddofbeonrcuoesizee)esaecdsa.31revsidacko.ntOoflerrmeocnmaoydby CS ond aneo id oar hh.3a plcshatsg ed3ccaone mvry uHtofc oltcocfchse areoYsihySetd.y Fs dnert idcave nd CCVor 3 oweso.The tre 0 edged 90.31_nSty ycontoolrmateiv1e0t3pheiychonromovi 0ed)fhe.ce,pre Fu) ibanks. 9.13C2 uCvoemmeaiolyeh)idibmekpi) stinnieve eif bleconvmaerliealmyasb(ewo iiedswiehudfoor :sd om ied. 91.33a unsSuummogcmsiecesmruyivcuomeley sniftlssusrngeemereidoieeh(eydmoogreb2ciukea.ipnregpaSr3eEcfSoon)m(r)ealwyiveblaarlkeswmiegxhoef 9.38hetilymo crail nvelva o,shenamedsdmr rks eybe stedsd il be ed 9.2 Sample Replicate `Samples pntswe eedsong chsoypool pctwos. SolidPhaseExacionEransdaAznssiysof srechemisl CompromBoluognsMdatsis Pages ots SMEnsoomentaLabortoy 3M EnvironmentalLaboratory Pa31gor2e16 Page 31 31615 Report 01-1256 Report E01.1255 PFOS: A Reproduction Study with the Mallard PROS: AReproStduduywcithtthieMaolnis 9.3 Surrogate standard {bSForneog3cosncannitdoin.incohempaonaeneogftoefstoey.alaspaluv,swpiikhedthwiteh xopgiofsaBdknSproioie1xtecisond iTympcipetaillmysmoavuyirbngegess pi1ke0dmduecstsayd meapdo,cts ohie mheehe1.0 1.pi0r.mc,ddtioicehdtoibnogmohgeineiersd.palrioerBreeorhveeefofdrocrhxiitamciiooonng..Hzcowererde, 9.4 Internal standard sFincnsoannidreiciacdoeamnpereonfoaf heirsiyoo.noflcnaep:lesaesiewih rlsadaferexcion tochin oT val. op ike lol the201m e ofexistins he15mLeis foge be,beesanslerng oe 9.5Lab Control Sample Labcontolsimples otscomportof his hod 9.6 Quality Control (aC) Sample liPrealpatrleoatauilvoyencoctnuteod.l f(ToQrC)iscshalOm1pCll0easpiyoiveaobreresnpeiorponfcfaiesnc,ysonfdhe1semeyrbie ceodeo d as cs fttlh "T3a.c0hCs12l)euslmyactobreopsrmas(o(nQCo)twialclhbe Smell exci onre Hrdoy vpreeplaroecdacfho noeQC dcyohfrsapdeinactne.cou(se5ofIhaels y. iAiy ocshdit es tb predon5 oyof Rionfo atcalofwehe) QmCy pprleessetil cploeucsocoefifomiosnaspdseda caach of ugeeeofvehseoafaryseo.nThvee elsitedbelowrybewe3dnd Lowles 3 0 SXbeLLOG, Mec: equivalent potshemideofhecalibsioncine, ighlve 80be L%OO TiucoonO,C wsialmpl3eieives aoefsGrneeQlCpaeeaeyvesry.enSh senblorknereensticonrnseeds0mploestbcotlsoybne sidaed chfor deemingwhenQCsams wil be syed. GcuCrssaemdpldeisncgchedcowriehof hpearkdlyrmsypheestbeedinbeblryeznetdbintshe.same abil. AOrCsimyples 1c6xsmacondfoemmuotbibleenxcikncioinBdoessseesyed noesnailrntenQCsimples fromthesane spe hEsscrhQiC s,pe3iminshovoeafn1a2cfihme OfCs75u1p28e4oafoehxpevcl. rAst ietusofmc2e3rso.1cQtfC,sap]ltlst .ee bee dyedonexmce. 9.7 SampleDilution ntCyrlsutonrladteitoinwocintshla.niaIfcsguewmisllebhewepneGrifholorimoefdohvehienhreasgeicocefpvalcseuseaundirvsleeesdsodbceoiutghedsrkolhe agieo.f Topoetrofnrntsheadmipolvlefdsswion1o0gneasamaplesiloessepuarlis,otrvoeprearsmate5sGangalens dGs.Bvhon10yml SoldPhase EtactEisrosdneAastnofsroychersicl Pageoof19 Compounds rom Boog Matices SMEnvronmentl Laborato 3M Environmental Laboratory Page 201216 Page 32 51818 Report EOI-1256 Repo on1258 PFOS: A Reproduction Study with the Mallard PROS: AReprooddyuwicthieMoatanr 0Srdvdccovitcisehsrhelnm0poksin0cr)irnoenc(adcchitiod (ixnigcddai0pndgrnodcider).sws.hilTmeheainctotenbdcprrocecousniofsiofihning dIeFbienethiivcehpleetr :icomef spro n riint15%fSortehecwno snamp.les ds singwilbereedfo 100CoCralblrbartatiioonnaannddSSttaonnddaradridzaitaiotnn 104 InstrumentCalibration 1Ox0nr3esciSolndataneocf 4ediewcirlalibeedporfyepnsaered9ft)ovmleo.dxAcdmeeonlidsifaiitenncuhrvessmaeymbstexraasethseson abaipessole cnCTierm.eisgBee1m0bmreLGaoonrencpeoreshpkpeertphieecnsosndpurceco.sfTdcih,oentdWinicelsloheleefeesiAowhhteerobgoeeGpiozendeco+ ohleotsgfoer:tbeo usma15enmdl Temes. ReFcoord0smchsaalcoit, hoame:naptphreopwrieagne,nofeotoclmaaicstieovnwe soskie,lkop.ment. Thi`ensdpuadncid.csotcsceonclttsalsto.ofnTshaenaud bse,krionoaf mtoasrbdBsekdnd aibnTdkboewry|tbaheydbdbeiwaked,3p0wGhepansnpddorayd,eoriiessoGndCe mei nance be, RUseeAcvehneC210.ck oae sl procphiefcomness 5 ofianbecclhthaeuctoocneinonnsdfshmewOCilgesid HoToteotspo,syyrbetes1kt0demssaulnryed,oiskfpoikeetv1i.o0rhme,r1d.10smlcL.nhGgreowgidehonwdsc, Glsaoprbenroeomrocvnedofeonr sacteion. payoenhme xltsc5mhtsssak ndesiovfe rrieetcrctc)ofnagcMts.Tyhecicvectaion wailederinbdy u eyseleicab hstmi2a0y77sbf7ee 4dp.1re2.9af dAlalnyesoi weioeobendl estewpi,oleedreegae rrebdioncv ol t 0xbcepkt h. emLLOeQwhlich Soli PraCse EoniEprcsronmsdoBAsoioanlusoyngiinoMifFeossrse IM Emicoments Laboratory 3M Emvironmental Laboratory Pero Page3301216 Page 33 o1617 Report E01-1256 Roper01-1266 PFOS: A Reproduction Study with the Mallard PROS: AReproSdueuywcntiiMaolanr Sohpaesnss ntMoamtiiondaattueadi1e5 | icFoiaatc20omoia.fvtolubemree [o T un Ts |S"T omwswogal| 1 amdmeaw]] osuI 150 T7 l0omsorognl| orswegmt || osmmuugmmt T Sioo00noggsgoorrnaggienT rt| | ssocoommggmmei [StuWnutn T14S0 | TDSSoenggoeorrmnpgmmi| | ZsooommmmL | smwutm TTeT|Sosnoogggcoorrnnggmmll| | sbooongnmeer] swum TT 7 ngageA | fooepm | [o-- oumo t 0 6500 |u moomopsoom rrnnggnntl| |-- ToomT seen]] Somopesdional| lo1enggorngm | Somat] 11 Procedures 14 Tissue Sample Preparation Onin ensupels oCftppreouvri 1es0t0e0fogrfmoidsuik1-,0n1t00lo0v,ionrgoeerepne0eOap.aevne. sin dicinpge.Thipr Weighie ve etyto redpacesrevil Record he eight otheweighivolamehee,xs ike, oe props cai, Remus tie he crxca tiontsse shavr ebchremned. AwhG.A2 mlofeenwir smuvil. thervolume ermine bybesn aoddocunredia ke. fHomiogtersizae tnhersairpaledPiutnteUl:Tara rie probe in he spesndgin or pros 2 msc,oc RbiyeetshepmrobdenoechmeereedconmikngfhoeFssrslgihP2K. .iL.ofsags de werocohervlan deli Take the rapa dls wih mt str acn hspe. Ree ETS.-52 es inrmtion. tee10tc3da0isanGmgyrotioonmdeadsibshyne0iy0e0an..dcstd(wocikm0ie+dg0i.e10mw0o2e)v0iefrdorecnadctoia,n8is)0w)eioghft 4jhofewkwo0ohlnees Solid PhaseExrcioEnsrnsdsAannaiisofFlorham) Compounds fom Bop Motes WM Enveonmenia Laboratory 3M Environmental Laboratory Peesof19 Page 3401216 Page 34 o1618 Report 01-1256 Repon01-1255 PFOS: A Reproduction Study with the Mallard PROS: AReproStduyuwichhtoMoalna 11.2 Fluid Sample Preparation J A -------- SLaebeetlac1h5emdwipaokoep(yA:TcHncestrwiWhorthkeaselcy)iramdboeer,retgngebIeD,rxeicne dpise.sdsnl is. 1V0or4 lamiix hnepucdvsaalmoplrecfloersspepoopilco1ntcio.rdsth snl 1.0mof filolespreamount Reta nedsrefee fe xnoseuss vebn ned. AdHoc0muLmofeenatenoitwantergto he 10m of hi for 16 ition,orother itionssdermisbyte ys. s1aevlolieooenshoasven 10mi i rermodforan ndvolume, dsste wrvolumesoning tomissinthe 11.3 Tissue and Fluld Sample Extraction liAesrneds1o5emmoprgfeiildesdslaepslcyofoeiisbepevnnroepnyc15ociond fsenctionnst11.11a0dm11.2,ooireserioopressevboyhmdJohe8 Reta edisedomogeiadpectonto eeestereos avebenrend Reso the volumereedontexeonwakes (Ascher Ao silawore, Spikeblank,samples. ndsnesesd forxraction wilhropesnd dscrbd inhismethod. Slklecsicaocnhicvaebsriinod sndichiOsCwsiellespree aus ofsanded 1 describedi his bod orth Vor i hesainuvesamples ndGC spl oxspray cons "sTocxanhsnp andan.ad50ml.ofseni, 3,ad vor isebyhdspoil 15 P0l0cpsmloprlosiclnsheihderseacosn6p.1o) repeed or20mittdq ting ofppcviily Rceimnogveoffsropm rhesaakye2s0n0d0cvmigortanhsoporopdrinn sepndfx1)10 ies 0adelpel species ArBaS4n0h0emSLpoefmraange1tahdeewther 0e3 c5e0mn.50umhi,.aciegfcagr:boet1.Remoocvecsoangfshfeomthcecenls loand Shain.Capademiibytvebinesvde esw,i Ion dsi ussd ofan rybecharged1. sa Neh heresi he SP cardedtach his serving ni 1 voc rfl. lNOoTwEo:f$Wh7emienn.ingFlhoewvsmaacyv,ythheouvghicarcehaebearetdshperKoPsAimsyeyb1S iKPsAe.dFo ihvoeabse psnodcsyeiaohnr mt ov endrmdo. POempelheoScPEocwaere.tabykwiandcairngoitce0swliohwsthpecoouil1 0rmtoefmyeetsafl,elaclhewabtyhspelus Btroeughithgcolisucmonmpldey,nepso.u hesamplei theresoiicardewitandalow lloftheled 1pas Run thevaca on ihforsponySines seq dy schSPEcrtide. Place cllction 1 mil.ppropyencevg bender chcageadciwih20lofmans Spikentbanks,spe,sdsdswih rlsind decribed nh hod, SoldPhaseExuactEioTnssndeAnasnys ofFsroshemical CompromBoluognsMdatses Pugeoorto IM Emienmonts Laboratory 3M Environmental Laboratory Page3sorzis Page 35 Ci1519 Report EO1-1256 ReponEO-1256 PFOS: A Reproduction Study with the Mallard PFOS: ARoproSudtuicntMollnrd aLxambtelbcexghdde,egnitdsiynaesoop)rnoLeInMarttSopmbp,p.iarwcif.rtohvesny,imser,sviil fcmcehoievednmceoerer,ospsel Tasercachchant13ssow no. 114 ExtractAnalysis . 14.1 Softwaresetup OtyheMeashs m a oi rotwn lsurpaes, sSkruanheSevtbestt3ishixnneodenipr1tfrntor,kLot 2digsof ExampleSurgeList [YYMoMrAOL2D020u8 =n ofhesane re4=A) YY=Tetyar MM= Tes mot2h) OD Teao0y =Fitsl it on)of hedy(he ctsale ndom) wld i, enc, csoitgalenm:auenogttsessme13nddeesisstsebranhfeo xsth2ilirso.fte stysmhsnd gh . Example ena:YYMMDDAB ALO205001 =nfsa Y=Teotyer : MM Tes cts 00 Teudy = Aflpiotrtofursturi heed ina meh me (MS)fo singwih eri. a oh9 01) kl,3boc ber,sn icin oe. MTmRuosMtcs,c("oixAlgdR.etnchtiecoksnomMniMosenitiohnnogsd)F.rdSanedbisotanpioinmheMesoM.ckSS5vS5etespqartoinopnnsdm6cesdtSItRIfS4M7iSeSfooibneRrnsep:rnpsnge `rAe.eoanisTorrboorta Fmainrotn rROL o a1ote. or Mw He nTapi, wl och esserebegswihye bly,shes is, nd etof ced min Sicaeimrpdleyedceo2sphccreaallyy omwiihrwpooOsiCbslierreasb ScAtVaEfernevder rohtscolndeinscailoneSvxevnabsbkkmsahyobued Solid PhaCseEocomnpEroranmdosBaAlnuasoyngsnsoMfdatFrlisocerschericl EnvironmentalLasoatory 3MEnvironmental Laboratory Page 10019 PoonB0t216 Page 36 31820 Report 01-1256 Repo 01-1256 PFOS: A Reproduction Studywiththe Mallard FOS: A ReproStduduywicththeiVaotanrd 1142 HPLC setup. `Setup sicmy ecgoh le otprepare. RSeedttheeauHPpLoCtoethe lhloinaconntion gccoonedoSsPhOeRsESt0consis peeorpin pons. [------ ects 1 Cte= 00mnses Powe - 0yLinn bicphae: Sobet A 2 Ars Ac Solent.Mebane. ! Soahsi eong: [ow] wo] [CwTw] [oe T=1 = IC IL 1143 Instrument setup FReifcniEth7a5n2A4,sOppereatiPornosnsdeMoiistioenrSooef?"MiGclraQs 1 Tre rangle Mas Sperone ChCeocckht theh see inHpPlLaCs ymtetseoi sdonfd es pief.ecUes:sencheeckets.Tetphoewit, oad des. epfobacon, usnie e robeand eptcteSk eli Tamandegen. Openteahg.Click pee nine ureHocksddestinhese pDeontoEnrHP:LC etddc ler or beg ys cli. cre wt 10-0Lninorss erie SILCpage bsedrops itcori utof pfere Afo it endbe osewih ison akingsod of bepoe, Ret hetpofth befn iss sened otocainesposimcy 10mes. 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Report 011255 PFOS: A Reproduction Study with the Mallard PFOS:AReprodSutcytwiihotnh Mollrd Coltevesinddeviation ingbe ll qo: RelativeStandard Devnion = SaarWDeenviation yg Catepertdvatobenluowisngienqgn oeten = Bp CopneedCCloaeb.esCone. 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AschmenAt Exction Worksheet Nebo Ravin 750.251.1 Same Timteponrt rr rr 17 [rr T 7 1] rrr 7 1 -- rr ----rr rr 1 -- rrr Tr 1111 1 ----r-- --r-- 1 ------r 1 -- 17 [-- 1 -- -- ----1 7 rr T1 rrrrrr [+1 1 1 rrrrrr 1 [Trrr C Sr Th1 Ahea[ pedTom T [1] S Mi en r n ons man 5 pope P & orTITee ReE Gr Gmyr ae n con" sn sar s) ihn rns T1o1CS onono s18rEm resTveaneppoe T r Mree aOH smT mi A so chm G go rs 55 Fo cc omo STr eeo A e shaoerord e.rone4h canto im ahcebe i is Ba E TE 7 eT ooe co on Fio oc amtn srt AtPA rganroaesy 47PA0 es 1im cn on Std hsCeEiocomnersormmpdaAndoopyetMaenseesrial ae 15019 aM EmicomanlLabora 3M Environmental Laboratory Page 201218 Page 42 V01828 Report E01-1256 Ropont01-1256 PFOS: AReproduction StudywiththeMallard PROS: AReproSdtuuywcihtheiNaolanrd tschmens B.- Sample WeightVolune Worksheet FAremDau:es: SSatmtpoledRMerabion: ESatupymeNunmtbNeorm:ber: Find Se&Tn NSumt ber: woiivr mt + RVeomuaoen i TTTr or -- I TT 1 Tr 1 7 1] rrr -- 1 rr rrr TT] 1 TT1 FomCoplinVesetty_____ Sold PhaseExcErsaaAnursofFach Camponisfo rpc Maes Page ar1e aM Envionmentl Lasoaioy 3M Environmental Laboratory Page 301216 Page 43 o1627 Report ferrin E01-1256 rs vy PFOS: A Reproduction Study with the Mallard HHbEH P E E S g=egooEaw crt T--a E E i --S== e L sLa LI a pl EaE EyTbEE , [FosooTT oem [500 Toiesr_To1600 EEL SEE SaSu oE a sra. e e [Cs Tool 17200 Tosesr Tose | BHP EE [so T oe--TT 50 Teieer |oie | E--He E ie Soo || oes 1300Toiesr |oie] H Tse npEe riEFere ET EReTe = [[m eor ] we yat p [ yLi esegtn0 TLioo0 g1 | ao1 lgoys]| [Crea Tose [oc es0 eT "eso | = Be B= Ce HHmEeH BB e B Twa [Ce] wpL a T mp SN 3MEnvironmentalLaboratory nase Page44. u1628 Report E01-1256 noes PFOS: A Reproduction Study with the Mallard ros A Repost Sliver atm im men ts LsTLuElE punt getemess SmpleNember |__| erection TuTu TwTvTvTu [v Comms[verieasy:| rrrrrrrr1 rr rrrr ---- rrrrrrrr 1 rr r rr rrr -- rrrrrrrT rTrrrrrr rrr TT rrT rr Tr1 -- Tr rrrrrr 7 -- TrrrTT1 rr1 rrrrTT 1 -- TTT 11 TTT 1 --rrrrrr ----rr rrrrT Co--er-- rrr111T 7 AANA srStm _--pind Enomtstroy 3M Environmental Laboratory tr Passe 50Pa1g6e 4259 Report EOI-1256 Roverton1266 PFOS: A Reproduction Study with the Mallard POS: A ReproSodywuicthieMootanrd ATTACHMENT B: DATA SUMMARY TABLES 3M EnvironmaeMnEtnavlonLmaebnotrsawLtaoobroryatory -- oPais z : Weed on 2 Beas sang : NH Tg Bee reas HY OHA [Penn nnn Hesse san W7 en sn 1 Zz BB 2 Hood ooo aH i Hees suey FR=EEll B| THIRETGOO $id in eR ny : t F dE i = BRU dn HH Boose] cones {| i Rd a fleconay mens pe| (FE ET~ E z Bann 1 RI | i : HE my LLHh 18 ER a ; : i i }5 3 ] 01631 I { 3 & H Eigeigeig Z i [Bsn Heian bl:cieoes: Fyre Ries : | |} gs Een IF << J ir 5 IREesn IF <1 I fleven 2 Hele SHEE Bea EERE B%E: eclevcfoe i s2slssyiss FsEzE <cfoecfee| i EERE BszEB <clessiees HI i[s23jsz5ls zg i d e WaT En [H M83E IE ! 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A RssSttyuwictokna Ewan anrrnanaadoGanvseya007.a0me7a7aey real | | | | | | | | || 1 1 | !| ||||| ---- 100 200 300 400 500 600 700 800 900 1000 3M Environmeonrtaol Lpabeorsat--or--y ~ [ros Page 75 001659 Report 01-1256 J EsSHiEonrvnirsonmmeTntaapleaNb,WaAGT [ir | i i PFOS: A Reproduction Study with the Mallard 0S A Rprhcton Sty ib ss ow annraoanadeavseyiToordoearSreend Se p=h: | | | | " i |1 i | | ! | | | | Oho R remRR e" R te ae we ae- Enger 3M Environmental Laboratory Pretost2e 9165Pa6g0e 76. nos Report E01-1256 E 1v0e8s r1-o03PPaM2,s6Male7, A,dult dio 100, ] | i i | of eASti Spurn PFOS: A Reproduction Study with the Mallard sBr a rdeavey 0707 zCo=] 233i0c8| || | | | | | Brrr err Tine| 100 200 300 400 500 600 700 __800 900 1000 | 3M Environmental Laboratory Page 77 001661 Report EOL-1256 Reponor1288 PFOS: A Reproduction Study with the Mallard PFS: AepSs oyio h heMn otard Dosed Group Adult Female Sera Samples [`3M@EnEvi1ron0me0n1t0a:lPOL5Wa,b2Fo0mat0e,,Adu h(.02y0228057 Sm i, 12) ia.no.n 28Fab-20G0a2v,ey170:72017 MRM of1Chomeslu5iiecg | | | | of OTrr akek shr e ee o 709 80r 0 r 800 1r 00T0i'ne 3M Environmental Laboratory Page 78 81662 FS nin PROS: A Rerun Sy with Malla 1108 Ars sp sits 454-109-3276, 10PPM, Fomale, Adult ;G C| mE 100 TT "davey 0701 TT emeoTnee = S13 Tic| | i | | smn 3M Environmental Laboratory | | ETE EE pens Page 79 001663 Report E01-1256 Raper aa5cM42-6E12n02v86i03r62o78n85m,menT(tiOan,lPP2LaW)b,Female, AG ' PFOS: AReproduction Studywiththe Mallard PFO. 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PFOS: A Reproduction Study with the Mallard PROS: A Repraducion Soywin he stars TT aresron 2M7-RFoMbo-f2"01d0Ca2v,hey0a40:7m506Ee:7Sl.| aaeziaec,|! | | | i | | { | | i ! | Shorr i MTT RTST TE MY TT 3M Environmental Laboratory Page 86 Report EOI-1256 Report E01.1260 [(fS41083260, TOPPW, Female, Adult "|[02022S6m06a8n. x2) I" |1 PFOS: A Reproduction Study with the Mallard PFOS: AReproduction Swa i the y larg Gavey 070793 = HofR 1ChamM elES.| Bay az | | . ||| | | | tl | | i || |]| | | rTTTea e e Ske e as 5%e eeabn rb - ae 5b iTeisme) 3M EnvironmentalLaboratory Page 87 Report E01-1256 Aap zor258 PFOS: A Reproduction Study with the Mallard PROS: ARproStcyuicthhteNoarnd DF 3oMsEendve ierGoranmo,l eunTpt0alMPao PLlaWbe, OMan fifss,prOinfgfSserparSiamnpgles aoe) zSn mon5) ohns || 1 || | Ga0R1 Mavro200e2G,ra1ym17:04S1rpkSoesr!] | | i ' | i * | | | Ora ee 100 200 300 400 S00 600 Jive 700 800 . 900 1000 3M Environmental Laboratory Page 88 01872 Report E01-1256 woman p0[4He54E-n1m0rm6o-9na6m2e5m,nta1a0liPLPiaMb, Male, Offspring || * | i| | t * PFOS: A Reproduction Study withthe Mallard 7708 RonnSt tes otE Mar-20`0da8v,Y ey101710874998 pon 2vi17 | | I | || | | | | | | ---- ge! 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Eoyz 2 gTl . || xf| | In | | |i | TEAR SR | | || | ha eh oe 3M EnvironmenEtamliLaboratnorny n Price Page 111 $1595 Report E01-1256 Roper Et1258 PFOS: A Reproduction Study with the Mallard PFOS:AReSptoytwusehaiaotan a[M0E2nv0i3rA o0nS6mme1n(1taa4nl 1L2a2)b --Eaent | J l | || |1 07-Mar-20G0a2v,e06r:31 {Mof 1CR hanesA liETnSeg-l on || | | | | |i | "10 Tina 200 300 400 500 600 700 800 900 1000 3M Environmental Laboratory Page 112 691696 Report EO1-1256 ResonEor1258 [[130MpEpnmviaro.n3men2taFl6LLiav6ber m0o 203065m11r2n, 122) | | | PFOS: A Reproduction Study with the Mallard PROS:AReproSdkyuwcintheiVolrnd 07-Mar-2G00a2v,e06r:08: 1o3r 1: MRMof 1ChamEe1i0Sl0c.0 ve | || || | { 3 To Eh 3h "4b 860 eb" 780 wh 560 10Taime 3M EnvironmeWnttEarlirLoarbaocrtatLoarbynory Pace 11301216 Page 113 91897 Report E01-1256 ReportEO1-1258 [10 pEinnviaro.n3m2e6nt8aFlLLiavber (802030S6m1(1M3n, 1:2) I | PFOS: A Reproduction Study with the Mallard PROS: AReproStuddyuwicntetMoallnard 07-Mar-2d0a02v,ey06:19: an 1: MRMof 1ChanneESl. tates 337 || | | | i. i 15076 soo 460 58 66 78 865 505 160T0ne 3M EnvironmeWnMtEalrLanboroatLoraybo Pace 114216 Page 114 001698 Report E01-1256 RaperE0126 aS[n2Mp0E0pn0m6v1i21r31o.5n3mm2e6(n4it,sF LLi2a)vber . PFOS: A Reproduction Study with the Mallard P78: AReprtotydwtuhocaorns or 07W-MRaro-2fG01a0C2vh,era05n:n5E7e:35l- ES 10, | | | | | || a TEE ahh Shak hak 5h fans 3M EnvironmeSnMtEanlicLmambeornatLoraybor Pan 11501218 Page 115 691899 Report EO1-1256 Repo Eon. 255 [130MpEnpvaim.ro3nm2eFn6LtLaivb0le.r (i|0020306067 Sim hin,12) | || | | || | |] | | PFOS: A Reproduction Study with the Mallard PFOS:AReproSdtuy icththeiNoarn 06-Mar-2G0a0v2e,y2G1:74087: Eonht 4:ofM1ChaRnnel0ME0"Si0.c | 100200 300 Tne 400500 600 700 800 900 1000 | 3M EnvironmeSnMtEanlvoLnambenotrsaltLoarboyratory Pace 1601216 Page 116 51700 Report EO1-1256 Reponcor1258 [1c02pnaEpdnmivoiaer1so.SnmrSenEitnaF,lLLi2va)ebr | PFOS: A Reproduction Study with the Mallard PFOS:AepSahytwuhctheiaotanrd on 0M6-Maa r-2G00aC2vh,eay2n1Oe:l73E07S:. siedr nas | [| p | i [| ] | || ohTER Shah ah ah 750 wh ae iTine | 3M Environmental Laboratory Page 117 631701 Report E01-1256 upon ot1250 PFOS: A Reproduction Study with the Mallard 705: ReproSduywcinthie aotns Dosed Group Male Offspring Liver Samples 00Mp20oE2n0mv7i0ar512onm9me6on3t6naWlL2Lia)vber |1 E50n 0TBMarNa2G01a02vR C,eh0ya00:mM 73a0057 : . 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PFOS: A Reproduction Study with the Mallard PFOS: AReproductionStudywiththeMallard |Dr Eo5s5em1d.Gt i5r6oun5p0Fevomsrale Offspring Liver Samples Fs =un || i || || [|i | | || 4 | |i |i I] I bl1 TR obPteara2S0eB0veaWraores ;7 | | | | || | | | SM Envirconmuenpt e--boone--y-- ---- Page 121 CLiv0s Report conor E01-1256 ATECAmeeLnrELa8ar |[1 | | -- PFOS: A Reproduction Study with the Mallard . o CarSteeTanSn As popod | | 3M Environmental Laboratory ago! Page 122 $1708 Report E01-1256 Raton 258 I [f1I20zpapamroa.e1.s9mn6.FL22iv)9 er | || [| | I PFOS: A Reproduction Study with the Mallard PROS: ARepriinpnahatts oSne o- 7R tar-2d0a0v8C e,y30:71C0:= 20=08 | | [1 | xJ | | || | | | | | | | | | i 10 200 300 450 "500 600 700 800 800 100Ti0me| 3M Environmental Laboratory Page 123 1707 Report E01-1256 Resa o-250 [i`03p2M0pE50nm7v0i41r7oS9nimm6eninFt,4LiL2va)8ebr | | | jl | PFOS: A Reproduction Study with the Mallard PROS:AaSrty iohboNnard. 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E- aoll | ||| ||i ||| L 0 ER ER ak 5k 6lL 3M Environmental Laboratory Page 125 31709 Report E01-1256 Repon ear 1256 0 pEpnvmiar1o.nm9e6n3t3aFl LLiavber [402030S7m0(4i5, 52) L | i | {7 PFOS: A Reproduction Study with the Mallard PROS: ARoproStdyuwichthie oatonr 07-Mar-2G0a0v2e,y23O:7271 4:ofM1ChaRncelMES. esos p es . | | || | | Too ER Sh 40 se 860 780 5h 5k gap. 3M Environmental Laboratory Page 126 651710 Report EOL-1256 Reponcov1256 F[CS1M0E2pnmvi01ronS0m5me8n84t4ianlF 5LLia)vser |! | | | | PFOS: A Reproduction Study with the Mallard PROS: AReprSoycwuinchio oatna = 2 08U-MRaro-2lG0Co02vr,er0a00n6:5e. ars ar=id | | i || 1| | | | i | | | || | | | ETE SREssw re ake ee 3M EnvironmEenrtaml Laabnorataorryi oun 700m Page 127 601711 Report E01-1256 ResonE01.1258 Control Group Male Sera Sample 0#2M0E2n02v56i0-3r38o2S4n3mm,en(0itns,PF1LW2a),b Wie, Adult | | PFOS: A Reproduction Study with the Mallard POS:A ReroSdhyawcishh ostanrs. on 2M 6Fob-o2R f01G0aC2h,va2emM 3OayT:l1E1S. ic Ld = oe | | i| | 1 |{ * | | | | | i [ v) \| TT a Errors shoo 3M Environmental Laboratory [-- Page 128 $5172 nomen Report E01-1256 QCoanetnoroolsne mG,ernoauTs lpPiFs,ehmaFloertS,er3a0S0ample wo) 1: Ate ti td PFOS: A Reproduction Study with the Mallard , r`eef5eoiis w a& | || || | | i | ol | 4| Ai AAAn ad || A TR ErroEro e ge 1713 Report EOL-1256 Ras eon-1258 PFOS: A Reproduction Study with the Mallard PROS: ARarStydiiarns. Control Group Male Offspring Sera Sample [[2:3@0442-E12n0v0:i19r35o7nm8m,ennt0aPlPLWa,b Hala, Ofapring an | 0 OM1.RMaOr20a10v2e,ayn14n0:70075. Tel 6.1p16r3) I |Ll l1 v il| Mihi" . J ToS a ake a ae Iime 3M EnvironmentalLaboratory Page 130 001714 Report amma E01-1256 108 Ai yit tts PFOS: A Reproduction Study with the Mallard Control Group Female Offspring Sera Sample Enbesneoor, (454-109-9589, 0 PPM, Female, Offspring 1 ere trot 74 davey 0707 TIC| 7.8803 Areal | | | | J| | I rrr TCT errr Time | 3M Environmental Laboratory Page 131 01715 Report nose E01-1256 SME ED rr a nLs Control Group Male Liver Sample |1| 1 | | [SS ---- PFOS: A Reproduction Study with the Mallard co o 2G0 r o1r:13:14 812 LJ 2Tic| 1.0704) | | || |[] LT i TRI 3M Environmental Laboratory Page 132 C171 Report E01-1256 f-- Control Group Female Liver Sample oSclcEananvTieorSnmsTomnnta.Cl e2La1ry ! | | | | .|| PFOS: A Reproduction Study with the Mallard 708ABarSytwrone ntat 0i8bMCar2r0G0a2va,er1v6oT18e | 1.p13e04 . I | oon C ER e O - 3M Environmental Laboratory coP1a5ge11733 Report 01-1256 wnorss I PFOS: AReproduction Study with the Mallard Control Group Male Offspring Liver Sample Ormman anri cn r Goe ver | 29.3303 | | I| |! | | | | | B i, | IM TET TTme M EnsiNmTToei ------ . 1, Report E01-1256 none ron Aa nt PFOS: A Reproduction Study with the Mallard CFSL orontmreolrE GroupTFheemrale Offspring Liver Sample oo| pa oT s aTl o ysairan] |. || | | | | \ | be T tt T e dh YT, SMEmironm[ ena Tam-- ers rae stn Page 135 o#1719 Report EO1-1256 Repo gov.1256 Extracted Sera Calibration Curve Point 05[:C2Mu0rEv2ne2vp0ir0oo1nn0mt5enptoanbl, iLna)sbara exact 7 PFOS: A Reproduction Study with the Mallard FOS: AReprSoyswuinceoatns an H 2FoboR 2f0d10a%hv,eayn1M n2.a25:E.A ES 34o50s4 || | | | | | | i | To Eh ahah Shs reek heeTime || 3M Environmental Laboratory -- P2ag1e712360 Report E01-1256 Sonor PFOS: A Reproduction Study with the Mallard rot:ARroSacykhootners ECSmxuHtravrEenanpbcrtloenndemLeinrpvtsearnaCbavlirbaravtricotn Curve Point " | =" ootiaGs0or0Ge2yaHm0e7e0sr=, pyh=: i | | | bth Ti IR IM EnvironmeEnanltrLeaborersmens rrr Page 137 e1721 Report E01-1256 RovortEot-1256 Unextracted Callbration Curve Point [[032M0E0n5-v1i5r4o,nm2e5nptpalbLuanbexiractedcurve |do2030008Sm i,122) || PFOS: A Reproduction Study with the Mallard POS: ARepraStuddyuwitchtih oatna 06-Mar-2d00a2v,e104y:21:21 aarn 12 of 1CM hanneM alcEtSie.cd es | | | | | |er Too 2r 05 36r 5 4 60 660 760 86 5B ioms e | 3M Environmental Laboratory Page 138 001722 Report -- E01-1256 SEPFOS: A Reproduction Study with the Mallard Extracted Sera Calibration Curve E E CT rTE i EE VA I, eve . || | . i [| | / ! | bo | | L| mm ET a TEs S | ---- 3M Environmental Laboratory a Page 139 091723 Report E01-1256 tin 1106 Asc is PFOS: A Reproduction Study with the Mallard Extracted Liver Calibration Curve T CeEET Ey EroEEiwoo [Response type: External Std, Aree. vn on -| | IN | | | |- | { | | | oof Wi--re--se--t | | onc| sr ge 1724 Report EOL-1256 Rees Mass Spectrometer Tune Settings PFOS: AReproduction Studywiththe Mallard MesAR-- --m---- Tuning Method Report Ta --AB--A ------, I RTS Page 1 : PRE SLal Be gt 880 57 FE ane fRdh Wexagole 1 nse 98 "S8eebl "RP toh Ee ios Bou ao 03 04 E . res 1 [i Energy 1 Be Eove tdum wn 30 0b7on Le -5- oe 4 EnsironR mentEoborR sons rartion Page 141 2172 Report EOI-1256 Repo E011258 PFOS: A Reproduction Study with the Mallard PFOS: ARopraStdyuwi cBieMaotanr HPLC Settings Mano port Matheadsme:e: pric: Poon CoUnMdaA.SSarLoYN1X,D2A02VE4V01E0TP1ORTO0M ToeMarnch1d,2e0626y837,50 HP1P1ump0ni0n1GoLnoCs SBoaoveon & 0050 5 a ViVveAassastvoccaoernett SHoFeiprTiooivensi) ()oa) 03ox o GenTompaC mreROC) 400 HP1Pum3pO0ra0nTLraCe Toe adnTrottcons 5answhich re TTfeoeh 0wA%ss weoot coo px o003% oorswm i$ im $ Ssmo Gwdaooo 000005 0g00o0 oooxww POOLEPumpExternalEver Teta TheTeta corto tiowhich are: wTaBinrMa Col%OuFrn Swichaon wa a Cooonrotact Coaonrtac? CoOonoftac &a HP1100AosamilpConldifrona DEDprracmm:PSSoppoessniddoinm(im)) 020000 iVSanpicTNornrbVeorrliunmee,s a11000 TTrormoonmsOsTnorpoatreC) 10 3M Environmental Laboratory Page 142 51728 Report 01-1256 Reon01-1256 PFOS: A Reproduction Study with the Mallard FOS: A ReprSdtyiwich tho Moalnard Mass Spectrometer Scanning Parameters [EE -- rage 1 MiaihoM:eatesea: Co1n\AoSuSnLI3O8\O1A5T:E3Y0O:720478290.03PRO\ACTTDR\AOKEN- FOS PYDA princess oe dar 19 08:30:32 2003 Solvent Delay (mtan ) 0.00 mmctio+1n Ma of 3 XassPaix ( 569-) SsSpEnaacnreer(ciDmaaamteelniDneala)+y ( Seca ) 93.0%03 ReEpoeatTsam,Eeri( nwninpea)rent Daughter 5D3v6e0l0l (seca) Coll Energy (ev) 1 aseo moo 030 o ' Come (V) " motion +2 Max of 1 Nass Far (ESP) SISpnEatneTr (craihmaiemvee(lniDaneala)1y ( + Secs ) 0a5.0003 ReEpeatks,Eninne parent Daughter 53Dve%ll (seca) Coll Energy (ev) 1 sme meee 030 2 Cone (V) 3MEnvironmental Laboratory Page 143 1727 Report EOL-1256 ReponEor 1258 PFOS: A Reproduction Study with the Mallard PROS: ARepraSdyuwicneiMootanrd eP ro e eeet eee er. ATTACHMENT D: SAMPLE PREPARATION SHEETS 3M EnvironmentEarldLambaornatosroycio Pon scr218 Page 144 C1728 Rs SyBspa dB): PFOS:(gf ioba leaTAigiIMallard `Amoounrt of Hoimvoagteentrztesd|| Poegenzed weighed (0) (mi) | OOpppmpaeils22i1r0Fmivveerr |E|[E 094| | [F22o 5o2y 4]) 0ppm al 32M1Liv8er [eas T1111 [(Eot|-1O3pp2ma6i322200F 5ver83| [04484] ] Lb] [E0i-1326-20601| Oppmai3222FLiver [1.07 11 Som etE nH E0011--11332266-.2209664367 E01-1326-29673|" 01-1326-20691 0 ppm a.. 32F2Liv4er 00ppppmm 0ppm a.ai.i.. a. 33322226MMF22LLLiiiv75vveeerrr 0ppm a.i. 32F2Liv8er 0.ppm a.i.32M2Liv0er 0Opppmaa.pl. 33m223310FMLLiivveerr 0 ppma.. 3232 F Liver [lea|s1 e 1 1 11 | fl0et %0e2d, L H L rr L + L r ] [Losi] IIN[A E_-- es| [I 111 [feoqug 0) 1 --- rr 130 1 I 1903 Tl E01-1326-297[18ommaimsuie Loaf LL E01-1326-20727 0 ppm ai.32F3Liv6er gob 1 01-1326-26736 0 ppm a.i. 3237 M Liver [Tied| T| | E00111-13322662-290| 775445. SOpppomam.a.i3s2a30sMeLvreirner|H[i14j9m3o9s| || | |ee 1 E01-1326.26765| Oppmais2d0F ver [lads| | | | | | E01-132629772| 01-1326-26781 Oppma. 324iMiver [1 asda I pp [ote 111 1 1 sme LS E01-1326-20700 01-1326-20808 0 ppm a.i. 3244F Liver 0 ppm a.i. 32M4Liv5er EF ---- a A ---- 01-1326-20826 | 0 0 pppmom a.. a. 32M4Liv7er 32F4Liv8er [A i Br -- [eoEE00r11i.-11s3322g66s.-22e09885632||| C0Qoppopmmmaa.al..D 332521M FM5Liivv0L eerr ]f| 1e400e8s:s 11 1 E0[T-1E 325-2E 9o871f TOpI pmai szT szFTTvTeY r [o0G]lo | 1 || -- I] ---- E01-1326-2[088C9 ommas stiier | 1>4ug - 1 E0o1t--1i3s26s-2209080978 | OpPppma 3256F ver [[1i0A266s65| | 1| |a | . -- E01-1326-20816 10 ppm aii. 32M5Liv7er T10oppppmmaa.i..s32z6s8amF Liivveerr oes HHH11 [119/92345|0] 0|H a| -- [ F-- || E01-1326-29943 0 ppmai. 32F6Lv0er [1.13274 | (| |EEo0-1-11332266--2200095621| 100pppommaia.i 332266i2MFLLviveerr [3 |2(.3905,|| 0 ppm 32M6Liv3er os | |T 1 T 1| rT E01-1326-20080 70 ppm a... 3264 F Liver 129 FH E01-1326-29989|1 __0pp 326m 5M La iveri| |wv 1 J nN 3M Environmental Laboratory Page 145 91729 a ~ Repu PEOS: A Regios bedi) og 283 ue weAighOedUO(0f)|bgyiigdanteed| HoMO(mSiE)PZ2| homboyglednatiezed EE0011--11332266..3300000176|| 1T0oppppmmaali33226676FMiLveerr 10ppmai 326FL8er |[ [I[a0i4l 07|9|o U\\dg o|| [ o 7|0 | n|| 1 [--] ToppmaiseriMiver [1.0235 | | | {| E0E101-.11332266--33[000067o10 |mm1a0ipspm ea..u3t2Fh7Lei4verr 1/292 9, {I Hf--| -- | E01-1326-30079. Toppmai sersMiver 10 ppm a. 32F7Liv6er fLuR=e| || [| rege 1 |Eoi-iaze-s0067| [ot taze30t06 | t0ppmeais277mMiver f0ppmais2r8Fiver [[00G24| [1966s | [| | 1 I| | [[EE0011--11332266::3300171254|| 01.1326-30133| 111000pppppm. mmaa.i 3S322268r01oMFMLLLiivvveeerrr_|||/1,I.-000G36e37os{|| r a r 1r EE0o1i--1i3a26z:630011e521|| 1f0opppmpma3i 2zez6MFiLvi3veerr _|(.|t0o7ar5es | [I | |1 | | E01-1326-30160 EO1.1326-30178| 1w0 pppmma. 32F 8Liv4er 10 ppma.. 32F8Liv6er [[L1.LA09:Eoss]11 1 E01-1326-30167 01-1326-30196_ 10 ppm a.i. 32M8Li7ver LT 050g FH 28 -- EEo011--11a32266..3900221243|| 1T00ppppmmaa.ii. 332020MF8Livv9eerr Toppa 329iMiver | [ro2e5e12,g Tog4is ||( IT1H I |1 L | L || || Foioro s dotar| 1100ppopmmaa.i332028MF0Laiv2rer h0e47eseet |J--TH--| 1----| 1-- E0011-.11332266--3300226580| "Eoi-1367:37295| 0Toppppmmaa.ii. d3ze2dMF0lLivve5err 1O0pppmpma.a...9382FF8L0Lii3ve6err [ D 2335,L E | [o C | e g mmt m| g roL e ] dl n | |[.1204| 3 oi) |EoEto-111936677:-331133007|1| EO1-1367:31313| 0Opppmapima.o . 95s 01MFLo iLivveerr Opp95m02 aFLvier | l2o4co1gB| s | [1.030050 I I ||] 1+ EE0011--11336677--3311331295.. 0ppm a... 95FL9iv8er [lize 1 o. EH 71 |E"OE1o-11-316376-73-13313373|1 00ppppm a.mS966a0160MF.LLiiviveerr 3rr I E01-1367-31343| EE0o1T--1130677--3311938469 | 0ppma. 9573F Liver 100 pppomma.a.1. 96255MM7LiLvi8evrer [apg HoNE--1---- Eo1-4387-31362| f0ppmai o620 Fiver [\.1|GF|C>| E011367-313| 68 f70oppoommaai9ses6sFrLi3ivveerr4_|i.05ion511]| | 1 -- r(l --1 E01-1267-31360| 01-1367-31386. 10 ppm a19645 F Liver 10 ppm a.i.96F4Liv8er HT (1 Ee. E0011--11336677--3311339928| 1100ppppmma.a.1 9966MM34LLiivv62eerr [ploassetts HH l T] I-- ] E01-1367-31404 E011367-31410 10ppma.i. 96F5Liv4er T0ppmaivesoriver losic:g|V 1U r 1J r } 3M EnvironmentalLaboratory Page 146 21730 Report EO1-1256 SPE Columns Extraction Worksheet STRAIT lib Roytoals: OKHOS fez Shr Ea 4, Prost]eevee Ee rm]mmm lel.| Jorsmsorn |ossanany | ove Joma | wa fee| feovsomsern|wsssvensanys | os faves | sownfrie||| Jovumseres|vansvrs |efovea |soucomoresfrie | || Jersey |ommmwozmmbimeimt| ios fovesits |omscrommseframe || | Jersumosmres |crmmnatmmmt| rs foie |woosfrie|| | Jevssmanres |comment | is [oioass |auwcaonesfrie | || Jeorsomorne |cmmmmasemntmems| ou feiss| susiomonas frame || | Jism | cmmmntmnmnent| ry [sar |ousomoresfrie|| | leossmormn |oomrnommimens| psfvmsate | smoresfries|| | Jerson| ormrinmmnien| rs fviscts |sousmonesfries|| | Jeorssmoomo |ormrmsominimemt| ious fovisin | ooutomorasfree | | | Jeosmonma |omnis| sf | mosses fies||| leosmsorss [oommimmintrem| osJovian | womenfrome || Jerse| ommnsomntmont|e[oiisier |sousomonssframe ||| Jor smames |orm | ors [ozs | sousoams[ime||| leonrsmsors |omits| ips [eves| sousomonssfrome || | Jeors2ms0rsr Jo orto comcetns| sve _favinisn |sousomonssfrome || 0 | EE on MAGo Amott S051 OD 11 meriennoo a AE TET ra oun Caavriarnftutgtescaomplrtegfonr 1t0womiern @b520r000aramia(npCentecHaErIEnAiEnS FC omemo ge eoc narsrmooa retee,Scar te ole ok gavel (8 toroqensijsus, Roowasf,hidnoekge oo elora: oe 9 SCT oareecsouoo mmwieinscssr wrpaedpsma oortdattPsaFvOn tAestnaoHnOtHmo_ronAOST 4Te tosprmeee t15mpcatgaemaesind_Qpd 3M Environmental Laboratory Page 147 c21731 Ferderal| Raeype T12-]56 SPE Columns Extraction Worke"n0eS:oAt Re65lugHLA ba iththe Mallard RPreoypoeaste: as; sKHmOnU 40 SMeuthodNRoorisii:n:EEa75n.8es], [---- ecu i Cems| aomoms |ao[omar|ovoomms[lm || | eCeemovvmsmosooenrs|||e omomcsaoimrnr sie||woeroem PFfPomosiias [T|i momewe wommnfeshsn fieme|T[1T| e| mmm | ommeimine | oe Pmam whTT [Cooeormmmass|||oeomimmusmmroow [|| oeoo fmfaoamd| |wwa p r poem T|TT]T | FCooanme||oetrmsine|| oeFmear||wb[11 1] [FCiernoimrmmmemern|[|ooormmemnsisersie||| oooeo ffFouaos=e||Twwa fhferew| [[11 |] nes|ommemron| ePa|who TT a ey yor ow gH [oormmon| ommuismrow| wo foes | wa frome |W] aevar transi 4S DR Blank verTNA-GO2D_;Amoo fiveu r: 8n -05t9 _g oK ao 00)PMfoucpeuiaing WA mastaoi oT rESN HOT be Emon 200gon LAMeeEte pm-- `Centritugesample for10min @2000rpm(Centrivgeins16ACY merma ea--------------------oSAr3S , Fa Tcolua mnwhmiandr sincateadr aoarf odnopHaette LT EoD_) into appropriate15migcrentriugme ensionspl 3M Environmental Laboratory Page 148 091732 Report E01-1256 oBEl GOEece: ssi i ST =m PFOS: A Reproduction Study with the Mallard fA m . eo irra) FkFe adboop Locr 81011 EElrimz . ny Eonson Liss oa an ; me] Emi |B EEE] 3M Environmental Laboratory LaoedlToedelbp WsWad de Page 149 031733 Report E01-1256 PFOS: A Reproduction Study with the Mallard Bottle-Top Dispenser Daily Calibration Check Fiamacares andMode: Date: DBisapleIannnsicetreiIaIlDDs::: VolumSoelv(emnLt):: mi: VR, Sal uz o7k9 0s Ancaedtoinae 34o*0% - VoStoluvmeentof 7 a swewn 1 oommee ||ssoowm|| [ 5 seowwa wT|omoms ||asoime|| Cs [sem 1 om |som| [Rrerses|Vo5l0u52m4e|: [FAT camo]e TOO]| pass [ -- evoi || mss Value, "PerformAacnccueraScpye,cifications cv. ol) % eo Iwo-me| si%e | Corrective Aeon Noe pecpeD ` [24 24 "Densit,y va=lsuepsectiakiecngrfarvoimtytahteyMercCkrIenfdeerx,re1d2towEdaitteiorna,tCXopyrCight 1996 n-Hexane d%, =0.660 Acetone d*, =0.788 Methanol 4%, =0.7866 Methylene Chloride d*, =1.3255 Acetonitrile d,= 0.7857 3M Environmental Laboratory 00P1a7ge34150 mle Rogen BOL135 rraogse as.350.28 SPE Columns Extraction Worksheet "gh Bs lard Moth Reon: ETE: Shir SS aomiepamr|samp tarodren et nv SEEEET-- Jeomsons| onsvornsamz| ave Joris |ooomnafiime ||| [orm | wmsuerusomz| won proms |sosooomeaficoe |[| femmes| omarion | amefaves| wa few |[ [orommst| opmosmmeon | wn fewer| wa fees ||] fromm|opmasm |eJair | wa frm|[| formar| opmuismirine|aofem | wa fue ||] ferommms| opmaomsmuer| we fuvmiti | wa from ||] foreman| opmumorue| wofms | wa few ||] formmms| opmusoruver| woe fev | wa from ||] [ome| opmumorie| wo fumes | na fee||] oom | opmuimomue| wn fowmess | wa fee|] [ome |opmuvoroe| wo fovmss | wa few|] [oom | opmuimamue | on fewer | wa fms||] [eromam| omarion |wn loess | wa pues|| fermmmo| pmosoni | ow fasts | wa frme |[| fmm | opmuuriw | oe poses | wa foes|] | fermmom | opmusmie| we fuvmasr | wa free |] feorsmmnr| opmursmoroe| we [rumen| wa free 11 formas| ommuisomon |we ower | wa fee [J] sau vksrostamtsy 0 CSaonttioenAmmCKoof2tA04140G100s2030Gt7raseCdrVrReSNSI4T1E50413) enrveentsamtrettrhoaaohtro5er0sewipwpnrgp RnU8 oFanrsCameoBosmtaycaraoatetdccsno ,deci rs iSoroconbto aeceoelmapetsha#a7n PFeOnsOrHrT2!00C80)14i5, or1 tt 150 macamn t, sie24 Tarra isptedn tov 3M Environmental Laboratory Page 151 1735 Report EOL-1236 SPE Columns Extraction Worksheet TS,aris AnParloypsDtasten:tias:3-5o0i}2 [meLSeumpemrberorsoon SMeotohrodoRmeviiseinoEn&:rEgTS-8-231 maarntipn, l | veee| entd ers id [eves| ommuimorim|ae Joma | wa fee||| [erm] ommuismiuve| on fumes | wa from |] | [osm | ommusmrom| on Jimas | wa prem || | [commu] ommuismmim| ou fowmas | wa fem ||| [erm]ommeiomtrim| on Jovem | wa from || | [evan] ommuomuw| aefomas | wa free [1 | [orimanor| ommursmarim|asfms| wa freee || [ovmame| ommuisrni | aefrm | wa fre || [eovmms| tommusmrie| onfumes | wa fom || | [corms| ommermsonin | ou fumes | wa fom ||| [eorommn| ommsismrin | on fowmesr | wa frm ||| [corms| ommursmui | oofumes | wa frm |[| [comm] tommuismrie| onfumes | wa fom || | [comame| opnusonn| we fon| wa free[VU | [(--1 --1-- 1-- 1 -- = 1 1 1 1 1 I-- "1 11 [-- 1 1 1 rw 11 1 | 1 H[ arogen-- cs bt-- wihKa--ye w--o A-- udofvl 40d451 SKointsmdptetsercto r15 aap on ests ow 602 CoShnakteisgnp mfpo 20m1in0@3m002o0n0(3kmar(WCIaRkSeNOA1E3R0OS) OaveormteottaHrao ivtv50 me ip tet careie Cohaneosnankgenpty fMo sHre(pTeA t00c0 g VFoou sGoanee viehacororuadche, cade Ste Kiaowccoonntio cnodmtpeedtaeut f ha OSOHTHAO18) issl 15mcargo o"ItM EsnevisronmenatalrLatboiratPorTyA sd ontT0146core 101. am at 24 Page 152 691738 Report E01-1256 PFOS: A Reproduction Study with the Mallard Bottle-Top Dispenser Daily Calibration Check i "Manufacturer and Model: Due: Dispenser I: Balance ID: VolumSeol(vmeLn)t:: Ds: wee VR, SmL. aiso0z < 2 of 0 Amceaodn3iitdisle [tome[3509] Mass of solvent | Densiuw)ty | VoSloluvmeentof 7 sew | omy |sow| 3 2 [ss ew | |e ounmss | |a ssoomme|| a 1 sweem1 || oomm ||ssoosmo|| [FAccurs0c0y% || Pass [cv 0a 7] pass [aman] PASS] Volune, mL) PerformaAcnccueraScpye,cifications ) cv2. ew |wows| siow | eTCor Ri pe feeped! "Density values taken from the Merck Index, 12* Edition, Copyright 1996 &, =specificgravityoHaetxyan*e*TM6%r, =e0.f66et0orwarteeradt ewe Acetone 0, =0.788 Methanol 6, =0.7866 `MethyleneChloride %, =1.3255 Acetonitrile 4", = 0.7857 3M Environmental Laboratory Page 153 091737 Fe = et Report E0I-1256 pRroppoate;sls;36O0F8 SPE Columns Extraction Worksheet. pHagt Ul StMuedtyhodNRuemvbiseiron: ETS-g8- am Hn ve Matrix Liver tmerion ann [mmr | owmowms| wefar | wa pum (wn | lorsmsms | smauimsana| ws [oom love |woven] ave fosmid | smuomosfiime || |sioommaafire || | | lessons [romneouvne] oo [oma | wa fom ||] linmoon lovin |omnusmron] oo [omar| |tommmonon] we fomai | nw pom || wa fue ||] lovismoe |omaniomrim| oo [oman | wpm||| limos [romanouue] oo forma | lovin |rommsrorue| we fms | wa fom || wa fm ||] lors |tommsamuune] oo limos |omnniomrue oo [mar | Lami | nw ow fume [|] fom || | lov | omnumrerun| we fom | wa poms||| lovmsoms [omnes] we oman | lovin |romm crore] ae limit | wa frm|] wn fm|] levrsmson |tommermri] we loves |omnemmrun] wo omar | fom | wn fume |] wa prem |] | | limos [romommiomui| oe Jom | wa fmm [| loves Tommi re foie | wpe ruierisnaepcrhTwbHauA0rl2tt5krAiamsyepovfetnn,.re57t3 to 68 4 StSratneamasemarmapAeuaCsrNsogyod 2eo0rc1100sr 133002si h5tS0oamdk) rrAWlnSsSNOAETSES) Cea ca tcc iayanr ts3oese wiInvoerrp cogs on. oFenaiCaooa eetatncaooo TdHsAki),dca Josbiastippecitbuebsearsaotiatydof lOnesarGHrTH sAGC1)4i5,pcacp1001757mcaartigiidn24 Sa sms ast tors 3M Environmental Laboratory |] Page 154 21738 Report EOL-1256 re]= , 3603 Teen as. OK or ese Pee], SPE Columns Extraction Workshaet pms : mn onsas 76-2 i Var tier 125% neat oom [orm [ommmmron] [musi] po we Pamir | ow foo fom | wf [1 || Coos[omen] oe Fam | wn fw|| oorommoms [[oommmuummomrioonn]]owoe [Pammier ||w wo f fu | [1|) mm[mri] wefms orm [rommumnoe] me [ami | ow foe [1 | wf 11 omen[omumron] eormomn[rommumnon] ws we mi fom | ow Fm[|] | wn fom || oom [mmmsmroe] [eos[ommmmnoe] we[mdi | wa fmm || we fmt |wf || e| rm--[ereommuimoron]-- oof-- ms |-- wa Pm -- |V -- -- I --rr 1 =r T-- 1 -- 11 P -- t 1 -- 1 1 t ur ere TwarAtrKASentrpr eTaotEroa o0:5t70ftie 4 So anAmCeeNs(i2o0niaAny3000psrhi4readrs8iAsRSNOA160 e otevb1ie0i tnats2t00m0ii prCpaanesScWeT608e1) C oesnaoyta yn1 OHn rsApoGpeOT)rg e Foe ctoco ctoongn rar4a7tsrosiFh,OnS sanOdr HTioAnnIC)Al,s pcape1l0071 5,cTarrpsb8e824 IM EnvironmentalLaboratory Page 155 631739 Report E01-1256 PFOS: A Reproduction Study with the Mallard Bottle-Top Dispenser Daily Calibration Check Vamtacirer odMode: Dtuase:: DisBpaelnasnecreIID:: VolamSea(vmeLr:: my: VR woo 0s Apccauivyie 400o%J mp | VSoolvuentof 1 ewwweT|omoms |swomm )| wa | omy |sow| Ce s 1 sowmT Tomoms |Isstoamn | [irere|svS0m61e_:} Fass 7 Pass Vomllu)me, ew Accuracy, Performance Specifications cvx. [wo [ e sioxs| Comes Ro: Mome Jodlou 2!693 oK eane &, =0.660 Densityvaluestakenfrom the Merck Index, 12* Edition, Copyright 1996 @, =specific gravityaty*TMC refetorwarteeradt X**TM Acetone dy =0.788 MethyMleetnheanHoolrdi%e, =40.78=616.3255 Acetonitrile *, = 0.7857 3MEnvironmentalLaboratory 5P5ag1e714560 mle Peale] -- | ReportE01-1256 propose: OK Analysts intals: >7eR) samplenumber denctpton SPE Columns Extraction WoFKteetRega Method Rovision: siajMsiard ETS-8:231 `MSatutdyhNumberLi:veEr 0112:51% 32J0) =_ radar erro]swsiasans| [ovis| wmsiisoms| oe oo fromr|smoomorspize [mir|moomafm || || | | [Feoemnmmaams||_ooommneerissosmomriie|| oocofFmuamre| | w ow ppoe em | | |] } Mansa | Cooma] omneimmrow| oofmer omnersorruw| wo[mar |w | ow fom fre [1 |] Peovoroe] cmmuromrine | oofram | Ceonmmaime| ommersworue| os Fumie | ow ow fue |] foe |] eons |oomersmouine| Penman| ommermorum | 0fms | wpe ocfume | w pom ||] |) Ceocnmross| ommeromruw| Ceesromse]ommersmoumun | oo omar oo fumes | ow fom 11 1 | wpe|T} Fennoose| Ceoemmares] ommeromuon tommeroomrom | | oc oo bomen| mer | wpm |T | ow foe || Donen | Coormmspe| ommusrue | omneswsrun | oo we Frm | ow foe | 1 omer |wf [1 | | Coenen| Fammosrse| ommeimeron | wommerssoron| oo mar | ow fue |] oofume | wom [1 | emrmaren| rommosmuow| os Fomine| ow foe [1 | Dome] Comme] ommermmue |ae rommerssiriom | oo [oma Frm ||w wn ff om| [1 || Lenmomse]_mmersasrun | oofm | wee [VV] iFlaocnmkotgvetenmrzoTefHhaeAr0w2iiho3Ka1A5nmdipyo!aowufrVanrro.tA5lmo0e5ub8re7eo0fwale aded45 i SShpaiSknedssaamSpnAlpelCsKfcorc( 2a0rmdionT lyG00HapmnA eShsakea) rrVtRe SIN 41680) CDe1er5ct0ar4ni0tvegrsosfaKmaipoyfcaoann1v0v7agiern @ob25e00s0w0ipipheoa(ptCeprkercWaegTEeRE13b)e Caonovnacmop sigwhiyhloMseOvH(pTrH-o4p.e6r0i09g iithrCsaomaentoiutgKhaconryWooeenncr.oamd,Gea rts BArSdooeecseoawegimsr tccromrppt llcetoaaomnoduarrdfPsFOeAr a(nMdeaOHnTHu-Ar-B02003)0i14o5,pGpornos1t0e.71o5m,camaonunetadtdbeed 2 Shaner sme io sprprmaattedatvyl 3MEnvironmental Laboratory Page 157 o1741 Report E01-1256 PFOS: A Reproduction Study with the Mallard Bottle-Top Dispenser Daily Calibration Check Fianatactarer and Model IDnutel:: DiBsapleansnecre IIDD:: VoluSmoelv(emnLt):: mr VR wom w3e2 709s9 ors Acneatodniitdrisle [ave soi] Dejnsmit)y' | VoSolluvmeentof [w | e ems |sow | 3 | | somwa[| onomss |[ss0owasr|| som | om sos | Cs [s [oo m |m 5056 | LTIL [s Deval 0a 0025 | [Cv] 028] pass [FesFair] PASS | Voluse, PerformaAncccueraScpye,cifications cv. L) ew Twe.ws| sixos | Corrective Action: joe fred! 2 7= ox Density,va=lsupeestciafkiecngrfarvoimttyhate YM#e*rTMc=kC rIendfeexr,e1d2t*o wEdaitteiorn,tCxop4y7right 1996. aHeane %, =0.660 Acetone a =0.788 Methanol 6, =0.7866 `Methylene Chloride 6", =1.3255 Acetoniirlle &*, = 07857 3M Environmental Laboratory Page 158 691742 Report E01-1256 PFOS: A Reproduction Study with the Mallard Aachen: Dilsons SummaryWorksheet - soarE" o1 ns|o-- 18 Efa.f She umber: eseoaP[F3A6.02 BoxNumber: 7-3C MatrixTimepoint: ff ALLARD CIVER) pre orBescipton [igTuioo [uv[v_[v |v_[Commons [Verified By:| thon woe gy <ufh5 YTHE Gomes [x[| | Eomesoon [x [|| | [ | [ | | | [71[| | 7-1|| [owes[x || | | fomesorn [=[111 | | | |[7 [| [71 | (povmeaose[= || | | | | [7 [oovmessme x|| [|| | [7 TT 1 TT} loves (x | | [| | | [7 lovers[x | | | | | | Aw] 1| || | owes[x [4| | | [/lofla lowes (p= || | 7|| || | TT | [ovwewm x|wl| | 7/1 | | wmeswr = [|| [71[[ | [1 T1 | lowmewns x| | | | 4 | [eocesons | [|[71 [|[1| 1| Peomeowa(x | ||7 | [omens[x | | CL | | [|1 A= | 1 | | ium Notes: eoud_oa fsamle +ed a _of solvent toed- don, or he chy es aur Ty Ore eK {2802 SM EnvironmentalLaboratory FormCompletion Verified By:[AAA 4+ccvg B fog 12 Wotlals Page 159 01743 Report E01-1256 PFOS: A Reproduction Study with the Mallard men: DisSummaryWorksheet SR BtoaxyN:umbpeom rriass01c-o1r3p2a6clped relaaaAeorns LijeRe Semper orDescipton [ig[yy [Emer[x | T[uu_[u_[u_[u_|Co|mVmerietendyw: | TTTT [14a] oes Domes [=|| | | | [+||| | | || || 7/1[| 7 [1 oases =|| | | | | [7 osesmo[x| | | | | | 7 [1 | [| Domes [x|_|[| | [7 Eoomesonns [=| | | I 71 [| [1 oes =| | | Mommesma x||| | |A| [| | || ||| [names[x || | | / fob Does [=| | | 7| | | |1| [|| ossesaos [x|| | ~21 | | | 1 a -- r == r1r A1 rrr 1 Tr| rr eee] -- 1 110 ditio=n jogd_ofsample + F2 A ofsolvent 3M Environmental Laboratory ormComplionvein: EN tly (CIE Page 160 Gt1744 SBE 6 B 2urrer. PFOS: A Reproduction Study with the Mallard Mholyloa Sey US otfaifsn atiquated Diutedwith| auto rm I cee == E52) Tree| E0011-11225566..2288666643|| rsa oben Nae 45445-410-91-0382-18321P09P0,M,$F. FMeamalleo,. hdl At _|| o & 50 g |jguo sIzllEngd bot |Gs | || Te /7e6 |FIT. -- 01-1256.20665| 454-109-3220, 0 PM, Female, AdGiL 0.57 |Eot-izss20867| S454o-10p6-3a222, 00P3M0L}Ma tot F| o0.r50 I-- eo T 1] HE 01.1256-28660| _ 454-109-3224, 0PPM,Female;Adult Fei 1 1 0011--11225566:-2208667710||_445544-1-019-03922-6502P02EB7MPH,,,FMeamlaol,eAAdduglt |0-a 57 ||elo F01-1256.28672| 454-109-3228, 0 PPM, Fmale, Addl | g Sv| | | sf I -- -- [E01-1256-20673| 01.1256.28674| 454-109-3225, 0 PPM, Malo.Adull 454-109-302P3P0M,Female. Adu | 5-50 o, .5 = ve 1 EEOn1v-i1z2s56s.p20o6s7e5|| 01125028677| d44o5e54r4-t-1e01s520-33322-3305002,R3bP1BPMW,,FMMaoallnee.,eAAddpuualtl |gpsr |I 57] 2I2e 1 1 E01-1755-26678| 01-1256.28679| 464-109-52340, 454-106-3236, 0 PM, Female, Adit| PPM, Female, Adbt| 0-55 a 57 || 01.1256.28680| 454-100-3237, 0 PIA Whale Adu | 3 7 i. 7F 2 & h 8 B [E01 1256-26682| 4544-15003--521360,5-30203PP,PEMW,, Mal.Femal, AAddil | #x5_ E01-1256-28683| 45109-3240, 0PPM, Female.Adu | 0.5 | ZZoo o |EEo011--11225566..2268668854|| 45445-1409--1320429,-3P204PP1MP,,,FMeimlael.eA.dAudult| o0r. _ TI ee | EE000111--111a22355866.-.722888060888867|||45445544-4-11009-5--332124446,0,0O00PBPPM,PW-M,F,o3MMmaaall2leee,,,4AddAidu5lblt,|| oor- | | os | | | -~ | -- 0011--11225566-.2288669809|| 45445-41-10000--35224467,, 0P0PPWW,,FeMmoallee,,AAdduult| |g..1"_ 1 7ca 1 FF=00011t---11122255066.6-22a88s66m991a2|a||g45445-41t0-o91o-0s30224-s830,2l040P,0PPw.WA,PMFFoeMrmamalale,el,,aAAG doyt_|| 0.5 -- 7a 5 0. TfI4 | E01-1256.28604| EE0o11-11225506-2286660965|| 454-100-325], 45445-41-0190-53-23522[500, 0PRMP,MFMeimael,eA,dAud 0APH,Malo,Ack |5.P5"d | 0, IH) s A-- @ EE0011--11225560--2298669978||454-415049--130285-43]250O5,FPAM.| a apt [ooss =| w EE0o1r--11275568..2288679090||4--545-41-10089-3-25312, 506TP0]PPPIl Make Ao |oG.r Ie] |E0o1t--11228566:-2266770021| EovizsoaeT0s| 45do4ox-w1o0i5t-e3sa2as5s8a0,ji01oP0oMPuP,fFMoaemlme.aAoddpdit eSr r | os | |e- 7 - E01-1256-28705 [4s 54-10i 9.3261,f1o0rPrP,FeWmaallee,AdiAtdull | | 0.5 =.5 E0v-1255.78706| 454-109-5264, 10 PPH. Male, Ac 0c 7) -- z7z s 00 askk OFFFanos di|Te -- 111]| @ oasis28707]i FEo0v1-t122s5s6-2238770080] _s4k5.4-u1n0a8-s3o26f1400,pPwP.M. FemaMallee, AduAlt || " G76..2. ot 1356 870 450-105-3267, 10 PM Male ok| 07 | ||14 | =FiPp Bory Tasties #40 Prost Ccor TobDoiot mien, MS 2:00. 3M Environmental Laboratory Page 161 GUL74S "RRepnortB OLY zeman PFOS: @A ReeprdoducStioen StUusdySwHith the Mallard oe 2083 rove] een]Je ; aiiquated] Dilutedwith| aiuted [[E[Es0e1-12| |5645-r 4-21065-7a3z21e6d92, TH1DREEPHF,eMamlael(pAdyer | x sr Ft----17 |I I E01-1256.20714| 454-100-3270, 10FPM,Famale,Agul_| ox 454-100-3271, 1hpel,Malaladin | or 11 T | | IT} EE0011--11225566--22867711[65|as45e4-t1o00o-s3o2r7e3, 1o0pPpPMF,Neamlae(Aduukt|| <".5 " ||| L Hi |IZ || E01-1256-28717| 01-1256.28710] 454-109-3274, F10e PPMm , alAeul, t| 45445-41-019-0592-7362,71500,PPPMP,M,FMealmea,,AdiAdtvi | o-7-- i 0|g-3 F | i | F e--e 4H] E01-t1a2s5e6.s28a7r2a1o||--4s54w-1100595-0327778,1,0OPPPRMWL, FNeremails.dAadu |F 05 e |1 r | tIl EE0011--11225566.-2286772232||44554-4100--52160,011060PFP-MP,N,F3eMam2lael,7eAdAu9dtu ,|| 0.52 _ [ee TT 2 0E1O1--11226566-.2268772245|| _454o454--411-00910-0.3932-62263,52,81110T,0OPEPPMPPM,;I,FMeVarimlsaeel.,e.AAAdduduiutt | oa..5 |or [To e e] | |[ee IT |1 EE0011-.11225566-.2288772208|| 44554445--411-001900--933-223062468,,5,11001P0PEEPMMP;,M,FFMeeamrlarela,e,AAdgulAudtult | or||1 T %e-- e 1H 1---- ] E01-1256.26730| 454-108-3287,10PPM, Mal, Adult z [E01-1256-28731| 454-109-3288, 10PPFM,emalAdeu .| o> ee--H--] Te Tt EE0011--11226566--2286770323|| _ 445544--110006--3329206,8,1010PM, TY FefnalgA,d HEH 1 I E0E011--11225566--2288773354| 4a54s-1s00u-32r912W0,ePPeM,Fe eda {oT dt oo | TL fo {1 [--] [ze 171 |& co0r1-12265662-28677376||_ 01-1256-26738| d4s45k54-4-i-1010009-5-7-3032429,011501,9P0PbMPPM,W,FMMeaamlleae,, AAddauult | | 00.7-7|||| | 0.5 La od % n |E01-1256-26739| 454-109-3296, 10 PPM, Foal, Aul|t 5-7 E01-1756.26740|454-100PP9M,-Fem9al5e,O6fp3rin,g| >.> ITT= 11 || | Fo +L} @ E01-1256-6742| dsa-100-650. ) PEWL Female, Ofsing | 7:3 lo EO1-1256-28743| 454-100-905P5E2M,Fdiale,Offspring| 7.2 | E01-1266-20744|454-109-905PP9A, Ofging| 0: BD zo [| 2 EEEo000t111-1t1572i5556s60--s9a28s8r77ii44775||a44]dsbs5s111406o5-0-56s016e10700046P.,PPEE0O0M0RFWEPF-FUaNmLa9aorle6,.OO0aofnflts3prireiinn.nggg||| 00|o..g505 |||I| ]| JAC -- -- I ---- --- 01-1256-26749| 454-109-9576, 0 PW, Wale,Offspring | . 01-1256-26750| 454-109-9625, 10 HEM,ble.Ofpling | o.2 | [4 [--] fa [4 11 @ o0r1-215265.62-027875531]| 44455544---1110090-0999-69923964,.313110,00 PPAMN,, Cora, ee] FFermale, OOetfftsp,ring| L 60/. [110 171 H -- H -- & |Eo0t7--11725566-2266775554|| E01-1756.28756| 445544--11000-90-6946s,41510,0PPAN],E. 454-103-9636,10 FEM, FFeamamlae,,OfOffssprgiinngg|| Mle, 0 = o s [1 --1-- a -- Tple E01-125628757| 454-109-96412,0 RPM,ile, Ofeping| o E01-1256-28750| 01-1256-28759| 454-109-9654, 454-109-9659, 10 10 PPM,Female, PPM, Female, Offspringle Offspring -- test VV 122 TV 8 8 3M Environmental Laboratory Page 162 GeL748 Fel== eee] -- FagorB0N-1255 SPE Columns Extraction Worksheet GH Ry he Prop Dat 252002 Method Revision: ETS-$:2310 preva 0 oe stan arg pa pein foto horseooms [ounmuwomwant| avefom [| wm foe [1] for | pe m fmt | [o ous s || |a formoseme[miei | ve [mer || momenfreer[| |] loosen | mem homens | | ry [it|| swuomaefier|| | | | a fom || svenfrre || || lovee | eer hovmoseze | et | spe fom ||momsfrre \| || |efier |[sue frier|| |] formosa loro [a|efet | oe |e[met |[sem fiie (| | Lovaas|| || loves | Te lovmoseza [om |e mer | re fm || apsomosfiree || | | |Loss |||] hlovoseormee[ [ Tm |m ge ffoormme |[|g owsos effreree ||||s | || ] fl omosese | o e r | |g ee ffmotr|[[n vvemm ffrrrrz ee JJII| [ o | | lors [Tam lovrmomme fmm | ns mer || veo freer [| | | toefrm | | ene frre[1 |} lovmeoms: Jems bomen oormws || e ae f[ooere[Jo]weemnn[fRioeV [11V ] ares be ewtswuaat bri Dt rent 3E--n MSeetss7enrFutk BeisGs,oms,imss,tfien d OnC EI 05 weeps orpiatiugsridintarts eeTv anoSHI2201% ) year a o ne va e aOwHam t TAAe CSIE SFnoCurosamreod coun, dcr irks t Bs n aa or TScss caT nJooe. pmeuti,s 2 wl IM Environmental Laboratory SEE [=]m= Fleet]| Resort Bin-1256 Propoats; 425 OR Analysts inials: OK [OT eset SPE Columns Extraction Worksheet: lt 3a Orothl2 wood roll E75.82010 cerain MStauidynNumberS:eraE01-1256 on] trai |eovmssms| comms |ae former | Lwumunfrie[| || [ovo |oot |ae fom | ovina [[1 [moses | acumms |wn for|Jessa (1 [eons [ror|, i | [o[ or oo |,m femalow fee ||] [omens| Tomi | pe [me || wa fee|] 1] [Cooma [oom |p, fre [| ow fe|] | [emma | emi | os me || wa fee |] || [Cevmemon [oeeomermn|,Pome || wa fre|] [| [Cenmmm |Pm | wefom [| wa fee|| [eon[oom fe (| ow free[| [| [Cooma |me|a fewer || ow fee[|] [Comes[Tomer fome || wa foe[|] | [roman[orem fom [Cemomos| mi | wofume Rit rndvrotsr601262pmapnmountmosoTf swaairanntwot 4mTm prove TERE, 5] 1s0ammytarenwaat s801 poebrewspilnoenc0S4i69rh)HeEbe Deoacmeanetsenaxtmraeectmiostonwcentristfugre taubereserwoeirthi0wan ct1er0 RFeiaoehscCaoomoetewishcaeomsnpiWao5rttsekidn, duc Ta rasm tna ary aonssourlnon manSO C5 IM Environmental Laboratory || ow free [TC wa few P| | cre 10. Tots mrss Ged Page 164 01718 Report EO1-1256 EE pa gr i wm PFOS: A Reproduction Study with the Mallard mre tow. CEo TETTEE EIZ|E|E E = 2lE = EEE E [(=TETE 2 = EeaEe ii l Err[82] ETE TohUS oglaalon E H Er l T Opin 201749 Report E01-1256 PFOS: A Reproduction Study with the Mallard Bottle-Top Dispenser Daily Calibration Check anatacturer and fMoood DispensietraIlD:: `VoBlaulmaenc(emLI)D:: Solvmeint:: 2VWhSL 27 hojok 79 Ss oro Aaccdoinidisle mi) VoSotlovmeentof 3 7 swemw | | oemms ||ssoomo|] [ o | 3 ses | oow mme ||sseown] Cems | oms |sow] Volume, mL) [iwio [[ AcSma e]pvTo oOtIoL] E_|| pass [ wcv. 020 | pass [Pass/Fail] PASS] Performance Specifications Accuracy, 5) cvx. |wows| siox | Corrective Aeon: Api Aehed BAS 2-20 "Density values taken from the Merck Index, 12* Edition, Copyright 1996 &, =specificgravitHyeaxtayne=4Cr%e,fe=r0r.e6d60towaterat x**TM Acetone, =0.788 Methanol 0, =0.7566 MethAycleeonneiCrhtleori4d%e, d", =1.3255 = 0.7857 3M Environmental Laboratory Page 166 51750 = me Pears] repo ananz Report 031285 Anas ntiss: OKHOS SPE Columns ExtractioH n o rtacrgion a] dani Kos teSsw uo b SMtaudrycNumberS.ora01.1256 foros Jouromssamams| wo Juveme | U fewer| | formes umsseamsaz| we Jovi | mvemonfrome || | Joorassasen [=n | | ga fer|[ for[m Toes| a, me ||fe|] osemen |=], Joma || me[0] omen |"un | ee pws | | free |[| fpor|m=semon| Jove | | fee |[| Formsenen [Tm | on fee | Vee [| SvoorwesSorawoog TAw-LlOB1ES5v _maAAounct ptofoseairwaha sind348m0 3|) SGhweaneviesnasrmaeeit2f0oimr1in0mG3@0 001TwaErcaB nRt ,ey `T| Add40miofKandiyohiwaterto50mi polypropelenecentrifugetube. | C m nhC on e n aot yMaeoOt rHe s(n pHAen GrORt sD) Fou sariBehseed oe,ascit e O tSrahronesosrteiensnawmncaoetdnasyvueraafPFsrOhAesslao npottG 5TmDcAI agT hn "3M Enironmental Laboratory ne DT mrtsis F2n Page 167 "01751 Report EO1-1256 : PFOS: A Reproduction Study with the Mallard SPE Columns Extraction Worksheet oyref $e 0s olailoa oe]ey laren] PrepDat: 202002 Analysts initials: OKHOJ MethoRdelision: ETS-8.231 CoMa ersE01-1256 on] nani freemen |SEI| oofre| po fees wa | ormomer | ERIN|osfmm || pes [1 fomomon [SEER] osfmm | | fee | fovmomon |EIN| fm | | foes || fomomnn [S fmE m || A feme |[] forse | STINE | fm | | pes [| fosean [SRR]oo, fmm || fee |TO fosoans |SEINE | onhme || fee [TT formas [SO fmmR | |E fee ] |] , formes |Sn| wofmm || BE [| fone [SER]opMme || fue [7 foray |SERRE] oe fm | | fee | foams [SER] 0fm || FRE | foam | EERE | oefmm |VRE r 1 r 1[1 --1 | Tf TT goagZ +1 [P= akTT 1 + TTT + [--t----1 1 <I--1 1 1TT] DouintksuernTwoh K G22o ,AmAmooun unrtoewr sa tisstnsd__540 p hat mit asi15mpsopoainn aamraonnn Tumni 0H745myoe hduStAensLG6T 4 Bl `ACnotnctoniumgesnacmapc lnefoyr 10amr einrh@oo2r50s0we 0iprpmso(ipCernptifeugec2e4r2g96) @) csoinsnicroumwtiysberHepeonrGOhRyD WFraahsCroelnBwunhaornodtrsok, daca te dow cto comptes ty SoSkMeaEnovinronmmenatatl sLaabroirsatPorroynsaronommt TEA coe. 100Tem amortnoma 2d Page 168 G21752 Report 01-1256 PFOS: A Reproduction Study with the Mallard Bottle-Top Dispenser Daily Calibration Check Viamatacture and Mode: tDoue: DiBsapleannsceer IIDD:: VohumSoelv(emnlt:: yA VR ST 26 Febuary 202 709 Accn5iie makiss geo oJ Density ym) | VoSolluvmeentof 7 wwme oonms [sseowm]] T e m smT | om son] CwwT om [som] [RA-- ccurey| TOG | pass [-- %Cv.]"047 1 pass [Pass/FPaAiSSl]| VomluLm)e, Accu%racy, Performance Specifications cv%. iwi -- T o.i@%| +io% | Corres Reo Mone peedend ok L526) "Density valuestakenfromthe Merck Index, 12* Edition, Copyright 1996 &, specificgravityaty*=Creferredtowaterat 45 weaned, =0.660 Acetone 4, =0.788 Metbanl *, =0.1866 MethAycelteonneitCrhilloeri0d"e, d=*,07=815.73255 3M Environmental Laboratory Page 169 $91753 Report E01-1256 SPE Columns Extacton rk EE 2 gh [om][mm ember] PrepDate: 9X02 Analysts intials: 9[</ ra [ma] me Method Revision: ETS-8-231.0 H`SetuedysNumber: E01-1256. komen feomsars | 0 Lori |ovemmefier [1 kama [ fom || |fe|| fosmsme foes || Sl| ppee [momaer ||| ||fpmeee|| ST i> IPR 2I I + I fmf[ oovemae | reli |= pefPmrma| || |f] emwme | ||| | bef[ oavema | Sr = |ePommama re |||| ffemem ] [ [1 | omar bozos | rei | |e] goyef[mmam || we |] ||fee |] boson [oe RS [pe [| boon | Sri | oe[mac | | pee[1 ee ore R eanE A p a , a ge wip 1696S &[Decan axtct hocain besvinwater contree Aperme ma mreasaossmernSSTTIR ene 0 Tt, mss Gp) "IM EnvironmentalLaboratory o Page 170 01754 Bepon 20j-125 SPE Columns Extraction Workahest: ERE a]we pAnraolpysDtastei;nalA:XTFOO2K) mrss | ampere Pel tea] e| ase Sofi B SMteutdhyodNRuemvbiesri:onE:OE1T-S1-285.6231.0 [[Coommmer [ ryo = Gor eae|Lm fE e [] ----] [oom [seem mmm] Re [| fr [1] [[CCenomoem=arane[|m= ossm pr |e,pFeoeg| EE e 1~ me 17 [CCooromrmmmaams|[FEo EfEmm|,fohge ||1|ffaoee[7[7 [Cuommmeos|TE RE| pm efpmear|LeE er [| TT eeT e T TT F] ] Tp] T TT o1 1 T r | 1] ] r TT 1r 11 1 T 1] rr r r7 r T1] T ST 1 1 1 TT--1] lankSoraTNA-GOIA_:Amo ofsaura aniuattad: m eorbyoiemsraaBaTri67eg 4145 tom ar 8] `ACdanat4it0ugmesaamKpalnefyoorn10wmatienr @o25000m0ippmopr(oCepnetlrnieugce 2aHne76tAe.12 | Dacantextract intocentrifugetubeswithwater en gy WashColumnwithKandiyohlWater i TTSs,e cota Soikesamoleswith intemalstandard PFOAstandardnumber T1DA Leone. 10 FU amount acdea owl ge 171 21755 Report E01-1256 PFOS: A Reproduction Study with the Mallard Bottle-Top Dispenser Daily Calibration Check Vianalacturer 323 Pode TaDtuats:: Dispenser ID: Vo`lBuamlaenc(emIiD:: Sovmar: VRS 27 Febuoary 2002 7 0% wsw ggrel) Ancacodiivaisle Density ) | VoSolluvmeentof s C To e SawT TTo|ommom w msesr |ssseoeewnr7]]] C e SwwT T n 1oommsy ssoom]] [Sh-- earer] T0127|] pass Passa] Pass_] Pass @VaLlu)e, Tew Accuracy, Performance Specifications cv%). Two. T3108 Corrective Rei: lowe neede: oF `aa Deasity valuestaken fromthe &, =speciicgravity at Merck YP Index, 12 Edlon, Copyright referretod water at <4F 199 nexane %, =0.660 Acetone, =0.788 Methanol 0%, =0.7866 Methylene Chloride, =1.3255 Acctonirte 4%, = 0.7857 3M Environmental Laboratory Page 172 C31758 pRreopnoornte0:1-1122506 8 SPE Colllumns ExEtrxatcrtaicotnion WoWorr kERSsf Ra eprdiiot)RSE emai ard [re] me Analystsinitials: KJ pres [eee]| _ mn recA`Study Number: E01-1256 fom osnerenisone| oe Fmd [emf |] foumene Poet | wo fame|| hI omme iFooii |wPPoRP= ama |I| ffem[1 aI | bboouronmes F[ oie | eeff| rmmemr|||[pomme [[| bf omme o Poer || oeeafa fmmmm[|m ||fpome [1n bonne fl rd|NgP,R maC5e|| fm500[I || bI omen [5ommTM|PoO fCmile| | pm500 I ffoorme PPoosite || eeee Bfommear|[|| pfmm[|] boone ome | fmar| fm[1 fbf oomm for|e me fPrimmea ||||fpe mw[ [1 1] ] fom FE | eefi|Um[GU] Se T I o JA L n SeEnTIeI tnon esE e 0 38 SE a pama meters | L E aarS e aaaD t : aisote)SOs Fiersampte throughconditicolnuemnd, discarsingtitrate 3M Environmental Laboratory Page 173 Report E01-1256 PFOS: A Reproduction Study with the Mallard Bottle-Top Dispenser Daily Calibration Check Fiamatacrer Moa Ddaattes: DisBpaelnasnecreIIDD:: VolumSeoe(msmsLt),:: RS 28 Feary 20o02 k a aad Awcacdo3isnecsi Via oroven | Demsmty | VoSolluvmeentar 2 7 T Swe TToom mm |ssaomw]] [ a T Se e T Toommsym m ||ssooom]] C Tows omer | sows | [Rversee|Vo50l6u3m5 e:| PASS [S Dev.t 002d 398 | PASS (Passa PASS | Voalulm)e, hee5y, Performance Specifications cvx. iwi wo.wex| si0x | Correa Kon lode peedeD LHR OK, "Density values takenfrom the Merck Index, 12 Edition, Copyright 1996 &, =specificgravityaty**TM*C referredtowaterat x*** n-Hexane d*, =0.660 Acetone d*, =0.788 Methanol *, =0.7866 Methylene Chloride d*, =1.3265 * Acetonitrile d, = 0.7857 3M Environmental Laboratory Page 174 C21758 Report E01-1256 PFOS: A Reproduction Study with the Mallard er Sm me eons,427 AttachmenDt:Dilutions Summary Worksheet : EOL ent/TN Number: 724 Box Number: co). 1p Clr Matris/Timepoint: ALLARD alRf 7 SmpeNember |Diem] orpeertoter [ito Junon[v[vTv [uu]Commons |Veriiany:| [EETuRsEsasn7s0s0TExS |ITTTTA TT4a I EEE A 7I E[EEortEzseamn[x | rrr E[poEwtEzseasrosIExo[4[ I AZA7 I [[pEoovivssseeaamrwoss[[x=[[x7 |1| [|[7d /7[1 T ]| (e[Bootnitzssseeaawsnnao[vx|1[|T | [71||y |] [Ese [x |[T/ [|T | | em Tepe - [[BEoasntcaaseasm|s[H x [| 7/A 7 | | || [eNoovtiemseam[x [VU |Ftp OD DituNons Wee MADE ONme SAME Ages E<TRACTIon/ eR THe DA ok ZL To@ okeHOR, Form Completion Verified By[: SY 4. lez 3M Environmental Laboratory 6 Page \ob2 WS, Page 175 001759 Report E01-1256 PFOS: A Reproduction Study with the Mallard I `Attachment D: rare ents Dilutions Summary Worksheet SJ/EFS ST BDiolxatNionoDatme/Abn0al1eys1tr:26:C6,D MEaxtrT actioni Date/Am nalyse t:2.s 2.50 2seZmF,OR E rSectT ieon [F | i ToE To Tm o o p o y , o [vin| fC eorsesr m =TT RZ T ma FFIF omrEreoEmeersef |T = 1T H H r Teu] A C7 EC A EE i A mmea C[oomvisPseseEsasma+T1a2g[ TZ 7 Ffeev rP] iPtperatd T r Fr e r Te r r ae peten| ee Notes: 1/10dilution = 15 of sample + Qo21f) ofsolvent hoods: lo ofsu auptle + QR ulof solvent Form Completion VerifiedBy:Yd o) cop 3M Environmental Laboratory - Page 176 1780 Report E01-1256 PFOS: A Reproduction Study with the Mallard oe AttachmenDt:Dilutions Summary Worksheet Heo oa-sys BSDtoiulxduytNi:uomnfbDoaeltr.e/2Ans1l5y2s6tgE:,6R4T1-102, $[or1s 5 SoMElxvtaeraarctt/imTonNoDNatnuem/btAenraf:lysgHt:ono z[7RS A SompleNamber [| fF Therion Diwtons tT 1 Trp] r rr r TTTr Tr rr 1 r 1 FF TTTTT Hable 1 rr TI T ITTTrr1r 11 rr TA T T Tr TrT --71-- AT1711 A TT rF r ZZ r [= Noir --F 1-- 1TT F J -- TF ] Joosleborie 1/10dilution= _M__ pt of sauple + 1948 ofsample +_af of4 solv-- ent of loc. Bok 508 Form CompletionVerifiedBy: DAX_4: Foy > pp @ Pop Lf L LS allen Burs fons P7 Ser8fei,an oe Gir PR IM Environmental Laboratory Page 177 31761 Report 01-1256 Rep E250 PROS: A Reproduction Study with the Mallard PFS: ARapcStcywct iveaornd A ATTACHMENT E: STUDY PROTOCOL, PROTOCOL AMENDMENTS, AND --, DEVIATIONS 3M Environmental Laboratory Page 178 1762 Report EOI-1256 PFOS: A Reproduction Study with the Mallard PROJECTNO.: 454-109, WIOUFEILTDNTERMTION eoviAassL AMENDMENT TO STUDY PROTOCOL STUDYTITLE:PFOS: AREPROSTD UDYUWIC THTTHEIMALOLANRD PROTOCOLNO: 454/120700MR/SUBA54 SPONSOR:3MCorporation EFFECTIVE DATE: Jamuary 24, 2002 AMENDMENT NO: 9 PROJECTNO.: 454-109, EO1-1256 AMENDMENT ``Tnheicseasmsaeraytdomceonmtpilnecltuedtehseaannalayttaicchalmepahtas(eAotfttahcihsmsetnutdyA.)whichprovidestheinformation REASON: `Theprotocoldidnotincludeinformationforcompletingtheanalysesrequiredbythesponsor. AMENDMENT: Harold Johnson i the Principal Analytical Investigator REASON: `Thesponsorroquestedthat aprincipalanalyticalinvestigatorbeaddedtotheprotocol, AMENDMENT: The3MEnviroomentaLaboratory retIdeotification Number obinchedwiththesudyis REASON: "Thesponsorrequestedthatthe 3MProject Identification Numberbeincludedintheprotocol, 3M Environmental Laboratory Page lof2 Page 179 1763 BORER vx ao wrest ware smal: A Repohcion Sudsgi I] JAN. 23.2002 5:25PM ENVIRONMENTAL LAB 2 3E 08 50.5293 P 3 | Hi Woreiw p emn PT ROJEo CTG NO.:u 45R 4.1 e | i Ju 0. Lully . `SeanP. Gallagher, C aden Dae he Mtr oT || r Lory es t ma hba i] HA 5 Te We Gea ! Wi e IM er ( i lea= ns pos= = alonoeo Ta itl 1 . i i Biron bebossnny Pagezaf2 Page 180 001764 Report EOI-1256 PFOS: A Reproduction Study with the Mallard --N LWIOLDLLT FIFEE E INTERR NATIN ONAL,A LTDTIONPA ROJEL CTNOE.L :O041l5-4I m1-12s0596e,D SeanP. Gallagher,SdyDirector Dae "LTaobourmaaBt.oBreyaMvaernsa,geWmiendte lwerational, UTD, Da "Far0oTomson, Principal AnalyticalTavesigaior Bae "WiLlalboiraamtoKr_yRMeaangaegne,m3eMntEnvironmental Laboratory, Dae RocheRlRlobeideas, Sponsor's Representative Date 3M Environmental Laboratory Page2012 Page 181 1755 Report E01-1256 PFOS: A Reproduction Study with the Mallard Protocol Amendment # 9 - Attachment A Wildlife International Ltd. # 454-108 STUDY TITLE PFOS: A Reproduction StudywiththeMallard `SPONSOR 3M Environmental Laboratory Building 2-3E-09 PO Box 33331 St. Paul, MN 55133-3331 PERFORMING ANALYTICAL LABORATORY 3M Environmental Laboratory `BPuiOldBiongx23-333E3-109 St. Paul, MN 55133-3331 LABORATORY PROJECT IDENTIFICATION 3M Environmental Laboratory: E01-1256 `Wildlife International Ltd. 454-109 3M Environmental Laboratory Page 182 01768 Report EOI-1256 PFOS: A Reproduction Study with the Mallard Sponsor Study Identification PFOS: A Reproduction Study with the Mallard B3uMilEdninvgir2o-n3m6e-n0t9al Laboratory PO Box 33331 St Paul, MN 55133-3331 Principal Analytical Investigator ASNtAuLdYyTILCoAcLatTiEoSnTsINGLABORATORY ANALYTICAL TESTING LABORATORY Harold Johnson 3M Environmental Laboratory Building 2-3E-09 PO Box 33331 St. Paul, MN 55133-3331 651-778-6479 3M EnvironmentalLaboratory Building 2-36-09 935 Bush Ave. PO Box 33331 St. Paul, MN 55133-3331 PACE Tier2 1700 Eim Street, Suite 200 Minneapolis, MN 55414 APNrAoLpYoTIsCeAdLSEtXuPEdRyITMiENmTeAtLabSlTeARTDATE DAANTAELYTICAL EXPERIMENTAL TERMWATION 01724102 oaran02 3M Environmental Laboratory 2 3M Environmental Laboratory Page 183 651767 Report EOI-1256 PFOS: A Reproduction Study with the Mallard 1. PURPOSE/OBJECTIVES Ipntheeinrliffephlasueofothirssptouotdayso,smiauclmlsaatrldts(waPeFrnOeSr)eegiunltsahreliuyrefxelpeodisfneodrotdoennrotmoiaenvaaltlduoaesteest,ohfe e`fafneaclyttsiocaflpdiheatsaeroyefxtphoessutruedyupiotnoaqduualnttsiofvyePrFaO2S1i-nwteheeklpievreiroadn.dTsehreapofubrotphcooofnstthreiosland tdooxsiceodlmoaglilcaarldhsi.sTtohpeatahnoalloygtiiccaallriensfuolrtmsaftoiomntmhaeyibn-eiufseepdotrtoicoonomfpathriesbwiirtdhstudy.Theinlifeportionofthestudywascompletedat WildlifeInternational,Ltd.instudy 454-109. 2. RThEiGsUaLnaAlyTtOicRaYlpChaOsMePstLuUdNyCwiEllbeconductedin accordancewiththeUnit.edStates EnvironmentalProtectionAgency GoodLaboratoryPractice Standards,40CFR 792. 3. QuauryAssurance s`tTuhdey3cMoEnndvuicrto,ndamtean,taanldLtahboerfaitnaolryreQpuoarltittoy AdsetseurrmainnceecosmpiltiwainlcleauwdiitthaGnaoloytdicLaalbpohraasteory P`PrroaccetidcuerSetsa.nTdhaerQdusaalnidtwyiAtshsu3rMaEnncveUinriontwmielnltarelpLoarbtolraltfoinrdyinSgtsantdotahredOpSeproantsionrg RepresanedtnhetStaudtyDiirevctoer. 4. REFERENCESUBSTANCE 4.1 PhysicalDescription-PerfluorooctpoatanssieumssaultlfrfoomLnota2t17eis,a 4.2 hPaurshbteyenasnhdoSwtnabtlolbletys--taTbhleepiunrmiettyohafnLooltso#l2u1t7iohnassfboereunpdettoe6rmmoinnetdhtsoatbaem8b6i.e9n%t. PFOS IntsetmpreurmaetnutrDeietnetchteivoanliLdiamtiitonDreetperomritnfatoimosntfuodryLPCS/OM1S3a,n"MdeGtCh/oMdSVAanliadlaytsiionsaonfdF.C807 CCoonmtproolu,nadnsdiRnefMeertehnancoedla.t"aRbeafseeritnotthheeC3eMrtEifnivciartoenomfeAnntaallyLsaibso(rsattoorreydi)fnotrhfeurTteshte,rpurity and stabilityinformation. 4.3 StorageConditions--Thetestarticlemaybestoredatambient temperatureorlower. 44 2R0eseCrv5eCSoarmpcolledser--aAndreissekrevpetsianmtphleeo3fMPEnFvOiSrfornmoemnLtoatl#La2b1o7rhataosrbye.en frozenat 4.5 CASNumbeCrAS--nTumbherie: 2795.39-3. 4.8 MwoelieghctuolfatrhWeealnigohnt--(TPhFOeSm)oilsec4u9l9ar(CwaeFigShOti)s.538 (C4FirSO:K). Note:Themolecular 3MEnvironmental Laboratory 3 3M Environmental Laboratory Page 184 1768 Report EOI-1256 PFOS: A Reproduction Study with the Mallard 5. CowTROL MATRICES Ttryapceeasbiolfictoynnturmoblemrastwriiclelsbesrndecthoeridresdoiunrtchee,rphaywsdicaatladaenscdriinpctliuond,esdtionrtahgeereiqnaulirreepmeonrtts, and 6. TestSvsrem `TWhieltdesetIsnytsetmeamtiisontahleLmtadll.adrudr(inAgntahsepilna-tfyirfehpyhnachsaeso)f. tThhisestteusdys)ywsitetmhwfoaosddporseepadr(eadtby mpipxminlegvPelF.OSAfwoiotdhfdeoesdeivneraifliacragteimonixvaelriidantaipopnrsotpurdiaytweapsorpteirofnosrtmoeadchbiyeWvieltdhleinfeominal 10 InVteerrinfaictaitoinoanlfuonrdtehresDteutdeyrmniunmabteiorno45f4PCF-O11S0i(n3AMv#iUa2nD7i2e3t)", "WAinladllyitfiecIanlteMrentahtioodnalverified pthhaesacetrueaplodrot.seMdalfloaorddfsoerrhuimssatnuddliyvaenrdstahmeprleessulwtesrweiclollbleecctoendtbayinWeidilnltiheeIinnt-elrinfaetWiiolndall,ife Ltd. andsentto 3MEnviroLabnormatoeryfnortanaalyslis, 61 MJaulstliafridcdautcikorneporfetshenetSweilledcbtiridopnoopfultathieonTseasntdStyhesytaermean EPArecommended. msapterciiecsebsefcoratuhseetsthuedyydios wteoldleitneramlianbeoirfatPoFryOeSnwvairsodnempeonsti.tTehdientusheeoifvtehreasnedserum `hoaftmcahltiinnggsawduilltsdettheartmwienreieffoPdFOPFSOwSa.spFassuedorntotmaanhtailynsgeiasdourfltthsm'eosfefomsaptrrriingc.eesfr,om 7. SOURCEOF SUPPLYFORTHETEST SYSTEM `fTohreibnifrodrmsawteiroenoabbtoauitnebdirbdyoWriilgdilniafteioInnltoecartnioant. ionLatld,. Seetheirpro(tstuody c454o-10l9) 8. SPECMENANDSAMPLERECEIPTANDMAINTENANCE ESnevriaraonndmleinvtearlwLearbeocroaltloercytfeodrbaynaWliylsdilsi.fTeIhnetem2a1t-iwoeneakle,nLdipdo.ianntdsserhaanidptliovtpehrseea3mdMples receivedbythe 3MEnvironmentalLaboratorywerefromthefollowingbirds: 4400ceoxnpterroilmeandtualltbaidrudlstb(i2r0dmsa(t2i0nmgaptaiiargsp)atihrasti)tnhgaetsitnegdefsotoeddcfoonotdaicnoinntgai0npinpgm1P0FpOpSm PROS 20firstgenerationoffspringbirdsthatingestedfoodcontaining 0ppmPFOS `dSameplsescwiinrltlbhieemmbeaitenhtoaddi.nTedhferoszaemnpelxecsewpitllwbheeknerpetmoisvoeladtfeodfrreoxmtrtahcetitoensatsnudbasntaalnycseidsuarsing storage. 3M EnvironmentalLaboratory 4 3M Environmental Laboratory Page 185 C01%r Report EOL-1256 PFOS: A Reproduction Study with the Mallard 9. SUB-CONTRACTEDANALYSIS 81 pAelrlfsoerrmaeadnadtliPvaecreexTtirearct2i,on1s7a0s0dEeltamiSlterdeeitn,thSiusiptreo2t0o0c,oMlianmneeaopdomleisn,twMiNllb5e5414, 92 Aaltl3sEMenrvaiarndolnimveenratnaallyLsaebsoarsadteotrayi,lBeudiilndtihnigs2p-r3oEt-o0c9o,l9a3m5enBdumsehnAtvweinluleb,epSte.rfPaourlm,ed MN $5106. 10. EXPERMENTAL CONDUCT Tahnael2yz1e-dwfeoerkPeFndOpSoqiunatntliivteireasnudsisnergtahseammpeltehsordesceliisvteedd(bseeleoswe.ction 8)will' beextractedand 10.1 ProparatoryMethods 10.1.1 UEsTiSn-g8H6PL,CE-xtErlaeccttiroonsopfrFalyu/oMraoscshSempieccatlroCmoemtpryo.undsfromLiverforAnalysis 10.1.2 UEsTiSn-g8H4P,LECx-tErlaeccttiroonsopfrFalyu/oMraoscshSepmeicctarloCmoemtproyundsfromSerumforAnalysis 10210.2.1AnaElTySt-i8c-a7l,MAentalhyosidssofFluorochemicalsinLiverExtracts Using HPLC10.2.2 EETSl-8-e5,cAnta/lyMrsaisososfSspPeopcttarrssoimauemtyrPyerfluorooctanesulofroOntahteer SFpleucotrroocmheetmryicailsn Serum Extracts Using HPLC-Electrospray/Mass 11. METHOD VaLoaTION CMeentthroedAvnaalliydtaitciaolnLfaoborrPaFtoOrSieqsu,aInntict.aitnisotnuidnym0a2l3l-a0rd4s4e.rTahaendmleitvheordwawislplebrefaoprpmleideadtto sampleanalyses withoutadditionalvalidation. 12. DATAQUALITYOBJECTIVESDURINGSAMPLEANALYSIS Tlehveelfsodlleowtingecrritiemnrsieiacwtinilloebne1d1m:etusingthevalidatedcalibrationlevelsandfortification 121 SSyysstteemmsuSiutiabtialbitiylwiiltlybedeterminedpriortothestartandatthecompletionof `reuancthharneael(y3t)miircdua-nll.ePverliuonretxottrahcetceadlciablriabtriaotnicounrsvteaandnadradfstweirltlhbeelaanstalsyazmepdl.eoTfhtehe `pmeoankiatorreeadpartetcihseiboengainnndirnegteanntditonhteiemnedporefctihseiornuannsedppaeraatkealsyy.mTmheetpreyawkialrbees tpirmeceimsuiosntmbuesetqbueaelqtouoarlltoeosrstlheassnt2h.a5n%2R.0S%DRaSnDd,tthheepperaekcaissiyomnmoefttryher(eftroenattiingonor styaisltienmg)smuiutsabtibleit0y.fa5i<lsA,F<sy2s.t0e,mwmhaeirneteAnFainsctehmeuasstybmemceotmrpylfeatcetodrp.rioIr tforiutanenmionngftyah.e 3M EnvironmentalLaboratory 5 3M Environmental Laboratory Page 186 i1770 Report E01-1256 PFOS: A Reproduction Study with the Mallard 122 123 se`csontdstaehterocaftlsiybisrtaentmiosgnu.itability samples andthe system suitability mustpassbefore Calibration It willconsistof a minimumofnine (9)levels,including ablankwithsurrogate and a blank without surrogate,theloweststandardwillbeat approximately 50% ofthe LLOQandthehigheststandardwillbeapproximately50% higherthanthe ULOQ. The standard curveequationwillbedeterminedbyregressionanalysisusing the peak areasof the analyte. Theaccuracy ofeachlevelwillbeverified.Anylevel T`ohutesicduer8ve0m%us-t12ha0v%eacaccourrraeclaytmiuosnotbfdeetdeeramctiinvaattieodn, a(ngdrreeagrteesrsitohnarneo-rcaelqcuualaltteod. 0".T9h8e5t,otAalllnulmevbeelrsmoufssttasnhdoarwdsaerxecslpuodnesdegmryeantoetretxhacnetedw2o0t%im.eIsfthtahteopfretcheedbilnagnk. ciiterionarenotmet,thecurveand samplesetwillbe reanalyzed. LiomfQuiantittatsion (LOG) `Thelowerlimitof quantitation(LLOQ)wasdetermined to be 10ng/ginliver and 10ng/mLserumduringthemethodvalidationasdescribedaboveinsection 11. TheLLOQmaybedeterminedtobehigher thanthatfound inthe validation study during ascreening tobedoneforendogenouslevelsofPFOSintheblankmatrices available at 3M EnvironmentalLaboratory.IfendogenouslevelsofPFOS are foundtobehigherthan theLLOQor ifthelevelsarefound to behighlyvariable, the LLOQwillbeadjustedtoaccommodatethis.`Thescreeningproceduresand dLaLtOaQaswdeeltelramibnaetiinognrweiplolrbteerdeicnotrhdeefdiinnalraenpootrett.oRefciloevaenrdykfeipctiweintchytahtetrhaewLsLtuOdyQ `willbedeterminedduring eachrunusing anextractedqualitycontrol sample l`odsupwirekiesndtgaaptartsuhsnei,ntLghLqeuOLaQlLiltOeyvcQeofln.otrrItofhltsahatesmqpupealclieifatinycdcraounnntwyrosoaulmslpadlmbepeslcbeoeanltsoitwdhteerhLeeLdntOeoQwblLeetvLehlOefnQaeimlxustst bereanalyzed `Theupperlimitof quantitation(ULOQ)wasdeterminedtobe 250ng/giin liver and250ng/mLinserumduring themethodvalidationasdescribedsbovein tsoecmteiaosnu1r1.erAecnoevxetrryaecftfeidcqiueanlciytaytctohnetUroLlOsQam.pIlefstphiekqeudalaitttyhcoenUtrLoOlsQawmiplllebaetutsheed 'ULOQ failsduring aruntheULOQforthatspecificrunwouldbeconsideredtobe tUhLeOneQxmthuisgthebsetrpeaasnsailnygzeqdu.alitycontrolsampleandanysamples abovethe new Anysamplewithanareagreater than thatofthehighestacceptablestandardwill inneteodtthoebreandgieluotfetdhienctourtvheerdaunrignegofantahleycsaelsiabrnadteionnocuugrvhes.amIpflsearmepmlaeisnasr,edaiploustte-drun ddiilluuttiioonnvvaalliiddaattiioonn,woinllebseapmeprlfeowrimledbteosveeprairfaytesdaimnptloetvwaolureesp.rTesoepnteartfiovresmatmhpeles 3M EnvironmentalLaboratory 6 3M Environmental Laboratory Page 187 691771 Report EO1-1256 PFOS: A Reproduction Study with the Mallard s(aGmep.ltewso)t1hmeLndailliuqtueodtussfionrgftlwuiodpsraomcpeldeusroers.tTwhoe1fgrrsatmpraomcoeudnutrsefcoornstiisstssuoe f diwhhitlientghtehseescaomnpdlperowcietdhuardedciotniosniasltmsaotfrdiixlpurtiionrgtthoeeextxrtarcatcitownit(hsesroalavdednitnpgossetr-a), extraction (methanolextractaddingadditionalmethanolsolve). dIefttehremvianleuewshaircehnvoatluwietshian1co5rr%eoctfreeparcehsoetnhteatriaodndoitfitohneasltaemstpilneg willberequired concentration. to 124 CAonnutnienxutriancgteCdamliidblreavteisotnaVnedrairfd(iccoanttiionunisngcalibrationverification --CCV)will cbaleiabnraatliyoznedcaufrtveer).evTehrye1ac0ciunrjeacctyioofnsth(setaCrCtiVngamfutsetrbtheewliatshiinn2je0c%ti.oDn aotftahmeayonly bceraeploirtbedcruiarfbvrteapicokioenttn)e.dbDyaptaasbsriancgkeCtCeVd'bsy(oonreaoCrCmVoarnefdatihliensgaCmCeV'lesvmelustbe: reanalyzed. 125 QuAamliintimyuCmoonfttrhorleSea(m3)pqluaelsitycontrolsamples (QC)willbepreparedwitheach saentaloytfes.aTmphlees.leTvhelesyarwei:llconsistof blankmatrixspikedwiththreelevelsof LMoiwd-leevveell:attthie LtmLhOeLQeL(O1sQ0,ng/mLinserumand 10 ng/gin liver), Highlevel: attheULOQ(25timestheLLOQ) 126 EQaCchPeQrCfiosrexmpaenccteedCtroitsehroiwaanaccuracyof 80-120%ofexpected. Aminimum boefr2e/-3anoafalylzleQdCormrues-temxtereatcttehdes(eascdrietceirdiea.dIbfyntoht,etShteuednytDiirresecatmoprl).esetmusteither 127 UCosnefiorfmatCoornyfmiertmhaotdosrayrMeetytpihcoaldlysnotneededwithLC/MS/MSanalysis. 128 PDFeOmSosnpsetcirfaitciitoynwoiflbSepseucbisftiacntiitaytedbychromatographicretentiontime,bythe characteristicprimaryion LCMSMS. (499), andthe characteristicproduct ion (99)using 13. SuB-CONTRACTEDANALYSS 73.9 A`llpfleuidraafntdoPtaircsesmuTeieeerx2tdr,a1ct7i0o0nEsalsmSdterteaeitl,eSduiintteh2i0s0p,rMoitonconlaemaenpdMomNeln5it5w4si1,l4l.be 3.2 A`lpelrffuorimdedanatd3tMiEsnsvuieraonnamleynstesalasLadbeortaitloerdyi,Bnutihldiisnpgro2t-o3c-o0l9a,m9e3n5dBmuesnhtwAivlenlubee, St. PaMuN5l51,06 3M EnvironmentalLaboratory 7 3M EnvironmentalLaboratory CoRgyms Report EO1-1256 PFOS: A Reproduction Study with the Mallard 13.3 PLaabcoeraAtnaolryytSitcaanldarSedrvOipceersa,tIinngc.PrwoicleldfuorlelsoawndatlhlefapopllliocwaibnlgeP3aMceEnAnvailryotincmaelInntca.l PSStaSn-dAadrmdiOnp-e0r1atiQnugalPirtoyceSdyusretse,m PSS-Admin-04 PSS-Admin-06 Laboratory Facilities Training Record Files Maintained by QAU PSS-ARC-02 PSS-ARC-04 ADirscphoisviitnigonDoatfaA,rScpheicviemMeantearnidalLsogbooks PSSDC-05 PSS-DM-03 LStaabtiNstoitcealbEovoaklsu,atLioognhoofoDkas,taand Phone Logs PSS-OPS-01 PSS-OPS-02 RUsaewaDnadtMaaintenanceofUltra-Turrax T25 Homogenizer PSS-OPS-03 PSS-OPS-04 Hazardous Waste Disposal Use and MaintenanceofN-Evap Analytical Evaporator PPSSSS--OOPPSS--0056 UUsseeoafndCoMmapirnetesnsaendcGeaosfeNsAiNn OthpeuLraeboIrIaWtaortyer Purification System PSS-OPS.07 PSS-OPS-08 LClaebaonriantgorNyonC-adlciuslpaotsiaobnlse Volumetric Pipettes PSS-OPS-09 PSS-OPS-10 ADneavliyattiicoanlsDferfionmitEisotnasblished Procedures PPSSSS--OOPPSS--1I13 UUsseeaannddCMaaliibnrtaetniaonncoefofaBLoatbtlRee-frTiogpeDraitsopresn,sFerreezers, and Ovens PSS-OPS-14 PSS-OPS-IS UGlsaesasnwdaCraelCilberaantiinognofSyringeswith aHamiltonChaney Adapter PPSSSS--OOPPSS--1167 UUssee aanndd MMaaiinntteennaanncceeoofftUhlterFaissohneircSWcaitenetrifBiactIhssot(eSmonpiFcraetoerzse)r PSS-OPS-18 PSS-OPS-24 UUsseeaannddMMaainitnentanecenoofafaVnoDrcetseeixccSahtaokrers PPSSSS--OOPPSS--3312 OUpseeraatnidonM,aiMnatiennatnecenoafnaScnhdeakCearlsibrationofLaboratory PSS-OPS-37 Operation, Electrodes Maintenance, and Calibrationof pH Meters and pH PSS-MC-01 PSS-MC-02 PReucrecihpatsoinfgLoafbLoarbaotroartyoSruyppSluipepslies PSS-MTR-01 PSS-MTR-02 CalibrationofCertified Weight Set CalibrationofCertifiedThermometers/Thermocouples PSS-MTR-05 PSS-MTR-06 CalibrationofEppendorf Pipettes VerificationofCalibrationof theEppendorfPipettor PSS-MTR-07 PSS-MTR-08 VNeeriwfEiqcautiiponmoefnCtalQiubarlaiftiicoantiaonndU(IsQe,oPfQA,n0alQy)tical Balances PSS-M:TR-09 UMosneiatnodriMngaDievnictesenofaFnischeerScientificElectronic Temperature PSS-Safety-01 PSS-Safety-02 General Use and Laboratory Safety Maintenanceof Biological Safety Cabinets 3M EnvironmentalLaboratory 8 3M Environmental Laboratory Page 189 631773 Report EO1-1256 PFOS: A Reproduction Study with the Mallard PSS-Safety-04 PSS-Safety-05 UEmseeragnednMcyEavaciuatnioonfPtrLoacbeeordauntroersayFunmeHcooeds PSS-TS-01 TrainingProcedures 134 A`pnearmfoernmdedmaetnltatboortahteorpireostootchoelrwtihlalnbtehwerPiattceenTiifeerxt2raocrti3onMsEannvdiarnoanlmyesnetsaalre Laboratory,respectively. 14. STATISTICALANALYSIS SEtxaatimsptliecaslomfetthheocdaslwcuillatbieolnismuisteedditnotthheeacnalacluylsaetsiwoinol fbmeienacnlsuadneddisnttahndeaarndadleyvtiiactailponhsa.se report. 15. Repor foAlflionwalarlelpGoLrtPwrielqlubierpermeepnatrse,dabnydtwhilel3inMcElnuvdeiraodnemscernitpatlioLnaobfoarlaltmoartye.rTihalesfainnad rmeeptohrotdwsill sed,including anarrativediscussionwith atabularpresentationofallanalysesresults, 16. LOCATION OFRaWDATA, RECORDS, ANDFINALREPORT `Whenthe final report icompleted,all origina paperdaa,includingprotocol,phase anraeployrtti,csatluddaytcao,wrrielsbpeonrdeteanicnee,dsianmtphleearreccheiivpetsaonfd t3rMaEcknivnigr,osnammepnlteaprleLpaabroartsitoonr,ya.nAdll `correspondingtraining records,calibration records,instrumentmaintenancelogs,standard T`oipeerra2tiongtphreo3ceMduEresn, evquiipmrentLoparbooncreadmtuorreeys,a,nasanpdtpmleicatahbollde.s willbe retainedeither at Pace 17. SecMENRETENTION aSnaamlyptliecsalosfttahnedtaerdsstswuiblsltbaenmcaei(natnayilneefdoivnetrhceolnatbroorlastoerryfoorlriavpeerrainoddsoafmtpilmeesa)sasnpdetcihfeied by sraegmupllaetsiownilolrnaostlboengmaaisntthaeiqnueadlmitoyroeftthhaenpr1e0pyaeraartsiaofntaefrftohredseefvfeacltuiavtedioant.eoHofwtehveefri,naltest rule if #pply to asppalmipcalbelre)e.te3MnEtnvtiiiomreonsn.mentalLaboratory StandardOperating Procedures also 18. RereReNces 18.1 Wwildti ifheeMItanltleamh radt"i,onal, Ltd. Protocol No. 454-109, "PFOS: AReproduction Study 182 MCeetathroedAsn"aElxyttriaccatliLoanboorfatPoortiaesss,iIunmc.PSetrufdyl0u2o3r-o0o4c4,a"tVaanliedsautiolofrnooOnftahAtneaerlytical FuEorolcheemiccaltCoSmprepcoturonodmsesFtrryop"amSnerdr"Euxymtfroa/crtAinoaMnloyfsaiPsoUtssaisnssgiHumPLC AnPaleysirsUsfinlg HuPLoC ElreocortrOotoshpercrayF/ltMuaosrasocSnhpeemceitcroasmlCetourmyp"lionunMfadlsloFarrndomSLaeirvutemrafneodr Liver" 3M EnvironmentalLaboratory 3M Environmental Laboratory Page 190 e017 Report E01-1256 PFOS: AReproduction Study with the Mallard 18.3 t3hMeSDtuedytU2e723r,omWfilPidFiOfnSeSiatnuAdtvyia4in5D4oiCe-t1n.1"0, "AnalyticalMethodVerificationfor 19. PROTOCOLAMENDMENTSANDDEVIATIONS SPltaundnyeDdircehcatnogreastndotthheeSprpootnoscoorlRweiplrlebseeintnatthievfeo.rmAofmwriettennawmieldnldbmemecnotnesssidiegnrneeddatbsypstahret foofrtmhoepfrwortiotctoenladenvdiwaitliolnbse,astitgancehdebdyttohteheSftiundaylpDriorteocctoolr.aAnndySoptohnseorcrhRaenpgreessewnitlabtievienatnhde filedwiththerawdata.Allchangestotheprotocolwillbeindicatedinthe inalreport. 3M EnvironmentalLaboratory 10 3M Environmental Laboratory Page 191 21775 FOGA931- 12565 FAL 410 8220832 WILDLIFE INTERNATIOREOS: A Reproduction Study guteMallar WIWILLDDULIFFEIINNTTEERRNATIONAALL,,LLTTDD eorlass PROJECT NO.: 454-109, E01-1256 AMENDMENT TO STUDY PROTOCOL . STUDYTITLE: PFOS: A REPRODUCTION STUDY WITHTHEMALLARD PROTOCOLNO.: 454/120700/MR/SUB454 SPONSOR: 3M Corporation EFFECTIVE DATE: Jamary 30, 2002 EET AMENDMENT NO.: 10 PROJECT NO.: 454-109, E01-1256 REASON: ``cTohmipsalemteenthdemeanntianclluydpehstaasnieaoctftaathclihsmesnttud(yA.ttTahcihsamtetnatcAh)mwehnitchArporpolvaicdeesstuhpedaattteadcihnmfeonrtmaAtiinonanmeccaedsmsaernytto9 ; ``uTphdeaatmetehneddmaetnatqu9aaltittay cohbjmeecnttivAesw,aasnudptdoactheadtngoietnchleuldieveardainfdfesreernatcexxttrraaccttiioonnlaoncadtaizoanl,yticalmethod, to - Scan P. Galagher, . Study. Date Soo, TE o,A WUEE-- rematiT ons, L-- TD, -- Laboratory Manage Fhrold 0. TobnaoeP,mipalAnalytical Ivesigator er. p= =D) eM `William K. Reagen, 3M Environmental Laboratory, een = oc/nloz. 01/5) fos Date. 9/314 . 1of9 3M Environmental Laboratory Page 192 Co1778 Report EOL-1256 WILDLIFE INTERNATIONAL, LTD PFOS: A Reproduction Study with the Mallard PROJECT NO 454-109, E0L1256 AMENDMENT TO STUDY PROTOCOL STUDY TITLE: PFOS: A REPRODUCTION STUDY WITH THE MALLARD PROTOCOL NO: 454/120700MR/SUBAS4 AMENDMENT NO: 10 SPONSOR: 3M Corporation PROJECT NO: 454-109, EO1-1256 EFFECTIVE DATE: January 30, 2002 `AMENDMENT: -- -- -- "0Thcisomapmleentdemtehnetanianlcyltuidceasl apnhaasteaocfhtmheisntst(utdya.chTmhiesntstAa)chwmheincthAprorevpildaecseusptdhaetaetdtiancfhomremnattAioninnecessary amendment. REASON: "Tuphdeaatemtheedantadq9uaamtlitteaycohnbmjeetncttivAesw,aasnudptdoatcehdantogientchleuldieveasdaifnfderseenrta eexxttrraaccttiioonnalnocdaatnioanl.yticalmethod,to "Scan? Gallagher, StdyDirector Date -- JLaobaonrnaBt.orByeaMvaenrasg,eWmiendte Intemational, LTD, Due "Harold O. Johnson, Principal Analytical nvesigator De -- -- LaboRraetoa"rWilyamgK Meannag,emMentEnvironmental Laboratory, Dae "RochellReRobideay,Sponsor's Represemaive Dae 100 3M Environmental Laboratory Page 193 GULVT Report E01-1256 PFOS: A Reproduction Study with the Mallard Protocol Amendment # 10 - Attachment A Wildlife International Ltd. # 454-109 STUDY TITLE PFOS: A Reproduction Study with the Mallard `SPONSOR 3M Environmental Laboratory Building 2-3E-09 PO Box 33331 St. Paul, MN 55133-3331 PERFORMING ANALYTICAL LABORATORY 3M Environmental Laboratory Building 2-3E-09 St. PauPlO, MBoNx 5353133331-3331 LABORATORY PROJECT IDENTIFICATION 3M Environmental Laboratory: E01-1256 `Wildlife International Ltd.: 454-109 3MEnvironmental Laboratory 20f9 3M EnvironmentalLaboratory Page 194 QOL77E Report E01-1256 PFOS: A Reproduction Study with the Mallard Sponsor Study Identification PFOS: A Reproduction Study with the Mallard 3M Environmental Laboratory Building 2-3E-09 PO Box 33331 St. Paul, MN 55133-3331 Principal Analytical Investigator SAtNuAdLyYTLIoCcAaLtTiEoSnTsING LABORATORY H3aMroElndvJiroohnnmseonntal Laboratory Building 2-36-09 PSt.OPBaoulx,3M33N3155133-3331 651-778-6479 3M Environmental Laboratory Building 2-3E-09 935 Bush Ave. PStO. PBaoulx,3M33N3155133-3331 APNrAoLpYoTIsCeAdLSEtXuPdERyITMiEmNTeAtLabSlTeARTDATE ANALYTICAL EXPERIMENTAL TERMINATION Dare 01/31/02 03/31/02 aM Environmental Laboratory 3019 3M Environmental Laboratory Page 195 91779 Report EOI-1256 PFOS: A Reproduction Study with the Mallard 2. REGULATORYCOMPLUNCE ' } 1 [PURPOSE/OBJECTIVES In the in-life phase ofthis study, mallards were regularly exposed to nominal doses of perfluorooctanesulfonate, potassium salt (PFOS) in their feed in order to evaluate the effectsofdietary exposure upon adults over a 21-week period. The purposeofthis. danoasleydtimcaalllpahradss,eofTthheeansatluydtiyciasl tionqfuoarnmtaitfiyonPmFaOyS in be tuhseedlitvoercaonmdpasrereawoiftbhoth control and toxicological/histopathological results from the in-life portionofthis bird study. The in- life portionofthe study was completed at `Wildlife International, Ltd. in study 454-109. "This analytical phase study will be conductedinaccordancewith the United States `Environmental Protection Agency Good Laboratory Practice Standards, 40 CFR 792. 3. `QUALITYASSURANCE The 3M Environmental Laboratory Quality Assurance Unit will audit analytical phase study conduct, data, and the final report to. determine compliance with Good Laboratory `PPrroaccetdicuereSst.anTdhaerdQsuaalnidtwyiAtshsu3rManEcneviUnriotnmweinltl arlepLoarbtoarlal tfoirnydiSntgasntdoartdheOpSeproantsionrg Representative and the Study Director. 4. [REFERENCE SUBSTANCE 4.1 Physical Description- Perfluorooctanesulfonate, potassium salt from Lot 217 isa `white crystalline material. 4.2 Purity and Stability--The purityofLot #217 has been determined 10 be 86.9%. PFOS has been shown to be stable in methanol solutions for up to 6 months at ambient temperature in the validation report from study PS013, "Method Validation and `Instrument Detection Limit Determination for LC/MS and GC/MS Analysis of FC807 Caonmdtsptealbiliintdy iRneffoerrmeantcioend.atabase in the 3M Environmental Laboratory) or further purity Compounds in Methanol." Refer to the CertificateofAnalysis (stored in the Test, 4.3 Storage Conditions--The test article may be. stored at ambient temperature or lower. 4.4 Reserve Samples--A reserve sampleof PFOS fromLot#217hasbeen frozeatn20C 5C or colder and is kept in the 3M Environmental Laboratory. 4.5 CAS Number--The CAS number is: 2795-39-3. 4.6 MweoilgehctuolfatrhWeeaingihont--(TPhFOeSm)olisec4u9l9ar(CwaeFi1g7htx)is.538 (CsF1sSO5K). Note: The molecular 3M Environmental Laboratory 4of9 3M Environmental Laboratory Page 196 31780 Report E01-1256 PFOS: A Reproduction Study with the Mallard 5 CTyopweTsoRofLcoMntArToRlImCaEtSrices and their source, physical description, storage requirements, and traceability mumbers will be recorded in the raw data and included in the final report. 6. TestSystem The test system is the mallard (Anas platyrhynchos). The test system was dosed (at `Wildlife Intemational Ltd. `mixing PFOS with feed in during a large tmhiexeinr-iinfeappphraosperoifattehipsorsttiuodnys)twoiath cfoohdtpihreenpeoamrviednaebly 10 `Ipntpemrnlaevteilo.nalAufnodoedr dsotsuedyvneruimfibcearti4o5n 4vCa-li1d1a0ti(on3Mst#uUdy27w2a3s),pe"rAfnoarlmyteidcably MWieltdhloidfe VveerriiffiiecdattihoenafcotrutahledoDesteedrfmoiondatfioorntohfisPsFtuOdSy ainndAvthieanreDsiueltts."wiWlillbdelicfoenItnatienrendatiinotnahle in-life `IWnitledrlniafteiopnhaal,seLtrde.poartn.d sMeanltltaord3sMerEunmviarnodnmleinvetralsaLmapbloersatwoerryefcoorlalneacltyesdisb.y Wildlife 61 JMuasltliarfdicdautcikonroepfrtesheentSweilledcbtiirodnpoopfultahteioTnessatndSythsetyeamre an EPA recommended s`mpaetcriiecsesbefcoarutshee tshteuydydioswteoldleitnerambioneraitfoPrFyOeSnvwiarsondmeeponsti.teTdheinutsheeolfitvheresaend ``msaetrruimcoefs mfartominhgatacdhullitnsgtshawitlwledreetefremdiPnReiOfS.PFFOuSrtwhearsmopraes,seadnaolnystiosomafttihnegseadults" offspring. 7. SOURCEOF SUPPLYFOR THETESTSYSTEM "The birds were obtained by Wildlife International, Ltd. Sec their protocol (study 454- 109) for information about bird origination location. 8 SPECIMEN AND SAMPLERECEIPTAND MAINTENANCE `ESnevriaraonndmelnivtearlwLearbeocroaltloercytefdorbaynaWliylsdils.ifeTIhnete2m1a-twioeneakl,enLdidp.oianntdssehraipapneddltiovetrhesa3mMples received by the 3M Environmental Laboratory were from the following birds: ++4400 ecoxnpterroilmeandutlatlbaidrudlst(b2i0rdmsa(t2i0ngmaptaiirnsg)ptahiarts)intgheasttiendgfeostoeddcfoonotadicnoinntga0inpinpgm1P0FpOpSm. PFOS 20 first generation offspring birds that ingested food containing 0 ppm PFOS `dSeasmcprliebsedwiilnltbhee mmaeitnhtoadi.neTdhfersoazemnpleexscewpitllwbheenkerptemiosovleadtefdorfreoxtmrtahcetitoensatnsduabsntaanlcyesdiausring storage. 3M Environmental Laboratory 50f9 3M Environmental Laboratory Page 197 91781 Report EOL-1256 PFOS: A Reproduction Study with the Mallard 9. SAlUlBse-rCa OanNdTlRivAerCeTxtErDactAiNonAsLaYndSIanSalyses as detailed in this protocol amendment will be `performed at 3M Environmental Laboratory, Building 2-3E-09, 935 Bush Avenue, St. Paul, MN 55106.55414. 10. TEhXePE2R1I.MwEeNekTAeLndCpOoiNnDtUlCivTer and sera samples received (see section 8) will be extracted and analyzed for PFOS quantities using the methods listed below. 10.110.4.4 PreEpTaSr-a8t:o2r3y1aSnoldidAnPahlaysteiEcxatlraMcetitohnoadnd AnalysisofFluoroche:mical Compounds from Biological Matrices. 11. DMAetThAoQdUvAaLlIidTaYtiOoBnJfEoCrTPIFVOESS qDuUaRntIiNtaGtSioAnMiPnLraEtAaNnAdLmYoSuIsSe sera and liver is in process in tphreec3lMudeEnavcirroosnsmveanltiadlatLiaonb,orhaotwoervyerst,utdhyeEEOO11--1122777.7 sLtiumdiytmeedtMhaoldlsarwdilclobnteraoplpmlaiterditxo sample analysesof Mallard sera and liver samples using thefollowingperformance based criteria: 11.1 SSyysstteemmsuSituaibtialbitiyliwitlyl be determined prior to the start and at the completion of reuancthharneaely(t3i)camlidr-unl.ePvreilourntexotrtahcetceadlicbarlaitbiroantciuonrvsetaannddaradfstweiltlhbeleasatnaslayzmepdl.eoTfhtehe pbeegaiknanrienagparnecditshieonenadndoftrehteentriuonnsteipmaeraptreelyc.isiTohnewpilelakbearmcoaniptreocriesdioant tmhuest be etoquoarllteossotrhlaenss2t.h5a%n 2R.S0D%.IRfSaDn,ytihetepmroefcitshieonsoyfsttheem rseutiteanbtiilointytifamielsm,ussytstbeemequal `Smaamipnlteesnaanncde tmhuesstybsetecmomsupilteatbieldiptryimoursttoprausnsnbienfgoresestcaorntdinsgettohefscaylsibtreamtisouni.tability 11.2 ATbhesoalbsuotleutReerceocovveerryyofthe method will be evaluated one time in both liver and smeirnuim.muFmoorfctawcho mlaetvrelisxoafmPiFnOiSmuthmaotfbtrraicpkleictattheesraamnpgleoefsawnialllybteefodrettiefiremdianetad for tLhOeQsafmoprlseasmp(li.ec.s,).atTnheearstahmephliegshewisltllbeveelexdtertacetremdintehdroiungshatmhpelmesetahnodd,ata~n1d50% of a"Tnhaelynzoend-ebxytrcaocmtpeadrsitsaonndawridtchaalinberxattieornnaclucravleisbrwialtliobnoefprneopna-reexdtriancmteetdhsatnaonld,aradnsd. bweilsltcaopnpsriosptrioatfae mreignreismsuiomnofwinllinbee(u9s)eldevteolsd,esicnrcilbeudtihinasgcmuertveha(nfoorlbeblsatnka.ccTuhraecy at all levelsofthe standards). 3M Environmental Laboratory 60f9 3M Environmental Laboratory Page 198 63178 ReportE01-1256 PFOS: A Reproduction Study with the Mallard Tdehteearcmciunreadcayt(c%acahbsleovleulteusriencgovtehrey)exatnerdnparleccailsiibornat(i%onCcVuorfvethfeorrqeucaonvteirtiaetsi)onw.ill be Tlehveelr.e iSshnooulcdonatrloelvellim(ihtigfohroarclcouwr)acnyo;tpmreeceitsitohinsmpursectibsieonb,etttheer tmheatnh2od0%wilalt eoanclhy b`meacyobnesicdoenrdeudcvtaeldidatfoorthleervellesvbelesttwoeeexnttehnedttwhoe avaclciedptlaebvellesr.anAgdedoitfitohnealmteetshtoidn.g 11.3 ACaclailbirbarattiioonn curve should be prepared in each matrix by spiking the matrix with kconnosiwsntocfonactenltearsattinoinnseosfttahnedaarndaclyutreveanpdoisnutrsrocgoavteer.inAg tchaeliebxrpaeticotnedcurravneges,hould iconnccleundtirnagttihoen-LrLeOsQp.onsTehreelsaitimopnlsehsitpmsohdoeulldtbhaetuasdeedq.uaTtheleyadcecsucrraicbyeosftehaech level wainldlrbeegrveesrisfiioend.rAe-ncaylculleavteeldo,uetxsciedpet7t5h%e L- L1O2Q5%wohficnhommiunsatlbmeuswittbheind3ea0ct%ivoafted, nbloamnikn.alA. mAlalxliemveulmsomfusftousrh(4o)awlerveelsspomnasye gbreeadteearcttihvaantetdwiicneatnhyatoonfetsheet,moartrtihxe set will be re-analyzed. 11.4 TLihmeiltosweorfQliumaintotfiqtuaatntiiotnat(iLoOnG()LLOQ) will be defined in liver (ng/g) and in sweitrhuimn(tnhge/7m0L%) a-s1t3h0e%lonwoemsitnaalccceprtaiblteaeenxdrtrwiaicttahedacnalainbarlayttieponeacukravrecpaoianttletahsatt 2is tkeipmteswtihtehbtlhaenkr.awTshteudLyLdOatQa adsetweerlmlinaastbieoinnwgilrlebpoertreedcoirndtehde ifnin2anlorteepotrot.file and `tThheehuipghpeesrtlaicmicteopftqaubalneteixttartaicotend(cUurLvOeQp)oiwnitltlhbaetdiesfwiintehdiinntlhieve7r5a%nd- i1n2s5e%rum as nominal criteria and includes applicable dilution factor corrctions. 11.5 AQumaliintiymCuomontfroonleSsaetmopflneinse (9) quality control samples (QC) will be prepared otrnieplitciamtee. inTehaecqhumaaltirtiyxc.onTthreoyl wsialmlpcloenssisshtooufldthbreeeprleepvaelrsedofainnaelaycthem,aetarcihx biny sbrpaickkientg tthhee csoanmtprlole mcoantcreinxtrwaittihoknnsodwetnercmonicneendtrianttihoenssotfudtyh:e analyte. The levels Low level: equivalent to an analyte concentration near or below the lowest level ofanalyte determined Mid-level: equivalent in to samples an analyte concentration near the middleofthe sample range High level: equivalent to an analyte concentration near or above the highest level of analyte determined in samples 11.6 Quality Control Sample Acceptable Recoveries 3M Environmental Laboratory Tol 3M Environmental Laboratory Page 199 u178 Report EO1-1256 PFOS: A Reproduction Study with the Mallard oEfac2/h3Q(C6 oiusteoxfpe9)cotefdatlol sQhCowmaunstacmceuertatchyoesfe 7cr5i-te1r2ia5a%onfdeaxmpeicntiemdu.moAfmoinneihmaulmf (s2amopulteofs3et)omufsttheitQhCerabteeraec-halneavleylzemdusort rmee-eetxttrhaecsteedcr(iatserdiae.ciIdfendobtytthhee ePnrtiinrceipal Analytical Investigator). 11.7 Matrix Spikes Two matrix spikes will be extracted with each sample preparation. The matrix sipnidkuepsliwcialtle.con1sftishteomfoanrexfsoprtiikfeicaantdi/onorlemvaetlriinxtshpeikreandguepolifctahtee sflalmpoluetss,ideexotrfa2ct5e%d accuracy, the curve, CCV's, matrix spikes and samples wil be reanalyzed. 11.8 BOlnaenckonstrol matrix and one water method blank will be extracted with each sample preparation. 11.9 TCownoteixnturiacntgedCsatlainbdraardtsio(ncoVnetriinfuiincgatciaolnibration verification -- CCV) will be acunravley)z.edTahfetearcecvuerraycy1o0fitnhjeecCtiConVs (msutsatrtibnegwaifttehritnh2e5l%as.t iDnajteactmioanyoofntlhyebcealibration rceuprovretpeodiinftb).racDkaettaebdrbacykpeatsesdibngyCoCneV'orsm(oorrea CfaCilVinganCdCtVhemsuasmtebleevreelancaallyizberda.tion 11.10 CUosnefiorfmaCtoonrfyimremtahtodosryarMeettyphiocadlsly not needed with LC/MS/MS analysis. 11.11 PDeFmOoSnssptecriafticiiotynwoilflSbpeecsuibfsitcainttyiated by chromatographic retention time, by the characteristic primary ion (499), and the characteristic product ion (99) using LC/MS/MS. 12. 12S4UB-COANlTlRflAuCidTaEnDdAtNiAssLuYeSeIxStractions and analyses as detailed in this protocol . a3Em-e0n9d,m9e3n5tBwuilslhbAevpeenrufeo,rSmte.dPat taheMu3NM5l5En1v0,i6r.onmental Laboratory, Building 2- 122 pAenrafmoernmeddmeatnltatbooratthoeripersotootchoelrwtihlalnbtehewr3itMteEnnivfierxotnrmaectnitoanlsLaanbdoarnaatloyrsye.sare 13. SStTaAtiTsItSicTaIlCmAeLtAhNoAdLsYwSilIlSbe limited to the calculationofmeans and standard deviations. Examplesofthe calculations used in the analyses will be included in the analytical phase report. 3M Environmental Laboratory. 8of9 3M Environmental Laboratory Page 200 1784 Report EO1-1256 PFOS: A Reproduction Study with the Mallard 14. RAefpinoaRlTreport will be prepared by the 3M Environmental Laboratory. The final report will ufsoeldl,owinalclluGdLinPg raenqaurirraetmievnetsd,isacnudsswiiolnl wiintchluadetaabudleasrcrpirpetsieonntoaftiaolnlofmaatleriaanlaslyasneds mreestuhltosd.s 15. LOCATIONOFRAW DATA, RECORDS, ANDFINAL REPORT `When the final report is completed, ll original paper data, including protocol, phase raenpaolrytt,icsatluddaytac,orwresbipoenrdeletnacilen,edsaimnptlhee raerccehiipvteasondf t3rMacEknivngi,rsoanmmpelnetaprleLpaabroartaitono,rya.ndAll cstoarnrdeasrpdonodpienrgattirnaginpirnogcreedcuorredss,,ecqauliibprmaetniotnprreoccoerddusr,eisn,satnrdummeentthmoadisntweilnlanbceerleotgasi,ned at the 3M Environmental Laboratory, as applicable. 16. SPECIMEN RETENTION a`nSaalmyptliecsaolfstthaendatersdtsswuiblsltbaencmea(ianntyailneefdtoivnerthceonltarboolrasetroaryorfolriaveprearnidosdoafmptliemse)aasndspetchiefied bsaymrpelgeuslawtiilolnnoortabselmoanignatsaitnheedqumaolriteyothfatnhe10pryeepaarrsaatfitone atfhfeoerfdfsecvtailvueadtaitoeno.fHtohweevfienral,test rule ifapplicable). 3M Environmental Laboratory Standard Operating Procedures also apply to sample retention times. 17. Rererences 18.1 Wildlife International, Lid. Protocol No. 454-109, "PFOS: A Reproduction Study 18.2 w3iMthStthuedMyaUl2la7e2d3",.Wildlife Study 454C-110, "Analytical Method Verification for the Determination of PFOS in Avian Diet." 18. PROTOCOL AMENDMENTS AND DEVIATIONS `SPtluadnyneDdircchcatnogreasntdo tthhee Spprootnoscoorl Rweiplrlebseenitnattihvee.forAmmoefnwdrmietntetns awmilelnbdemecnotnssisdiegrneeddabsypatrhte offotrhmeofprwortiotctoelnadnedviwaitlilonbse, astitgancehdedbytotthheeSftiundaly pDriorteocctoolr. aAnndySoptohnesrocrhRaenpgreessewniltlatbieveinatnhde fled with the raw data. All changes to the protocol will be indicated in the final report. `3M Environmental Laboratory 90f9 3M Environmental Laboratory Page 201 63178 Report E0I-1256 PFOS: A Reproduction Study withthe Mallard WILDLIFE INTERNATIONAL, LTD PROJECTNO.: 454-109, E01-1256 AMENTOD STUMDYPERON TOCTOL STUDYTITLE: PFOS: AREPROSTDUDYUWICTHTTHEIMAOLLANRD PROTOCOLNO.: 454/120700QRISUB4S4 SPONSOR: 3MCorporation AMENDMENTNO: 11 PROJECTNO: 454-109, EOI-1256 EFFECTIVE DATE:March27,2002 AMENDMENT. Sedion S1a1 meced Change:Trehteenpteioankairmeeampruesctibsieonomquuaslttboeorqlueaslstthoaonl2e5ss%thRaSnD2..0%RSD,theprecisionofthe "To:rTehteenpteiaoknatriemaempruescitsbieoenqmuuaslttboeorolqeusasltthoaonr2l.e5ss%tRhSanD5..0% RSD,theprecision ofthe "REASON:aIrnfeoarcmoautnitonsrcecoemimvoednftrooUmVoudreitnescttorrasmpeenctisfuipcpaltiioenrsi.ndMiacsatsesstpheatc8t2r.0o%mRewSthDiecfrhowsrt,ohe `cuasnebdfeosrutphpirsesstsueddy,bayroetmhoerrsepseecniscistpirve,sicnagteinnetrhaelsaanmdptlheefmaacttrtihxaatnadnamloybilioenpihzaastei.on mcalekanelairneesasraerperotdhuecdiebtielrimtyimnoinrgefcahcatlolrcsa,bgiuntgt<2o.m0ai%ntasitni.lSaabmiptlaeggarnedsssoiuvrefcoer mass spec. TheapplicationchemistsatMicromass,theinstrumeatvendor,suggest 2value of <5.0%. AMENDMENT: Sec11.t3,Seinteoncen5. Change:rAencayllceuvlealteodu,tseixdcee7pt5th%eL- 1L2O5Q%wohfincohmminuasltvbaeluweimthuisnt3b0e%doeafctniovmaitnaeld.,andregression "To:iInncsloumdeedcianstehsethlienleoawersatncguerovienpfoliunetn,caeltthheoulgohwoeustesniddsotfhtohe3c0u%rnveo.miOnnlayloronqcupioretr,aetah,erlooawyebset lqeuvaentliptoaitnito,nc.aTnhbeelliemittionffqouarntthiitsaptuiropnowsiel.lIbtewtihlelnnoetxbtopouisnetdotnotdheetceurmrivneemteheetilinmgitthoef30% nominal requirement, REASON:Tcahliebrreatmioovnaplooinftthtoeldeovwieasttecbayligbrraatteirontchuarnve3po0i%n.tRienmsoovmaleocafstehsicspaouisnetsitnhtenuenxctaluosweesst {chaloinberxatticoanlpiobirnattsiionnpsoionmtetcoadsecvsicoaubldycgornetaitneruetuhnatni3l0th%e.reTahriesvceornytfiemwepddoienltison of 3M Environmental Laboratory. Page lof3 Page202 63178, Report EO1-1256 PFOSA: Reproduction Study with the Mallard r30%eimsuaseiidnttnoheiicnufnrluvgeen.cTethheeinlcolwuesrieonnodoffatchuercvuerpvoeianntwdiitshpaodteuvsieadtfioonrgdreetaetremritnhaatinon oftheLOQ. AMENDMENT: Section 11.3,thelastsentence. Change: Aremanaaxliyzmeud.moffour (4)levels maybedeactivatedinanyoneset,othestwillbe "To:Thecalibrationcurvewillcontain&misimumofsix (6)calibration carvepoints. "REASON:TIhnemloasrtgceansuemstbheercoaflipborianttisoinncutrhveecsacrovnetiasiunsgeredattoesretlheacntninaen(g9e)rceaplriebsreanttiaotnipvoeitnotts.he scaalmipblreast.iLoinrmaintginegntohtrereempovraleosfoenonlfyttfhoaeustra(im4)pvploeeisntsinsome casescould causes AMENDMENT: Section 113 Add:Thecoefficientofdeterminationforth calibrationcurveshouldbe > 0.985. "REASON: Nreomcooevfefidcpireinotrotfodpertinetrimnignoaftitohnefiiinnacllcuodpeyd.intheprotocol. Iwasinadvertently 3M Environmental Laboratory Page2003 Page 203 L01787 Report E01-1256 PFOS: A Reproduction Study with the Mallard WWILDLiIFE IoNTERNrATIONeAL, iLwToD reRuPROTnECTNoO:e4[05w110e5,e -1256 `Sean P. Gallagher, Study Director Cia Joann B. Beavers, Wildlife International, LTD 0.1 ipal Analytical Investigator 22 FZ Zz -- a= `WilliamK Reagen, 3M Environmental Laboratory, Date. Date i} F.2.07_ Date O 2a) da Date: 3M Environmental Laboratory 3 Page 204 GI1788 BromB73 max 410 822 0ss2 wioLtre ivTERriiag A Reproduction Studyviththe Mallard BueLE 19:29 RSD INF TECH 22-01 + eats No.ses poss | Wpure INTERNATIONAL, LTD. PROTECTNO: 454-109, B0J-12%6 : i vy Qa DR. E Seap. Gallagher, ! ul ox Dae. Soko Mangeemeent -- -- Be Maley : 1 Willig K_Rosen, 34 geal Laborsory, Dutc' + R Soe S t Sr . Fk Lh i iii ry a . 3M Environmental Laboratory Pan3ets i i ; i Page 205 05178: Report EOL-1256 PROS: A Reproduction Study with the Mallard WUWIOLLDLFIFEEIINNTTEERRNATIONAL, LLTDD PROJECTNO 454-105, BE0oL-1t25s6 AMENDMENT TO STUDY PROTOCOL STUDYTITLE: PROS: AREPROSTDUDYUWITCHTTHEIMALOLANRD PROTOCOL NO.: 454/120700/QRISUBAS4 SPONSOR: 3M Corporation EFFECTIVE DATE: August 16,2002 AMENDMENTNO;: 12 PROJECTNO. 454-103, E01-1256 AVENOMENT -- ---- Cthheansgtued:y TishBeO3L-M12E5n5v.ironmental Laboratory Project enifcation Numb (LIMS) tobe included with "tEThOoeL:'s1tT3uh6dey7.misaEiOnI3-1M25E6n.viArdodnimteinotnaall LtraabcokriantgonryumPbreojresctasdsoecnitatietdiwoitnhNthuimsbsetrdy(aLrIeMSU)27tob25e,EiDnIc-l1ud3e2d6,waitnhd REASON: pMeealrrltaaarsidsnisigantnmogepdltehasLsewIeMsarSmptrlreaeccsek,iivnhegednyiuwnmetbrheeer3c.hMeNcEokntevdiarwioannrmoeeodnfittfahelreasencstoepv3eMroaflLIihMimsSeoppraoonjieysco.tts.hUepLroIpnaMrSativpcaruollja,ercssttanumudpmylbeesrs aasshigonfedthte0stehipsrosjteucdtys ipnecrltuadienitnhge0fotlhlioswisntgu:dyUw2e7r2e3,anEaDlIy-z1e2d56u,ndEeOrIo-n1e32i6,nunsdtEudDy1-m1o36b7e.rSEaOmTpLlIeSs56i.n AMENDMENT: Change: Harold Johnson isthe Principal Analytical Investigator. "To:Lisa A. Stevenson is the Principal Analytical Investigator. REASON: To change role ofthe Principal Analytical vestigate. 3M Environmental Laboratory Page 102 Page 206 31790 Report E01-1256 PFOS: A Reproduction Study with the Mallard WIWILLDDLLIIFFEEIINNTTERNAATTIIOONNAALL, LLTTDD rag 21] Sean.Gallagher, Study LJaobaonrnaBt.oro y Mar nage`mWielndltife International, LTD, Lisa A Stevenson, Principal Analytical investigator WillieKs.ReaZgn 3M BovironmenialLaborer, --Laboratory -- -- Management KSoolaeid KaobiSpdereRieapseenemmm,ine moins PROJECT NO.: 454-109, E01-1256 for Te Date Date Di%,Sogo Be5/20/02 3M Environmental Laboratory Page 2012 Page 207 0179; Report E0L-1256 PFOS: A Reproduction Study with the Mallard W`IWLIDLLDLIIFFEEIINNTTEERRNNAATTIIOONNAALL,LLTTDD Boas PROJECT NO.: 454-109, E01-1256 AMENDMENT TO STUDY PROTOCOL STUDY TITLE: PROS: A REPRODUCTION STUDY WITH THE MALLARD PROTOCOL NO.: 454/120700/QR/SUB454 AMENDMENTNO.: 13 |, SPONSOR: 3MCorporation EFFECTIVE DATE: September 27,2002 PROJECT NO.: 454-109, E01-1256 EON. (Change: Rochelle R. Robideau isthe Sponsor Represcntativ. To: Susan A. Beach sth Sponsor Representative REASON: "To change ole ofthe Sponsor Represenaive. ' 20 Q . )} = `Sean P. Gallagher, Study Dir toliloy. Date. Tounn 8. Berean, WHE Teron] C75 Laboratory Management ue BES 6:fsa A.AS.teSvelneswont,aPgroinncipal Analytical Tvestgaior LWabjriu2 oryllia5m K.7MRaenaaggeemne3--nM,tEnvironmental Laboratory, Susah A. Beach, SponGso.r's Representative Date0a/azlea. Dato e b, Daae /az/o 3M Environmental Laboratory Page 1of1 Page 208 31782 Report E01-1256 3M Confidential PFOS: A Reproduction Study with the Mallard Record of Deviation SEhoald-y12P5r6oject No. Deviation type ESOP D(oCchuecmkenontem)uber ETS4-400Protocol I. Identification [Method 0 Equipment Procedure [J Other: 2D3111900a,02,o321tf5o21c502c0s,u2r3,e0)2n2c2e,61307,02027.02, I 22812, 22202, REequTiredSinptreomc4aelduchr-aei/npor4focceoss0so:dy `"WTihtehiinnttehrneala5c.haTihneofcfoursmtosdyhfoorbmelft0lbeded iwsieth syackaatl moovtehmeernretleofvsanptsiaemspledocimers. - SItnAoctrtreuodallcprhreioscaeerodfuFrLues./tpoArdloiecsseswhsoe:msogoentiziendg lvreaackds.almupslteisngnsdiemspampelxesawcetr.Srincee drienceF~irpteseasmpl3eswere Untilexraciondate. Sempleremained fozenuni exracion - (sh 05 amTein,dmAecnttiosunesd, TSaOkPenvison Devision tsSOFvis. rn -- erm - Recorded by BousAe o J {fo Authorized by Date $902. Date Shy Dinche: Jag. dablwpdoy(ees SnDDeviatPioentNLoe ,EO Tot Sr Chek Np 2p tz eter Auachment A 3M Environmental Laboratory DocumentatiEoTn oSf 4De4vi2ations Page sof 1 Page 209 651793 Report EO1-1256 PFOS: A Reproduction Study with the Mallard Record of Deviation T. Identification Stu/Prdojeyct No.E01-1256 I D(eCvhieactikoonnTe)ype OsPoroptocol OOMeOtthheor:d 0 Equipment Procedure Document Number:ETS-8231.1 | Date(s)ofoccurrence/25/02, 2/26/02,2/27/02, 2128/02, 31/02, 3/4/02, 3/5/02, 3/6102, 3/7/02, 3/8/02, Il. Description: tRheoqsueilriestdedP,rtohceeydwuirlel/bperodcoecsusm:eSnetcetdiionnt1h2.e1r,aCwaldcautlaa.tions: Ifother calculations are us_ed than A(`c1St/u0ubdaualgmEPLO)rIo-i1cl3oe4d2|-um 3r6e0o1/f0pL ,vrPosecpeossrhsoe:gesnsp.iTnhi"oCFroorEvgeTePniocnc--onpsigst f5IGFv,erwpastpr4e5pmpe._dwbye.siSnine20m0L.0So2ut0ho0f1S8o6m. Homapgeepe veindg SoPEp,pheeaGcho aruict 2s0amn.do,f MSeoOfH. oTeHER0E1FO)REo.f ve spiked. Afr hshomaisgikeed (20) (1.00gPFmOlS. MeOH) (1 0mLI1000uL) (1000/1.0ug) = 200g PROS ont SPE column T{2S0hi0engceePatheiRsts/tOa2rn0dSmartodshMrueenncOioHrsd=ebde0innggmpPepRsbOs,SehmseLcaonMdmeerOepHiotrsteordne1eS0hnrogTkmP.pohoFigf MOyeOeSHn). Similary, he lowingstatements re (200g FOS 1.0m.homage()Om. homogenate0. vr) = 200gPROS glives cThhriomealtaocgornasphhiipc srehsouwltshthtesfacntonronf2.0 sed to "Samet the unis when calultihne findrs in gg omthe SFEaOmT-e12C42u:30t%4s8,:Oppm i. 333 M iver" CNhromoatomgraophwiictghr3e.es0miLs.nva10te.e76,dnndgaLr(e1p0r%eofvlalisv2e08w.e4iagh.ed,Ssiinncceeheiv1er03d3e3nsgitnytofl1,s0am0p1lse wmee)ioifgvaheerdt5forthe nie SPEprocaret,e calculation is follows: (107605PROS!mL.MEOH)(mLMeOH /0.103 give) =2084ngPROS-/g lver `MSSiaEmmppCllHeeCEsoDlpIle-a1dt3i4to3on.:3I60L17v,eCr1b0oopgpenba"ie:.This QC spe i prepared by adduli.of n0200g153 (5.020 PFOS mi. (4) 5.0(2mL0O0)0L) (000.10 5liverm )=200g805 P)EOS giver UPsiRnOgS:t1hge xiveri,thcelrleaciovoenry,itsh(e2a7na1l/yt2i0ca0lSrXesIu0l0t1o-f131354S9%g/mi.causes 0271, Sg/g ive. Sincehespike lvei 2008 3MEnFvoirrmonEmTenStAal8L0aboratory 3M Environmental Laboratory (aig StdDic oDrervijatiLondaNo.. andofm__a2dorprj) Page 210 63179. Report E01-1256 PFOS: A Reproduction Study with the Mallard Record of Deviation ~ ll. Actions Taken: (such as amendment issued, SOP revision, etc.) Issuingofthis SOP deviation and a note to file. ~ Rep By < A - IV. Impact on Stu/Prdojeyct Date - 4. (aeoy_ There will be no impact on the study as this is for clarification purposes. Authorized By (Study Director / Project Lead) heat As shy Och: La, ef.RATVIA Adon Uh Nagrand: SA clefonba Date dia 3M EFnovrirmoEnTmSen.t4a.lL8a0boratory 3M Environmental Laboratory gt StyDrorDorePvriojaetcitLoenwdNto.h ndof_m3.dapc) Page 211 691795 Report EO1-1256 PFOS: A Reproduction Study with the Mallard Record of Deviation I. Identification Study / Project No. 01-1256 Deviation Type (Check one) TSOP Protocol TT TT 0 Method 0 Equipment Procedure 0 Other: `Document Number: ETS-8-231.1 | Date(s)of occurrence: Throughout the study Ti. Description: RSeeqcutiiorned11P.3r,ocSeendtuernec/epr5oscaetsess::_An_y l_evel_out_side_75%- 125% of nominal value must be deactivated, and regression recalculate... aMpaenxyofofthtehecuhrivgeh.caWlhibernatiaocnaploiibrnattsiionntphoiisntstluideys aarbeovkeepttheinatpheex,cuirtivsecdoensspiidteerbeediinngdaetbeorvmeinthaent c(ableculleadtewd,itnhoapner1ceanntddnioffceornecnecnetirsactailocnulisatceadlcfuolraetveadlfuoartitnheg wsthaentdhaerrd.oIrfnnootctohantcesnttarnadtairodniiss within the stated criteria. Removal of these points in most cases causes the next calibration point then be above the apex of the curve. This continued deletion of points could continue until there are no points remaining onthecurve. Therefore, calibration pointsabovethe apex were included in the range ofthe curve with no evaluation ofpercent deviation criteria. Ti. Actions Taken: een (S050.08Gagrilmaenst ssised,SOF.revision,ete) |Tnheixtsdhigehestviactaliwiaobrsnatwirointtepno,inatnwoetreetorfeialnealwyazsedw. riatndtdateapnoin,ts which were above the (1 RR ------] 1 Lisa A. Stevenson (yc A Destnon 08/16/02 atfiuloy `Authorized By (Study Director / Project Lead) Date dy poche Hake} Ny don Lahorahony Maragerent' FA f-- 8/20/02 3MEFnvoirrmonEmTeSni4a8l0Laboratory idbySoyDict DePviraottiLoenwdNao. _nd_of3d_y o_F_) 3M Environmental Laboratory Page 212 3917 Report E01-1256 PFOS: A Reproduction Study with the Mallard Record of Deviation T. Identification Study /ProNoj.Ee 01-c12t 56 Deviation Type (Checkone) SOP TOMethod 0Equipment Procedure OProtocol 0Other: Document Number: ETS-8-231.1 | Date(s) ofoccurrence:Entire Study Il. Description: SReesqiounir12e.1d, CPrloecetdnurse/fprooceecssl: on re setanhse td hey willbedomtheervddi (SAacntdu5aadl1P02ro5c62e-d3u06mrl4e./0o/pfrPporoec0lpeessdsso2e:cs.sTciie edint"e10sperecrosnsvoefSplo.ns"rwsipoyreSpopme,dwitsiSnpg cLS| lT GOaOoTfS4oT0m. "pileddsnrdsri espdr0vrienpSrPeeEchfexaactcedesan2d0r,.TAoDfoMfetOheH,mTLHfERsEFO"RpEi.ke.A 1.0m ofiidses 4 (SagPROS mLMeOH) * 4 * (101/100) * 1000.00 = 00gPROS:cot SPEcoum T2{0eS0isgnPerFeOshSme1ar2ne0doman MaecOkoHrsd=ebd1e0ngg0PsR7Or,Setihm,caMorOepHoa.iissoen0gSHPORMOSSEISMHEEsH)r. SiamniglaPtRyOdSe!f1olmo.widngisedesems)ies4wne0. . ser 20m. nialsr) =400gPROS!iSern Trienretlt4onPshRipOshSo.wsSteesfrocmohoefc40hroorm2so.g0rmphMierOeHl0.h05t Saenrg)Fi ROS/" L MeOHthe itswhenclung hein SC"ahErDnoImn1a2et5oC6g-lr2oa8lp7uh0i1ic,o4ns5.4u.1i0s9.33420835r,1g0,pMmOcMm,lp, eitd. ve 13612sg.Ser.Soethe LOrl samplevolumeof (S3e4r0.30d6iPtReOSw!ilh130R 2m0mM.ewT OaH)e ES (i00mJ.iM8cOiRcYi0f.onr5mehe.inSneex)S=PE13p6r12o0c4PeF,OoSsmcLlSeraa ni follows: fSMriOHe)s1pik2ed 5to m8Li2tocd5sas5r0pop.010ThmiLn.oQfCstpaes1).reprebydn 1.of 2101.53 (0.200PROS: /ml (50200p/mL) * 1D * ImLII0O0L)* 1000Ngh) (0.05ml.Sere) = 10040 PROS:mL.Sern 1ri0n0gg hePcRaOtSemcll.utiSe.ont,htheeneanyicl1e36t3of2160400A6nHIgO.OIc1a0l5c2l5t.s 0 05624nr.Se. Sinethespclends Ill. Actions Taken: (suchasamendment issued, SOP revision, etc.) This deviation was written and a note to file was written. ReLicsoarAd.eSdteBvyenson A A Dtrion Date " 08/16/02 08/1u fog `AuthorizBeyd(StudyDirector /ProjectLead) AD ade Date dy Deck Aiwy{ Ah 2 tae Lr abora mk,VHEp ETZ Fon T5480 Zr.Deviation to. __4_ (eidSdDic PctLend 5 dof yo) 3M Environmental Laboratory Page 213 Co1797 Report EOI-1256 PFOS: A Reproduction Study with the Mallard Record of Deviation 1. Identification |Study/Project No.EOI-1256 D(eCvhieactkioonnTey)pe, TOPSrOotPocol 0 MOetthhero:d 0 Equipment Procedure Document Number:ETS-8-231.1 I Datofeocc(urrsenc)e: Througthheostuudty Ti Description: SReecqtuiiorne1d3.3Proofctehdeurmee/tphroocdesstast:es: Twothirdsof llquality controlsamplesand 172of cach quality control sampleat ach levelar expected to show an of 75-125%. AAclltu2a5l pPprbocmeadlulraer/dpsreorcaeqsusal:ity controlsample recoveries were>125%. (such as ameTnild,meAncttiisosnused,TSaOkePn:revision, etc. | "`Tahnidsdqualeityvcionawtraotslwidraitotatennno,t sweirtahdiantcariteiraaerpatfoltahgregletdowiernadtnhegeroafwtdhateac.urve may bebiased high, ReLicsoarAd.eSdtBevyenson (hc A Jhtuenion AuthBoy(rSwidyzDireectdor /Project Lead) ( dy Deel uy P Mey Lobsheyhy MonagpmntMagn EZ -- folio orate [0b 826a 02 3Jaulos Date L| 3M EFnvoirrmonEmTeSn.t4a.l8L0aboratory 3M Environmental Laboratory oir tty DiocDePvicattiLondNo. _nd_ofSy_o_pr_o) Page 214 91798 Report EOI-1256 PFOS: A Reproduction Study with the Mallard Record of Deviation StojyNo. BOI-1356 1. Identification De(vCihaetcikononTey)pe. OVSPOrPocol 0 MOemtehord OEquipmentProcedure - "Document NumETbS3e53r11 |TD3aatrem2,osfvceec,ur6e0n2c,e7235110022,, 2330600,0, F775, 32008, FTF. I. Description: RiellqbueirdedoPrcocuedmuireet/hepnrrootcweedsast:da.Section 12.1, Calcuions: Ifthe calulaoanes used ha thos ised thy. "hAicswdiePvirsoieondupredrpsroceevsasio:n_#1_x_p__i__v_e__.io_n___ SL SOamnLdO haomEoIg.mep1noate31i mv2afd6n fPp.erepL 3smhace7agcth) ed8cesscc.8ripTdth,iiosn abCnoadmroavgree,Pris1in5e0--oofn0he5s5$o0if5n9Si70ve5"07,.wia0sk1p0rep7p3sped40b58y d5swp7iak5ien5g,0S,hesofww0e2o00+1.t66 T0H5E9R7EgROvRE spiked".Ane osbomogent 4AKed130 epredsrgSPE. costes 0m of MeOH. (QOL) 1.00ug PROSmLMeOH) (1.0mLJ1000ul) * 1005510) = 0.03PROS"ntoSPEcom 2(h0Se0isgcaPiFeOshSe/aU2nni0dtmasribieMngerOmHets=se18d0gs1P0dRgO,gShoenekcdoMnoeensOhHerihsAO11T5APOEROSc/.nofMeOH) Simla,the ollsoewmeinins mge. Q008PROS 10mLhomoge) * (1.0mi orogenic/0.10107 g ve) 198 PROSg vee "`ESDm0u1e32a6l9a9i1o6n.ype 1.3257 M ver" C moarwig tos5.l0mn msi31tt4re 6,nogsLgrsepapidv0ihl0isi7210s7cSnPgE .PrSoicnucreeth,e1.c065ueil empll wo,eiofgvehri 1068/00mLwater + 1.064 giver) = 0105848 fer 10mlhorogensieremovefoxr. 81.460gPFOS/mi. MEOH) * mi MeOH0105848 ve) 10=72077 ngPROS / vee Sa`MSOnamHppl)eeCs"pBai0lk1oe-nd1i3n2ot6n.:3m67L95li,vOerhoCmogSe.Thi QCsample iprardbyaddingTu,of0200-53(502005PROS a. (ul)* (Sag)* (1nLJI000L) * (1000ngg) (O0ICTS vr = 57 0PROS ver POUsiSng)hgeicvaeteirecaelcclaoio,nhe(n7ly1H+ e(s0l0o)f1348.58%7.nm.cect 0571ng vBhe,Siethespikelvl 49g. Testing of 5 SOPdeviation. suchasamenMid.meAncttiisosnused,TaSkOePn:revision, et Recorded y Lis Stevenson (YAi Sheyonion ~ | Daeme oak ASidiorzoed Bey (dyGlDircor/Prajer Lead)Q\ h 01 \y x Bee d Ly e E LiFtormEb TS480brL iSmom Ronge 27 ins Sn DisZcroDPoovtiLtewdoino._dtb_yo_P_r) 3M Environmental Laboratory Page 215 1799 Report E01-1256 Repo Eot1258 PFOS: A Reproduction Study with the Mallard PROS:ARepraStouywcihtiMaotanr ee emer ATTACHMENT F: EXAMPLE CALCULATIONS eeeee semeee ee eee eee [FORMULAUSEDFORSERAANALYSESIN STUDY E01-1256 AR (ng/mL. MeOH) x OF x Ditton (diuted sera) = nin. Sera Golculaton Used for ED1-1256.28701, 454-109-3258, 10 pom Female dull (nl volurbe = 0.8 mi) 340.3 ng/mL MeOH x 1x40. = 13600ng/ml. seem 3rote oEEpe memes FORMULA USEDFOR LIVERANALYSES IN STUDYE01-1256 AR (ng/mLMeOH) x DF x amountFiofnavleVrolinumdei(vmedL)sample (5) =nglgLiver Calculation Used for EO1-1326.29925, 10 ppm 1. 3258F Liver (ital weight = 1.0034 6) 355.07ngimLMeOH x 1x 021000m3L0M6eOLiHver = 7080nglg Liver --_-- DAFR == ADnialltyotnalfarcotsourlt from MassLyn summary Dilution(diuted Amount of sea sienrlau)t=edFisnaalmpvloel(muimLe)(=mLaYmaomuoruonftsrofssuesraadi(nndLilouttaedl`a'msoaumrpleo(fmLso)ra + ten) RAommoougnotnoifzivnegr(miLnoig)ed sample(o) = amount vorweighed amountof vr waghedi) +waaraed for -- ExamTpiTos------------------ AOmhotuonnt(odfusiadasinedirte)s=anmapllveoe)m=ea2mo0unmtLoYfasmeournutsofds(o0r.a5mnyidaasmamopulneto(0.0f5 8 m+=wa4t0er (10m)= 0.05mL. Amountof ar ingfe same) =amountof erweig(h1.e00d34 gofu vorwoioht d(100345)water `addedforhomogen(9i.0z0miLn)=g 1.0 9/100.3 00344g = o0s08 o 3MEnvironmen0taEl nLanboraatLoarbyo,r Pace 216218 Page216 +05 BON679, 31800