Document 10j4dD2ojMg3raZZ2Ok4OZmxj

PROTOCOL DETERMINATION OF THE WATER SOLUBILITY OF PFOS mw BY THE SHAKE FLASK METHOD ml `OECD GuidelineWfaortetrheSToelsutbiingloyf Chemicals, 105 of SM Lab Request No. U2723 ul -- 1 3M Corporation Environmental Laboratory 1 St PauPl.,O.MiBmoexs3o3t3a3155133 m WILDLIFE INTERNATIONAL LTD. 8598 Commerce Drive nm } Easto1n0, )M8a2ry2l:a3n6d0201601 | Deceamber2, 1998 mn 000140 m PROTOCOL NO.: 454/120298/830.7840/SUB4S4. 3M LAB REQUEST NO. U2723 Pe WIE LDLIFE INTEe RNA ATIONAL LTD.rie 2. DETERMINATION OF THE WATER SOLUBILITY OF PFOS BY THE SHAKE FLASK METHOD SPONSOR E3nMviCroornpmoernattailonLaboratory P.O. Box 33331 St. Paul, Minnesota 55133 `SPONSOR'SREPRESENTATIVE: Ms.Susan A. Beach TESTING FACILITY: Wilde Intemational Lid 8598 Commerce Drive Easton, Maryland 21601 STUDYDIRECTOR: --Rondartaccts RaykmVaondlnawedn, PhD. --Senior EhemistScientich LABORATORYMANAGEMENT: Willard B. Nixon, Ph.D. Manager of Chemistry FOR LABORATORY USE ONLY _ Proposed Dates: || sExtpaetrDiumee:ntal__oJto__J99 proto: AMCSOV Test Substance No: --AGT5 1 tExepmeirmimueinotnalDue: 3/0/20| yupwe _Bllaloltr ReceiptDate: --_10l20fig PROTOCOLAPPROVAL 4 : // L i Ii OR altel gt DATE | LABORATORYMANAGEMENT SPONSOR'S REPREASENTATIVE PROTOCOLNO.: 454/120298/830.7840/SUB454 24 DATE Ja DA [2] 98 000141 3M LAB REQUEST NO. U2723 W-_I--LDLIFE INTERNATIONALtLrTD. 3- 0000000 INTRODUCTION CperflWuiolrdolcicfteaneIsnutlefmoantiicoaniadl, pLtodt.asswiiulml saetx)p.erTihmeensttauldlyyvidletbeermcionneducttheed watattehre WsiolldubiifleitIynteorfnaPtiFoOnaSl gLiudi.daanncaelyptriecsalenctheedmiinsttrhye OfaEciCliDty GiunidEaesltionne,foMrarTyelsatnidn.gofTChheemstiucdaylw,il105b:e pWeartfeorrmSeoldubfiolliltoywi(n1g) tfhore usnhdaekreEfPlaAskPmreotdhuocdtolProogpye.rtiTehsiTssetsutdGyuiidseliinnteesn,deOdPtPoTmSee8t30d.a7t8a4r0e,qWuairteemreSnotlsubuinldietyr:thCisolguuimdnelEilnuetainodn MSeectthioodn;18S4h0:akWeaFtlearsSkoMluebtihloitdy ((32)). aTndheTmSeCtAhoTdiotlfean4a0lyosfitshefoFreqduearnatliCtaotdieonofprRoevgiudleadtiboynst,hePSaprton7s9o6r, willbe verifiedatWildlife International Lud. Raw data for al work performed at Wildlife International Ltd. and a c Intemational opyofthe final report will be filed Lid. site or a an alternative locati by on t project o be spe number in archives located cified i the fina report. on the Wildlife "The pu rpo seofthis study is to determine PU the RPOSE water solu bil ity of P FO S at 20 05C by the shake flask method. Determination of water solubility by the shake flask method is applicable to test `substances with water solubilities equal to or exceeding 0.01 gramyLiter (g/L). not be applicable to surfaceactiveor volatile test substances The methodology may "The water solubilityof EXPERIMENTALDESIGN PFOS willbe determined at temperatureof20:+0.5C. A preliminary toefstawdidliltbieopnesrfoofrmiendcrteoaessitnigmlayteltahrgeewaatmeorusonltusbiloiftywaattoeor mtoteampkenroatwunrew.iTghhetpofrtlestismubtisetsatnnccoaensruinstytisl esstoilumbaitliezdawtaiotneisseoflufbeicltietdyogrretahteesrotlhubainl0it.y01is ge/sLt,imadaetfeidntiotibveetleesstwtihlanlb0e.p0e1rfg/oLr.meFdo.r Tsuhbesdtaenfceisnwiittihtevasent | consistsof equilibration of an excess amountoftest substance with water at an elevated temperature, - 30C, followed by equilibration at 20C. | MATEARNIDMAETLHOSDS L TestSubstance "Thetestsubstanwiclelbethehigpurhityeavasilabtle. Thetetsubstshaounldcbeatleast 99% { spuubrsetabnycew,eiigfhatv.ailaTbhlee:Sponsorwill be astkopreoviddethefollowing information concerning the test | { PROTOCOL NO.: 454/120298/830.7840/SUBAS4 000142 3MLABREQUESTNO. U2723 nN om om IN on ml im nm im I I w 0 H n n I I ----m WiLoLiFe INTERNATIONAL 1p : a. DCEimhspesimoricicicaaatllioNFnoarCmmoeunlstaaanntd/inorWaMtoleerculaWr eight CLhoetmoircaBlatPcuhriNtyu:mber MExeptihroadtoiofnADnaatleysis SVtaoproargePrCeosnsduirteions alnodngtTewshitietnhtgaaoMcfaththeeerdieafslotrSmseuIbysDtEaDnaNcteTaIShFeIs,CwAiTllIObOeFNusTdEStTpSrUoBviSTinAfNorCmEatiBoYn nSePceOssNaSryOfRo (tAhpepheannddilxinI), substance containers at the end . The Sponsor ofthe study. agrees to acceptanyunused test substance andor g test Fae smoalyvebneWtasntweeirleltdhbaftomeheetstAiSaTlM TmyeptehoIdsotanpdraerpdasra(tiAoSnTofMstoc1k19s3-l91)iwilalnbdeaunsaelydt(i4c)a.l sOttahnedr solvents inletswith teheAqCSuraeagnenttogfirtahdtestoaersttbseutibesrt,oanacnned, vill be determined to be ards, freeofcontaminants All that PreliTmesitPnroacerdurye A preliminary test will {emperature. Approximately be 10 conducted mgofthe to test estimate the solubility of the test substance at room volumes of wate w il be added stepwisea ss h substance own below. wi llbe placed in a plastic tu b e. Increasing Totalvolumeof water added (mL) Approximate solubility (g/L) OL 0s 1 5 200 20 0 5 tgfesetrosusrch afooroaupnprsoofsialmattyelye1d0 mitnhuetesstaatnvdovliusmuaelliynceixcaamtidn,ehdefcronutnadiinsesrolwvileldbteesctapped and shaken sohankfiengr,betsdhetocaaonnlictasetngortdconitaisnesr aaonfdtelwaavtdedrieatidodndofor10 mLn,olfvwoaltuem,ethe10co9nate.ntsFoofltlhoewcisounnbgtscataiapnnceperi.nwiIllftbhoe EdLi)camtaeyavbeatpresroafliounbreirmlwibityyl<tb0ae.nvisguLa.lly Pcrheelcikmeidnfaorry utnleissstoolifvtenhdgemastoelruibaill,itiy .atluonwdiesrscoolnvceedntmrataetriioanls w(go<au0n.l1dd he st ith esetamount sering the contents ofhe 100g, festsubstan, e.5, 1mg Amou vessel 10a 1-L vessel or reinitating vdoleumefsoofcwoantdeurcmoafyhbeepruesleidm.inary suc, ager amountsoftongtssuabnstdavnocleuwmietshnportoepodrstiboonvaellayrelaornglery 000143 PROTOCOL NO.: 454/120298/830.7340/5UBA434 3M LAB REQUEST NO, 2723 a H n WIE LDLIFE INETERRNAAo TIOe NAL LTD.,-- u > a DefinitiveTestProcedure fi thpr`Thiemqueanytitsyto.ftesTtosubvsotalnceeonfewcesrsaryitodsaitulratdeeptheenddesnitrehdevoalulmetofswamteres etssntdihmsatieodlfldryom range. Greater than (or equal to) five times the quantityoftest substance required to achieve water 0 solubilitywill be transferred to a mirimumofthre test vessels (plastic andlor other suitable container materia). The desired volumeofwater will be added to each vessel and the vessels sealed. The closed i vesselswillbe agitated (shakenorstirred)at 30 1.0Cin awaterbath. Afer 1 day,oneofthevessels willberemovedandre-equilbratedfor24hoursat 20 + 0.5Cwithoccasionalshakingor tiring. The d contentsofthe vessel will ten be centrifuged in a centrifuge regulated at 20C. The concentration of thetes substancsin amirimum oftwo aliquotsofthe aqueos phase will be determined. The remaining i two vessels are trated similarly following initial equilibration periodsof 2 and 3 days at 30 + 10C. The test will be terminated if the concentrations of the test substance in the aqueous phase of two. consecutive vessels agree within 15%. If greate variation is observed andlor at the request of the a Sponsor,the test may bereinitiated with longer equilibration periods: Method "The analytical method for quantitationofthetestsubstance will be based on procedures provided bytheSponsor.Themethodwillbeappended tothi protocolin AppendixIIandreferencedinthe report. The method may be verified as partofthe preliminary test(s) and may be modified to measure. o theobserved test substance concentrations. Majormodifications will be approvedby the Sponsorand Study Director, and documented in the raw data. nuo Calculations `Theconcentrationof thetestsubstanceineachvesselwillbeexpresseding/L,mg/Lor ug/Lin H `water as appropriate. The average solubility for test vessels with solubilities within 15%ofcach other will be averaged and reported. SampleHandlingandSafety m `TheSponsorwill idenantysipefciaylhandlingor safetyprecautionstobeusedwiththe above referenced test substance. All normal precautions with respect to handling and storage will be taken. a 000144 an PROTOCOL NO.: 454/120298/830.7840/SUB454. 3M LAB REQUEST NO. U2723 iH . om WILDLIFE INTERNATIONAL LTD. on -6 mn `SamplUeraonndTceosmptlSeutbisotnaoncfeRseitenn,tiopnornsofth st btn sd 8 pit of is stywil be disposed of in accordance with federal, state and local regulations. Any unused portionofthe test nm substance will be returned to the Sponsor. REC TOBOEMR AIND TAIS NED no Recordstobe maintainedfo datageneratedbyWildife InternatioLniadl. will inclbuutdnoetb,e limited to om 1. Acopyof thesignedprotocol. 2. Identification and characterizationofthe test substance, ifprovided by the Sponsor. ml 3. Datesofinitiation and completionofthe study. 4. Datesofexperimentalstartand termination. i] 5. Storage conditionsofthe test substance. 6. Test substance use log. ml 7. Concentration calculations and recordsofsolution preparation. 8. Instrument operating conditions and chromatograms, ifapplicable 9. Statistical calculations 1 10. Test conditions. 1 11. Acopyofthefinalreport. i| Mm mm [7] . mm mm FINALREPORT Afinalreport oftheresultsofthestudywillbepreparedbyWildlifeIntemational Ltd. The report will include, but not be limited to the following, when applicable: 1. Name and addressofthe facility performing the stds. 2. Datesuponwhichthestudywasinitiatedandcompleted. 3. A statement of compliance signed by the Study Director addressing any exceptions to Good Laboratory Practice Standards. 4. Purposeandprocedure, assatedinth approvedprotocol,includingallamendmentsanddeviations tothe protocol. 5. The test substance identification, including name or code number, purity, empirical formula, molecular formula, lot or batch number, methodofanalysis, and any other information provided. by the Sponsor 6. Descriptionofthetestmethod o referencetothemethodusedalongwithanymodifications made. 000145 PROTOCOL NO: 454/120298/830.7840/SUB4S4 3M LAB REQUEST NO, U2723 SWIeLeDLIFE INTERNe ATIONs AL LTe D. 7. 7. The individual concentrationsofcach sample. 8. The means and standard deviations of solubility determinations at cach interval for cach temperature tested. | 9. Descofarnypirobplemts exiperoienncedand how they wereresolved. 10. A statement preparedbytheQuality Assurance Unit listing the datesthat study inspections and | auditsweremadeandfindingsreportdtotheStuyDirectorand Management | CHANOFGPRIOTNOCGOL Plannedchangestotheprotocol will be intheform ofwriten amendments sibgytnheSetuddy DiranedcthetSpoonsorr. Amendmentswillbeconsideredaspartoftheprotocolandwillbeattached. | tothefinalprotocol. Anyotherchangeswillbein the.form ofwritendeviationsfiled withtherawdata | All changes to the protocol will be indicated in the final report. GOODLABORATORYPRACTICES | "This studywillbeconducted according to the Good Laboratory Practices descriniObEeCdD (ISBN 92-84-12367-9) and EPA (40 CFR Part 792). Each study conducted by Wildlife International LidsroutinelyexaminedbytheWilde International Ltd. Quality Assuranc Unit for compliance with | `Good Laboratory Practices, Standard Operating Procedures and the specified protocol. A statement of | `compliancewithGoodLaboratoryPracticeswillbepreparedfor llportionsofthe studyconductedby `Wilde Intemational Lud. The Sponsor vill be responsibe for compliance with Good Laboratory Practicesfor procedures performed by othr laboratories. Raw data for all work performed at Wildlife | IntemationalLid.and copyofthefinalreportwilbefiledbyproject numberinarchives locatedonthe `Wildlife International Lid. ite of at an alternative location to be specified in the final report | | I | I 100146 I PROTOCOL NO.: 454/120298/830.7840/SUB454 3M LABREQUEST NO. U2723 uN W_I--LDLIFE INTERNATIa ONAL. LTD. se | REFERENCES 000000000 n 1 COhregmainciaslast,i1o0n5:forWaEtceornSoolmuibciliCtoyo.peration and Development. 1995. GuidelineforTestionfg 2 EPlruotdiuocntMePtrhoopde:rtSiheaskeTeFsltasGkuiMdeetlhionde.s. 199. OPPTS 830.7840. Water Solubility: Column o 3 TSCA Tile 40 of he Bhs Coe of Repos. 1595 Fst 756, Ssin 14, ae Solubility. n A'mDeIr19i3c-a9n1,SAucSiTtMy fSoercTtisoinnIlgWaatnedrMaandteEnrv,iro1n9m9e,ntaSliTnedcS hnologp y, Vol. e 11.f0o1.Rc 45e-g47e.ni Weer, I| 000147 4 PROTOCOL NO.: 454/120298/830.7840/SUBAS4 3MLABREQUESTNO. U2723 1 WILDLIFE INTERNATIONAL L7D. 5. I -_-- 1 _-- IDENTIFICATION OFATErSmToSUrBySTANCE BY SPONSOR To be Completed by Sponsor | URS rt mhpromptoibsng cis | I. RTeesfterSeunbcsetaSntcaenIddeanrtditGyf (anppalmiectabolbe)e:usAendaliynttihcealreSptoartn)d:arPdE: OS_(NP/AerfluorooetaneSulfonicAcidPotassium Salt I Test Substance Sample Code or BatchINnutemrbnealr:Standda_r_odL:otz2P117.e1.r28HfHlHvorooScultfonaicAncied_ | IL TTeesstt SSuubbssttaanncceeCPhuarriatcyt(er%izAacttiiovne Ingredient): __98.9 Expiration Date: _2008 Have theidentity,strength, purity andcompositionorothercharsetristi IL dTesteSutbstepanrcireorSmttoortiasgensCeoinendittdhiiossntsudyin accordawnicteh GLP Standards? Yes__ No_X || PleaseAimnbdiiecnattertohoemretceompmemreantduered storage conditions at Wildlife oternational Lid | SOHaetshertdhpeeeretminstiaebilnnitytgsotfabtiheleicttyoesidntafsonurbcmsawttiaionlnc:eOunLdSerthnes 5 conditions Yes_No_X -_-- 000 i IV. Test Concentrations --X_bAadsjeudstutpeosnttchonecpeunnttryat(i%on)togi1ve0n0a%boav.e. | Doain. oTteastdtjhuestmaetterciaol AnScS,ern0 100% V.. Toxicity Information | Mammalian: RatLDSO_251mgkg MouscLDSO_NA | Aquatic: Invertebrate Toxicity (EC/LCS0) Daphnia magna: 27 mg/L Fish Toxicity (LCS0) Rainbow Trout: 1 mg/L | Other Toxicity InformDataipohnni(ainmclaugdnian;g f5i0ndmingg/sLofchronic and subFcahtrhoenaidcMeistnsn)o:w: 38 mg/L Please see MSDS, [ 000148 ! PROTOCOL NO: 454/120298/830.7840/SUB454 3M LAB REQUEST NO. U2723 W--I_--LDLIFE INTERNATIONAL LTD. -10- APPENDIX II ANALYTICAL METHOD Analytical Method fo the Determination of PFOS in Water detectionPF(OLCSMSm)a.y bSeadmeptleermpirneepdariantwiaotnefrorustihnegfhoirgthifpiceartfioonrmsaanmcpelelsiquwiidllchinrvoomlavteodgirlaupthioynw(iutshinmgastshesspeacmterommaettrriixc wfoallro)winigntporetsheetcsonacpepnrtorxaitmiaotnercahnrgoemaotfogirnastprhuimcenctoanldirteisopnosnsfeo.r LCMaMtSrixquabnltaintkastiowinllofbPeFOdiSr.ectlCyhrionmjeactteodg.rapThhiec conditions of PFOS. may be changed to provide conditions more optimized for retention and/or chromatographic separation Instrument; Hewlett-Packard Model 1090A HPLC Columa: Keystone Betacil C-18, 100mm x2.0mm, Sum | | FMolboiwlReatPeh:ase2:50MueLth/amnionlu:teAmmonium Acetate Buffered Water 65:35 (vx), isocratic | Column Temperature: 40C Injection Volume: 100 uL Ton Source: Turbo lonSpray Mass Spectrometer: Perkin-Elmer APL100 Run Time: 6.0 minutes PROTOCOL NO.: 454/120298/830.7840/SUB454 000149 3M LAB REQUEST NO. 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