Document eBObk8ZnZkqxvZXOOp91vmp9

-I . . Determinationof the MeltingPoint/MeltinRgange of PFOS MELTING POINT TEST SUBSTANCE Identity:Perfluorooctanesulfonatmea;y alsobe referredtoas PFOS or FC-95. (1-Octanesulfoniaccid,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8heptadecafluoro-p,otassiumsalt,CAS # 2795-39-3) Remarks: The testsubstanceisa whitepowder. Sample was taken from 3M lotnumber 217. Sample was storedunder ambient conditions priortotestingP.uritydeterminedtobe 90.49% by LC/MS, 'H-HMR, '9FNMR and elementalanalysestechniques. METHOD Method: OECD 102 GLP: Yes Year completed: 1998 Remarks: Study utilizeadBOchi MeltingPointB-540 instrument, calibratedand inspectedjustpriortouse usinganthraquinoneand 1,8naphthalimide. RESULTS Melting pointvalue in*C: >4000C (No meltingobserved). Decomposition (yes-temperatureOC/ no /ambiguous): No Sublimation (yes/no/ambiguous): No Remarks: Measurements ofthe meltingpoint/meltingrange were limitedto :54000C,the maximum specificatiofnorthe instrumentused. Fine dropletswere notobserved toadhere uniformlyorotherwisetothe wallsofthe meltingpointtubes. CONCLUSIONS The meltingpoint/meltingrange was notobserved and thereforecould not be determined. Remarks: While no meltingofthe testsubstance was evident, discoloratioonfthe testsamples was observed. The whitepowder turned toa lightbrown and eventuallyblackas temperaturesrose. Submifter: 3M Company, EnvironmentalLaboratory,P.O. Box 33331, St.Paul,Minnesota,55133 DATA QUALITY ReliabilityK:limischranking1. REFERENCES Study conducted at the requestof3M Company by WildlifIenternational, Ltd.of Easton,Maryiand. OTHER Last changed: 5/3/00 DEITYlvENATIONOF THE MELTING POINT/MELTING RANGE OF PFOS WILDLIFE INTERNATIONAL LTD. PROJECT NUMBEIL 454C- 106 OECD GuidelineforTestingofChemicals,102 MeltingPoint/MeltinRgange AUTHORS. Ronda L. Jacobs WillardB. Nixon,Ph-D. STUDY INITIATION DATE: December 18,1998 STUDY COWLETION DATE: Febnuay 24,1999 WILDLIFE Submittedto: 3M Cmparadon EavkonmeaW Labomtory P.O.Box 33331 St PauL Kmnesota 55133 INTERNATIONAL 8598 Comma= Diive Easton,Maryland 21601 (410)822-8600 Page I of 12 LTo. WILDLIFE INTERNATIONAL LTD. -2- PROJECT NO.: 454C-106 GOOD LABORATORY PRACNCE COMPLLANCE STATEMEENT SPONSOR: 3M Corporation TITLE: DeterminationoftheMeltingPointMeltingRange of PFOS WILDLIFE INTERNATIONAL LTD. PROJECT NUMBEF- 454C-106 STUDY COMPLETION: February24,1999 Tlw sb* was conductedin compliancevnth Good LaboratoryPracticeStandardsas publishedby the U.S. EnvirommentalProtectionAgency in40 CFR Part792, 17 August 1989 and OECD Principleosf Good LaboratoryPracticeO,CDE/GD (92)32,EnvironmentMonograph No. 45,Paris1992. STUDYDIRECTO .Ronda L. Jacobs,B.S6,,I' Senior Chemist WildlifeInternationLatlcL Z171c;" 9p DATE WILDLIFF- INTF-RNATIONAL LTD. -3 PROJECT NO.: 454C-106 QUALITY ASSURANCE STATEMENT Tiussb* was ommmod forcompliancewith Good LaboratoryPracticeStandardsaspublishedby the U.S. EnvirommentalProtectionAgency in40 CFR Part792, 17 August 1989 and OECD Principleosf Good LaboratoryPracticeO,CDEIGD (92)32, EnvirontaentMonograph No. 45, Paris1992. The datesof all inspectionsand auditsand the datesthatany finchngswere reportedto the Study Directorand Laboratory Management were as follows: AC=Y: MeltingPoint Dmft Reportand Data FinalReport DATE CONDUCTED: December 18,1998 D ecember 23, 1998 Feb=q 1,1999 DATE REPORTED TO:' STUDY DHZECTOR: MANAGE2vDENT: December 19, 1998 December 18, 1998 December 23, 1998 Deccmber 23,1998 Febmary 1,1999 FebnuiTy1,1999 Linda R. Mitchell,B.S. Manager, QualityAssurance DATE WILDLIFE INTERNATIONAL LTD. -4- PROJECT NO.: 454C-106 REPORT APPROVAL SPONSOR. 3M Corporation TrrLE: Determinationof theMeltingPoint/MeltingRange ofPFOS W]ILDLEFE RMRNATIONAL LTD. PROJECT NUMBER- 454C-106 STUDY DIUCTOR: Ronda L. Jacobs g@@' SeniorChemist MANAGEMENT: WillardB. Nixon,Ph.D. Manager, AnalyticalChemistry DATE BA-TE WILDLIFF- INTE:RNATIONAL LTD. PROJECT NO.: 454C- 106 TABLE OF CONTENTS TitletCoverPage .......................................................I ............ Good LaboratoryPracticeCompliance Statement ...................................2.......... QualityAssurance Statement ...............................................3............ ReportApproval ......................................................4............ Table of Contents ......................................................5............ Summary...........................................................6.............. Introduction..........................................................7............. Purpose ............................................................7............ ExperimentalDesign .....................................................7............. Materia@sand Methods ...................................................8............ Test Substance ...................................................8 ........... Test Procedure ...........................I ................................8....... Results .............................................................9............ MeltingPointand MeltingRange ........................................9............ Conclusions .........................................................9............ References ...............................................................1.0 ........... TABLE Table 1 -DeterminationofMelting Pointand Melting Range forPerfluorooctanSeulfonicAcid,Potassium Salt(PFOS) .......................I.I..... APPENDIX Appendix I-PersonnelInvolvedintheSh* .....................................1.2.......... WILDLIFE INTERNATIONAL LTD. .6- SUNDIARY SPONSOR: SPONSOR'S REPREsENTATrvE: LOCATION OF STUDY, RAW DATA AND A COPY OF THE FINAL REPORT: 3M Corporation Ms. SusanA. Beach EnvironmentaLlaboratory P.O.Box 33331 St.PauL Minnesota55133 Wil&deInternatiLotnda.l Easton,Maryland 21601 PROJECT NO . 454C-106 WILDLWE INTERNATIONAL PROJECT NUMBER: LTD. TEST SUBSTANCE: STUDR. TEST DArEs: 454C-106 PerfluorooetaSnuelfoniAccid,PotassiumSalt(PFOS) DeterminatioonftheMeltingPoint/MeltinRgange of PFOS ExpmimentalStart-December 18,1998 XE!@@ Terminatio-nDwmber 18,1998 ProductChemistryTest IAELNNO P019r: R.esults None, k400*C, discoloratioobnserved Method WILDLIFE INTERNATIONAL LTD. -7INTRODUCTION PROJECT NO.: 454C- 106 WildlifeIntmTiationLatlcLaamnpted to detmmme themeltingpointand meltmg range of thetestsubstance PFOS (perfluorooetasnuelfaaicacid,potassiumsalt).Thisstudywas conductedby WildlifeInternationaLltd. for3M CorporationattheWildlifehitmmationaLltcLanalyticaclhenustryfacilitiynEaston,Maryland. The study was performed followingprocedures in the OECD Guiddine for Testing of Chemicals, 102, Melting PoinbMelting Range (1).The Werimental portionof thisstudywas conductedon December 18, 1998. The originarlaw datageneratedby WildlifeInternationaLltd.and a copy ofthefinalreportarefiledunderProject Number 454C- 106 in archivesloratedon the.WildlifeInternationaLltcLsite. PURPOSE The purposeof tiussb* was todetermme themeltingpomt and meltingrange of PerfluorooctaneSulfome, Acid,PotassiumSalt(PFOS). EXPERIMENTAL DESIGN The meltingpointisdefinedasthetemperatureatwhich dw phasetransitiofni-oma solidtoa liquidstate at&nospberic press= occurs.For some substances,thetransitioonccursover a range of temperaturesdefined as the meltingrange. Subsamples of the testsubstancewere heatedin a meltingpointtube in a temperaturecontrolledheatingblork. Measurements of the meltingpomt/meltingrange were limitedto K400'C (approdmately673 -K),diemaximum sp=ficationforthemsummtation usecl The temperatureatwhich fine dropletsA&ere uniformlytothewallof themeltingpointtubewould be acceptedas themeltingpoint Ifa ----_ maturermigewas notedbetween theformationof thefinedroplets(be&ning of melting)and transitiotno a liquid(endof melfing)a,meltingrangewould be reported.A BZchi Melting PointB-540 instrumentwas used. WILDLIFE INTE:RNATIONAL LTD. -8MATEPJALS AND MFTHODS PROJECT NO.: 454C- 106 TestSubstance The testsubstancewas receivedfrom 3M Corporationon October29, 1998 and was assignedWildlife intmnationaLltd.identificatinounmber 4675 upon receiptThe testsubstancea,whitepowder,was identified as:FC-95,LotNumber 217,ExpirationDate:2008.The testsubstancewas storedunder ambientconditions. Test Procedure A BBchiMeltingPointB-540 instrumenwtithmeltingpointtubessuppliedby Bf)chiwas used. The B6chi Melting PointB-540 instrumentwas calibrateadnd inspectejdustpriortouse usinganthraquinoneand 1,8naphthalimide. The meltingpointand meltingrangedeterminatioanttemptswere performedasfollows.Subsamples of thetestsubstancweeretrawfeffedtofourmeltmg pointcapillartyubestoa depthof approximately3 irnm The tubes were tamped topack thetestsubstance.One subsamplewas subjectedto a rapidtemperaturescan to determme an appmxunate meltmg point An approxanatemeltingpointcouldnotbe determine& The test substmm mmad alighbtrown colorand thenblackened Fine dropletwsere notobserved.The msbumwt was thenprogrammed to incrementthetemperatureovera rangeof 300 to4000C at-a rateof IOC/niimft.Ilm meltingpointand range fortheremainingffim subsampleswere attempted.At no fim during the testinogf PerfluorooctanSeulfonicAcid PotassiumSalt(PFOS) were 6= dropletosbservedto adhere unifom2lyorotherwiseto thewaus ofdiemeltingpointtubes.The threeremainingsubsamplesreactedin a similarmanner as therapidtemperatursecansubsample.The whitepowder tamed toa lightbrown. As'the ,I I nwm hi=ased,PerfluorooctaSnuelfoniAccid,PotassiumSalt(PFOS) darkeneduntiliteventualltyurned black. When approaching400*C, some ofthetestsubstancelosttheblackenedcolorand turnedto a clear, . crystal-lipkaerticulateT.he remainingtestsubstancestayedbladl The barometricpressurewas recordedat thetimeofthemeltingpointtmeltinrgangedeterminations. WILDLIFE INTERNATIONAL L-rD. -9- RESULTS PROJECT NO.: 454C- 106 MeltinPgoinatndMeltinRgange The resultosfthemeltingpointandmeltingrangedewnninafionasrepresentedinTable 1. Finedroplets werenotobservedtoadhereuniformloyrotherwisteothewallsofthemeltingpointtubes.Thereforea,melting pomt/meltingrangeforPerfluorooctaSnuelfoniAccid@PotassiumSalt(PFOS) was notdetermined. CONCLUSIONS A productchemistrytestwas performedtodeterminethephysicalcharacteristoifcsthetestsubstance PcrfluoroocumSulfoniAccid,PotassiumSalt(PFOS). The meltingpoint/meltirnagngewas notobservedand thereforceouldnotbe determined. WILDLIFE INTERNATIONAL L-rD. -10- PROJECT NO.: 454C-106 REFERENCES 1. OrganisatiofnorEconomic Cooperationand Development 102.GuidelineforTestingofChemicals, 102:MeltingPointIMeltinRgange. WILDLIFF- INTF-RNATIONAL LTD. PROJECT NO.: 454C-106 Table1 DetmmainatioonfMeltmg Pomt andMeltingRange for PerfluorooetaSnuelfoniAccid,PotassiumSalt(PFOS) Subsample ID Rep 1 Subsample Amount (MM) 3 b2sbunent Gradient (OC/Min) 1 Barometric Pressure (mmHg) 770 Rep 2 3 1 770 Rep 3 770 Melting Point (-Cand-K) None observed None observed None observed Melting Range (-Cand-K) None observed None observed None observed WILDLIFF- INTERNATIONAL LTD. -12- APPENDIX I PersonnelInvolvedintheStudy PROJECT NO.: 454C-106 The followinkgeyWildlifIentmuationaLltcLpersomelwereinvolved"M'theconductormanagement of thish*: 1. WillardB.Nixon,Ph.D.,Manager,AnalyticaClhemistry 2. Ronda L.Jacobs,SeniorChemist 3. KeriLeach,Technician PROTOCOL DETERMINATION OF THE MELTING POINT/MELTING RANGE OFPFOS OECD GuidelineforTestingof Chemicals,103 MeltingPointMeltingRange 3M Lab RequestNo. U2723 Submittedto 3M Caporafim Laboratory P.O. Box 33331 St.Paul,Mftmesota 55133 WILDLIFE INTERNATIONAL 8598 Commerce Drive Easton,Maryland 21601 (410)822-8600 LTE). December 2,1998 PROTOCOL NO.: 4541120298/103/SUB454 3M LAB REQUEST NO. U2723 WILDLIFE INTERNATIONAL L-rD. -2- DETERMINATION OF THE NCELNNG POR4T/UELTING OF PFOS RANGE SPONSO 3M Corporation EnvironmentalLaboratory P.O. Box 33331 St Pmd, Minmota 55133 SPONSOR!S REPRESENTATIW- TESTING FAC Ms. Susan A. Beach VrddlifeIntm-nationLatl(i 8598 Commmw Drive E&ston,Maryland 21601 STUDYDIRRR-TOR- Ronda Jacobs SeniorChemist LABORATORY MANAGEMENT Vrdlud B. Nixon,Ph.D. Manager of Chemistry FOR LABORATORY Proposed Dates: Experimental StartDate: Pmjqct No.: I Fr c- 9 o' z4Se4Cl-e)&- Test Substance No.: USE ONLY Experimental TerminationDate: Int/Date: I ReceiptDa te@ All-1 Z9 OD @>,p c@ 9,@ PROTOCOL APPROVAL DIRECTOR @Vh SPONSOR!S REPRESENTATIVE PROTOCOL NO.: 454/120298/103/SUB454 / ? &. DATE 9,p DATE /<7 DAT9 3M LAB REQUEST NO. U2723 WILDLIFE INTERNATIONAL LTD. -3- INTRODUCRION WildlifeInternationaLltd. willdeterminethe melting pointor meltingrange of PFOS (p@@ sulfoniaccidp,otassiumsalt)T.he sb* willbe conductedattheWildlifIenternational Ltd.analyticcahlemistrybm* inFmton, Marylon& Ile sb* willbe performedfollowingprocedures' inOECD CjW&IineforTestingofChemicals,102,MeltingPointImeltingRange (1).Raw dataforall work performed atWildlifelatmmationaLltd.and a copy of the fitw reportwillbe filedby project munber inarchiveslocatedatWildlifeInternationaLltcLor atan alternativleocationtobe specifieidn thefinalreparl PURPOSE The purpose of thisstudy isto determinethemeltingpointor meltingrange of PFOS. E20EERMNTAL DESIGN The meltingpointisdefinedas thetemperatureatwhich thephase transitiofntm a solidto a liquidstateatatmosphericpressureoccurs.For some substances,the transitioonccurs over a range of ten4=aam definedas themeltingrange. Subsamples of the testsubstancewillbe heatedin a pointUibeinakmpagm-m@Ucd heatingblockcmuuung a meltmg pointcapillaryM=m=cnt of meltingpointswillbe limitedto :@400*C (approxim@ly 673*K), themwdmmn specifiefdorthe mmutattm used.The wmperat= atwhich finedropletasdhereumfm* tothewallof themelting pointtubewillbe acceptedas themeltingpoint Ifa rangeof tm4wature isnoted between the formation ofthefim droplets(beghmingofmelbng) andtransititoona liquid(endofmelfing),a meltingrangewill be reported. MATERIALS AND METHODS TestSubg= The Sponsor willbe asked to providethefollowinginformationconcerningthetestsubstance, ifavailable: ChemicalName (ordesignation) Lot or Batch Number Picity Composition(formulti-CO@@ Empiricalformula(s) ExpirationDate mi-Ilum) The attachefdorm EI)EMMCATION OF TEST SUBSTANCE BY SPONSOR (Appendix 1) istobe usedtoprovideavailablien@@on. no Sponsor isresponsiblfeorinformationon thepurity and compositionof thetestsubstance,as well as allinformationrelatedto the safehandlingof the test PROTOCOL NO.: 454/120298/103/SUB454 3M LAB REQUEST NO. U2723 WILDLIFE INTERNATIONAL LTD. -4- substance. The Sponsor alsoagreesto acceptany unused testsubstanceor testsubstancecontainers remainingatthe end of the study. Test Procedure Mx meltingpointorrangewillbe ddammed usinga BficluMeltingPointB-540 instrumentwith meltingpointtubessuppliedby Bachi. The instrumentwillbe calibratepdriortousewith a minimum oftwo referencsetandards.Subsamples of thetestsubstancewillbe transfmtedto a minimum of three capillarytubes to a depth of approximately3 irnrnTubes willbe tamped to pack the testsubstance. Following an initiarlapidscan(s)to determinean approximatemeltingpoint,thefishument willbe programmed to ft==ent the temperatureover the meltmg pointor range at a ratenot to exceed I'Chntmft The WMeralm atwinch finedropletusniformlyadh= tothetubewallwillbe accepted asthemeltingpoint ifthetempmt= inwmm significant(laypproximatel2y*C or more) between theformationofthefinedropletsadming tothetubewaN untilhquificatioan,meltmg rangewillbe reported. The nrltingpointorrangewfflbe reomded in *C and reportedboth in OC and OK The barometric pressurewillbe recordedatthe time of measurement of themeltingpointor range. Sw=te Handling and gafdy The Sponsor willidentifyany specialhandlingor safetyprecautionsto be used with the above referencedtestsubsu=. An normal precautionswithrespecttohandlingand storageVAU be twkcm SuWga and Test Substance Upon completionof testingp,ortionsof thetestsubstanceused as partof tiusstudywillbe disposedof in accordancewith fakral stateand localregulationsA.ny wmsed portionof the test substancewillbe returnedto the Sponsor. RECORDS TO BE MAI Records to be maintainedfordata generatedby WildlifeIntmnationalLtd.willinclude,but not be limitedto: I. A copy of ffiscignedprotocol 2. Identificatiaonnd dwactaizafion ofthetestsubstance,ifprovidedby theSponsor. 3. Dates of initiatioand completionof thestudy. PROTOCOL NO.: 454/120298/103/SUB454 3M LAB REQUEST NO. U2723 WILDLIFE INTERNATIONAL L-rD. 4. Dates of experimentalstartand termination. 5. Storageconditionsof thetestsubstance. 6. Test substanceuse log. 7. The instrumenttemperatureprogram. 8. Individualand mean meltingpointmeasurements expressed in *C and *K. 9. Statisticaclalculations. 10. Test conditions. 11. A copy offl@t'finrgeporl FINAL REPORT A firwreportoftheresultosfd3csb* willbe preparedby WildlifeInternationaLltd. The report willincludeb,ut notbe limitedtothefollowingw,hen applicable: I. Name and addressof the facilitpyerformingthe study. 2. Dates upon wlnch the studywas unuated and completed. 3. A statementof compliancesignedby de Statr Directoraddressingany exceptionsto Good-, LaboratoryPracticeStandards 4. Purpose and procedure,as statedin the approved pmtorol mclu(hng allamendments and deviationsto theprotocol. 5. The testsubstanceidentlficatiomne,hidmg name, chemical abstractnumber or code number, purity,compontion,empiricalformula,molecularformula,manufachutes lot/batchnumber, dissociatioinnwater,method of analysiso,rotherinformationprovidedby theSponsor 6. Dmcriptionoffliteestnv:thodorrefaa= tothemethod used alongwith any modificationsmade. 7. Individualandmean valuesobtainedforthenwltingpointor rangeexpressedin *C and *K 8. Descriptionof any problems experiencedand how they were resolved. 9. A smement preparedby theQualitykumm= Unitlistintghedatesthatsb* ins@ons and auditswere made and any findingsthatwere recorded. CHANGING OF PROTOCOI,. Plmied changes to the protocolwillbe inthe form of writtenamendments signedby the Study DiectorandtheSponsor. Amendments willbe consideredas-partoftheprotocoland willbe attached tothefinaplrotocolAny odw &wigm willbe intheform ofwrittendeviationsfiledwiththeraw data. Allchangestoffipcrotocolwillbe indicatedinthefinalreporl PROTOCOL NO.: 454/120298/103/SU]3454 3M LAB REQUEST NO. U2723 WILDLIFE INTERNATIONAL LTD. -6- GOOD LABORATORY PRACRICES Tlus studywillbe conductedaccordingtotheGood laboratoryPracticedsescribeidnOECD (ISBN 92-84-12367-9a)ndEPA (40CFR Parts160 and/or792).Each studyconductedby Wildlife InternationLatld.isroutmelyexw=ed by theWildlifleatmmabonalLtd.QualitAyssuranceUnitfor compliancewithGood LaboratoryPractoesS,tandardOperatingProceduresand thespecifiepdrotocol. A statemenotfcompliancewithGood LaboratorPyracticewsillbe preparedforallportionsof thestudy conductedby WildlifIenternationLatld. The SponsorwillberesponsiblfeorcompliancevnthGood LabmtoryRacbcc@forpmce&m performedby od=W*ratones. Raw dataforallwork performed atWildlifIenternationLatld.and a copyofthefinarleportwillbe filebdy projecntumber inwreves locatedon theWildlifIenternationLatld.siteoratan altemativleocatiotnobe specifieidnthefinal reporl PROTOCOL NO.: 454/120298/103/SUB454 3M LAB REQUEST NO. U2723 WILDLIFE INTERNATIONAL L-rD. -7- RMEENCES 1. OrganisatiofnorEconomic Cooperationand Development.102.CjWdeline'forTwfimot ChcmicalsM,eldng PoinbMeltinRgange. PROTOCOL NO.: 454/1202981103/SUB454 3M LAB REQUEST NO. U2723 WILDLIFE INTERNATIONAL LTD. -8- -.WMCATION APPENDIXI OF TEST SUBSTANCE BY SPONSOR To be Completed by Sponsor I. TestSubstance Identit(yname tobe used inthereport): tmb=Qglam SulfonicAcid- Potassium Salt Sample Code orBatch Number. Lot 217 Purity(/oActiveIngredient)9:8.90/9 ExpirationDate: 2008 U. Test Substance Charactmizafion Have the*Iden!ttiy,ig,FlI-4Ik purityand compositionorotherchwactedstics which appmO?Lat* defim thetestsubstancebeen dckmiinw prior tothe to thissktudyinaccarda= with GLP Standards? Yes-No X M. Test Substance StorageConditions Plem indicatetherecommended storageconditionsatWildlifeInternatiorLwtd. Ambient mbm kmpm=- Has thestabilitoyfthetestsubstanceunder thesestorageconditions been determinedin accordancewith GLP Standards? Yes No X Otherpartiamtstabiliitnyfmnfion: IV. ToxicityInfomnfion: mammalian: Rat LD50 251 mg&g Mouse LD50 Aquatic: InvertebratTeoxicity(ECtLC50) FishToxicity(LC50) piamagan- 27 mgl Rainbow trout4II mgil amimia mague 50 mWL Fatheadmina= 38 mr)L Other Tomcity Information(mcludmg finchngsof dvmc See MSDS. and subchronictests): PROTOCOL NO - 454/12029R/I 0'1/.RTTR4rtA '2)6ifT A13 OlUfNTTV"'kTfN TVINPFIN"