Document 06b1me47qJ4OBRn8bomdDXvaJ

I Determination ofthe Vapor Pressure of PFOS Using the Spinning Rotor Guage Method VAPOR PRESSURE TEST SUBSTANCE Identity:Peffluorooctanesulfonatmea;y alsobe referredtoas PFOS or FC-95. (1-Octanesulfonicacid,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 testsubstance isa whitepowder. Sample was taken from 3M lotnumber 217. Sample was storedunder ambientconditions priortotestingP.uritydeterminedto be 90.49% by LC/MS, 'H-HMR, '9FNMR and elementalanalyses techniques. METHOD Method: OECD 104, U.S. EPA OPPTS 830.7950 GLP (YIN): Yes Year completed: 1999 Remarks: Determinationofthe vapour pressurewas done by using the SpinningRotor Gauge method. RESULTS VaporPressure: 3.31XIO-4Pa Temperature OC: ' 200C Decomposition (yes/no/ambiguous): No Remarks: The measured vapour pressurewas repeatable. CONCLUSIONS Remarks: The vapor pressureofthetestsubstance was determinedto be 3.31Xl 0-4 Pa at 200C usingthespinningrotorgauge method. 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, Maryland. OTHER Last changed: 5/3/00 DETERMINATION OF THE VAPOR PRESSURE OF PFOS USING THE SPBQNING ROTOR GAUGE METHOD WILDLIFE INTERNAT10NAL LTD. PROJECT NUMBER. 454C-105 OECD Guideline104 Vapour PressureCurve U.S. EPA OPPTS 930.7950 Vapor Pressure AUTHORS: Raymond L.Van Hoven, Ph.D. JoelL Stenzel WfflardB. Nbwn, Ph.D. STUDY RUMTION DATE: January12,1999 STUDY COMPLETION DATE: May 5,1999 Submittedto 3M Cwparation EavionniontdLaboratory 935 Bush Avenue 3M Building2-3E-09 P.O.Box 33331 St PauL Mimmota 55133 .WILDLIFE INTERNATIONAL LTD. 8599 Commm-ce Drive EuM Maryland21601 (410)822-8600 Page I of26 WILDLIFE INTERNATIC)NAL LTD. -2- PROJECT NO.: 454C-105 GOOD LABORATORY PRAMCE CONTLIANCE STATEMENT .SPONSOR. 3M Corporation TITLE: DeterminatioonftheVapor PressureofPFOS UsingtheSpinningRotorGauge Method WILDLIFE INTERNATIONAL LTD. PROJECT NUMBEP, 454C-105 STUDY COMPLETION: May 5,1999 Ttussu* was conductedincompliancewithGood LaboratoryPracticSetandardsaspublishedby theU.S. EnvironmentdProtectioAngency in40 CFR Part792, 17 August 1989;OECD Principleosf Good Laboratory PracticeO,CDE/GD (92)32,EnviromuentMonograph No. 45,Paris1992;and JapanMAFF, 59 NohSan, NotificatiNoon. 3950,AgriculturParloductioBnureau,10 August1984,withdw followinegxceptions: The testand refm-encseubstanceswere notcharacterizeidncompliancewithGood LaboratoryPractices Standards. The stabiliotfythetestsubstanceand referencsetandardsundertheconditionastthetestsitewas not testedincompliancewithGood LaboratoryPracticSetandards. STUDYDIRECTO &. l@/VVan/Hz@nv@enH,c@h.D. Scientist SPONSOR APPROVAL: Sponsor DATE DATE WILDLIFE INTERNATIONAL LTD. -3- PROJECTNO.: 454C-105 QUALITY ASSURANCE STATEMENT SPONSOR- 3M Corporation TITLE: Determinatioonf theVapor PressureofPFOS Using theSphming RotorGauge Method WU,DLU@E INTERNA NONAL LTD. PROJECT NUIVMER- 454C-105 Thisstudywas exanunedforcompliancewithGood laboratoryPracticSetandardsaspublishedby the U.S.EnvironmentaPlrotectioAngency in40 CFR Part792, 17 August 1989;OECD Principleosf Good LaboratoryPracticeO,CDEIGD (92)32,EnvironmentMonograph No. 45,Paris1992;andJapanMAFF, 59 NohSan,NotificatiNoon. 3850,AgriculturParloductioBnureva,10August 1984.The datesof allinspections and auditsandthedatesdid anyfmcbngswerereportetdotheSb* Dinzwr andLaboratoryManagement were as follows: ACTrVrrY: TestSubstancPeremalion and TestInitiation Measurement One DraftReportand Data FinalReport DATE CONDUCTED: January27, 1999 January29,1999 FabniM 24,1999 May 5,1999 DATE REPORTED TO: STUDYDnuzmp- MANAGEIVIENT: Januar2y7. 1999 January29,1999 February24,1999 May 5,1999 Januezy27,1999 January29, 1999 Febnimy 25,1999 May 5,1999 LisaT.Drottar DATE QualitAyssuranceRopm=utive WILDLIFE INTERNATIONAL LTD. -4- PROJECTNO.: 454C-105 REPORT APPROVAL SPONSOR-- 3M Corporation TITLE: DetenninatioonftheVapor PressureofPFOS UsingtheSpinningRotorGauge Method W]ILDLJFE INTERNATIONAL LTD. PROJECT NUMBEIL- 454C-105 STUDY DIRECTOR. RwymYt@dL.-@tanHoven, Ph.D. scientist MANAGEhffi'NT WfllardB. Nixon,Ph.D. Manager,Analy&d Ch=istry DATE DATE WILDLIFE INTERNATIONAL PROJECTNO.: 454C-105 TABLE OF CONTENTS Title/CovePrage..........................................................................1 ............... Good LaboratoryPracticCeomplianceStatement...............................................2................ QualityAssuranceStatement...............................................................3................ ReportApproval.............................................................:........................4............................ TableofContents...................................................................................................5............................... Summary ...............................................................................7............... Introducti.o.n...........................................................................8............... Objectiv.e....................................................:....................................................8.............................. ExperimentalDesign......................................................................8............... Materialasnd Methods...........................................................................8............... Resultsand Discussion...................................................................1.2............... Conclusion.............................................................................1.3.............. Refertmees.............................................................................1.4.............. TABLES Table1. Steady-StaPtreessureofPFOS Sample..............................................1.5.............. Table2. PressureIncreasoefPFOS Sample..................................................1.6............... Table3. Steady-StatPeressureofControlSample.............................................1.7.............. Table4. PressureIncreaseofControlSample................................................1.8.............. WILDLIFE INTERNATIONAL LTD. -6- PROJECTNO.: 454C-105 TABLE OF CONTENTS Continued- FIGURES Figure1. Diagramofhighvacuum systemconfigurati.o.n.....................................1.9................ Figure2. Diagramofsampleintroduefisoynstem..............................................................2.0................ Figure3. Graphicaplresentatioofnoffsemteasurement.......................................2.1................ Figure4,. Sw*-state pressureandpressureincreasoefHexachlorobenzmesample................2.2.............. Figure5. Steady-statperessureand pressureincreasoef DDT sample............................2.3................ Figure6. Stm4-statepressureandpressureincreasoefPFOS sample...........................2.4................ Figure7. Steacbr.-stparteessureand pressureincreasoef Controlsample..........................2.5................ AppendixL APPENDICES PersomelInvolvedintheStudy...............................................2.6................ WILDLIFE INTERNATIONAL LTD. ,7" SPONS01;L SPONSOleS REPRESENTATM: LOCATION O'FSTUDY, RAW DATAANDA COPY OF THE FR-4AL REPORT: SUAUAARY 3M Corporation Ms. Susan A. Beach WildlifIenternationLatld. Easton,Maryland 21601 PROJECTNO.: 454C-105 WMD= INTERNATIONAL LTD. PROJECT NUMBER: TEST SUBSTANCE: STUDY: TEST DATES: 454C-105 PFOS (PerfluorooetaSnuelfonicAcid,PotassiumSalt) Detmmiinationof theVapor PressureofPFOS Using the SpinningRotor Gaugr,Method ExperimentalStart-January27, 1999 Termination-Febmuy 12,_l999 SUMMARY: The vaporpressuroefPFOS was determinetdobe3.31x 10'4 Pa at20*C mg the spinningrotorgauge method. Wi LD LiFE NTER NATI 0 NAL LTD. -8- PROJECTNO.: 454C-105 INTRODUMON ThistudwyasconductbeydWildliIfneternatiLotndaf.lor3M CorporataitotnheWildliIfneternational LtcLanalyticcahlemistryfaciliitnyEaston,Maryland.Testswere performedusingthe spinningrotorgauge method. Ilm vaporpressuroefthetestsubstancweas ana4-zedfromJanuary27 toFebmary 12,1999. Raw data generatebdy WildlifIenternationLatlcLanda copy ofthefinarleportarefileudnderPmjectNumber 454C-105 inarchivelsocateodn theWildlifeInternationLatld.site. OBJECTIVE The objectivoefthisstudywas todeterminethevaporpressureofPFOS at200C usingthespfimingrotor gauge method. EXPERIMNTAL DESIGN The spinningrotorgauge(SRG) systemwas usedtodeterminevaporpressure.The SRG measuredthe rotationaflrequenryof a stainlesssteeblaU thatwas magneticallsyuspendedvnthm a vacuum chamber T"ne deceleratiroanteoftheballwas used todeterminethegaspressure.The systemwas configurewdithtwo sample chambers.One ofthesmnplechamberscontaineadsampleofdietestsubstancew,hiletheod= remained=VtY tomake omtrolmeasurements.The systemswady-statperessureand pimsurem=ase ofthetestsubstanceand controslamplesweremeasureddnw U=. MATERL4LS AND M[ETHODS Thisstudywas conductedbasedon procedureosutlineidnOECD GuidelineMse,thod 104 (1);andEPA OPPTS 930.7950(2).The spinningrotorgaugemethod was usedtodeterminethevaporpressureofthetest substance. TestSubstance The testsubstancewas receivefdrom 3M Corporatioonn October29, 1998,and was assignedWildlife IntmmationaLltd.identificatniuomnber 4675 upon receiptT.he testsubstancea,whitepowder,was identified WILDLIFE INTERNATIONAL LTD. -9- PROJECTNO.: 454C-105 as: FC-95,Lot217,3M M#: 98-0211-3916-1.Based on informatiosnuppliedby theSponsor,thetest substanchead a purityof 98.9% and an averagemolecularweightof538 AMIJ. The testsubstancewas stored underambientconditions. Refemee Substances The hcxachlorobenzenreeferencesubstancewas receivedfrom Aldnch ChenucalCompany on February10,1997,andwas assigaedWildlifIenternationLatlcLidentificatniuomnber 3948 upon receiptThe refemce substancea,whitepowder,was identifiaesd:Heutchlorobenzene;'catanloo.g17105-0,CAS Number 119-74-1. The referencseubstancehad a reportedpurityof 99%, andwas storedunderambientconditions. The DDT referencseubstancewas receivedfrom AldrichChemicalCompany on January20, 1999,and was assignedWddlifbInternationLatld.identificatniuomnber 4749 upon receiptT.he referencseubstancea, whitepowder,was ideatifiaesd:1,1-bis@Chlorophenyl)-2,2,2-Tricbloroleoftlnmuwm;ber 77 H3614; catalog no.C8894, CAS Number 50-29-3.The refemce substanchead a reportedpurityof 99.3%,andwas storedin a refrigerator. Aj@paratusC onfiMnt@ion I'helughvacuum systemconsisteodfa vacuum pump (LoyboldTRIVAC S 1,6B),a Wrbomolecularpump (IAyboldTURBOVAC 50),an iongauge andcontroll(eMretra731 DigitaIlonGauge Controllera)S,P*M*=9 rotorgauge(LvjMd VISCOVAC VM 212),a samplekto4uWm systm@ and varioustainless-stc.ocne-lflat fitbngsi,ncludintgb= valves.Ilm em-flatfiumgswereassembledusingcoppergl*ets.The valvesw= used toisolattehesamplechambers,thespinningrotorgaugeand/orthevacimm pumps. Ile sp@@ rotorgauge controllwears connectedto a computerviatheseriailnterfac(eRS-232port).A diag= of theapparatus configuratiiosnpresentedinFigure1. The sampleintroductiosnystemwas customdesignedand manufachu-edby At-Mar GlassCo. (Kennett Square,PA). IU wistemconsisteodf twohighvacuum glasssampletubes.Duringthestudyo,ne tubecontained a sampleofthetestorreferencseubstancewhiletheothertuberemainedempty (control)T.he temperaturoef thesamplesweremaintainedby iinmrsingthesampleUA= ina waterbath.The temperaturoefthewaterbath was periodicalmloynitoredusinganASTM 44C m=ury thermomew. The tubeswereindependentlvyented and connectedtothevacuum systemusingthreeground-glasstopcocks.A glassto metaltransitiofnlange Wl LD LlFE INTER NATI 0 NAL L-m. -10- PROJECTNO.: 454C-105 connectedthesampleintroductisoynstemtothevacuum system A diagramofthesampleintroductiosnystem ispresentedinFigure2. A steelbaU was inserteidntothespinningrotorgauge tubebeforethetubewas connectedto thehigh vacuum systenlThe con-flaftittingasndvalvesofthehighvacuum systmnwerewrapped inheattape.The temperaturoeftheheattapewas controlleudsingarheostatThe surfacetrmperaturoefthevacuum Vsternwas periodicalmloynitoredusingan Omega Model HH23 digitatlhermometer(Omega Engineming,Inc.S,tamford, CT) witha thermocouplpelacedbetw= theheattapeandtheoutersurfacoefthefittingsT.he airtemperature alsowas periodicalmloynitoredusingthedigitatlhermometer. Procedures The highvacuum systemwas heatedtoapproximately80'C and evacuatedforatleast18 hourspriorto maldng anymeasurements.Afterheatingd,w systemwas allowedtocooluntirleachingroom temperature.ne steelbaU insidethesphmingrotorgaugetubewas suspendedina magneticfieldand driventoa rotational frequencyofapproximatel4y15 Hz. The deceleratiornateof thebaH was monitoredusingthespinningrotor gauge. The parametersof the spbmingrotorpuge were setto recorda deceleratimoenasurementevery 30 secondsbasedm themoleculawreight(28.96g/mole)andviscosit(y18.2x IV Pa-s)ofair.The offsevtalue was determinefdoreachsampletubewhen dw deceleratirmatereacheda plateau.The offsetvalue(mean deceleratiroante)was enteredintothespmmng rotorgauge controller A sampleofhmachlorobenzenewas placedinone ofthesamplechambers,whiletheodw chamber remainedempty (control)1.1@-p.arametersofft spmmng mtor gmigewerechangedtorecordpressurei,nPascal (Pa),every30 so=ids. Thissettinwgas usedforallsubsequentmea urements.The molecularweightparameter was setto284.78and viscositwyas settozero.The samplechamberwas evacuatedto achieve'aswady-state pressure.Temperatureswere periodicalrleycorded.Afterthe systemreachedtemperatureand pressure equilibriumt,hesteady-staptreessureofthesamplewas measuredwiththesphmingrotorgauge.Ilm valvesto thevacuum pumps werethenclosed,and thepressureincreasweas monitoredforatleastwo hours. A sampleofDDT was placedinone ofthesamplechambers,whiletheotherchamber remainedempty (control)T.he moleculawreigbtparameterwas setto354.5andviscositwyas settozero.The samplechamber was evacuatedtoachievea steady-staptreessure.Temperatureswereperiodicalrleycorded.Afterthesystem WILDLIFE INTERNATIONAL LTD. PROJECTNO.: 454C-105 reachedtemperatureand pressureequilibriumt,hesteady-statperessureof thesample was measured with the spinningrotorgauge. The valvesto thevacuum pumps were thenclosed,and thepressureincreasewas monitoredforatleasttwo hours. A smallsample of thetestsubstancewas placedinone of thesample chambers,whiletheotherchamber remainedempty (control)n.e molecularweightparameterwas setto538,and viscositwyas.settozero.The sample chamber was opened tothevacuum system and pumped-down toa stady-statperessure.Temperatures were penodicaflyrecorded.Afterthesystemreachedtemperatm*eand pressureequilibriumt,he steady-statr, pressureofthesample was measured withthesphming rotorgauge. The valvestothevacuum pumps were then closed,and thepressureincreasewas monitoredforatleastatleasttwo hours.Mc&sw=ents thenalternated betwetm thePFOS sample and thecontrolsample(empty sample chamber)fora totalofthree Of each. Calculations The steady-statperessureswere determinedby averagingthepressurevaluesrecordedpriorto.closingthe valvestothevacuum pumps duringeachmeasurement. Standarddeviationasnd 95% confidencefiftrvalwsere alsocalculated. The pressureiname datawere analyzedusingleast-squam-filtinearegressioannalysisA.linewas fit totheportionofthedatathatwas determinedtohave achievedequilibriupmressurewithdw soVIe. The slope and intercepwtere calculatefdorea& meammmt. Correlatiocnoefficienatnsd 95% confidencekdwvals for each parameterwere alsocalculate&The out-gassmgratewas determinedfi-omtheslopeof the lineand the vapor pressurewas determinedfrom dw hitercept-value. The means and standarddeviationosfthereplicatmeeasurements of thecontroland PFOS sample were alsocalculated. WILDLIFE INTERNATIONAL LTD. -12- PROJFCTNO.: 454C-105 RESULTS AND DISCUSSION A graphicaplresentatioofntheoffsemteasurementisshmm inFigure3. Thegraphsshow datacollected forapproximatel2y hoursfrom eachsampletube.The mean offsetvaluewas basedon theaveragedeceleration ratenimured fromleft(7.877x 10-3s-')andright(6.838x 10-8i@-1s)an3plechamberson January6,1999. The offsetvaluewas determinedtobe 7.357x 10-8s-'. I The steady-staptreessuraendpressureincreasoefh=chlarobenzent'weredetmmlinedon January14,1999, and arepresentedinFig= 4. The steady-staptreessurewas 1.24x 10'sPa and thevaporpressurewas determinetdobe 8.30x 10' Pa. The vaporpressurewas consistenwtiththerangefoundintheliteratu(r2e). The steady-staptreessureand pressureincreasoef DDT were determinedon January22, 1999,and are presenteidnFigute5. The ste@-statepressurewas 4.81x 10-6Pa and ft vaporpressurewas determinedto be 1..7x6 10-4 P& The vaporpressurewas consis@t withtherangefoundintheliteratu(r3e). The stra@-statpcressureandpressurem=ase ofPFOS were ddmnuned m February3,5 and 12,1999. The mean swady-statepressurewas 4.51 x 10-6Pa (Table 1). For each associatedpressureincrease measurement,theslopeofthepressureincreasdeatabecame constantaftearpproximatelnyimv minutes.This indicatetdhesystemhad achievedsaturationf thegasfrom ffiPcFOS sample.A linewas fittothisregionof thedata,andtheslopeandintercepwteredetermined.The int=cptvaluesrepresentedde vaporpress= ofthe smnple.The me= vaporpressuroefPFOS was 3.31 x 10'4 Pa (Table 2). A representative graphical presentation ofthedataisshown inFigure6. - The sW-ady-statp@r-e.ssureand pressureincreaseof thecontrolsamplewere det=iirtedon February2,4, and 8,1999.The mean baselinperessurewas -1.22x 10'6Pa (Table3).Foreachmeasur=en@ dieslopeofthe pressuremereasedatabecame constantafterapproximatelythirtmymutes, indicatantghesystemhad achieved equilibriumA linewas fitothisregionofthedata,and theslopeand intmreptweredetermined.The slope valuesrepresentetdheout-gassinrgateof thesystem.The mean out-gassinrgatewas 4.78 x 10" Pa/see. (Table4).The intercepvtaluesrepresentetdhebackgroundpressureofthesystmn.The mean background pressurewas 1.51x 10-,P5a. The backgroundpressurewas consideredinsignificacnotmpared to thevapor WILDLIFE INTERNATIONAL LTD. -13- PPOIECT NO.: 454C-105 pressureof PFOS and was notsubtractefdrom thosevalues.A representafigvreaphicaplresentatioonfthedata isshown inFigure7. Occasionalldyuringthestudy,a leakdevelopedatone ofthegroundglassjointosfthesampleinb-odwtion system Thiswas c=ectedby adjustmgtheswpc@ and/orepositiomntghesampletubes-The spmnmg rotor gaugedisplayeedithe"rMnhffi TOO LONG* or"BAD SIGNAL"messages duringthestudyb,utwas restuw withoutanydifficulteiaecshtime. The mean temperatureof the,waterbath,duringmeasurementsof thePFOS sample,was 20.1*C and rangedfrom 19.50to20.500C. The airtemperaturreangedfrom 19.0to22.3"C,andthesurfacetemperature ofthevacuum systemrangedfrom 19.5to22.9-C. CONCLUSION Based on theresultfsrom threesetsof measurementscollectefdrom thesphmingrotorgauge,thevapor press= ofPFOS was determinedtobe 3.31x I Pa at200C. WILDLIFE INTERNATIONAL LTD. -14- PROJECTNO.: 454C-105 REFERENCES 1 OrgwiisatiofnorEconomic Cooperationand Development 1995.GuidelinfeorTestingofChemicals, Method 104,"VapourPressureCurve". 2 U.S.EnvironmentalProtectionAgency. 1996.OPPTS 830.7950,VaporPressureW.ashington,D.C. 3 TinsleyI,.J.1979.ChemicalConceptsinPollutioBnehavior.Vv-ileIynterscienNcew, York. WILDLIFE INTERNATIONAL LTD. -15- PROJFCTNO.: 454C-105 TrialNumber 1 2 3 Table 1 Steady-StatPeressureof PFOS Sample Date, 2/3/99 2/5/99 2/12/99 Mean = Si&Dev.= Steady-State Pressure (Pascal) 7.1440E-6 5.6664E-6 7.2968E-7 4.513E-6 3.359E-6 Standard Deviation 5.8716E-7 4.8038E-7 5.2793E-7 95% Confidence Interval 6.1426E-8 6.1158E-8 6.0657E-8 WILDLIFE INTERNATIONAL LTD. -16- PROJECT NO.: 454C-105 Table 2 PressureIncreaseofPFOS Sample Trial Number 1 2 3 Slope 95% Confidence (Pa/see.) interval 3.5926B-7 2.3696E-7 1.1970 E-7 3.5808to3.6044E-7 2.3607to2.3785E-1 1.1949 to1.1992 E-7 Means 2.386E-7 Std.Dev. 1.198 E-7 intm-cept (Pascal) 3.2796E-4 4.6090E-4 2.0452E-4 3.311E-4 1.282E-4 95% Confidence interval 3.1615to3.3977E-4 4.5107to4.7072E-4 2.0190to2.0715E4 Correlation Coefficient 0.99904 0.99875 0.99978 WILDLIFE INTERNATIONAL LTD. -17- PROJECTNO.: 454C-105 TrialNumber 1 2 3 Table3 Steady-SteAPcressureof ControlSample Date 2/2/99 2/4/99 2/g/99 me= = Std.Dev.= Baseline Pressure (pascal) -3.4529E-6 3.1513E-7 -5.2957E-7 -1.222E-6 1.977E-6 Standard Deviation 5.2286E-7 4.0515E-7 1.8258E-7 95% Cmfidcnce Interval *7.3013E-8 :t4.1621E-8 *2.2633E-8 WILDLIFE INTERNATIONAL LTD. -19- PROJECT NO.: 454C-105 Table4 PressureIncreasoef ControlSample Trial Number 1 2 3 Slope (Pa/see.) 95% Confidence Interval 5.2256 E-8 5.1886 E-8 3.9377 E-8 5.217'to5.234 E-8 5.186 to 5.191 E-8 3.936 to3.939 E-8 Means Std.Dev. 4.7940 E-8 0.7331 E-8 Intmrept (Pascal) 1.9635 E-5 1.7799 E-5 7.8875 E-6 1.5107 E-5 0.6319 E-5 95% Confidence Interval 1.917to 2.010 E-5 1.762 to 1.798E-5 7.781 to 7.994 E-6 Correlation Coefficient 0.99990 0.99998 0.99999 WILDLIFE INTERNATIONAL LTD. -19- PROJECT NO.: 454C-105 CS 07 6. ol C4"" 1. vacuum pump 6. turbomolecular pump 2. turbopump controller 7. Ion gauge tube 3. sample lntra.system 8. Ion gauge controller 4. constant temp. water bath 9. spinning rotor gauge controller 5. spinning rotor gauge head 10. personal computer I Figure1.Diagramofhighvacuum ratem configuration. WILDLIFE INTERNATIONAL L7D. -20- PROJECT NO.: 454C-105 ---U6 glasstometaltransition ground-glassstopcocks sample tubes water bath scissorslack Fig= 2. Diagramofsampleintroductiroinsterm WILDLIFE INTERNATIONAL LTD. -21- PROJECT NO.: 454C-105 I.OE-07- OffsetMeasurements 9.OE-08- 8.OE-08 7.OE-08 6.OE-08 I 5.OE-08 P.WtS-n* Tube 6.S4E4 @@ 0- ------o LcaSRMPT'uEbe 7.BSE4 4.OE-09 1/6/999:00 116/9910:00 1/6/9911:00 1/6/9912:00 1/6/9913:00 1/6t9914:00 time Figure3. Graphicalpresentationfoffsetmeasurement. WILDLIFE INTERNATIONAL LTD. -22- PROJECTNO.: 454C-105 2.2E-03 Steady@StatePressure and PressureIncrease ofHexachlorobenzene Sample 2.OE-03 1.8E-03 1.6E-03 1.4E-03 1.2E-03 1.OE-03 8.OE-04 6.OE-04 9.30E-M 4.OE-04 2.OE-04 O.OE+00 1/14/9914:00 1/14/9915:00 1/14/9916:00 Time 1/14/9917:00 Figure4. SWacly-statperessureand pressureinacaseof Hexachlorobenzenesample. WILDLIFE INTERNATIONAL LTD. -23- PROJECTNO.: 454C-105 1.4E-03 Steady-StatePressureand PressureIncrease of DDT Sample 1.2E-03 I.OE-03 8.OE-04 -- 6.OE-04 4.OE-04 -- 2.OE-04 -- L76E-04 O.OE+00 I 1/22/9911:00 1/22/9912:00 1/22/9913:00 Time Figure5. Steady-staptreessureand pressureinaeaseofDDT sample. 1/22/9914:00 WILDLIFE INTERNATIONAL LTD. -24- PROJECTNO.: 454C-105 3.5E-3 - Steady-StatePressureand PressureIncrease ofPFOS Sample 3.OE-3 - 2.5E-1 2.OE,-3 1.5E-3 I.OE-3 - 5.OE-4 - 3.2&E-04 O.OE+O 2/3/9911:30 2/3/9912:30 2/3/9913:30 Time Figure6. Swady-statperessureandpressurem=ase ofPFOS sample. 2/3/9914:30 WILDLIFE INTERNATIONAL LTD. -25- PROJECT NO.: 454C-105 4.OE-04 - Steady-StatePressureand PressureIncrease ofControl Sample 3.5E-04 - 3.OE-04 -- 2.5E-04 2.OE-04 -- 1.5E-04 -- 1.OE-.04 -- 5.OE-05 O.OE+00 212/99 12:30 d 2/2199 13:30 2/2/9914:30 Time Figure7. Swady-statperessureandpressm-cin=ase of Controlsample. 2/2/9915:30 WILDLIFE INTERNATIONAL LTD. -26- PROJECT NO.: 454C-105 APPENDDC I PersonnelInvolvedm theStudy The fouowmg keyWildlifeInternationLatld.persomelwereinvolvedm theconductor management of thisstudy: 1. WillardB.Nixon,Ph.D.,Manager,AnalyticaClhemistry 2. Raymond L.VanHoven, Ph.D.,Scientist 3. JoelI.StenzeLB.S.,SystemsAnalyst 4. KeriLeach,B.S.,LaboratoryTechnician PROTOCOL DETERMINATION OF THE VAPOR PRESSURE OF PFOS USING THE SPINNING ROTOR GAUGE METHOD OECD GuidelineforTestingof Chemicals,104 Vapor PressureCurve 3M Lab RequestNo. U2723 WILDLIFE Submittedto 3M Corporation EnvironmentalLaboratory P.O.Box 33331 St.Paul,Minnesota 55133 INTERNATIONAL 8598 Con=erce Drive Easton,Maryland 21601 (410)822-8600 LTD. November 24, 1998 PROTOCOL NO.: 454/112498n950/SUB454 3M LAB REQUEST NO. U2723 WILDLIFE INTERNATIONAL LiD. -2- DETERMNATION OF THE VAPOR PRESSURE OF PFOS USING THE SPINNING ROTOR GAUGE METHOD SPONSOR- 3M Corporation EnvironmentalLaboratory P.O. Box 33331 St.Paul,Mimesota 55133 SPONSOR!S REPRESENTAT TESTING FACILITY: Ms. Susan A. Beach Widdhfe InternationaLltd. 8598 Commerce Drive Easton,Maryland 21601 ST'IJDY DIRECTO LABORATORY MANAGEMENT: -jeol-s@lC"Y"4 t WillardB.Nixon, PILD. Manager ofChemistry FOR LABORATORY USE ONLY Proposed Dates: Experimental StartDate: ProjectNo.: oi-1.2-qq q,540-- Test Concentrations: QA TestSubstanceNo.: IGI:IA Experimental TerminationDate: o p qq ReferenceSubstanceNo. (ifapplicable): NA NOME_-, Bt@ PROTOCOL APPROVAL STU15Y'DIAECTOR b DATE ORY MANAGBfvENT DATE 4eo", 6- POA jd,-t, S NSOR!S REPREStffTATIVE PROTOCOLNO.: 454/11249gn950/SUB454 3M LAB REQUEST NO. U2723 WILDLIFE INTERNATIONAL LTD. -3- INTRODUCRIO WildliIfneternatiLotnda.wlildletermitnheevaporpressuorfePFOS (perfluoroocstualnfeonic acid,potassimnsaltu)singthespmmng rotorgaugemethod. The studywillbe conducted attheWildlife InternationaLltcLanalyticaclhemistryfacilitiyn Easton,Maryland. The studywillbe performed forovangproceduresintheOECD GuidelinfeorTestingof Chenucals,104, Vapor PressureCurve (1) and ProductPropertieTsestGuidelinesO,PPTS 830.7950,Vapor Pressure (2).Raw dataforallwork performedatWildlifLe*mational LtcLand a copy ofthefinalreportwillbe filedby projectnumber in archiveslocatedatWildlifeInternationaLltd.or atan alternativleocationtobe specifiedinthefinal report. PURPOSE The purpose of thisstudyisto determinethe vapor pressureof PFOS using the spinningrotorgauge method. at approximately20 0C EXPERIMENTAL DEST The spfimingrotorgauge (SRG) method describedin thisprotocolisapplicableto both liquids and solidswithvapor pressuresintheapproximaterangeof 0.5 to 10' Pascal(Pa).The vapor pressure of a controlsample (emptysample chamber)and a singlesample of the testsubstancewillbe detemiined threetimes each. The temperatureof the sample chambers willbe maintainedat20.0:L 0.5*C. Test Substance MATERIALS AND WTHODS The Sponsorwillbe asked toprovidethefollowinginformationconcerningthetestsubstance,if available: ChemicalName (ordesignation) Lot orBatch Number Purity MolecularWeight Composition(formulti-componentmlxtures) Empiricalformula(s) ExpirationDate The alladiefdorm EDENTIECATION OF TEST SUBSTANCE BY SPONSOR (Appenchx 1) isto be used toprovideavailablienfmmation. The Sponsor isresponsibleforinformationon thepurity and compositionof thetestsubstance,as wellas allinformationrelatedto the safehandlingof the test substance. The Sponsor also agreesto acceptany unused testsubstanceor testsubstancecontainers remaining atthe end of the study. PROTOCOL NO.: 454/112498n950/SUB454 .3M LAB REQUEST NO. U2723 WILDLIFE INTERNATIONAL LTD. -4- Apparatus The high vacuum system consistosf a turbomoleculaprump (LeyboldTURBOVAC 50) and roughpump (LeyboldTRIVAC S 1,6B)fittewdithan iongauge and controlle(rMetra 731 DigitalIon Gauge Controller)a,spfimingrotorgauge (LeyboldVR200), and sample introductiosnystem. The sample introductiosnystemconsistosf two high vacuum glasssample chambers with valvesand a glass tometaltransitiofnlangedmt connectsto thevacuum system. The apparatusispresentedschematically in Figure 1. Test Procedure The highvacuum system,with attachedsample introductiornystem and SRG, willbe evacuated tohigh vacuum priorto takingmeasurements. The system willbe heatedtoatleast50*C fortwelve hours or more, then allowedto coolto room temperature.The SRG willbe used to measure the deceleratiornateatthePistmn'sultimatevacuum (offset)T.he offsetvaluewillbe enteredand the SRG used to measure vapor pressures. A sample of the testsubstancewillbe placedin one of the sample chambers; the othersample chamber willremainempty. The chamber containingtestsubstanceand theblank sample chamber will be degassedthoroughlyt,ypicallsyeveralhours,toremove entrappedairand water vapor. The sample chamber tempmmiim willbe controlleadt20+-0.5'C.The vapor pressureof each sample chamber will be measured atleasthreetimesas follows:The sample chamber willbe opened to thevacumn system. The SRG willmonitorand recordpressureat30-swond intervalsT.he system willbe allowedto achieve a swaly-statepressuret,henthevalvestothe vacuum pumps willbe closed.The SRG willmonitor and recordchanges inpressureat 30-serond intervalfsorat least10 minutes. The system willbe allowed to achievecquih-briumwitthhesample The valveswillbe opened againand themeasurements repeated. Calculations The mean and slmdarddeviationof thesteady-statperessurewillbe calculatedfrom the pressure measurements made justpriorto closingthevalvesto the vacuum pumps. A linearregressionOeast squares fit)willbe performed on thevapor pressuremeasurements collecteadfterthevalvestothe vacuum pumps arecloseclThe out-gassingrateofthePystemwillbe equaltothe slopeof the regression equation fortheblank sample. The uncon=ted vapor pressureof the sample willbe equalto the interceptof theregressionequation,i.e.thevapor pressureatthemoment thevalveswere closeclIf significant@hevaporpressuredeterminedforthe blank sample chamber willbe consideredthe baseline or background pressureand willbe subtractedfrom each vapor pressuremeasurement for thetest substancechamber The means and standard&viationsof thevapor pressuresand out-gassmg rateswill be calculated. PROTOCOL NO.: 454/112498/7950/SLJB454 3M LAB REQUEST NO. U2723 WILDLIFE INTERNATIONAL LTD. Eli" Smple Handling and S"@ The Sponsor willidentifayny specialhandlingor safetyprecautionstobe used withtheabove referencedtestsubstance.All normal precautionswith respectto handlingand storagewillbe taken. Smple and Test SubstanceRetention Upon completionof testin&portionsof thetestsubstanceused as partof thisstudywillbe disposedof in accordancewith federals,tateand localregulations.Any unused portionof thetest substancewillbe returnedto the Sponsor. RECORDS TO BE MAINTAINED Records to be maintainedfordatageneratedby WildlifehitemationalLtd.willinclude,but not be limitedto: 1. A copy of thesignedprotocol. 2. Identificatiaond characterizatiofnthe testsubstance,ifprovidedby theSponsor. 3. Dates of initiatioannd completionof the study. 4. Dates ofexperimentalstartand tenninatiorl 5. Storageconditionsof thetestsubstance. 6. Test substanceuse log. 7. Spinningrotorgauge pressurereadings. 8. Statisticcaallculations. 9. Test conditions. 10. A copy ofthefmalreport. FINAL REPORT A finarleportoftheresultosfthestudywillbe preparedby WildlifeIntemabonalLtd. The report willincludeb,ut notbe limitedtothefouowing,when applicable: 1. Name and addressof thefacilitpyerformingthe study. 2. Dates upon which the studywas initiateadnd completecl 3. A statementof compliancesignedby the Sh* Directoraddressingany exceptionsto Good Laboratory PracticeStandards 4. Purpose and procedure,as statedin the approved protocol,includingallamendments and deviationsto theprotocol. 5. The testsubstanceidentificatioinn,cludingname, chemicalabstractnumber or code number, purity,composition,empiricalformula,molecularformula,manufachirer'lsot/batchnwnber, dissociatioinnwater,method of analysiso,r otherinformationprovidedby theSponsor. 6. Descriptionofthetestmethod orreferencteo themethod used along with any modificationsmade. PROTOCOL NO.: 454/112498/7950/SUB454 3M LAB REQTJEST NO. U2723 WILDLIFE INTERNATIONAL LTD. -6- 7. Individualand mean valuesobtainedfor out-gassingratesand vapor pressure. 8. Descriptionof any problems experiencedand how they were resolved. 9. A statementpreparedby the QualityAssurance Unit listintghedatesthatstudyinspectionsand auditswere made and any findingsthatwere recorded. CHANGWG OF PROTOCOL Planned changes to the protocolwillbe in theform of writtenainenchnentsignedby the Study Directorand the Sponsor. Amendments willbe consideredas partof theprotocoland willbe attached tothefinalprotocol.Any otherchangeswillbe in the form of writtendeviationsfiledwith the raw data. Allchanges totheprotocolwillbe indicatedinthefinalreport. GOOD LABORATORY PRACTICES This studywillbe conductedaccordingtotheGood LaboratoryPracticesdescribedinOECD (ISBN 92-84-12367-9)and EPA (40 CFR Parts160 and/or792). Each studyconductedby Wildlife InternationaLltd.isroutineleyxamined by theWildlifeInternationLatld.QualityAssurance Unitfor compliancewithGood LaboratoryPracbces,StandardOperatingProceduresand thespecifiedprotocol. A statementofcoinphancewithGood LaboratoryPracticewsillbe preparedfor allportionsof thestudy conductedby WildlifeInternationaLltcL The Sponsor willbe responsibleforcompliancewith Good LaboratoryPracticefsorproceduresperformed by otherlaboratoriesR.aw dataforallwork performed atWildlifeInternationaLltd.and a copy ofthefinalreportwillbe filedby projectnumber inarchives locatedon theWildlifeInternationaLltd.siteor atan alternativleocationtobe specifieidnthefinal report. PROTOCOLNO.: 454/112498/7950/SUB454 3M LAB REQUEST NO. U2723 WILDLIFE INTERNATIONAL LTD. -7- REFERENCES I OrganisationforEconomic Cooperation and Development. 1995.GuidelineforTestingof Chemicals,104:Vapor PressureCurve. 2 Product PropertiesTest Guidelines 1996.OPPTS 830.7950.Vapor Pressure. it [i PROTOCOL NO.: 454/112498/7950/SUB454 ai 3M LAB REQUEST NO. U2723 WILDLIFE INTERNATIONAL LTD. -8- APPENDIX I IDENTIFICATION OF TEST SUBSTANCE BY SPONSOR To be Completed by Sponsor 1. TestSubstanceIdentit(yname tobe usedinthereport): PerfliLq=tane ulfonicAcid-PotassimnSalt (PFOS) Sample Code orBatchNumber: Lot 217 Purity("/AoctiveIngredient)9:8.9% ExpirationDate: 2008 H. Test Substance Charactmization Have theidentitys,tm ke .Vuntyand compositionor othercharacteristics which approyriately@deegthetestsubstancebeen determinedprior tothestarto thisftudyinaccordancewithGLP Standards? Yes-No X III. Test Substance StorageConditions Pleaseindicatetherecommended storageconditionsat WildlifeInternationaLltcL Ambient room t=erature, Has thestabilitoyf thetestsubstanceunder thesestorageconditions been determinedin accordancewith GLP Standards? Other pm-dnent stabilitiynformation: Yes No X IV. ToxicityInformation: Mammalian: Rat]LD50 251 mg&e Mouse LD50 N/A Aquatic: InvmtebrateToxicity(EC/LC50) FishToxicity(LC50) Daphnia magm: 27 me/L Rainbow trout:11 mgil DopMa map-nap50 mpJL Fathead mixmow& 38 mgl Other ToxicityInformation(mcludingfindingsofchronicand subchronictests): See MSDS. PROTOCOL NO.: 454/112498n950/SUB454 3M LAB REQUEST NO. U2723 WILDLIFE INTERNATIONAL LTD. -9Figure 1. Schematicof SpinningRotor Gauge Apparatus. ......... C2) 1. vacuum pump 2. turbovac controller 3. sample chambers 4. water bath S. spinning rotor gauge head 6. turbomolecular pump 7. Ion gauge 8. !on gauge controller 9. spinning rotor gauge 10. comptner Pl@OTOCOLNO.: 454/112498/7950/SUB454 3M LAB REQUEST NO. 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