Document RJYLJq7bgoM7OD6x8y9zwJe17
AR 126-0043
:
DETERMINATION OFTHE VAPOR | PRESSURE OF PFOS `USING THE SPINNING ROTOR GAUGEMETHOD
`WILDLIFE INTERNATIONAL LTD. "PROJECT NUMBER: 454C-105 `OECD Guideline 104 VapourPressureCurve U.S. EPA OPPTS 830.7950 Vapor Pressure
AUTHORS: Raymond L. Van Hoven,PhD.
Joel I. Stenzel `Willard B. Nixon, Ph.D.
STUDY INITIATION DATE: January 12,1999 STUDY COMPLETION DATE: May S, 1999
Submitted to
3MCorporation : `Environmental Laboratory 935 Bush Avenue 3MBuilding 2-3E-09 P.0. Box 33331 St. Paul, Minnesota 55133
WILDLIFE INTERNATIONAL LTD. 3
410)822-8600 8598 Commerce Drive
Easton, Maryland 21601
Page 10026
. 000057
WILDLIFE INTERNATIONAL Lt.
-2-
PROJECT NO.: 454C-105
GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT
!
SPONSOR: 3M Corporation TITLE: Determination ofthe Vapor Pressureof PFOS Using the Spinning Rotor Gauge Method
WILDLIFE INTERNATIONAL LTD. PROJECT NUMBER: 454C-105
STUDYCOMPLETION: May 5, 1999
Enviro"nTmheinstsatludPyrowtaesctcioonnduAcgteendciyn cino4mp0lCiaFnRcPeweirtth7G9o2,o1dL7aAbuogruatsotry1P9r8a9c;tiOcEeCStDaPndraridsnecspiuobpflGlisoehoesddbLyatbhoeraUtSoSr.y NProatcitfiiccea,tiOonCNDoE./3G8D50(,9A2g)ri3c2u,ltEunrvailrPornomdeuncttiMoonnBougrreaaup,h1N0oA.u4g5e,stPa1r9is841,w99i2t;hantdh fJoalpoawniMngAcFxo,ept5i9onNs:obSen,
"ThetestandreferencesubstanceswerenotcharacterizedincompliancewithGoodLaboratory Practices Standards. {estedi"TnhcestaboilitmyofwptihthetGleosotsdiuLbasbtsoarnactneoarnyPdcrraecfteeirceencSetsatnadanrddasr.dsundertheconditionsa thetes stewasnot
STUDYDIRECTOR: fan Zan Hoven, PhD. V.
S DATE E 5 flo [24 DA'
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a. WILDLIFE INTERNATIONAL Lo.
PROJECT NO.: 454C-105
QUALITY ASSURANCE STATEMENT
SPONSOR: 3M Corporation
TITLE:
Determination ofthe VaporPressureof PFOSUsingtheSpinning Rotor Gauge Method
`WILDLIFE INTERNATIONAL LTD. PROJECT NUMBER:454C-105
te tolows`Thisstudy wasexaminedforcompliancewith Good LaboratoryPracticeStandardsaspublishedbythe
U.S. Environmental Protection Agency in 40 CFR Part 792, 17 August 1989; OECD Principles of Good `Laboratory Practice, OCDE/GD (92) 32, EnvironmenMt onograph No. 45, Paris 1992; and Japan MAFF, 59
a`nNdohaSuadni,tsNaontditfhiecdaatteiNsotonh.a3t8a5n0y, fAignrdiciunlgtsuwrearlePrreopdourctteidonoBtuhreeSatuu,d1y0DiAruegcutsotra1n9d8L4.abTohreadtaotreysMaofnaalgleimnespnetctwieornse.:
acm: em-- Miro Datos Fister
DATEGONDUCTED: Sy 27,199 ey 29,1599 Fey24,199 Nays, 1958
STUDYDRECDTAOTRE:REPORMTAENDATGOE!MENT:
rn yz, Fema 15 ----
Jem 7,199 Joma 29,159 Feary 25,1599 --
RoR ees
Lisa T. Drottar `QualityAssurance Representative
<<
DATE
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PROJECTNO:: 454C-105
REPORT APPROVAL '
SPONSOR: 3M Corporation
TITLE. DeteorftmheViaponrPraestsurieofoPFnOS UsingtheSpinRontoirGnaugge Method
WILDLIFE INTERNATIONAL LTD. PROJECT NUMBER: 454C-105
'
STUDYDIRECTOR:
nye.
Scientist jan Hoven, Ph.D.
MANAGEMENT:
WMialnlaagredrB,.ANniaxloynt,icPaLDCh.emist4ry
55.09
DATE DATE
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THIGICOVET PAGE...
TAOFBCONLTENETS
PROJECT NO. 454C-105 |
TaOFb COlEeRLS..csrrssmm
3
OBJGEHVE sss
8
TABLES Table 1. SteaPrdessyure-OfSPFtOSSaEtPeIC....vcvsmssmss: 1S Tabl2e. PressureIncreassOf PFOS SHIPIE. ovis: 16 Table3. SteaPrdessyure-ofCSOMtFOlate SAPIE....vcvvrvcnssms: IT
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`TABLE OF CONTENTS - Continue-d
FIGURES
Figare2. DiagramofSampleintroduSYcStE.ion vss 20
Figur3e. Graphical proseatation Of OffSetEASES...
21
Figured, Steady-state pressureandpressureincreaseofHexachlOrobenzene Sample... 22.
Figur5e. Steady-statepressure adprESSure 06reageOfDDT SADIE...
23
Figur6e. Steady-statepressureandpressure crease Of PFOS SAmPIE..vvrrscve 24
Figure7. Steady-statepressureandpressureincreaseOfCOBTOL APIE..rrrrvn 25.
APPENDICES Appendix. PerIOsI oinnthenSYel ccs26
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Ey `SPONSOR'S REPRESENTATIVE: DLATOAACNDAOAFCSTOTPUYIDOYFO,TRHNAEW FINALREPORT:
SUMMARY
SMCorporation Ms. Susan A. Beach E`aWsitldoinf,eIMnatreyrlnaantdion2a1lL6t0d1
P--RO--JE--CT-- NO.: -- 454C-105 .
WILDLIFE INTERNATIONAL LTD, PROJECTNUMBER: TEST SUBSTANCE: stub:
TEST DATES:
454C-105 PFOS (Perfluorooctans Sulfoic Acid, Potassium Selt) DeSterpminiaRtoitonnoorGfnathuiegeVaMnpeotrhgPordessure of PROSUsingthe. EExxppeerriimemnetanltal STert-mJiaannuaartr-yi2to7n, 19Februay9912, 1999
SUMMARY:
"ThevaporpressureofPFOSwasdeterminedtobe 3.31 x 10 Paat20Cusingthe spinningrotorgauge method.
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INTRODUCTION
"ThisstudywasconductedbyWildlifeInternationalLtd.for 3MCorporationattheWildlifeInternational Ltd.analyticalchemistry facilityinEaston,Maryland.Testswereperformedusingthespinningrotor gauge `method.Thevaporpressureofth tetsubstancewasanalyzedfrom January27to February12,1999.Rawdata `gebnyWeillrifeaIntteraetiodnal Lid.and acopyofthefinaleport arefiledunder ProjectNumber454C-105 inarchiveslocatedontheWildlifeInternationalLtd. ite.
OBJECTIVE
"Theobjectiveofthsstudywastodetermine the vaporpressureofPFOSat20Cusingth spinningrotor gaugemethod.
EXPERIMENTAL DESIGN
`Thespinningrotorgauge (SRG)systemwasusedtodetevrapomrpirosnsureo. The SRGmeasuredthe: rotationalfrequencyof astainlesssteelballthatwasmagneticallysuspendedwithin #vacuumchamber. The decelerationrateofthebal wasusedtodeterminethegaspressure. Thesystem wasconfwiitghtuworsaempdle chambers.Oneofthesamplechamberscontained asampleofth testsubstance,whiletheotherremainedeupty tomakecontrolmeasurements. Thesystemsteady-statepressureandpressureincreaseofth testsubstanceand controlsamplesweremeasuredthreetimes.
MATEARNDIMEATHLODSS "Thisstudywasconductedbasedonproceduresoutlinedin OECDGuidelines, Method104(1);and EPA OPPTS 830.7950(2). The spinningrotor gengemethod wasusedtodeterminethevaporpressureofthetest substance.
Test Substance
"Thetest substancewasreceivedfrom 3MCorporation onOctober29,1998, and wasassignedWildiife IntemationalLtd. identification numbes4675uponreceipt.Thetes substance,awhitepowder,was identified
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as: FC-95, Lot 217, 3M ID#: 98-0211-3916-1. Based on information supplied by the Sponsor, the test `substancehad apuorf9i 8.9t%ay nd an averagemolewceiughtlofa5r38 AMU.Thetest substanwcase stored underambientconditions.
ReferenceSubstances
Thehexachlorobenzenereferencesubstancewasreceived fromAldrichChemicalCompany on
February 10,1997,and was assigned WildlifeInternationalLid. identificationnumber 3948 upon receipt. The referencesubstance, awhitepowder,wasidentified as: Hexachlorobecantzaleong neo;. 1710CA5SN-um0be,r
118-74-1. The reference substance had areported purity of 99%, andwas stored under ambient conditions.
The DDTreference substance wasreceivedfromAldrichChemical Comp onaJan nuayry 20, 1999, and `wasassigned WildlifeIntemationalLtd.identification number 4749 uponreceipt. The reference substance, a
`white powwads ie denr tifi,ed as: 1,1-bis(p-Chlorophenyl)-2,2,2-Trichlaroethane;lot numbe7r7 H3614; catalog 10. C8894, CAS Number 50-20-3, The reference subhas da rt epora ted pn uritc y ofe 99.3%, and wasstoredin
arefrigerator.
`Apparatus Configuration
.
"The high vacuumsystemconsistedof 8 vacuumpump(LeyboldTRIVAC 1,6 B), aturbomolecupluamrp
(Leybold TURBOVAC 50), an iongauge and controller (Metra 731Digitallon Gauge Controller), aspinning
rotorgauge(Leybold VISCOVACVM212), asampleintroductionsystem,and variousstainless-steelcon-flat
fittings,including threevalves.Thecon-flatfittingswereassembledusing coppergaskets. Thevalveswereused. toisolatethesample chambers,thespinningrotorgaugeand/orthe vacuumpumps.Thespinrontoir ganugge.
controllerwasconnectedto acomputerviatheserialinterface(RS-232port). A dia ofg ther appa aram tus
`confiisgpreuserntaedtiniFiogurne 1.
`The sampleintroductionsystem wascustomdesignedandmanufactured by At-Mar Glass Co.(Kennett
`Square, PA).The system consisted of two high vacuumglass sample tubes. During thestudy, onetube contained `a sample ofthe testorreference substance whiletheother tube remained empty (control). The temperaturofe
thesamplesweremaintainedbyimmersingthe sampletubesin a waterbath.Thetempeorftahetatuerrbateh
`was periodicallymonitoredusinganASTM 44Cmercurythermometer.`Thetubeswere independentlyvented
andconnected 1the vacuumsystemusingthreegroundglassstopeocks. Agltaomsetsal transitionflange
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`connectedthesampleintroductionsystem tothe vacuum system. A diagramofthe sampleintroducstysitoenm ispreseinnFitguree d2.
Asteelballwasinsertedintothespinningrotor gaugetubebeforethe tube wasconnected tothehigh `vacuumsystem. "Thecon-flatfittingsand valvesofthe highvacuumsystemwerewrappedinheattape. The `temperatureoftheheattapewascontrolledusing arheostat.`Thesurfacetemperature ofthevacuumsystemwas `periodicallymonitoredusinganOmegaModelHH23digitalthermometer (OmegaEngineering, Inc.,Stamford,
CT)with a thermocouple placed between the heattape and the outer surface ofthefittings.`Theairtemperature alsowas periodicallymonitoredusing the digital thermometer.
`Procedures
Thehighvacuum system was heatedto approximately 80Cand evacuatedforat least 18hourspriorto
`maanyk measiurenmeng ts. Afterheating,thesystem was allowedtocooluntil reachingroom temperature. The
steelballinsidethespinning rotor gaugetubewassuspendedin amagneticfieldanddriven to a rotational
freofq appu roxiematn ely4c15y Hz.Thedeceleration rateoftheballwasmonitoredusingthespinningrotor gauge. Theparameters of thespinningrotorgaugeweresettorecord a decelerationmeasurement every
30secondsbasedonthemolecularweight(28.96g/mole)andviscosity (18.2 x 10Pass) of air. "Theoffsetvalue
wasdeterminedfo eachsample tubewhe thedecelerationraereached aplateau.Theoffvalsue(emetan
`decelerationrate)was enteredintothespinningrotorgaugecontroller.
Asampleofhexachlorobenzenewasplacedinoneofthe samplechambers,whiletheotherchamber
remainedempty(control). Theparametersofthespinningrotorgaugewerechangedto recordpressure,inPascal
(Pa), every30 seconds. Thissetting was usedfor allsubsequent measurements.`Themolecular weightparameter
`wasset to 284.78andviscositywassettozero.Thesamplechamberwas evacuated toachicve aseady-state pressure. Tempweerr epeariodticaullyrrece ordsed.Afterthesystemreachedtemperatureandpressure `equilibrium,thesteady-statepressureofthesample wasmeasuredwiththespinningrotorgauge.Thevalves to
the vacuum pumps werethen closed,andthe pressureincreasewasmonitoredforat leasttwohours.
A sample of DDTwasplaced inoneofthe samplechambers,whiletheotherchamberremainedempty
(control).Themolecularweightparameter wassetto 354.5andviscositywas set 02f0. "Thesamplechamber
was evacuated to achieveasteady-sprtesasturee. Tempweerrepeariot dicaullyrreceordsed. Afthte seystrem
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reachedtemperaandtpruesrsuereequilibrium,thesteady-statepressureofthesample wasmeasuredwiththe
`spinningrotorgauge. Thevalvestothe vacuumpumpswerethen closed,andthepressureincrease was. `mofnori at t leasottwroheoud rs.
Asmallsampleofthetestsubstance wasplacedinone ofthesamplechambers,whiletheotherchamber `remema ptyi(cnonterold). The molecular weight parameterwas setto 538, andviscosity was.set to zero.The
samplechamberwasopenedtothevacuumsystemandpumped-down 0 asteady-statepressure. Temperatures wereperiodicallyrecorded. Afterthesystemreached temperatureandpressureequilibrium,thesteady-state: pressureofthe samplewasmeasuredwiththespinningrotorgauge.The valvestothevacuum pumps eethea
closed, andthepressure increasewas monitored for at leastatleast twohours. Measurementsthenalternated `betweenthe PFOSsampleandthecontrolsample (emptysample chamber)for totalofthreedeteaninationsof each.
Calelations
`Thesteady-statepressuresweredeterminedbyaveragingthepressurevaluesrecordedprior toclosingthe `valvestothe vacuumpumpsduringeachmeasurement.`Standard deviationsand95%confidenceintervalswere. also calculated.
Thepressureincreasedatawereanalyzedusing leastsquares-itlinea regressionanalysis.A linewas it
totheportionofthedata thatwasdetermined tohaveachievedequilibriumpressurewiththe sample."Theslope `andinterceptwerecalculatedforcachmeasurement.Correlation coefficients and 95%confidenceintervals for each parameterwere alsocalculated.`Theout-gassingratewasdeterminedfromtheslopeofthelineandthe `vapor pressurewas determined fromthe interceptvalue.
`Themeansand standard deviations of the replicatemeasurements of the control and PFOS sample were: also calculated.
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RES ANU D DIL SCUT SSIS ON
Agraphical presentation ofthe offset measurementisshownin Figure3. "Thegraphsshowdatacollected for approximately 2 hours fromeach sample tube."Themeanoffsetvaluewasbasedontheaveragedeceleration rate meafrsomu lefr t(7e .87d 7x 10% 5)andrigh(t6.838 x10* 5) samplechambersonJanuary 6, 1999. The offset valuewesdetermtionbeed 7.357 x 10%sTM.
Thesteady-statepressureandpressureincrease ofhexchlorobenzeneweredeterminedon January14,1999,
and arepreseinnFitguered4. Thesteady-statepressure was 1.24 x10Paandthevaporpressurewas
detetorbem8.3i0xn10ePda.The vaporpressurewasconsistentwiththerange foundintheliterature(2).
Thesteady-statepressureand pressureincrease of DDTweredeterminedonJanuary22, 1999,andare.
presienFnigturee5d. The steady.-statepressurewas 4 81 x 10Paand the vaporpressure wasdeterminedto `be1.x170*6 Pa.The vaporpressure wasconsistentwiththerange foundin theliterature(3).
`Thesteady-statepressureandpressureincreaseofPFOSweredeterminedon February3, 5and12, 1999.
Themeansteadpyre-ssusretwaast4.e51 x 1P0 a (T eble 1). For cachassociated pressure increase. `measurement,theslope ofthepressureincreasedatabecameconstantafterapproximatelyninetyminutes. This
indicatedthesystemhad achieved saturationofthegasfromthe PFOSsample. Alinewasfit tothisregionof
thedats, and theslopeandinterceptweredetermined. Theinterceptvalues representedthevapor pressureofthe: `sample. Themean vaporpressureof PFOS was 3.31 x10 Pa(Table2). Arepresgerapnhitcaalprteseiatvatieon
`ofthedatais showninFigure6.
Thesteady-statepressureandpressureincreaseofthecontrol sampleweredeterminedon February2, 4,
an8d, 1999.Themeanbaselinepressurewas -1.22 x 1P0 a (Ta ble 3). For cachmeasurtehemsloepenoftth,e
equilibrium. Alinewas fittothisregionofthedata,andthe slopeand interceptweredetermined.Theslope values represeatedtheoutgassingrateofthesystem.The meanout-garatsesweis4n.g78 x 10% Pasco. (Table 4). The interceptvaluesrepresentedthebackground pressureofthesystem. Themean background prewass 1.s51ux 1r0Pea.The background pressurewasconsideredinsignificantcomparedtothevapor
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PROJECT NO.: 454C-105
`presosf uPFrOeSandwas notsubtrfarocmttheosde.values. Arepregras phie caln prestenta atit onoi fthv edaeta. isshio nFiw gurn e7.
Occasionally during thestudy, leak developedatoneofthegroundglassjoint ofthesampleintroduction
system.Thiswascorrectedbyadjustingthestopeocksand/orrepositioningthesampletubes. Thespinning rotor
`gaugedisplayedcither"MTIME TOOLONG" ox"BADSIGNAL messagesduringthestudy,butwesrestarted `without any difficuealcth tiiemes.
`Themean temperatureof thewaterbath,duringmeasurementsofthePFOSsample,was20.1Cand `rangedfrom 19.50t0 20.50C.. Theairtemperraangtedufrroem19.0 to 22.an3 d thesuCrfa, ce temperature ofthe vacuum system rangedfrom 19.510 22.9C.
`CONCLUSION
`Basedontheresults fromthree setsof measurementscollectedfromthespinningrotorgauge, the vapor pressureof PFOSwas determtoibne3e.3d1 x 10 Paat 20C.
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REFERENCES
1
Organisation for Economic CooperationandDevelopment. 1995. Guideline for TesoftChiemincalgs, Method 104, "Vapour Pressure Curve".
2 US. Eavironmental Protection Agency. 1996. OPPTS 30.7950, Vapor Pressure, Washington, D.C.
3 Tinsley, LJ. 1979. Chemical Concepts in Pollution Behavior, Wiley InterscienNceew, York.
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_--
"Trial Number 1 23
Table 1 Steady-State PressureofPFOS Sample
Date 2399 22/0152//9999
Mem=
sabe
Steady-State Pressure (Pascal) 71440 E-6 56664 E-6 72968 7 45BES
aaE6
Standard Deviation S8716B7 | 48038 E7 52793 E7
55% Confidence: Interval 61426E3 61158 E-3 260657 E-3
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Tabl2e
`Pressure Increaseof PFOSSample
--_-------- "Trial Siope 95%Confidence
Interoept
95%Confidence
Correlation
Number (Pulses)
Interval ee(Pascal)
Interval
r Coeffie ciente
21 233S669EETT 323S6M0S710032G3M78MSEETT IA2GMO06EE44 4LSII60I7S0W4L7I0I2TEE44 |090999980745
_-- 3 LI90ET LI4901I92ET 2042E4 2010020715E4 099978
Meas SWDev.
2386E7 1198E7
31321812EE44
- ---
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_-- oo T"rTrailalNNuummbbeerr
21 3
-_
Table 3 Steady-State PressureofCoatrol Sample
DDawte 222149999 2899
Mem= SWDev.=
Baseline Pressure (pascal) 334S5132E976 5.29577
-1222E6 L9TTE6
Standard Deviation 4502321856E77 18258 E-7
95% Confidence Interval
+73013E48 41621 E48 22633 E8
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_-- Trial Number
Slope (Pulsec)
1 52256E8 --_-- 23 S3I983876TEESS
SMdeDewvs. 407743031EESS _a
Tabled PressureIncreaseofControl Sample:
95%Confidence Interval
52171052E34S 3591386611053199119EE88
Intercept (Pascal) 1963SE-S LT781I9SEESS 15107E-5 06319ES
95%Confidence Interval
Comelation Coefficient
1917102010E5 1762017%8ES *
099590 099998
IIB0TINES 0.99999
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f
|i
y && O o re] = 98 & f[a9d
lve]
@
21.. vtuarcbuoupmumppumcopntraller
3. sample Intro. system 4. constant temp. water bath 5. spinning rotor gauge head
r i =Eosd E ;. t 3
na EE
75.. tlornbgoamulgeecutluaber pump
8. fon gauge controller
9. spinning rotor gauge controller
3
10. personal computer
Figure 1. Diagramofhigh vacuum system configuration.
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3glass to metal transition
3 --, ground-glass stopeacks
=
5 sample tubes ------ waterbath
Figure 2. Diagramof sampleintroducsytsitoemn.
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Offset Measurements
10807
=
i
.
3
9.0E-08
1
_ soe
&
|i 7.0E-08
coms}
50808
NN
o
om seers cme
rs
---- Omen
.
40808 V6999:00
1991000
UGS ILO0
GSI1200
GSI 1300
UHI 1400
Timo
Figure3. Graphicalpreseofnofftsea tmetasuireo mennt.
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Steady-oSftaHteexaPrcehslsourroebeannzdePnreeSssaumrpelIencrease 22803
2.0803
1.8803
168-03
148-03
F 12E03
L0oBmo
=,7
>
oo
808-04
amor Ld
6.0804
4.0E-04
208-04
0.0400 1/14/99 14:00
114199 15:00 Time 1/14/99 16:00
`.
. 1/1419917:00
Figure 4, Steady-state pressure and pressure increaseofHesachlorobeazzae snp.
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Steady-State Pressure and Pressure Increase ofDDT Sample
148-03
12B:03
108-03
8.0804
3
.
& 6.0804
4.0B-04
208-04 0.0E+00
1122/99 11:00
yy
yy
een &
.
1/22/99 12:00 Time 1/22/99 13:00
Figure S. Steady-statepressureandpressureincrease of DDT sample.
.
1/22/99 14:00
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3.5E-3
Steady-State PorfePssRuOreSaSnadmpPrleessure Increase
3.0E-3
2.5E-3
i J _ 20B3
153
7
1.0E3
ry
5.084
rd
same
0.0E+0
2399 11:30
2399 12:30 Time 23991330
Figur6e. Steady-statepressure andpressureincreaseofPFOSsample.
23/99 14:30
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4.0B-04
Steady-StatePressure and Pressure Increase of Control Sample
3.5E-04
3.08-04
2.58.04
3
g
208-04
158-04
108-04
A
5.0805
py
19005 off
.
0.0E+00
22/9912:30
2/2/99 13:30
212/99 14:30
22/99 15:30
Time
Figur7e. Steady-statepressureandpressureincreaseofControlsample.
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APPENDIX Personnel Involved in the Study `ThefollowingkeyWildiife IntemationalLid.personnelwereinvolvedintheconductofmanagementof this study:
1. Willard B. Nixon, Ph.D, Manager, Analytical Chemistry 2. RaymonLd. VenHoPhDv,Seciennti,st 3. JoelL Stenzel, BS, Systems Analyst 4. Keri Leach, BS,LaboratoryTechnician
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