Document 6RyZp37ozzqKpox9KRodGk30m
PROTOCOL
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DETERMINATION OF THE VAPOR PRESSURE OF PFOS
"USING THE SPINNING ROTOR GAUGE METHOD
(OECD GuidelVianpeofrorPrTeessstuirneg Curve ofChemicals, 104
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3MLab Request No. U2723
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Envir3onMmeCnotraplorLaatbioornatory
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St. PauPl.0,.MiBnonxes3o3t3a3155133
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WILDLIFE INTERNATIONAL LTD.
8598 Commerce Drive
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Easton, Maryland 21601 (410) 822-8600
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November 24, 1998
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000083
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PROTOCOL NO.: 454/112498/7950/SUB454
3MLAB REQUEST NO. U2723
I WILDLIFE INTERNATIONAL LTD.
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DET"EUSRIMNIGNTAHTEISOPNIONFNITNHGERVOATPOORRGPARUEGSESUMREETOHFOPDFOS
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SPONSOR
E3nvMirCoonrpmoernattailoLnaboratory
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PS.t0.PaBulo,xM3i3n3n3e1sota 55133
SPONSOR'SREPRESENTATIVE: Ms. SusanA. Beach
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`TESTINGFACILITY:
W8i5l9d8iiCfeomInmteerrncaetiDornialveLid.
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Easton, Maryland 21601
STUDYDIRECTOR:
JoctStensel Ray NanHoven, PhD +
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LABORATORYMANAGEMENT: WMilalanrBdo.afNCihgxeomnei,sPtrrAyD.
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-- FO FORR LABORL ATORA Y USEB ONLYRA
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| Proposed Dates:
| Experimental Start Date:
01-12-92
ExTpeemriinmaetnitoanlDate: 09-10-41
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pero: 4540-105
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Test Substance No: AGTHA ReferenceSubstanceNo. (ifapplicable): NA
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PROTOCOLAPPROVAL
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LABPRATORYMANAGE
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SPONSOR'S REPRESENTATIVE
BA1T1/30/49 8
00084
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PROTOCOLNO.: 454/112498/7950/SUB454
3MLABREQUENSOT. U2723
n WILDLIFE INTERNATIONAL LTD.
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Intemational
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will
INTRODUCTION determinethe vapor pressure
of
PFOS
(perfluorooctane
sulfonic
acid, potassium sa)using thespinroto gauge method. The study will be conducted at the Wildife
fIonltleomwaitnigonpraolceLtddu.resanianlytthiecOalECchDeGmiusitdrlyinfagcifloitryTienstEiansgtoonf,ChMeamriyclaalnsd,. 10T4h,eVasptoudryPrwielslsubreepCeurrfvoerm(e1d)
apnd PerirckatPWfriolpdeloritfieesrInTteesmmtaGtuiioednealliLdnieds.,aOnPdPTacSopy30o.f7t9h50,finVaalporrePproetwssurie (lf2i)l.eldRbyapbwrdoajeteactornualml wboerirnk
archives located at Wildlife IntemationalLd.o a an atermative location tobe specifiedi the final
port
The purpose of this studyi todeterPmUiRtnPheOvSaEpor pressure of BFOS at approximately 20C using thespinningrotor gauge method.
Thespianingrotor gauge (SERXGP)EmeRtIhModEdeNsTcrAibLedDiEntShIisGNprotocol i applicabletoboth liquids aonfdascoolnitdowlsiathmvpalpo(rapnrpetsyssuaremspilnethcehaambperp)ranodaxsiirnagmnlgeaesotafmepl0e.5otfot1h0eteBsatsscuabls(tPaan)ceTwihlelvbaopodreptreersmsiunreed
threetimes each. The tempoftehesrampalecthaumberrsweillbe maintaati20n.0e1%d 0.5C.
MATEARNDIMEATHLODSS
TestSubstance:
si"cTheSponsorwillbe
asked
toprovidethefolowinginformation
concering
the
est
substance,if
LChoetmiocBaoltNcahmNeum(borerdeigaation) Purity
ECmopmiproisciatlifonor(mfourlmausli-component mixtures) Expiration Date
Molecular Weight
{sto'b"eTuhseeadtttoacphreodvifdoeramvaIiDlaEbNleTIfoFrImCatAiToInO.NTOhFeTSpEoSnTsorSUiBrSesTpAonNsCibElefBoYr iSnPfoOrNmaStiOoRn o(nAptpheepnudriixt)y asnudbsctoamnpcoes,itiTohne oSfptohnstoerstaslusbsatgarnceee,taos awceclepatsaanly iunformsateisotnesrueblsatd taendceoothfetessatfesuhbasntdalnicnegocfotnhteatiensst remaat thiennd ofithenstugdy:
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PROTOCOL NO: 454/112498/7950/SUB454
000085
3MLABREQUENSOT, U2723
o WILDLIFE INTERNATIONAL LTD.
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a . Appara"tTuhs high vacuum system consistofa trbomoleule pup (bold TURBOVAC 50) and
rough pump (Leybold TRIVACS 1,6B) fited with an fon gauge and controler (Metra 731 Digital on
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sGeamupglee iCnotnrtordoulclteiro)n,saysstpeimncnoinnsgisrtostoorftgwaougheig(hLevyabcouludmVRgl2a0s0s)s,amapnldescahmapmlbeerisntwriotduhcvtailovnessyastnedma. glTahses
to metal transition flangethatconnectsto the vacuum syste. The apparatus is presented schematically
oa
in Figure 1.
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TestPr"oTcheedhuigrhevacuum system, with attached sample introduction system and SRG, will be evacuated
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tohighvacuum prior to takingmeasurements. Thesystemwillbeheated 0atleast S0Cfortwelve
hours or more, then allowed to cool to room temperature. The SRG vill be used to measure the
deceleration a atthesystem' imatevacuum (offset). Theoffsetvaluovillbecteredandthe SRG:
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usedtomeasure vapor pressures.
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A samofpthle eestsubstancewillbeplacedinoneofthesamplechambers;theothersample:
chambes will main copy. The chamber containing test substance and the blank samplechambervil
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bedegassedthoroughly,typicallyseveral hours,toremove entrappedairandwatervapor.The sample:
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chambertemperaturesvil becontroled at 20:0.5C. Thevaporpressureofeachsamplechambervil
bemeasure atlasthr timesas follows: The samplechamberwill be opencdtothevacuumsystem.
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The SRGwillmonitorand recordpressureat30-sccondintervals. Thesystemwilbeallowedtoachieve
astady-sate pressure, thntvhalves tothe vacuum pumps will be closed. The SRG vill monitor and
;
recordchangesin pressureat30-socondintervalsforat least 10minutes.Thesywsilltbeaellomwed
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toachieveequilviitbhtrheisaumplme.Thevalveswillbe openedagainandthemeasurementsrepeated.
1)
Calaulations "Themean
and
standarddeviationof
thesieady-state
pressure
willbe
calculatedfrom
the
pressure
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`measuremeatsmade justpriortoclosingthe valves tothe vacuum pumps. Alinearregression (least
squares ft) will be performed on the vapor pressure measuremeatscollectedaftr the valves to the
vacuapumpsareclosed. Theout-gasing ateofthesystemwillbeequaltotheslopeoftheregression
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equation for the blank sample. The uncorrected vapor pressureofthesamplewill be equal to the
interceptofthe regression equation, i. the vapor pressure at the moment the valves were closed. If
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significant,th vaporpressuredetermined fortheblanksamplechambervillbeconsideredthebaseline
or background pressure and vill be subtracted from each vapor pressure measurement for the test
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bsuebcstaalneuacthoadm.ber.Themeansandstandarddeviationsofthevapor pressuresandout-garsasteiswn0ilg0l 0086
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PROTOCOL NO: 454/112498/7950/SUB454
3M LAB REQUEST NO. U2723
a WILDLIFE INTERNATIONAL LTD.
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. `SampleHandling ondSafety "The Sponsor will identify
any
special
handling
or
safety
precautions
o
be
used
with
the
sbove
referenced test substance. All normal precautions with respect to handling and storage will be taken.
`Upon completion of testing, portions of the test substance used as partof this study will be
disposedofin accordance with federal, state and local regulations. Any unused portionofthe test
`substancewillbereturnedtothe Sponsor.
REC TOO BE MR AIND TAIS NED
`Records to be maintained for data generated by Wildlife International Ltd. will include, but not
be limited to:
1.
2
Acopy of thesignedprotocol.
Identification and characterizationof
the
tet
substance,
if
provided
by
the
Sponsor.
3.
4.
DDaatteessooffiexnpeirimtenaitnadlacsottmarpitleaontdinotneromfitnhaetisotnu.dy.
5.
67..
Spiing ir mgs rss endings. Storage conditionsofthe test substance.
Test substance use log
8. Statistical calculations.
9. Test conditions.
10. A copy of the final report.
FINALREPORT
Afinal report ofthe resultsofthestudywillbopreparedby WildlifeIntemational Ltd. The report
will include, but not be limited tothe following, when applicable:
1. Nameand addressofthe facility perforthmesitundyg.
2. Dates`upon whichthestudy wasinitiated andcompleted.
3. A statement of compliance signed by the Study Director addressing any exceptions toGood
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Laboratory
Purpose an
Practice Standar
dprocedure, as
ds
statedin
t
he
approved
protocol,
i
nc
l
udingal
l
amendments
end
deviations tothe protocol.
5. The test substance identification, including name, chemical abstract umber or`code number,
`purity, composition, empirical formula, molecular formula, manufacturer's lot/batch number,
6. Dedsicssroicpitaitoinoonfinthweatteesrt,mm etheodt oorfrhaenfaeo lryesnd icse,tootrhoetmheetrhiondfoursmeadtailononpgrwoivitdheadnbyym`othde iSpfoinscoar.timoadnes.
PROTOCOLNO.: 454/112498/7950/SUBA454
3MLAB REQUEST NO. U2723
000087
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WILDLIFE INTERNATIONAL LTD.
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ou 7. Individualandmean values obtained for outgassing rates and vapor pressure
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8 Descriptionofany problems experienced and how they were resolved.
9. Astatement prepared by the Quality Assurance Unit listing the dates that study inspections and
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audits weremadeandanyfindings thatwererecorded.
CHANOFGPRIOTNOCGOL
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Plannedchangestotheprotocolwillbeintheformofwrittenamendmentssignedbythe Study
Directorandthe Sponsor. Amendments will be considered as pastofthe protocol and will be attached
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10the finalprotocol.Anyother changes willbe intheform of written deviations filedwith the raw data.
All changes tothe protocol will be indicated in th final report
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GOODLABORATORYPRACTICES
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"This study willbeconducted according to the Good Laboratory Practices described in OECD
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(ISBN 92-84-12367-9) and EPA (40 CFR Parts 160 and/or 792). Each study condbuycWitldelidfe
International Ltd. is routinely examined by the Wildlife International Ltd. Quality Assurance Unit for
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compliancevithGoodLaboratoryPratis, Standard Operating Procedures and the specified protocol.
A statementofcompliancewith Good Laboratory Practices vil be preparedfo all potionsofthe study
:
conducted by Wildiie Intemational Lid. The Sponsor will be responsible for compliance with Good
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LaboratoryPractices forprocedures perfobrymotehedr laboratories. Raw data for all work performed
at Wildlife International Ltd. and a copyofthe final report wil be filed by project number in archives
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located on the Wildlife International Ltd. site or at a altemative location tobespecified inth final
report.
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PROTOCOLNO: 454/112498/7950/SUB4S4
000088
3MLABREQUEST NO. U2723
| WILDLIFE INTERNATIONAL LTD.
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11 3| COPhrregomadinucicastlastP,iroo1pn0e4f:rotriVeaEspcTooernsoPtrmeiGscusiuCdroeeolpiCneuerrsvaet.i19o9n6.anOdPDPeTvSel8o3p0m.7e9n5t0.. 1V9a95p.orGPreussiurdef.oerTlesitinngoef
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PROTOCOLNO: 454/112498/7950/SUB454
000089
3MLABREQUEST NO. U2723
WILDLIFE INTERNATIONAL LTD.
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IDENTIFICATION OFATPEPSTENSDUIBXSTANCE BY SPONSOR
[N "Tokbe Ceompn leS ted by Sponsor S
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L Tes Substance Kent(ame to be sed ntherepor). BefySgulforni oAcicd. PtotasasiumnSaelt.
| SPuarmiptlye(%CoAdcetoivreBIatcnh Ngumrbere9:8L.do9t%i21e?2nt): Expiration Date: _2008
| IL Test Substance Characterization
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YHaovethetS he ideOE nFtihtyi,ssotrSehngatdha,yinDacLpcurity oanbrdadcwoniamtcpnhoesGcipLteePioenSdtoarenodtarrhdeesr?cdharpacotreristics Yes No X_
IL Test Substance Storage Conditions
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Please indicate the recommended storage conditions at Wildlife International Lid.
.
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bHeacsnthde steabiltityoeifntarhcecotmredstainscuebnwstiatenhceGudLnPdeSrttahnedsaersdtso?rage conditions.
Yes__ No X_
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Other pertinent stability information:
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IV. Toxicity Information:
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Mammalian: RatLDS0 251mg/g MouseLDSONA.
Aquatic
Invertebrate Toxicity (EC/LCS0)
Fish Toxicity (LCS0)
DsphniSa0mmgfla,gna: Eathcadminnow:38mgll
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Other ToxicityInfor(imncahitngfiinodinngsofcharndsoubchnroniictescts):
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PROTOCOL NO: 454/112498/7950/SUB454
000090
3MLABREQUEST NO. U2723
on WILDLIFE INTERNATIONAL LTD
a " on
Figure 1. Schematic of Spinning Rotor Gauge Apparatus.
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Ffha]tsoe
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1A oi =fr03 Nypy tEiaEl
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Lm wiolieBd=lL ll cecil oa
& 4 o Pp
8
@po
1. vacuum pump
6. turbomolecular pump
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2.turbovac controller 3. sample chambers
87..iioonn ggaauuggee: controller
4. water bath
9. spinning rotor gaisge
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5. spinning rotor gauge head 10. computer
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PROTOCOLNO.: 454/112498/7950/SUB454
000091
3M LAB REQUEST NO. U2723