Document 2q163Rp7oX84yRpEVa1rze1XN
TestingResults:Air-WatoPrartitioCnoefficie(nKtAw) for PFOS
AIRIWATER PARTITION COEFFICIENT
TEST SUBSTANCE
Identity:Perfluorooctanseulfonatem;ay alsobe referretdoas PFOS or FC-95. (1-Octanesulfoniaccid,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8heptadecafluoro-p,otassium saltC,AS # 2795-39-3)
Remarks:
The testsubstance isa whitepowder. No information was recordedon the purity.
METHOD
Method: There isno standardizedmethodology used todetermine thisvalueforregulatorpyurposes. The experimentwas designed by Dr.RichardPurdy of3M's Environmental Laboratoryand Don Mackay ofD. Mackay Environmental Research Limited.
GLP (Y/N): No Year completed: 1999
Remarks: The followingmethod was devised and used:
1 . Weigh approximatelz0.01 gram ofthe testsubstance directliyntoa
tared250-mL Pyrex beaker. Record weight.
.
2. Transfer200 mL ofNANOpure water intothe beaker usinga
Class A glaisvolumetricpipet.
3. Prepare solventblanksample. Using a gas-tighstyringe,transfear
250 pL aliquotofNANOpuie water intoa 25-mL Class A glass
volumetdc flaskpartiallfyillewdith50% methanol /50% ammonium
acetatebufferreagent.Bringto volume with50% methanol /50%
ammonium acetatebufferreagent.Ampulate inan amber glass
autosampler vial.
4. Mix and sonicatethetestsubstance inwater sample (50 pg test
substance/mL targetnominalconcentrationf)orapproximately10
minutestoensure dissolutioonfthetestmaterial.
5. Prepare the controlsample. Transfera 250 pL aliquotofthetest
substance inwater sample intoa 25-mL Class A glassvolumetric
flaskpartiallfyillewdith50% methanol 150% ammonium acetate.
bufferreagent.Bringtovolume with50% methanol /50%
ammonium acetatebufferreagent.Ampulate inan amber glass
autosampler vial.
6. Place the testsubstance inwater sample beaker on a hotplateand bringsolutiontoa boil.Afterapproximately10 mLs (5%) ofwater has evaporated,remove beaker from hotplateand coolto room temperatureinan ice-waterbath.Transfercontentsofsample into a graduated cylinderand recordactualvolume.
7. Process a 250 pL aliquotofsample as describedabove forsolvent blankand controlsamples.
8. Return sample tooriginableaker and bringsample toboil. 9. Repeat steps6-8 untilsample has evaporatedto100 mLs. Submit
allampulated samples forLCMS analysis.
RESULTS
[,(,,0:* TemperatureOC: Notrecorded.
Remarks: *DonMackayprovidetdhefollowiinngterpretaotfitohne analyticarlesults:
"As Iinterpretthelab resultstheyestablishedan initial concentrationof50 mg/L in200 mL water then distliiedoff10 m Laliquotsand analyzed theresidue.They then calculatedthe percentage oftheoriginatlestsubstance presentwhich remained in thebeaker unevaporated.These 'percentagerecoveries'r;anged from 136 to 105 withno realtrend.Iconclude thatthetest substance didnotevaporatetoany measurable extent.This isa verysensitivemethod ofmeasuring low air-waterpartition coefficient*sI.tcan be shown thatifwaterand thesoluteevaporate equally(e.g.t,hecontentsdo notchange incompositionas would occurwithan azeotrope)then K,, or H isidenticaflorwater and the solute.For water,H isapproximately2400 Pa (approximately 200C) dividedby 55000 MOUM3 or 0.044 Pa m3/r@olor a Kw of about 2 x 10-5 . The testsubstance must thushave a Kaw considerablylessthan this,i.e.lessthan 2 x 10-6.Itisthus essentiallnyon-volatilferom aqueous solution.Thisisprobably because ofitsionicnature.The simpleexpedientistoassign ita K,w ofzero,i.e.isa type2 involatilcehemicalinour nomenclature."
DATA QUALITY
RellabliltyK:Jimischranking2. Data has limitdereliabiliStaym.ple purity was notnoted. Study temperaturewas notreco* rded.
CONCLUSIONS
Testingindicatetshissubstanceisessentiallnyon-volatiflreom aqueous solution.
Submifter: 3M Company, EnvironmentalLaboratoryP,.O.Box 33331, St.Paul,Minnesota,55133
REFERENCES
Study conductedattherequestof3M Company by WildlifIenternational, Ltd.of Easton,Maryland.
Study reviewby Don Mackay ofD. Mackay EnvironmentalResearch Limited,
OTHER
Last changed: 5/1/00
I.,.ITERNALCORRESPONDENCE/3M
TO: Dale Bacon - Env Lab 2-3E-09 CraigBurton- FC Tech. Center 236-3C-89 Mike Nash- OGC 220-12E-02 BilWleppner- Chem EHS&R 236-IB-10
CC: Rich Purdy - Env Lab 2-3E-09 Joseph Fiksel- BattellCeolumbus Denise Appleton- Env. Lab 2-3E-09 Janine Seiffer-tEnv. Lab 2-3E-09
FROM: SUSAN A. BEACH
SUBJECT: TesfingResults:Air-WaterPartitioCnoefficien(tKAw)forPFOS
DATE: March 19,1999
WildlifIenternationaclonducted a studytoestimatethe air-wateprartitiocnoefficien(tKAw)forPFOS. There isno standardizedmethodology used todeterminethisvalueforregulatorpyurposes;thusitwas conducted as a nonGLP study.The experimentwas designed by Rich Purdy and Don Mackay. WildlifIenternationaplrovidedRich and Don withanalyticarlesultsD;on providedtheinterpretatiboenlow:
"As Iinterpretthelabresultstheyestablishedan inrdacloncentrationof50 mg/L in200 mL waterthen distilloefdf 10 mL aliquotsand analyzedtheresidue.They then calculatedthe percentageofthe originaPlFOS present which remained inthebeaker unevaporated.These "percentrecoveriesr'anged fmm 136 to 105 withno real trend. Iconcludethatthe PFOS didnotevaporatetoany measurable extent.Thisisa very sensitivemethod of measuring low air-wateprartitiocnoefficientsI.tcan be shown thatifwater and thesoluteevaporateequally(i.e. the contentsdo notchange incompositionas would occurwithan azeotrope)then KAw or H isidenticaflorwater and thesolute.Forwater,H isapproximately2400 Pa (approximatel2y00C) dividedby 55000 moVrT? or 0.044 Pa m3/mol or a KAw of about 2 x 10 -6.PFOS must thus have a KAw considerablylessthan this,i.e.lessthan 2 x 10-6.Itisthus essentiallnyon-volatilferom aqueous solution.Thisisprobablybecause ofitsionicnature.The simple expedientisto assignita KAw ofzero,i.e.itisa type 2 involaticlheemical inour nomenclature".
Please see the attachedanalyticarlesultsformore information.
Questions should be directedtoRich Purdy.
Regards,
S'u,sus4A. Beachh
Attachment (1)
W ildilfe
8598 Commerce Drive 0 EastonM,aryland0 21601
Phone:(410)822-8600 0 FAX: (410)822-0632
International
Ltd*
FAX TRANSMISSION
Ifthistransmissioinsnot receivedcorrectloyr ifpagesare missing,pleasecallWildlifIenternationaLltd.at (410)822-8600
Date:
anuary
PLE PSSEE@'DDE
From:
NOTES:
R( 0:
Fax Number: (651)778-6176
3 page(s)followthiscoversheet.
RichPurdy
3M Corporation 3NfEnviro=ental Technology and SafetyServices
Raymond L. Van Hoven Scientist
Rich:
Enclosedyou willfinda completed datasummary thePFOS air-wateprartitiocnoefficienetxperunentincludingthe datasuamiary,method oud=, and instrumentaclonditionsummary. Pleasedo not hesitateto contactme to discuss thefindingso,rtoprovideany additionaelxpmmneataldetuls.I look forwardto spealcmgwith you inthe nearfuture.
wmDLim uTnERNAMONAI, PFOS Air-WatorPalidM COCTIDCW Sequeme LD.: 12JAN" Projed No.:454C-101 Due of Anabn&.01/12/99
LTD.
Sample Nxm 467SA-OOlA4
467SA-MIA3 467SA-OOIA2 4675A-OOIAI 467SA-WIA4 4675-OOIA2 3736-OOIA4 3736-OOIA3 3736-OOIA2 3736-OOIAI
AWP1.XLS
(UWML)
1
250
2
Soo
3
750
4
1000
9
250
13
750
is
250
19
Soo
20
750
21
1000
Peak Arn 4155337
7399923 10491144
13024361 4246955 11036778 4309756 949377.4 lon"lo 13561071
12195.2 53733 0.985 515.1 1.1526P+14 #NA
1437081."l 35SQt.549 473031.497
8.000 17900703$MOI
#NtA
Fit 222.9372 498.0412 742.4307 950.1538 230.4007 787.1725 235.4790 573.6429 770.5794 994.1639
Y4ntercept SLOPE R2
14000= 12OW000 -IDOOOODO -8000000.-
pa" I
400=
2000=
0 0
2DO
400 ODO
800 1000
Carmntmdon (ngftl)
1437OS2 12195 0.9M7
Nominal
sampk
Concattradon Vbd
Identinestion
(UgftL) NO.
454C,101-REB-1
0.0
5
454C-101-AWP-1
50.00
6
4%C-101-AWP-2
52.63
7
454C-101-AWP-3
57.14
t
454C-101-AWP-4
60.61
10
454C-101-AWP-5
64.94
11
4W-101-AWP-6
69.44
12
454C-101-AWP-7
7S.63
14
454C-101-AWP-8
$0.65
is
454C-101-AWP-9
97.72
16
454C-101-5tmbffity
50.00
22
Peak Ana 172690 975W$ tWl77 SS11737 96420" 10220321 11137255 11133423 11851738 13073257 7SM9$
iniual vaium (-L)
0.250 0.250 0.250 0.250 0250 0.250 0.250 0.250 0.250 0.250 0.250
Y-"dude (ng'mL-)0-k mv"-bta-pt)/siope) AMoed resul(tn&'mL)- (Y-nWude * diludmfea") Dibman bctw -(FuW vobxwfmtudvolum) Pa-t r-vay - [walyucerlmdt (r4tmLYnmuW cwmtrabm (rgfml)xltoo Allspmadshed adailkiormperfannedusingEOCCEL 5.0V inda fullprecisiomnade.
Flow vow=
(-L) 25.0 25.0 25.0 25.0
25.0 25.0
25.0 25.0 25.0 25.0 25.0
Ditudes Fwtar 100.000 100.000 100.000 100.000 100.000 100.000 100.000 100.000
100.ODO 100.ODO
Y-Evaluate AnalyUcalResult
(ughnl) (uglinl)
<M
-CS.0
6213597
62.1959
597.8639 604.7197
59.7864 60.4720
672.9047
67.2805
720.2233
72.0223
795.4116
79.5412
795.0914
79.SW7
853.9990
85.3999
"4.1632 S27.4492
95.4163 52.7448
percent Reco-y
(%) NA 138.4 111.7 105.8 lii.0 110.9 114.5 IC)5.i 105.9 10&8 105.5
CERTIFIED COPY OF THE ORIGINAL
---MMALS oi isitt I I
DATFJ uj 441L
WildlifeInternationLatlcL
M[ETHOD OUTLINE FOR THE DETERMINATION AIR-WATER PARTITION COEFFICIENT
ProjectNumber:454C- 10 1
OF PFOS
1. Weigh appproximately0.01gram ofPFOS (WIL# 4675A) directliyntoa tared250-mL Pyrex*beaker. Record weight.
2. Transfer200 mL of Nanopurde water intothebeakerusinga ClassA glassvolumetricpipet.
3. Preparesolventblank sample. Using a gas-tighWtxinge,transfera 250 gL aliquotofNanopure" water intoa 25-mL ClassA glassvolumetricflaskpartiallfyillewdith50% methanol/50% ammonium acetatebufferreagent.Bring to volume with 50% methanol/50% ammonium acetatebufferreagent. Ampulate in an amber glassautosamplervial.
4. Mix and sonicatethePFOS inwatersample (50ligPFOS/mL targetnominal concentrationf)or approximately10 minutes to ensuredissolutioonf thetestmaterial.
5. Preparethe controlsample. Transfera 250 gL aliquotof the PFOS inwater sample intoa 25-mL ClassA glassvolumetricflaskpartiallfyillewdith 50% methanol/50% ammoniwn acetatebuffer reagent.Bring to volume with SOO/omedmol/50% ammonium acetatebufferreagent.Ampulate inan amber glassautosamplervial.
6. PlacethePFOS inwater sample beaker on a hotplateand bringsolutionto a boil.Afterapproximately 10 mLs (5%) of water has evaporated,remove beakerfrom hotplateand cool toroom temperaturein an ice-waterbath. Transfercontentsof sample intoa graduatedcyuinderand recordactualvolume.
7. Processa 250 glaliquotof sample as describedabove forsolventblank and controlsamples.
8. Return sample tooriginalbeaker and bringsample toboil.
9. Repeat steps6-8 untilsample has evaporatedto 100 mLs. Submit allampulated samples forLCMS analysis.
WILDLIFE INTERNATIONAL'LTD.
LC/MS OperationalParameters forthe DeterminationofPFOS Air-Water Partition
Coefficient
MASS SPECTROMETER:
ION SOURCE: ION POLARITY: ION SOURCE VOLTAGE: ION SOURCE TENTERATURE: IONMONITORED: LIQUID CHROMATOGRAPH: ANALYTICAL COLUMN:
MOBILE PHASE:
FLOW RATE: INJECTION VOLLTNffi: RUN TIME:
Perkin-ElmerSciex API 100 LC Mass Spectrometer
Perkin-EhnerTurbo lonspray
Negative
5200 V
450 OC
498.6 amu
HewletlC-Packard1090 Series]I
Keystone BetacilC- 18 (2 mm D:),100 mm, 3 gm particlesize)
65% methanol/35% ammonium water
acetatebuffered
240gUniin
10 gL
8 minutes
P 92
,DMER
D. Mackay Environmental Research Limited
1604 C;hamplainDeive Peterborough,Ontario Ceiiada K9L IN6 lial(705)740-Pgl *I GST Reg. #R-101420263
3M991
'ro:Y)r.RichPurdy,3M 1.)rJ.oyc-cNwAlKCuoper, DaiLeDe
I)aw Rich and Joycc
I reecivedthe"Fluorochemical1.,U,&,aMcoidteyling Requiremnts" statcnientI.tisgenerallyin agreementwithour expectationasnd we willdo our bestto satisfyyour needs.The principal problem will,1 suspect,be &ratherintgheh4mt datilWe can keep inclosecontactwith you regarxiintghe uiodeldevelopment.
We obtainedfrom you thePL,'OSair-wateprartitionindgata.As,I interpretthelabresulttshey e.-;tabU,qahnediniticaolncentratioonf 50 mg/T.in200 mL wathrthcndistilloefdf10 mL aliquoto. and analysedtheresidue.7UY thencalcuhitetdheperccntagcof theoriginaPlL-'OSpresentwhich mtmine d inthebeakerunevapomted. 'I'hes"epercentrecoveriesr"angedfrom 136 to 105 with no realt' rend.I co=lude thatthePFOS didnotevaporateto any nxwumble extent.'Jchisa veryscnsitivmcethod of measuringlow air-w-.iptacrtitiocnocfficientIst.can be shown thatif waterand thesolutecvdporateequally(Le.thecontentsdo notclonge inconw.-.itioans would oc= withana7wtrope)thenKAw or H isidenticaflorwaterand the.-.olutFeo.r waterH is approxhnutel2y400 Pa (appmximatcly20*C)dividedby 55000 nwitni3or 0.044Pa rnl/nwl.oar KAw ofabout 2 x 10--.PPOS must thushave a KAw considetabllyessthanthis,Le.lessthan2 x 10. Itisthusessentialnloyn-vt)latitkhim aqueoussolution'.rhisisprobablybecauseor its ionicnature.Ilm simpleexpedientisto &-.siginta KAw of zero,Le.itisa type2 invok"c clwnicalinour normiielature.
We didsampleEQC model ruinsusinga KAw of zert)a,nd punitionca)eflicieLn/tksg forsog-water of2.4,%ediment-wateror4.8 and rish-wate(rdimensionlesso)f 1000. The dimensionle%p,asititic)n coefficienatrsehigherby a fitctocrorrespondintgo thedensity.ilm degradationhalfliveswere allml at 10 yem. I attachtheLevel1,11and IIIresults.
The TevelI resultsshow that?FOS hasa.,%trutnegndencyto remaininwater,i.e.typicallgyoo/o with20% iisioil.
I'hclevel11resultsshow an identicadlistribution. rmjor lossisby advectioninwater with
p 93
onlyveryslow degradation.The overau persistenceina regioniscontrollebdy the.water row;dcm-ctiim. The LevelIIIrcsuhssht)wdiat:Ifdischargedtoairitwillrapidlydepositto soil(900/oa)nd water(101/*). IfdischargedtosoU ittendsto renviinthcrewith themajor lossbeingrun-offto watcr because of itslow sorptiontendency. Ifdisrhargcdtowater itt=W,.toremain in.solutionand issubjectto removalby advectiveflow (9(rla-) *rhereL-l;ittlscurptk-)tno sedimenls. In summary, itbehaves much as one would expect of mongly ioniccompound. I believeitisimportanttomeasure rcalpartitiocnoefficientfsorinclusioinnthe model and perhaps rcflnethe halffive-.I.n thepre.,4ernctgwatory climatea substs, which isso persistenits going to come undcr veryclosescrutiny.I wonder ifitispossibleto builda degradation weaknf.-,i4nstothe mlcculc? In conclusion,wc arereadyand willingtodo modeling atyour request.Pleaw M-gardthiqasjust a!;mallLimistop. Your.%truly
c@@ Don Mackay DM/mm