Document 5b7k4RMN7OJ1XXMkv9nVbb04e
SOIL ADSORPTION - REVISED
TEST SUBSTANCE
sS i T EETl ram ry productionlotofFC-95. Purity determined to be 97.9% by LC/MS, 'H-HMR, "F-NMR
wEWOO
[=EE Ea SS[oEm EmES E Rea ES,ReeEen mmS[eEiTseemu|speeiee[n0 5n===5e5] [Lothmber| o02i0r| oodos|eezes|ooas|zi|
PDoeuSiCnPaHON | i 1.000m., mdaioro-p | r1.0e00m4dmdaio,eop |die1d,0005"mdomop|| ie1d0005"mdemop| | "2h00emnecseh
ff[heEoeermT[T===m[T[=e=[[[[oo==mm [[[o==wm[a[2]7:|] :
a
"Value iforpH inwaternot pH in 0.1MCaCl
E[8 :22 z=
CONTAIN NO CBI
000255
--
`sAluddsgoersp)twieornsKeiqnueitliibcrsa:tedRebpylsihcaatkeinsgtfuodryastamlepalsets1c2ohnotauirnsiantg rtoheomsotesmp(oerrsaetduirmeewnitths 0o.r01 M CaCl. Study samples were dosed with the test substance at approximately 0.5 mg.
and placed on an orbital shaker. Replicate setsof thesestudysamples were removed at
rs po posal st rs. So sa wren prepared and analyzedfor the target analyte. The adsorption kinetics were determined i ri a using this data. The lastsetofstudy samples (48 hour) were saved and used for the
Desorption Kinetics (One concentration): After the adsorption kinetics
a 23erenoouCoyaIisnnaamm pwywarowohoapSrooomo mapoil removed. Thevolumeofsolutionremovedwasreplacedbyanequalvolumeof0.01 M
RESULTS
Adsorption Kinetics of PFOS, 1:5 Soil:Solution Ratio,
E[E mtnE [on|EEE| LC 48 Hour Time Point
Ce oen w on a ee mwe=
[[Chowmsmon [0 va[ [w ww w||
[Comms | com | me| ores |
Brn
----
Apparent Desorption Kineticsof PFOS, 1:5 Soil:Solution Ratio,
e em| e emo 48 hour Time Point e iw e ] C mo e m e e e s] ]
000256
ib HNe og iaees di `Theriversedimentdisplayedthemostdesorptionat39%after48hours.Thesludgesamplesdid
significantly.
[rAodsrormponn o[threorasrs[IGTT ] SoFretee | FeezCo [ om T owo [[owno[|m ow mi [e n i] e w [[ovmwsmoammes|| e03[[mo2o[ | w wos o |mor]| [oman 20[om|mow]
`unitsare(ug) Kg")
ernie [sormme [ogtem,[RET|Pewsymein ReorsiGonin [mFiooe[ior[Toeo[a oes [] wm] [[oosmeer||5r9s0s[[swwsi || owroz[w |o] s|
`accurately, the units are (ug "(L)"Kg")
J bn oeseo-- samt
CONCLUSIONS
oe scoomreenssCER laole i ame eD a Perflucrooctanesulfonate (PFOS) appeared to adsorb to allof the soilisediment/siudge: fSurbmeitn, d3sCompas,EnecnmatalLaboratory, PO,Sax3501, 1. Pc,
000257
DATA QUALITY Reliability: Kimisch ranking 1. REFERENCES 3PeMrfTieucohrnoioccatlanReespuolrftona"Staeil(PAFdOsSoYr'p.lioMna/rDkesEo.rpEtliloefnsSont,udPyroojfecPtoNtausmsbieurm 00-1311, Final Report Completion Date June 4, 2001. Amended Report Completion Date May 24, 2002. oTHER Last Changed: June 12, 2002
000258
Study Title Soil Adsorption/Desorption StudyofPotassium Perfluorooctanesulfonate (PFOS)
Data Requirement Based on OECD 106
Author Mark E. Ellefson Study Initiation Date October 17,2000 Study Completion Date
DaofStigneing PerformingLaboratory 3MEavironmentalLaboratory Building 2-3E-09, 935Bush Avenue.
St Paul, MN 55106 Project Identification 3MLaboratoryReportNo:E00-1311 AmendedFinal Report Total Number ofPages
0
000259
`Thispage hasbeenreservedforspecific countryrequirements.
`3MEnvironmentalLaboratory
000260 Page20f703
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GLP Compliance Statement
i Study Title: @Fos) Soil Adsorption/Desorption StudyofPotassium Perfluorooctanesulfonate
`StudyIdentificationNumber:~ E00-1311
`Thisstudy was conductedincompliancewith ToxicSubstances ControlAct (TSCA) Good
LaboratoryPractice (GLP)Standardswiththeexceptionslistedbelow:
Exceptions toGLPcompliance: 40CFR 972.Th1 ere3 isn0ot( aneclec) tro: nicaudittrailofcorrections. The
authenticatedhardcopyprintoutsare constheioridginealrrawedatda.
=
N
E.
v, StudyDirector
Willip amK. Rt eagen,rTesing Faclly Management
2G fog) /e,
oDratbe it,
3MEnvironmental Laboratory !
000261
Page 3 of 703
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`Quality Assurance Statement
4 SudyTide: Soil Adsorption/DesofoProtpatsisiounm Perflorooctanesulfonate (FOS)
`StudyIdentification Number: E00-1311
This study wasauditedby the 3M Environmental Laboratory Quality Assurance Unit (QAU), as
minadniacagteemdeinntthe following table. The findings were reported to thestudydirector and laboratory
oo oe
[om
ee[oe [on| erm [| |
eon| | |
| ene | mm |oem|
CAT = hepresave
GBa0 e
aM Ensionerontal Laboratory
Page 401703 000262
--
`Table of Contents GLP COMPHACESETI
sss snd
LISOfTUBIES.sssmssssss mss
THI Rassias ----------------
ee
|
Appendix A:StudyProt060l BO-I3L1e crs
25
ADP'EETDS-I8X-B15:5A"RPrRepIarVatEionMoEfDSOoBilSSurplsrfx o reliminary(Ter r)SoptonStos ic fo Forochersials 51
ETStSu-d0i-e1f6o0r"FPuroerpaorcabtoimonicolfsSao5iltSeuTpelsetsSUfobrSSOc0reEe"nv ing(FerI)sndAdv vanced TirTH)S: orption 7 E`TOSEC8D-110565 ""AAndasloyrsipstoifoP-noDteasosrspituimoPnefUosoirogocaBtaantecshlfEonqaiuoiFObMeesiFloodorc ocheaicasr isWasteSo ain89
[ETS-3-110 "Analysisof PtasiumPeorooctancsulonatc ofOberFuoxochermicasfnWater
APPEDix D: [iVidUa] SAOPIC DIR.
191
AppiB:Qality CoRrol SATPIe DA...
281
Appendix F: Notes 0File nd DEVIGtOn FOS vss 24
ADDEnCix H: Rew DAta SWRIAIICS vss
483
APPCOAiEx TraGeAbilY IfOBHO....rsssssssssssns 594
3M EnvironmentalLaboratory
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List of Tables
Table 1. Summary Tableof PFOS Adsorb/Desorb Tier I SUES...
T
Table 2. Summary TaobfPlFOeS Adsorb/Desorb Tier I SWes vv
`Table 3. Summary Tableof PFOS Adsorb/Desocb Tier I SEES..vvvvsvrrn
`Tabl4e. CSUhBSaAOCrESar cotfteherm TeistzSubasts tanice,oTenst SysantdAenalmyti,cal Reference 10
"Table 5. Test System Distribution for Study LRN-EO0-1311 rrr 13
Table 6. Sample Collection and Preparation for Study LRN-EO-I311 ccs 1
Table 7. Suitable Analytical Method Determination...
1
Table 8. Suitable Test Vessel DEICTNRHON vv
11
Table 9.EquilibriumTime for AJSOPYOR Of PFOS
srr 18
"Table 10: Suitable DesordSOIVEDt,MERA...
19
Table 11. StabilityofPFOS during the Study Period.
20
`Table 12. Adsorption Kinetics ofPFOS, 1:5 Soil:Solution Ratio, 48 hourTime POint..........20
Table 13. Desorption Kineticsof PFOS, 1:5 Soi:Solution Ratio, 48 hour Tite Point... 21
Table 14. AJSOIPHOD ISOctrcDETTIS.
2
Table 15. DESORPHOD INES...
23
Study Personnel and Contributors StudyDirector Ma3rMkEnEv.irEloincmfesnotnal Laboratory B9u3i5lBduisngh2A3v5e-n0u9e St.Paul, MN55106
Sponsor `3WiMllEianmviKro.nRmeeangtaanl,LLabaorbatoorryaMtanoargeyr 9B3u5ilBduisngh2A3v5en0u9e St.PaMuNl551,06
`3MEavironmentalLaboratoryand ProSferveicessContiriboutinngPerasonlnel (PCaicnedyAnMal.ytCicaarllSesrovnices, Toc, 1700ElmSt,Micucapolis,MN 55144) (BLrianudnanAi.tGeooCdosrppoereatdion, 6875WashingionAve.South,MianeapMaNl55i4s39,) (BKrraiustninInLt.rTtecrCroerplolration,6875 WashingronAve.Sout,Miancapolis,MN55439) M(Barraukn ILn.teArntedeeCrosrpoonration,6875WashingAtvoen. South, Minneapolis, MN 55439)
`3MEnvironmental Laboratory
Page 6of703
000264
_--_--mmmm
A ---- LocationofArchives
`Thetestmaterialsandanalyticalreferencestandardreservesamples,aswellasthesamples. `pertainingtotheanalyticalphaseofthisstudyarearchivedatthe3M Environmental Laboratory.
Reservesamples,digitalcopiesoforiginaldataandalloriginalpaperdatawillberetainedinthe
arcofh3M Einvivronemenstal Laboforrapaeritodoofartleyast 10yearsfolltohewefifecntigve
date of the applifincalatebstrlulee.
Summary
ld rt te Apreliminary,screening,andadvancedstudy ofthesoiladsorption/desorptionofPotassium
Perfluowar s po erfoo rmec dtotbeta terun ndee rstas ndpu artil tiof ningo undn eraa vart ietye of
tested. Analyseswereconductedasdescribedby3MEnvironmental LaboratoryAnalytical
`MethodsETS-8-159"PreparationofSoil SamplesforPrelimi(nTiaerrIy) SorptionStudiesfor
S SSEm mei E FluorochernicalsastheTestSubstance"andETS-8-160"PreparationofSoilSamplesfor
`Resultsofthestudyarepresentedinthefollowingtables:
"Table1.SummaryTable of PFOSAdsorb/DesorbTier I Studies
[Gestion
TComiwn
meEbR eI E i [i r ma o mmstein
[me rtmma]
ema
astm
000265
meee----------------------
Table 2.SummaryTableofPROSAdsorbDTeersIoSturdibes
[omommmeerra T T om T a ] we |mses [mw a [ommesperse| sm | wm | wm |
`Table3.Summary Table of PFOSAdsorb/DesorbTierIIIStudies
smn | wo
[Comtem TwTe a
[em Te
[Cocoa |b
a
[omen |eT|e a |
Introduction Nose:Theanitsfortheisothermsassume thatthetera r=]. Moreaccurately,theunits are(ug (1) kg)
EF EFT kf EF
F~EN N IN INOYN F P Ye
yr
POTASSIUM PERFLUOROOCTANESULFONATE (PFOS)
(CAS Number: 2795-393
Chemical Formula: CyF 780K.
`Molecular Weight: 538.22 g/mol
Purpose
C`hAedmsiocrpatlisoann/ddestohrepstidoinsstrubduiteisoanrienutsheefsuillf,orwagtenee,raatdingiescsmenpteiarliimnefnotrmofaotivoonnbatshephmrobei.liTtyeoyf `crannsbfeorumsaetdiionnthaenpdruedpiackteibonyoorregsatnimiastmisonloefathcehaivaniglabpirloifteyso,foacahemticaflrfoomrsdoegfraadnadtioonf, f mfordoemllainndgspauporsesf.inatocnateursal waters. Adsodar tacpant alsi obeousn edforcomparatainvde
3MEnvironmentalLaboratory
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`oTnhedniustmrbibeurtoiofndoifffearcenhtefmaicctaolrbs:etthweecehnesmoiiclaalnndaatquureeooufstphheassuebssitsan8cec,otmhpelcehxarparcotcereissstdiecpsoenfdtihneg `oplh,enaonmdecnlaiamnadtomfeacchtaonrisssumcsihnavsoralivnefdaliln,ttheemppreorcaetusrse,ofsadusonrpltaionindogwfihancdth.emTicahlbtyhusenoiulsmcearn,onuost `bveecn fothimsatptdeemflpitnceeadnbntyoatasedidmrplelsisfyiacldlolfatbhoeraetnovriyrmoondmeelnstualcphoasssitbihlepitrieesse,inttpgruoivdieldiensve.alHuoawbelveer, informationontheenvironmental relevanceoftheadsorptionofa chemical.' s`oOiElC.DTghuegoialdis1et0o6loisbiaaiinnmaeesdoartpetsitoinmvaatliunegtthheatacadnbseousredptotpriedoicntbpe/ahradtviiteoirosonifonag rusnupdbestrtaaincoeonn `vcahorefemnintvioivrecaornaimteolautsysalolcsoanditdieotnse.rmTihneerdefaosrea,fuenqcutiiloinbroifusmialdcshoarrpatcitoenrciosctifcTsi.ieDnitfsffeorerntsoil t`yopcecusrmruinsgstoblesu. sTdhiensooridlepratraomceutlearsttehtahteairnetbeerlaicetvieodnsmoofstagiimvpeonrstanutfobrasdwtistoahnrantpuarctralieelpyoHn, oarrgedaensicicganrebdtonoceovnatleunatt,ectlhaeyacdosnotrepntti,oannofsaoiclhteemxitcuarel.oTndhiefpfrroecnetdsuorielsotyuptelsintehadtihnatvhee avaryiguindegline rangeofpH,organiocarbon content,andsoltexture,Theguideline iscomporftihrse etiedrs: 11 Tierl:ThePreliminStaurdy
LLL Theprelstudiyismdesiignendtoadeterrmiyne: 2) suitableanalyticalmethod b)theadsorptionofthetestsubstanceontothesurfacesofth testvessels )attheecqquuiilliibbratiiuomn timeforadsorptionandtheamountoftestsubstanceadsorbed asuitable desorption solvent the soil:asqoluutieonoruatsio 9thestabilityofthe test substance duringthe study period.
112 LTahbeorparetpoarryaMteortyhmoedtEhToSd-o8l-o1g5yf5:oPrrTeiparraLtiisdoneoscfrSiobieldSianmtphlee3sfMoErnPvrierloinmmiennatrayl (`TOiEeCrDG)SuoirdpetliionneSt1u0d6i)e.sforFluorochermicalsastheTestSubstance (basedon
. 12 T1i2e.r1Ii:TSchreesecnrienegSntiundgsyt:udyisdesignedtostudytheadsorptionofthetestsubstancein three differntsoil systems,onesediment, andonedriedsludgebymeansof: 4)adsorption kinetics atasingleconcentration b)determination ofdistribution coeficients KyandKoc
122 LTahbeorparetpoarryaMteortyhmoedtEhToSd-o8l-o1g6y0f:orPTreipearraItiisodneosfcSroiibleSdaimnptlhees3fMoErSncvriereonnimnegnt(aTiler 1)andAdvanced(TierII)SorptionStudiesforFhuorochemmicalsasthe Test Substance (based on OECD Guideline 106).
13 T1ie3r1IN:ThAedsoarptdionvIssotatuhdcyrnimsadecnsdiDgeenseodrtdpot:ion Kinctics/DesoIrspotthieromns 4)determinetheFreundlichadsorption isotherms that,inturn, determinethe
hc1cOaECDrGusldenn1g06 3M Environmental Laboratory
Page 9.0f703
000267
m-- r-- p ----------------------
trly da esptionn by meansofdeters deorpionKinet Freunich influenceofconcentration on the extentofadsorption onto the soils, sediment
and sludge.
SimbedeonGa3 nGdsn 106, 132 LTahbeorpartepoarryatMoertyhmoedthEoTdSo-l8o-g1y6f0o:rPTreipearrIaltliiosnodefscSroiibleSdaimnptlhees3fMorESncvriereonnimnegn(tTailer 11) andAdvanced(TierIIT)Sorption Studies for Fluorochernicaalssthe Test `
Materials and Methods
`Chemical Characterization
Table. Cather Tos Saba an,Ttyc stem nda Antsl Reine
`Substances
[mse
we | mee]
[I == -- [awe -- lIoo-- m |
[om ee er n es r]
C-- ThT fo -- fw |
I oni --T-- eT t -- e
e To e TIp Sy e] e ST For FOSsabilty formations fo 3 EnverLabtey prt AllsolubilitydeterminationsofPROSTCR-00017-046wereconductedat22-25C. WAST PFOS
`hydrolysis study).
[O--
Page toot
000268
_--_--m--m
[o=e[=[=T [T eZE] T |Some [apie [gic [apie [Acie [Agiw [ost |
CEB=L=SEEeeenlm m ffoI en ffm m=ee effame fr o[[= mfoe| [Smad [lex
[esi Tame [owTew
[sow Tom
we
[2m [aon Jaw
[see [am [2% [ew Tam Jw
[WA | wa | [wa |
TETes a titl Saei MethodSummaries
SultableAnalyticalMethod:
ar Asoilofhighadsorbability (highorganiccarbonandclaycontent)isagitated withan
`appropriate volumeof 0.01 M CaCl,solutionata1:5(w:v)ratiofor aminimumof 4 `hours.The mixtureiscentrifugedandthe aqueousphase filtered, ifnecessary.This
`volumetricflasktoreach anominal concentrationwithintheconcentrationrangethat is likelytooccurduringthetest.This "studysample"isthenanalyzedusing HPLC/MS.
EE Afterthestudysample hasbeen analyzed, adeterminationismadeastowhether imMaER S BSSa pHEaemIitoRi nEE De r ne Ri E seRpA L m t SDa RAe E Ts E i E egt eea t eL eatrs rgeaE,r+e * SelectionofOptimalSoil:Aqueous SolutionRatio,DeterminationofEquilibration
000269
--
tuSb0e0smcyaLnbPeRrOeSmtoov.ecdaotnincteervnalts (orsfap$atn.nOiimngog/nL0.toS4u8ffhirc)ieannttdutbheesaaqueeopruesppaorretdisounchthat tainmael.yzTzhde.oEpqutiilmiablrsiouiml:isodleuttieornmianteidbiydpeltoetrimnigntehdebaydscoormpptaiorninogftohfettheesatmsoubusnttanocfe over asdasmoprlpetsi.onAocftcheteesptvastulbusaetsaanbcreelasotieel:qsuoilluitbiiounrmaftoioththvaargiiovuessaodielp:lestoiloinoonftrhaettoessttudy cdehteemrimcianlgerebayteartmhaasns2ba0l%aancneddperteefremrianbaltyiognrefaotllotwhianng 5a0m%eathtacnqoulielxitbrraicutmi.onStoaftbhielsiiotysl `gTihveemsaasdsepblaeltainocneodfettehremtiensattcihonemiisccaolnadbuocvtee2d0o%oatnhedoprnefseorla:bsloyluatbioovn e a5t0o%peart soilthat equilibrium. SuitableDesorptionSotvent: Mheitghhacnlaoylcwoantseinntvseositligwaatseddoasstehdewsiuitthatbhleetdeesstosrupbtsitoannscoelvaenttwoflorevtehlste0t.s7u5bpsgt,an7c.e5.ugA). ``TThheetceosmtbsiunbestdamnectehwaansotlhexetnraecxttsraacrteetdhfernopmrtehpeasrteuddfyosaamnpalleysstihsbryeeHtPiLmeCs/wMiSt.hmethanol.
Ieqnuailllibcraasteiso,ansdteeqpusawteerqeupaelirtfyoarsmseurdaantc1es9atmop3l0edsewgerreeesprCe.paredand analyzed.The
= ETS.8160"PreparationofSoil SamplesforScreening(Tier11) andAdvanced(Tier TIT)Sorption Studiesfor FluorocahstehemTeisteSucbsatalnces" TierTI: AdsKoinetris(pOnetconcientroationn): Asptpurdoypsraimaptleessociolnstaanidnoirngstehdeismaeinltss(oarndsleodrismlenutdsgeosrwselruedsgeelse)cateeedqfuoiltihberastteuddby.ysRhepalkiicnagte f`owirtah tlheasetst1s2huobsutrasncateraotoamptpreomxpiemraatteulrye0w.itmhg0/.L01anMdCplaaCcle.dSotnuadnyosrbiatalmsphaarkleerd.eossed R4e8phlicaotiesmeetuspeorfritohde.sSesttuuddyyssaammpplleessaarreetrheemnporveepdaarteddeasnidgnaantaeldytziedmfeoproitnhtesttahrrgoetughouta a`nSaalmyptlee,(T4h8ehaodusro)rpstrieosnaKvineedtaincsduasr eddeftoerrtmhiendeedsuosripntgitohniksindeattic.sTphoerltaisotn softothfesmteutdhyod. Tier Il: DesKoinetrics(pOnetconcientroationn): AtfhteaertqheaduspohreapsteioorneKmuionvetesidc.s eTxhpeevriomleunmte,otfheso4l8uhtoiounrsrteumdoyvseadmipslreesplaarceceednbtyraifnuegqeudaalnd vdoelsourmpteioonfe0q.u0i1liMbCriauCmliswiretahcohuetdt.eDsutsruibnsgtaan4c8e.hTouhrepnereiwodm,ixatturdeefiinaegdtitiamteeidnuenrtvialtlhse, `esxmpalelriamlieqnutottsheonfctohnetaiqnuueesowuispthhatsheoarriegrinealmmoixvtuearned,dTanhaeldyezseodrfpotitohnkitnaertgiectsaanarleyte. The determinedusingthisdaa. TierII: Adsorption Isotherms(Fiveconcentrations): Fsiavmepleesstscuobntsatiannicnegcosnoiclen(torrastioens adreouirsseldmu,dcgoeevse)rniinncgtotnwtoasocrtdweirtsho0f.m0a1gMriCtauCdel.aSrteudy weithqtesutsiubfsoltraancime.ibnTihmreusmaofa1t2maheorupcdrtshl.enAgefeenrtsley qagituateid ulnttihlieasdbtsourrdpytsiaaomnptclqeuisialoberidnooms,eisd Trheaecshendd.ySsaammpplleessetasreatrheernpermeopvaerdefdroamntdhaneoarlbyizteadlfsohatkhertaatrdgeestisgnnaaltyetdet.Timheeiandtseorrvpatlsi.on
34EnvironmentalLaboratory
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000270
_---,m.m,A_M,eorH.nr _._,.,..ee--
S R Er R isothermsarecalcuusilngathtisdeatda.Thestudysamplesfromthelasttimeinterval NcThestudysamplesfromtheadsorptionisotherm studyareusedforthedesorption
isothermstudy. Thesesamplesarecentrifugedandtheaqueouslayerremoved. An equalvolumeof fresh 0.01 M CaCl,solutioncontainingnotestsubstanceisaddedto cach sample. The samples are placedinthe orbital shaker and equilibrated for48 hours. Thesamples arethenpreparedand analyzed forthetargetanalyte. (These study `samplesaresavedand usedtodeterminemassbalance.)Thedesorption isothermsare. deteursimngithnisdeatda.
`Thestudysamplesfromthe desorption isothermstudyareusedforthemassbalance study.Thestudysamplesarecentrifugedandthe aqueouslayerremoved. Three `portionsofmethanolare addedtothestudysamples.With each addioftmeithaononl, thestudysamplesarcagitated,centrifuged,and themethanolremovedandplacedina
``secaondcnofnotaaritnhleert.ayTrhgeeztsaenseaulbystdee.quMeanst s(bmaetlhaanncoeli)ssdtuedystameplreussmianrgeitthhniesndepartedap.aredand.
mEoRm l AE TEa |Il [ConmoiBlans| 15 | 15 |
DesorptionSolvent" Solutions
e=a ee Alii Citi
Spikes.
iE=mi a | `TierIl"Adsorption | Test Substance| 144+48Matrix
Kinetics"
Solutions
Spikes
gy Kinetics"
Solutions
spikes. Spikes
Spikes
000271
E--E------------------------
`Tier I "Adsorption | TestSubstance 180+60Matrix 180 + 60MatrixSpikes
IsothermsTM
Solutions. orSpmikeas n| 367 Zmarkepies
spikes
TierTibDeersmorsp"tion | TeSsotluStuiobnsse| 90+S3p0iMtearix | 89+30MarSpies
TierIT"Mass,
Balance"
TestSubstance | 90+30Matrix. '89-+ 30MatrixSpikes
Solutions.
Spikes
`Control Blanks| 18+ matrixspikes | 18+ 6matrixspikes __|
`SpecimenCollectionandAnalysis `Duringthecourseofthestudy,aliquotsofthetestsystemswerecollectedatpredeterminedtime
sianmtpelrvianlgs.reSgoimmeensaimnpfolremaatiloni: qweuredoiltutsed with methanol. The foltlabloedewsciribnestghe "Tabl6e.SampleCollection ndProgaraton orStudyLRN-E00-1311
"STienrblle || Esxhcahgotarhmoeteqsoilu ,bweiheiOd0iIcMntCaane dltihen||dEoasecdh-mmaupsolluton,"s|| Sampl1e1s0a2li6q0uoted AnaWlyotikcal|rtermiponlvidectadthew.arThdiiosns"emgdatwsriihhxsiohlneutisotnu"biasebteaheens, `controlsampleisprepared. "STuiralble || Fotmeoripaloscfeossteesohctcehtofsatdanicfeffaoxt||doEsxecdh ptweoocfocncopritinosns|,| aAliqcuootweds1p1i1e4s00 Contin" | f24orhoours.sTthosremanlingmsesshusianymnlaowys0a|| aprnedpaereod.fEcveorlyvseselis || aMiihoapnoeldcx1t1c1t5i/o0s0
hecoonmainr,yThtetebtvceeeldaenxeybtce || xhsabwiactacheanoeslbdefer Tl |sTtooebdpesotfosohleaidmfedhwoichomoeers.s |Exhpemoif,sdaosledsaf|Mobo] tons D"eSwripnieon|| ms staooi tianvdstea esso.lTmhn eexcxia, covair ||towfoccoonrtsorornompdlaa.ssst| aliquoted 12201 Sovet| combined sboidnyosfbeestvoemrets.es he
"STertton| s"Tooolplessoaolhtloateepirkopaensdrhmeaeptetnesol | conxbicstohnsapeetpreidn||sAigenoend1m729s00.
OpSianioSnot:||Sur mp ro o retahreemdett isenveerroife etpstye.to|| t efccoeocmdl anwrsc, o,ol ||Methan1o2l4ex0r0stons
MaRsoBslnadc||dereicohno th oneq iaddaofi st, ebscinon
prepa
suo 12700
ionsperiod
IMEmironmonta Laboratory
Page tac700 000272
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"AdTseolplion ||pTrhepraersedi,toheosseodiss,soun honeiinsdhicdoagteesndien||1Esapchesoeloipnspacoinrcbiaoe,moidnone|| aAldiuceuootneds2p1i0e1s.
Kinetic? | theeTsirtusbtusdtyo.cTehansdpluacepdonodaosshsakewrie,th|| maanrdeasiektoifscpoenrttroorlesd, pe
samparlheenspulled sevetirmepaoinlts
reared
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loberme"|thhoeTeisetsbsstuadnyc.eTh(aetosacmoplfeSscarondeocsteidwoinlh)|| mpatresepiikpneirasipplerircoaete,moedod. snl
ond quiredforor4c8hoew.
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Totem"|`vaeqssueeloaunsdCthehveossetlspilaceaodadennd03shihakeesrftor|| epverryeh5ipdasmaaarxlespleisd
"shou.
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came ot thesmeves
`Dainlaultyezdedsuasmipnlgehsig(hi-.pesrafmoprlmoanexcteractqsu)icdocnhtraionmiantgog2r5a0pnhgy//mmaLsTssHpPeFctOrSomaestriny(teHmPalLCst/aMnSda)ridnwtehree fnreogamt2i.v5ei-o10n0m0odnge/.mPL.FPOFSOSleavenldsw2e5r0enegv/amlLua.tTeHdPvFerOsSu.ssItnatnerdnaarldSctuarnvdeasrrdanqugainntgiifinccaotnicoennwtarsatuisoend dteopbreosttofniattaenddTrHePpoFrOttShe(damtza.=4T2a7r)g.etionsweredeprotonated PFOS(mz =499),and AEnnavliyrtoincmaelntdaealiLlasbaorreaitnocrlyu;dtehdeisntutdhyeffiolldoeritshlioscsattueddyitnhattheis3mMaianrtcahiinveesdb.Ayltlhest3uMdy samples weregeneratedandanalyzedatthe 3MEnvironmentalLaboratory. Nochainofcustodyforms weregeneorraretquieredd. tRheese3rMveEsnavmiprloensmoenftraelfLearbeoncreatmaotreyrfioarlsafpreormiotdheno3tMlEenssvtihraonnm1e0nyteaalrLsfaoblolroawtionrgytwhielelfbfeecsttiovreeddaatte osfamtphleefsionaflttheestrreuflee,reonrcuenmtaitletrhieaqlusaflriotmy othfetchoenptrreapcatrlaatbioornantoorlyowniglelrabfefroertudrsneevadtluoatthieonI. MR.eserve EnviLabroraotorynfo mreteentionnantdarcahivilng.
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Results and Discussion DataQualityObjectives "qTuhaelfiotlylobojweicntgidvaetswaeqruealmiettyo,bejxeccetipvteassadozcfurmoemnttheedmientrhaowddsautsae.dinthepresentstudy. Thedata + aCcotuertfvhfeeiscwlioeewrnaetn0od.f9iD8ge5thoeerrngmrdiesnaoattfeitro.hneT(hcrue*rc)v.ueT.rhQvueeascdworeeafrtfeiieccxiceaunmtrsiveonfefddtwectaleosrsameiplnypfaltoiireoadnctco(cu*)arlfaiocbryraotthfieoqcnuaalnitbirtaattiioonn
tstoatnhdeadradtsa.andsample datatoimprovequantitationovetheconcentrationrangeappropriste + MperetpharoadtioBnl,adniklsut.iMoen,thnoddbalnaanlkysss(psrpopcleisasb)lpersoavmipdleedmaatmreiaxstuarkenotfharboourgshttohreyecnotnitraemisnaamtpiolne.
d`Aecfcienpetdablreevianlausetshfeocrotnhceebnltarnaktsiwoenoreflheessltohwaens5ts0t%anodfatrhde. limitofquantitation (LO), + MgartorupisxuSspedikientRheecsovteurdiyewsa.sApproesptaprreedpbayraatdodriymnagatlriiqxusotpskoefsatemsptlaenfaolryecsaoclhuotifotnhaecscaomrpdlien:g 1a0c3ceMptMaeblteh(odE1T300S%0-).5Ia.n1dn156s90.wThtheersaepsipkniekreecrceocvoeevreiresisefsoorut>s8i0de%oofftthheecsoanimrpollersawnegreew.ere
bscrvedsreindiicnApapetndeixdE. Sample `Twhernaitlapstl80i%ocfTtahheemRtewleeartei.lveeSstsatnhdaanordrDeeqvuiaatitoon3s0o%fwQi-ptlisctastewesraempulseesdwetoreexacclcuedpetable
outilndiatearsess. + aCnaolnyttienwualsggCraelaltbratthlaonn30Ve%riffircoamtithon.tIrfetvhaelpuercreelnattidvieffteortehnce ifotratlhsetaamndoaurndctoufrqvu,aontnilfyied
trheomsaeisnaimnpglseasmapnlaelsywzeerdebaenfaolryetzheedwliastthacacneeptwacbulrevcea.librationcheckstandardwere sed.The. Limt calibeatoifonQucaunrtviet.ation(LOQ).TheLOQwasequal tothe lowestacceptablestandardinthe + C1a0l1i0br0a0tnigonPSFtOaSn/dmaLrdmse.tEblaenvolenwsetraonudasrds rfaorngtihngcialnicborantcieonntcruartvieosn.froCamlsipbprraotxiiocmnuartevleysw2e.5re
runbeforeandafeover analyticalsequence. + SolventBlau.Solvent(Methanolblanksprovide ameasureof instrumental
qcuoannttaimtiantaitoino,nd.efAicnceedptbearbelienvaasltuheeslfoowretshtebcallainbkrsawtieornesltaensdatrhda.n50%ofthelimit of SydsetmoenmstrSautletdabbiyltayc.ceWptiatbhloeutipnestrrfuomremntianlgachmeectkhso(dc.v5a.liadabtibon,rsyestviemziscuhiateactbkilteiutnydev,aos full
auto-tuneroutines).
Saad Caine `sMofetawnasraen.dCsatlacnudlaartdiodnsewitvh tihewareartwedciaaltcoauwlneartseedmausdiengfuosnincgtitohensepqruoavtiidoendsidnesMcicrriobseiodnftheExOceElCD Me10t6(seh cAppo endid xB).
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DaaSom sndDeion
Avpendics Dent maeindivi ere msso
stlrtn. Renpsrsheantiavaioo mtoup mess
egpntto dni
`abe, SaleAmat ethod oermaatn ResultsoftheTier Istudyarepresentedintable 7through11:
I IB Te eI TS NT-- -- [[sotvoerrses||mwoorreenmmonmoann|| wwsn| [wmwm ]]
[osmeroo|mormvonan| an| w ] --
ae To wm [T wa] Cree eTpT S om oa emSei|oralw.eeTom Frm `tubeshad the least amountofextractable PFOS, and were theonlytubeswithacceptable matrix
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000275
--_--mm
Table.Equiv TimefrAdsorptionof FOS
C oT T me
| EE E oe T o= w
El aTo= n
o ----T -- en --
| EE
wm
aTom|
= ------e-- w--
Ta 1 w|
aT am]
itm
: | `Adsorption Equilibrium Plot
i
2 1000 Ter
i
ERR be ail]
feoofo late oy Se| o LEi ER R ERE
= Ecuitbrum Time,hours
irae esa
|
rn
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Flac f 7 me | | 1000
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5 18 Sao
Adsorption Equilibrium Plot
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[x5ao wo
7Ratio Sediment)
ai
2m] |-m 1:5 Rato(sediment|)
NT om TI |e 125ratosodmeny|
oo Mi BEAT SA 0 0 40 eo Equilibrium Time, hours:
"`TThheetcelsatysaupbpsetaarnecdetaoppteaakreemdotroerteiamcehteqouriclaicbhreiquumialfitberri2u4m,htohuerrseifnoraeltlhof4t8hheosouirl:siomluetpiooinnrtawtiaoss. w`eusredeagsitvheenaeqmupilleibtriimuemttoimeeqfuiolribtrhaeter.emainderof thestudy. Thisensuredthatallfiveofthesoils.
Table 10:SuitableDes Solvent,Methanol
Foirpioras
ph
RETR
| Eee a
[ow
mew]
[ww ww |
`Despitcusingmet[ hanol,o an excelw lentsolventforPROS,ta ho averagepeT rcentrece overyofw PFOS
rafrnom g7210 eto 9d6%. It isunlikely that a differentsolventwouldyieldbeterrecovery.
Pardesvoirobuesdroestulhtsisnitlh,iasnsdtiusdynohalviekeilnyditcoabteedctohmaptltheetlteysetxtsruabcstteadncferiosmreia.dilyandrapidly
`7Th5hie%sorpnatctilimoaadylem1son5so 5t%raitiendl soadr:viaemtres ianogwteo .aadssldoertu petrit moinnipeedro tcoenbnteage1:s5o(f PrFOetSorf Taanbegliern9gfforroampspplipcraobxliemdaaetal)y.
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Tube1.SitofPFSdaintheSn Prod
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es Tw
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AeeetoornntiTngeeOtECyDa oif deltr 1h0g,antveassleeiT etonoORp EopAeiw TEataS9e%o1h -- E irphon " Be o Br lpersotte Thereleft TieTsay repre fnTable 12:
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[ovemrems T on T| [[CComosmemmmeerreaT [ w5 w 0w 5| [Commeroe| mwTw]
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200278
wp oR HY i `AdsorptionPercentage as aFunctionofTime.
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gw a on DaaREL Hoe
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i
J
10
20
30
40
50
:
`Time,hours
:
Al ofthe solsdimentludgematicsadsorbedth test substancetovaryingdegrecs.The
`sludgesamples,in the adsorptionportionofthekineticsstudy,demonstratedthemostadsorption
(w9i6th%in)tah nfdrPeFtOeSwwhaosunrsotodfextepcotseudrisnatnhdestahmpelesss.uTbhsteadnacteaGionndciceantreasitohnatdaodcssorBpotvioanroyccurred signi aftefr ti he1c6ha ourntit meploiy nt. "Th resultsoftheTi I dyarepresentedin bls13trough15: "Table13,DesorptionKinetics ofPROS,1:5Sal:Soltion ato, 8 hourTim Pot
me mes newm ] me seme n T ew ]|
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es eee as
os i . oimin
DesorptionPercentage 2 a FunctionofTina
|
mel S Te R To0 on |T pTpT o aTR ARY,bil
i
# oooa p{eIIlNSEL S i Se ERRE) caiyyLoam
woo [3] IEE ly HT | SayLoam
sofoiinak TCn ae ii E HTTs eResadiment
wo {BAA el |
6 oTm ontoom ew
`cSTolhimeygtpelsstsaaudbr.sctTrahandceberrwqedassuSpioso,erlaytdteesSoerbpee8dyhfroaothmntnhoeetstopoiolfe/osebtodeiamnennte/ssstl,uncdtgeD em5at5rc%iocnae eesntdrtuar8taiinp oHgGntohde.r4Tto 8h-hoviuersy
Table 14.Adsorption others
F[oonme 0 ve 1 Tn wi [omwa | | w || [CoomsmeeT am | awne | [T owwe | | a a || Cosel ao 11 | om |
Note:Theunitsfortheisothermassumethatthetemu=1. Moresccaraely,theunits re (45 (1) Kg)
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Table15 Desorption satherms
I
f
Fae
eLe
mn | wr | oem | Las
[CoowiomTi| oa | ows | wm |
[west | 16 1 ws | 0| om |
(ome| 50 | ow | om | wm |
Note:Theunitsfor theisothermassume thattheterma=1..Mareaccurately,theunitsare (ug (L)*Kg")
Freundlichisothermsrelate theamountof testsubstanceadsorbedonthesoiltotheamount
pirnedsiceantteitnhtahtteahqeudeaotuaosbstoaliunteiodnfoartteqhueitleisbtrsiuubms.tTanhceevoavleuretswcoaolrcudleartseodffomratghneirteugdreeasrsieosnlciognhsttlyant
non-linear.
References
1. Adsorption-DesorptionUsing a BatchEquilMietbhord(iOuECmD 106), January 2000.
Report Amendments
Theorganiccarbon normalizedadsorptioncoefficient (Kovaluescontainedintables 2 and12, wiseorthceoremveatlueedsfcololownintg cailniatianeblseetsi3do,n o1f4alned1s5iaosnwseldleassrearwtseidpOrBCeaioddnsepanhgee1s026c0. 5t-Ta2s b3l3e pa13gheawda2smvaolduiefsisedwtio itndciacnhatdeewtahdiss ceoprorrecttehda. bTohcecaomnecnludseido.nTs heesigcwnaat tsurri eempoovgen dw.aTshroestiitglneed
folltho eamweni dmenntg s.
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Signatures "Tthheaasbmeenedneidsfsiuneadlbdyr:aftoftisreportis atruereprescatationof th dat developedinthisstudy.
"e7Eligfon,Sut Direc
5, Date
WillD iam K. Reat gan,TA esti-- ng Fa-- cilityManagement
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SM Environment! Laboratory
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