Document qmrV7M5mY24KoYzL5qq5Vo5LR
ARRAG -- 1366
LABORATORY-SCALE THERMAL DEGRADATION OF PERFLUORO-
'OCTANYL SULFONATE AND RELATED SUBSTANCES
TEST SUBSTANCE
Identity: Perfluorooctanesulfonate; may also be referred to as PFOS or C1a1F.2127,S3O,53K4,"4..5(,15-,O6c,t6a,n7e,s7u,l8f,o8n,i8c-ahceipdt,adecafluoro-, potassium
salt, CAS # 2795-39-3). Sample container was a clear glass
v9i8a-l0w2i1t1h-b3l9a1c6k-1p,laLstoitc2s1c7r"e.wTohnecpaupr.ityLaobfetlhirsesaudb"sCta8nFc1e7SisO3K", 86.9%. Storage conditions were not described.
Remarks: Thermal degradation of FC-807A and FC-1395 (Cs
pPeFrfOlSuorinootchteylensvuilrfoonnmaemnitd.esF)Cw-a8s07aAlsios eavamlixutautreed oafsmaonpoot-enatinadl dsio-urce of p(hHoOsCpHha2tCeHe2sNte(rRs)oSf Ofl2uCorBoFch1e7)m.iFcCal-8a0l7coAhohlasd previously been used in uprroedtuhcatnieonpooflyomiel-rretsoiwsthaincthpatpheerfsluaonrdocphaemcikcaaglinaglcmoahtoelriiaslb.ouFnCd-1t3h9r5ouigsha
urethane linkages. FC-1395 had previously been used as a carpet
tTrheeatsmaemnptlmeatceornitaalinperirofrotroFtCh-e8p0r7oAduwcatisonmaphdaeseo-foculteairn gDleacssemwbitehra20m0e0t.al 8sc0r7eAw/8c5a8p.1/TBhCeASL/aTbiemlef:or1t1h:i1s0s/uLbosttNaon.ce30r1e7a7d/D"MrautmerTi4al/SFtCe-p/Date: 12-222K/Sampled by C. Senior." The sample container for FC-1395 was an
amber glass vial with black plastic screw on cap. The label for this
csounbdsittainocnse wreearde "nNotamdee:scFrCi-b1e3d9f5o/rLoFtC#-:809700A8a6n/DdatFeC:-11319/57./00.P"uriSttyowraagsealso
not noted for these test substances.
METHOD
EMnevtihroodn:menMteatlhoSdcideenvceelsoapnedd
by Takahiro Engineering
Yamada and Philip H. Taylor, Group, University of Daylon
Research Institute, based on the use of batch-charged continuous flow
rmeaatcetroiraslsd(eRvuebloepyeadnadt CUaDmReIst,o 1s9t8u5d,y RthuebtehyeramnadlGsrtaanbitl,it1y9o8f8o).rganic
Method comments: Laboratory-scale study simulating a full-scale hazardous waste incinerator. The System for Thermal Diagnostic Studies
s(eSvTeDrSal) mwaajsorusceodmfpoorntehnetsi:ncaintehreartmioanl srteuadcyt.ioTnhceomipnasrttrmuemenntt;caontsriasntsfseorf
line; an analytical gas chromatograph (GC), a mass selective detector and
a computer workstation.
002026
1
:
Year completed: Phase | testing began in 2001 and the final report was written and completed in 2003.
GLP: No
Test Overview:
Testing was completed in 3 phases. Phase|tested the initial test protocol and project objectives, Phase Il consisted of the method development work, and Phase Ill revised and applied the test protocol. The overall goal of this study was to determineif incineration is a potential source of perfluoroalkyl sulfonates, .g., perfluoro-octanyl sulfonates (PFOS), which has been found widespread in wildife tissue samples
Phase I:
Objectives of Phase | were to determine if Cs perfluorosulfonamides form
pceormfbluusortoiopnrepcruordsuocrtosfipnetrhfelufoorromocoftapneerfsullufoornoaotcet,anteo dseutlefornmaitnee(tPhFeOeSx)toenrta
of conversion of PFOS under conditions representative of hazardous or
pmruondiuccitpsa,l awnadstteo dinectienrermaitnieonif,tthoeidseunltfiufryptrheesemnatjoirn tfhlueoPriFnOatSedicsombustion
quantitatively converted sulfuryl fluoride (SOzF2)
to at
sulfur dioxide and/or thionyl high temperature, fuel-lean
fluoride (SOF2) combustion
and
conditions.
`The development of the test protocol was based on the use of batch-
scthaabirlgietydocfoonrtgiannuiocusmaftleorwiarlesa.ctAonrasldyesivselwoapsedpeartfUoDrRme!dtoussitnugdyint-lhienethgearsmal
chromatography/mass spectrometry (GC/MS). The analytical focus was
identification of stable quantification of sulfur
fluorinated organic intermediates and oxides in an attempt to recover 100%
the of the
initial
sulfur in the sample. Sulfur selective detector (MSD).
quantification
was
performed
using
a
mass
tGeamsp-eprhaatsuerethneeremdaeldsttaobiglaistiyfaynsalaymspilse,wa2s) fpetrhfeoprhmaedsetochdaentegremiisnteh1e)rtehseult
of evaporation or deposited by the
decomposition, and 3)if a sample. Then testing was
non-volatile residue is performed to assess whether
the gasification products reactor conditions.
have
the
ability
to
be
transported
under
the
flow
The STDS chosen as
twhaesfuseellefocrtesdamtoplceasythoauttwtehries
incineration study. hydrogen deficient.
Methane Two
was
ptreemlpiemriantauryrecsom(6b0u0stainodn 9t0es0tsC.) were selected for the study base0d o0n2027
:|
Phase II:
The purpose of PhaseIl of the incineration study was to verify gasification
of PFOS and transport of PFOS through the
system. Recovery efficiencies and detection
UDRI
limits
thermal instrumentation
for sulfur compounds
(SOz, SOF,
precursoorf
and SOF) and perfluorooctane
PFOS) were determined through
sulfonyl fluoride
analysis using a
(POSF,
GC/MS
a
system. Measurements were performed in duplicates.
Hexafluoropropene (HFP) was selected as the surrogate volatile
fluorocarbon. Recovery efficiencies and detection limitsofvolatile Cy-Cy
fluorocarbons were also established. A quantitative method osf ampling
the reactor effluent was established. ORBO PUF cartridges were used for
sampling PFOS and precursors from the reactor effluent.
|] (: peakary 3: concentration Linear Fit Equations and Detection Limits Linear Fit
Lik Detection
[ SO, |V-58813E3"X[-003078 1|5471 85E5| [ SOF,|V=8333E3"X-[0799.9401]2637 0364|
[[PSOOSF E | |vV==11.003314E42'X+31.E8275366X--[[01..B909d70|8o] d2ad011es]|
[WFP | V=-14075E4'X[0-992978|25339E6|
Transport Efficienc
[SystemTransport | Directinjecton [ PeakAra | PeakAra
|Efficiency | | (%) |
[Sample T T 2dTAVGH| 1 | 2[AVE[ayemin]
[S0, |"9130332| 8980717 | 9055525 |11952302 | 1762367] Liss7285] [SOF; | 25244352| 25203780| 35224066 |24862639 | 24773683|24818161|
76.4] 1016]
[SOs:| 86850304| 85572809| 86211557 |84435720 | 79738316| 82087018] 105.0]
[BFP 148670354 | 145606343 | 147142849| 148372504 | 142271896 | 145322200] 1013]
Phase Ill:
Phase Ill consistedof 8 different tests (SO, Transfer Efficiency Tests, Laboratory Spike Analysis for PFOS, Heated Blank Combustion Test,
`Combustion Tests for PFOS and two Cs perfluorosulfonamides, Heated
Blank Combustion Test (repeat), Transfer EfficiencyTest for PFOS, Sulfur Recovery Analysis as SO, and Extracted lon Analysis). In-line and off-
line GC/MS analysis was conducted So the combustion gases. The off-
line GC/MS analysiis was used in repplliiccataete runs ii n ordelerto capy ture 002028
3
more volatile compounds and because there were resolution issues with t(hpeoliynu-rlientehsanaempfloianmg)acpopllreocatciohnfoofr tthhee sruelafcutrorreecfoflvueernytraanted. chPeUmFical
`extraction of the reactor and associated transfer lines was completed.
LPCU/FMSc.artridges and extracts were delivered to 3Mforanalysis of PFOS by SO; Transfer Efficiency Tests were performed to confirm rests from spyhsatseemIlc.onTthaemiHneaattioend.BlFaonukr CaonamlbyussetsiownerTeesctosndwuecrteeudsfeodr tthoeexHaeamtiende sBlaamnpkleCoamnabluysstisi,onoftfe-sitne(nG-Cn/eMGSCa/naMlSysainsaulyssiinsg,TPeUdlFarcoblalge,ctaenddoff-gas
reactorftransfer line system extraction using methanol).
RESULTS
SSOO;;
tTrraannsspforetr
Efficiency Test: efficiency was 83.7%
in
Phase
Il,
slightly
higher
than
the
tPrhaansspeorIltreefsfitcsi,en7cy6.f4or%,SOwhFi;cwhagsiv1es00a%veirnaPgehavsaelsueIlofan8d0.I1l.%. The
Laboratory Spike Analyses for PFOS:
Phase Ill laboratory spikes included fourteen 1 pg and twelve 10 ug spikes
osifnPglFeO1Su(gasPtFhOeSPsFpOiSkea(naisont)heinPtoFtOhSeKPUsFa'lst)(osfetehAeptpuebnidngixus5.e)d, aansdtahe rspeiakcitnogr s(ocloumtbiuonstwiaosn cinhjaemcbteedr)juastndbetlroawnstfheer sliunref.aFceo,r tahnedPaUllFowsepdikteos,drtyhefor 8302%moinfutthese,PaFnOdSthweansexrtercaocvteerdedasfrinomthtehetes1tnpgroPcUedFursep.ikAens waivtehraagreeloaftive standard deviation of 10%. An averageof 92%ofthe PFOS was
croemcobvuesrteidonfrcohmatmhbeer10spuigkePUinFvoslpviekdesinwjietcthiangnaR1SDugofsa7m%p.leTohfePsFiOngSleinto
tbhleowrienagctwoirthashiagh1 puugri/tly snoilturtoigoenn.inAfHtPerLdCrygirnga,dethmeettrhaannsofle,r alinnde wdraysingby wbaayssspheuimnmbgplsie.ndg~otTofhte5h.et5ortmealaLcPtooFfrOmaSerntedhcatonhvoeel1r.ty1hfrmrooLumgvhotthlhiuesmraeesaascsestmeobmrlbfyliiyrnawtnwaslosifnseeeerxqtusrepanictktieeadl was 188%. This single spike result suggests that an errr likely occurred
during preparation, extraction or analysis. Nevertheless, this spike result
confirms that PFOS can be extracted from reactor/transfer lines.
ull PFOS Laboratory Reactor/Transfer Line Spike Analysis: [PFOSTTM 1 232 | 716 |
002029
4
=e [Brace Extracts
T7171]
HTehaetfeldowBplraofnikleCaonmdbucasrtriieornflAonwalvyosliusm:e used for the heated blank analyses at 600C and 900C are given in the following two tables.
|rime[ owe Raa | otame| Vou: Flow RateRPeraocfitloerfo|r HeaPtyerdopBrloabnek A|nalyTsoitsalatF6l0o0wC| Total |Sampled
(milmin) (milmin) (mimi (mi) (mi)
[0-7201 705 ~T" 080 | 1130 | 2260] 20.0]
[120-130| 705 "10805463"[11301463 | 2.16] 1.9]
Hal pe Las 1 [40-|791063(0Hel| 453(Hef|
GE 1356
[aml | 452]
ow 4.19]
I "Linear increase (a1 pproximate). *~ SwTitocthaedltVoohuelmleum(mfo)r|swee3p1..8 0Sa]mp2le0d.13]
volume for PUF andTedlarbag collection.
BAERdeal do Flow Rate Profile for Heated Blank Analysis at 900C F(mliomwiRna)te | F(lmiolwmiRna)te (mRialmtien) Volmiu)me| Volmui)me*
[0-150| 760 [070[830 | 2075] 18.05] [150-160|" 760 [0705463 |830>1223| 171] 154] [160-170| 760 1 463 [| 1223. | 204] 17] [70-750 [7654 He"| 453(Hef| 11.07 | 369] 3.36]
CL *LiI near increase (approT ximato e). l > SwiV tcheo d tou hellum m foreswe2e( 8p..*1m 9S]am) p2le5d.| 02] volume for PUF and Tedlar bag collection.
T0h0erCe)wfaosr bnoothmeian-sluirneabalned cooffn-tlainmeinGaCt/ioMnSfoarnaeliytshiesr.teAmpsemraaltluarmeo(u6n0t0 oafnd PheFaOteSd(0b.l0a8nukgc)owmabsustdeitoenctteesdt.inTthhee aremaocutonrtfotfraPnsFfOerSlienxeterxatcrtaecdtiinn tthhee first second heated blank combustion test was below detection limits.
Combustion Tests for PFOS and two Cy perfluorosulfonamides:
tPhEeOfSourinsTerqaunesnfteira-lLcionmebEuxsttriacotns:teTsatbsloen5.P4F.O1.S1,ofatthoetalreopofrt1.s83hmowgsotfhPatFOiSn . were gasified in the pyroprobe.
045+0.38+0.5+0.5 = 1.83 mg
002030
5
cTaobmlbeusst5i.o4.n2.t1esatsndon5.F4C.3-.810o7fAtahendreFpCor-t13s9h5o,wttohtaatl,soifn t2h.e16fomurgsaeqnuden2t.i0a2l
mg, respectively, of product dry mass were gasified example, for FC-807A:
in
the
pyroprobe.
For
0.50+0.59+0.45+0.53 = 2.16 mg
The toa
gasified samples then combustion chamber.
passed through heated (260C) In the combustion chamber the
transfer lines volatlized
gases 1395)
omriexxecdewsistahinre(arP-FsOtSoi)chainodmewterrice
amountsofair (FC-807A and FCexposed to 600or 900Cfor about
2
streacnosnfdesr.linFersotmo ahemrbei,enthtetecmopmebruasttuiroen pporloyduurcettshpaanessfeodamthcroonutgahin2i6n0gC
cartridges or Tedlar bags.
oFfoltlhoewsinegcotnhde chaolmfboufsttiheoncotmesbtusstatio9n00chCa,mtbweorsaenqduetnhteiatlramnestfheranloinlesexdtorwacnt-s
streamofthe combustion following table shows the
chamber were analyzed for concentration and amounts
PFOS. The of PFOS (as
the
K
sal), detected in the chamberfiransfer line. This is the amount that
tawcocuamtu6l0at0edC ianntdhetwcohaamtb9e0r0/tCra,nfsofreeralcinhepfrroodmuctth.eTfhoeurtsoteaqlueanmtoiualntteosfts,
PFOS PFOS
dgaestiefciteeddininetahcehexoftrtahcetfsowuratsesetqsuiovra,laenststhooawbnouitn
0.04% of the the following
equation, tests.
0.009%of
the
1.83
mg
of
PFOS
gasified
in
the
four
sequential
100 X (0.00011+0.00005)1.83 = 0.009%
pFeorlfllouwoirnogotchteylfsouulrfsoenqaumeindteiparlocdoucmtbsu,stPiFoOnStewstassobneeloawchdoeftetchteiotnwloimits in
t`haemocuhnatmobfePrfFirOaSnstfheartlcionueledxthraavctes.beBeansperdesoenntthien deeatcehcotfiotnhleimtitwso, the
gseiqvueennitniatlheexTtarbalcet w1aosnlpeassgeth7aonf0A.p0p3e5nudgi.xB4a,stehde o2.n1t6hemgstaoincdhi2o.m0e2trmyg of
FC-807A formed a
moraxFCi-m1u3m95ofs1o.li8d7smggasiofrie1d.5i5n
the four sequential tests could mgof PFOS (as the K salt),
have
respectively. For example, for FC-807A:
2.16 mg X 0.519/0.600 = 1.87 mg
`(wahsetrhee0K.5s1al9t)a.ndTh0e.6f0o0llaorweintgheshforawcstihonoswofthfilsuocrailnceuliantiFoCn-w8a0s7Adoanned fPorFOS PFOS using the data in Table 1, page 7 of Appendix 4:
002031
6
|
:
Fraction F in PFOSK' = (1917)/(12'8+19"17+16*3+32*1+30.11) =0.600
cWahrebroen,1o9,xy1g2e,n,16a,n3d2paontdas3s9i.u1m,arreestpheectmiovleelyc.ular weightsoffluorine,
Tlihnuess,wtahsislaensaslytshiasn s0h.o0w0s4%thaenadmloeusnstthoafnP0F.O0S05i%n otfhethcehammabexrifmtruamnsafmeorunt
of PFOS that respectively.
could have been For example, for
fFoCr-m8e0d7Af:rom
FC-807A
or
FC-1385
100 X (< 0.000035+ < 0.000035)/1.87 = < 0.004%.
Transfer-Line Extraction Results:
[E2 xtraction TPFOSK (pgal] |PFOSK (ug) ||
se
Ton
[2
"Test
Joos
| |
[Eases
7
|
bo le
Teo
Tess
|
Two
Jeo
|
[Fcsora-- 7 ---- ------
OO
T<o0
Too
Two
Joos
|
PEOS table,
in PUF Extracts: The calculation below, shows that the amount of PFOS making
using data in it through the
the following combustion
system and the 0.45 mg
extracted of PFOS
from the PUFs gasified at 600
was C.
equivalent
to
less
than
0.5%
of
100 X (0.00062 + 0.0016)10.45 = 0.49%
g`aTshiefdiaedtaatin9t0h0isCtamblaekaelssoitsthhoouwghthtatthaebsoyustt0e.m07an%d owfatsheex0t.r5acmtgedoffrPoFmOSth.e PUFs.
100 X (0.00011 +0.00022)/0.5 = 0.066% SPuUbFstEaxntcreactio|n TReesmuplts:
[PFOS [FCA395
1600 Teo Teo Tso
"142
[251.640 [062.16 |
THM2 -- Ta31.901_Joi1.022 |
112 -- T<500,<600 [<012,<012 |
112[<500.|< <016 2.<0 0.120|
002032
7
[Fe8oA Teo Tso
Tiz 42
[00.600 [<02.002 | [<500,<600[0.12 <0.12 ]
`cTohmebuPsUtFioEnxtorfacpteirofnluRoersoualltksyltsaubllfeon(aambiodvee)coamlspoousnhdosw,s ntohatP,FfoOlSlowwiansg
dqueatnetcitfeidcaitnioPnU(FLLeOxQt)ra.ctBsasatedcoonncetnhteradteitoencstiaobnolvimeittsh,ethleowaemroluimnitt oefxtracted
farnodm0e.a5c5hmogf tofheFtCw-o80se7qAueanntdiaFlCP-U13F9s5wgaassilfeiesdsattha9n000.C1,2 cugo.mObfustthieon0.45
`could sal),
have formed respectively.
a maximum For example
of 0.39 mgor for FC-807A:
0.42
mg
of
PFOS
(as
the
K
0.45'0.519/0.6 = 0.39 mg
wKhsearlter0e.s5pe1c9tiavnedly0..6T0h0eafroelltohweinfgraecqtiuoantsioofnfsltuhoruisnsehionwFtCh-a8t0t7hAe aanmdouPnFtOoSf 0P.F0O7S% ionftthheecPoFmObiSntehdatPcUoFuledxthraavcetsboefetnhefo9r0m0edCftreosmtsbwotahsFlCe-s8s0t7hAa:n
100 X (<0.12 + <0.12)380 = <0.062%
and FC-1395:
100 X (<0.12 + <0.12)/420 = 0.057%.
TTrharneseptoyrptesEfoffitceisetnscwyeTreestcosnfdourcPteFdOSto:examine transport efficiency. Tgehneesreatteesdtsduwreirneg tdhoencetomobvuasltidiaotneofthfaltuoPrFoOchSemciocualldsbien dtehteetcetsetdsyifsittewme.re Tpyhreopfirrostbteesatnedxtarmainnseposrttheed ttrharnosufgehr etfhfeicrieeancctyoroftosatmheplPeUsFgacsairftireiddgienst.heThe sceocnodnednsteedstoinnvtehsetiwgaaltlessotfhtehpeopsysriobiplriotbyet/hraetatchteorvotlraatnisifzeerdlPinFe.OSThe third tbeesttreaxnasmfeirnreesd thootwhemuPUcFh'sPFanOdShvoolwatmiulczehd winoutlhde ccoomnbduesntsieoninrtehaector could reactorftransfer line tubing.
fIonltlhoewi1n*g Ttarbalnesfsehroewfsfitchiaetncnyotedsette0c.t4a8blmegaofmPoFOuoSfntwhtaes vvoollaattiilliizzeedd.PTFhOSe.
wsaamsprleecwovaesreeditfherromthtehremaPlUlyFdciasrstorciidagte.edTihnitsherepsuylrtopinrdoibceatcehstahmabtetrheor the
gasified transfer
sample was line tubing.
completely
condensed
in
the
pyroprobelreactor
i
PUF Extraction Results for 1* Transfer Efficiency Test
002033
3
PFOS
(pg/uh)
[7[1[<a50s 0 [i 0.n 2|
Tmheaesnuerxatbtlweoatmaobulnestsshofowthteha0t.,47inmtgheo2f"PtFrOanSsftehratefwfaicsievnoclyattiesitz,ed survive tpryarnoslfyesrislicnoesn.ditHioownesovfetr,henopydreotpercotbaeb,leaanmdocuonlltecotfePdFinOtShesuhrevaitveeds transit tothe PUF sampling cartridge.
Methanol Extraction Results for 2 Transfer Efficiency Test
[PEOSTT | sor| 21 | T7727T<i00|<024|
PUF Extraction Results for 2" Transfer Efficiency Test
PFOS | [>
17 1<10.0 |<05| a]
thThehiasettifenosgtl,liotPwtiFonO5g7St5wwoCa.tsTahbvleoelsafitsrishitzotewadbrlieenstsuhlhetoscwoosfmttbhhuaestt3mieoatnrscaunhrsaafmberlbeeefrafmi(croieueannccttyosrt)eosfbt.y In
dvaoltaatiflrzoemd tPheFOfiSrstpoafstsheedsefrtoambltehsesrheoacwtotrhatto 1t2he.8P%UFosf.thCea0lc.u4l6atmigonosf using
PFOS PFOS
volatiized volatilzed
iinn
aHier.
reached
the
PUF,
as
did
5.2%ofthe
0.48
mg
of
100 X (0.058 + 0.0011)0.46 = 12.8%
100 X 0.025/0.48 = 5.2%
Ttrhaenssfeercoefnfdictiaebnlceybteeslto.wThsehsoewswemreethfarnoomleexxttrraaccttsdoaf:ta1o)btthaein2e6d0inCthe 3 arseascotcoiraftterdantsrfaenrslfienreltiunbeitnugbainngdj2us)ttuhepsrtoroemamteomfptehreatPuUrFe vcaarltvreidagneds. oCfalPcFulOaStio(n5s.6u%sianigr,d3a9t.a3f%roHme)thiasccsuemcuolnadtteadblien hthoe wreatchtaotrlfatrrgaenrsfaemroluinnetss upstream of the PUF cartridges. The majority of the PFOS accumulated in
002034
9
the portionofthe transfer line heated to 260C, suggesting that this
`compound could condense, or was in a particulate form, at this temperature.
100 X (0.024 + 0.00045 + 0.0024 + 0.000079)/0.48 = 5.6% 100 X (0.171 + 0.0019 + 0.0077 + 0.00035)/0.46 = 39.3%
meg Tere ogy| ay| 3" Transfer Efficiency Test PUF Extraction Results
[7 T23g3l0)[|
(ng)
s8
|
Ar | [2 Te 7 ae 4 1 1r 215 ||
[ 2" <i00[<0.1|2
3 Transfer Efficiency Test ReactorValve Transfer Line Extraction Results
Air
Notes:
actor' | 1% 171|90 248|
[Feo Valve"
Ti"
ee 2} 16|0246|
Reactor' [ [12%71722183[|05013 77190||
VaveTM ||" 27 T7925101 8[|1797||
[2%T7110 032 5]
1. The location labeled "Reactor" included the secondhalf of the
combustion chamber (575C) and the heated (260C) transfer
2.
Tlliehnaeedillneogacdafitrnioognmftr"hoVemalvtvahele,v"eciotnmocbltuuhsedteiPdoUtnFh.echvTaahlmevbevearalnvtdeo
tthhee vtarlavnes.fer line and this transfer
line were at room temperature during the test.
Sulfur Recovery Rate: StBh0ae2s.oefdfNlooinneStOGheFC;/inMa- nSadnsdSyOosf;tfeF-lm;inwweeeGrrSee/mdMeutScehcatnesadhl.ayrspBeeser,castuuhlasfneurStwOhae;sSpOfeo,auknpsdeoambkassienurlsvyienadgs ruessiunlgtsitnoinqueanGtCi/taMtSiv,elitywaansaldyezceitdheedstuolfuusreroefcfo-vienreyGaCs/SMOS.analytical 002035
10
SO, Calibration Results Using the off-line PLOT Column
aInpptrhoeaSchO-;thteraansvfeerraegfefirceiceoncvyertyesrtactoenwdausct7e5d.6u%si.ngThtihse
off-line
is very
analysis
similator
the
recovery rates obtained from the in-line analysis, i.e. 83.7 and 76.4%,
suggesting that the lack in 100% recovery is due to sample losses in the
combustion system and not the sampling and analysis procedures.
RlPY id Standard SO; Transfer Efficien
[223lt0sotoa7 136E-06 | 1636-06 | 834 |
[2213 [estso87] 111E06 |163606| 678 | CTT T Aveage| 756 |
Extracted lon Analysis: `The following ions (51-CF2H, 69-CFs, 119-C;Fs, and 67-SOF) were `PaFmOoSn,g athloosweerexmtorlaectceudlafrrwoemitghhettpoetralfliuoonrocahlrkyolmsautlofognraatmes(dfersoimgnteasttesdoans PliFnXeSa)n,daonffd-ltihnee GCsC/pMerSflaunoarloyssuelfsoinnamoirddeesr.toTahinsalwyazse fdoorntehefoprrbeostehnctheeofinpinearbfilluitoyritnoadteedteacntdthseul6f7o-naStOeF-cioonntaiinnainngy ionfttehrmeesdeiaatneasl.ysIemsposrutgagnetlsyt,edthleow levels or an absence of perfluoroalkylsulfonyl compounds in the cnootmbliuksetlyiotno bperoaduscitgsn.ifiTcahnitssroeusurlcteostfrocnogmlyposuugngdessttshatthaarteinecnivnierroantimoenntisa.l cprhercoumrastorosgorfamPsFfOoSr 51o,r o6t9h,earnpder1fl1u9oriooanlsk,ywlhseulnfoenvaatleusa.teEdxtirnaccotnejdunicontion with hydrogen flame ionization detector (HFID) chromatograms, suggest that tr and tetrafluoromethane and hexafluoroethane were likely combustion products.
PDuFeOStotaesnt,aptpheareexnttralcotsesdoifosnenasniatliyvsiitysogfetnheeraitne-ldinferMomSPdFetOeSctcoormdbuursitngiotnhe.
did not indicate the presenceoffluorinated combustion products, unlike
tHhFeIrDesdualttas
ifnorcaolnljoutnhcetriocnowmiptohutnhdesHFteIsDteadn.d
An evaluation extracted ion
of the PFOS analysis data
for
lower molecular weight perfiuoroalkylsulfonate (PFXS) strongly
uuR036
1
:
fsluugogreosctheedmitchaalt cPoFmObuSstcioomnbupsrtoidoucntas.lsTohgeenPeFraXtSeddastoamsehovowleatdile (low MW)
fluorochemicals were present at the same retention time as HFID peaks.
APdFdiXtSioncaolmlbyu,stthieornetweenrtieonnetairmleysidoefnttihcealH.FITDhurse,stphoensseamfreofmlPuoFrOocSheamnidcal
combustion products likely formed from these two different compounds.
aTphperofxolilmoawtienlgyt1w%o toafbtlheastsahto6w00thaCt.thTehiHsFrIeDsulptesaukgagreesatsatn9ea0r0lyCcoismplete
destruction of fluorochemicals combustion products at 900C.
Integrated HFID Peak Area of PNFeXtSAmaondunPtFoOfS at 600C TaGasified Sample
[PFXS |1190193| 052 | [PFOs [35|4706 3814|
Integrated HFID Peak Area of PFOS at 900C
Net Amount of
G=asified Sample
[Fos |30041 | 050 |
INCLUSIONS
dTehgirsaldaabtoiroantocroyndsittuidoynsusleikdelay tsoysotcecumrddeusriignngemdutnoicsiipmaullaotrehtahzeatrhdeorumsalwaste incineration. When perfluorooctane sulfonamide containing products (FCw1e3r9e5 1an0d0F2C5-%80a7nAd) LwCe/reMSexapnaolsyesdistoshthoewseedcothnadtitnioonqsu,anStOi;fiarbelceovaemroiuesnts tohfePsFyOsStem(.<0T.0h7e%SoOf;thraetssttosicshuigogmeetsrtictahlaltytphoespsiebrlfei)ucwreorseulrfeolneaamsieddesfrwoemre isnucbisntearnattiiaolnloyfdpeesrtfriouyoerdoaonctdatnheesLulCf/oMnSamriedseulstwsosutlrodnngloyt rseulgegaessetPthFaOt S to etmhiesesnivoinrso,nsmehnotw.edFuarnthaebrsmeonrec,eomfas6s7-sSpOecFtriaolnse.xtrTahcetesdeiioonnsanaarleysis of the tirndaincsaftoirvem toof pPeFrfOlSucrionatlhkeylesnuvlfiornoynlmecnotm.poTuhnedsa,bswehniccehocfoutlhde p6o7te-nStOiaFlliyons
suggests that the carbon-sulfur bond was completely destroyed (and did
enontvirreofnomremn)tianltthreancsofmobrmuasttiioonnoftecsotsm.buTshtiisonrespurlotdsuuctgsgetsotfsotrhmatPFOS is
also unlikely.
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12
When PFOS was exposed to this combustion system, sulfur recoveries varied from 50 to 60% and LC/MS analysis showed that only a small
faruatchtoirons osfpetchuelPatFeOtShatthlatowwasuslfvuorlarteicloivzeedrimeasdweeritetlhirkoeluyghdutehetosystem. The cthoendseynsstaetmiotno wtihtehiPnUtFhse daeppcarreaatsuesd. aTshtehefrtaecmtipoenraotfuPrFeOoSf tphaescsoimnbgutshtriooungh chamber increased. At 600 C, about 0.5% of the gasified PFOS made it
completely through the system and was collected on the PUFs. When the
`PcFomObSusctoilolneccthedamobnetrhetePmUpFersatwuarse dweacsreianscerdeatsoedabtoou9t000.0C7,%t.he amount of
CdiyfiouroCr;oeftlhueonreoa(lPkFanOeSs o(nlliyke)lyanprdod1,u2c-tdsifalrueoeriotehtehrenCeHF(sF,C-C1F39,5oornlCyF))w,er1e,1the only highly fluorinated compounds observed in the system effluent. Fiuorobenzene was also detected (FC-1395 and FC-807A only). No
higher molecular weight fluorinated polycyclic aromatic hydrocarbons, and
no perfluorooctane sulfonyl precursors of PFOS were present in the
system effluent at detectable levels.
Tinhdeicraetpeosrtthsattaptreosptehraltytohpeerdaattianfgrfoumllt-hsicsalleabionrcainteorrayt-isocnalseysintceimnsercatainon study aIndceiqnueartaetiloynodifstphoesseeofflPuoFrOinSataedndcotmhepoCusnpdesrfilsunoortolsiuklefloyntaomibdeesa. significant source of PFOS into the environment. With the exception of stable Cs and eCm2itfltueodrdoucrairnbgontsh,efilnucoirnienraatteidonorogfanPiFcOiSntoerrmpeedrifaltueosroaorcetaunnleiskeullyfotonabmeides.
Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331,
St. Paul, Minnesota, 55133
DATA QUALITY
Reliability: Kiimisch ranking 2. Purity/Compositionof 1395 were not properly characterized in the study.
FC-807A
and
FC-
REFERENCES
SRteusdeyarccohndIunscttietudtea.t the request of 3M Company by University of Dayton OTHER
Last changed: 7/03/03
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