Document dMeeBGX1G7ozw05wkL8oMR66
OCTANOLMATER PARTITION COEFFICIENT
TEST SUBSTANCE
Identity:
Nre2f-e(rNr-emdettohyalspeNr-flMueoFrOooScEtAa,nesourlMfeonFaOmSidEoA).-et(h2y-lPracorpyelnaotie;c
amcaidy,
also 2-
be
[itheptadecafiuorooctysulfonylmethylaminolethyl ester, CAS #
25268-77-3)
cReommaprokusn:d asM"aTt-e5r8ia6l9"is(aBnatacmhb2e4r0,8)w.axSyamsopllide. puTrhietytiesstgilvaebnoraasto"ry96i%de.ntiTfhiees the remaining 5% of the product was not characterized.
METHOD
Method: ~~ OECD 117 & EEC-Directive 92/69 EEC, Annex V, Part A8 YGeLaPr(cYoImNp):letYeeds: 1994 Analytical: HPLC with Spectrophotometric detector
rReefmearernkcses:.
TTheessteinsguubssetdansciexsswuebrsteaunsceeds
twoitchalkinborawtne
log the
ePlouytivoanltuiemseaisn
units
of
/
109 Pou.
[ReBefnezryelanlcoeohsoulbstance |16gPox |
[Fl1uo4ra-ntdheinec(9h8%i) or| oben8z4en|e
[Obenzyi|(e405%)|
2,4-DDT (99%)
62
AmLstaoccektosnoilturtiiloenaonfdtshoentiecsattisnugbsfotra2ncmeinwuatsesp.reTphaeresdtobcyk
dsioslsuotlivoinngwa2s87dimlguteidn
50.0 10
times with mobile phase, resulting in the test solution (574 mgiL).
Mobile phase is a 75/25 (viv) solution of acetonitrile / Milipore-Q water
respectively.
RESULTS
Susan | Tos gPu |
TBoenlzuyelnaelcohol
2T7i
1,4-dichlorobenzene
34m
000095
Fluoranthene, Dibenzyl
ar 48"
2,4-DDT
62"
Peak T (major comp.)
56
PPeeaakk 32
54 53
Several small peaks
07/52"
+"+ lTongtePrpoolvataelduefsroamcctohredirneggtreostshieonOiEneC:Dyg=ui0de.li2ne8s8.~ 0.730 (=0 972, n=6)
CONCLUSIONS
This study estimates the log Pou for MeFOSEA.
Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133
DATA QUALITY
Reliability: Kiimisch ranking 2
-per OECD. HPLC methods enables partition coefficients to be estimated in the 10g Pow range between 0 and 6.
-Notox states impurities are of minor importance in HPLC method, however
OECD states, HPLC method is less sensitive to the presence of impurities in the
test substance impurities can
than make
the the
Shake Flask method. interpretationofthe
Nevertheless, in results difficult due
stoomuencecratsaeisnty
in
peak lower
assignments. Mixtures limits of log Poy Should
which result in an unresolved be stated. Duplicate analysis
band, upper and should be reported
in
order to show confidence range of +/- 0.1 log units)
in ~
the data
measurement (log Poy values should provided mean value therefore can't
fall within show
a
confidence. pH of eluant is critical of ionizable compounds.
"The study did not include any fluorochemicals among the reference substances.
Without fluorochemical reference compounds, itis not known whether the same
relationship between the capacity factor k' and Kow exists for compounds with
perfluoroalkyl portions as exits for nonfluorinated reference materials such as
tihnjoesceteudsienddienpetnhidsensttuldyy.toTihnesurreefaeprpernocperciaotmeproeutnendtsiosnhtoiumled ahsasviegnbeedentoaelascoh
trheefemreenacne rceotmepnotiuonnd.timReedfaetraenicsegisvuebnstfoarncthees rweefreereinncjeecstuebdsttwaincec,eshotwhuesver only
repeatability of the retention times is not clear. It was not demonstrated that the
test material was soluble in the acetonitrile stock solution or in the mobile phase.
No demonstration that the major components of the test substance are
detectable at UV A = 210 nm. UV adsorption spectra is needed of the purified
main components of the test substance. Assumptions are made that the major
:
oT
000096 ~~
peak from the HPLC of the test substance is the major component. No attempt was made to confirm this (e.g. Mass spec analysis to show the material detected has the appropriate mass). It is not known whether the major components even `comeoff the column. Some K' values reported are calculated incorrectly. REFERENCES Study conducted at the request of 3M Company by NOTOX Safety & Environmental Research B.V., The Netheriands, April 7, 1994. OTHER Last changed: 5/17/00
000097
_a
- 7-5669.4 ge erm
REPORT
DETERMINATION OF THE PARTITION COEFFICIENT (N-OCTANOL/WATER) OF
T-586944
BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC)
NOTOX Project 121286
3
NOTOX substance 38196
|
- Page 1 of 14 -
000098
RECEIVED
NV -9 1994
3m TOXICOLOGY
T5869
NOTOK Project 121286
STATEMENT OF GLP COWPLIANCE NOTOX B.V., *s-Hertogenbosch, The Netherlands
The study described in this report was conducted in compliance with the
most recent edition of:
The OECD Principles of Good Laboratory Practice
which are essentially in conformity with:
@:
RTheeguUlnaittieodnsStPaarttes5F.ood and Drug Administration. Title 21 Code of Federal
oTfheFeUdneirtaeld RSteagtuelsatiEonnvsiroPnamretnt1a6l0.Protection Agency (FIFRA). Title 40 Code
FTehdeerUanliteRdegSutlaatteisonsEnPvairrtonm7e9n2t.al Protection Agency (TSCA). Title 40 Code of
Study Director:
i
Ors. R. de Vries
a eA e
Date: Tmo TotRAN
- page - 000099
T-5869
NOTOX Project 121286
QUALITY ASSURANCE STATEMENT
NOTOX B.V., 's-Hertogenbosch, The Netherlands.
Study study
procedures were subject specific processes were
to periodic inspections and general non also inspected at periodic intervals.
Tmheitshodrsepoarntd wraessulatusdiatcecdurbaytetlhye NrOeTfOlXectQuatlhietyrawAssdautraa.nce Unit and the
DATES OFAUQADUITSINSPECTION/S
REPORTING DATES
25 March 1994
28 March 1994
21 April 1994
25 March 1994
28 March 1994
21 April 1994
Quality Assurance Manager
C.J. Mitchell B.Sc.
Date:0G- ot-aL
- Pages -
000100
T-5869 REPORT APPROVAL STUDY DIRECTOR:
}
MANAGEMENT:
<
NOTOX Project 121286
Ors. R. de Vries
od-- --2--
vate: eae 9. aan 2AMN. van Helvoirt
Section head Physico Chemistry
Nn
J _~--"brlona c. Eninga
everiieeiiiiiiiiie.. |TechnicalDirector vate: og lobliggw
- paged -
000101
7-5869
NOTOX Project 121286
PREFACE
sponsor
Study Monitor Testing Facility
Study Director
study plan
3CManaBdealsgtiruamat- C1h1emical EBC 8B-e2l0g7i0umZWLINORECHT Mr. RH. Cox NHOaTnObXakeB.nVw.etering 3 5Th2e31Ne0Dthe'rsl-aHnedrstogenbosch ors. R. de Vries sCtoamrptl:ete3d0: Ma07rchApr1i9l941994
TEST SUBSTANCE
Identification Description
5869 Cream solid
Batch
2408
Purity
95%
Storage conditions
At room temperature in the dark
cosntadbiitliiotnysunder storage stable
:
Expiry date
denuary 01, 1%
<
- Pages -
000102
T-5869
NOTOX Project 121286
PURPOSE AND PRINCIPLE
tTheestpusrubpsotsaencoef btehetwesetnudyn-owcatsantooldeantdermwaitneer.the partition coefficient of the
Tofhethpearteiqtuiiolnibrciouenffcicoinecnetntr(ant-ioocntsanoiln/waattewro) ph(aPsoey) syisstedmeficnoendsisatsintgheofratio n-octanol and water.
T1h1equirdetCehnrtioomnatotginreaphoyf a(HPsLuCb)stacnhcreomaitnogararpehviecrsesdy-spthemaseisHirgehlaPteerdfotromaintcse
pThaertiHtPiLoCnmectoheofdficiisenutsef(unl-ofcotrano1l0/gwaPtoeyr)values between 0 and 6.
.
Umsuisntgaltshoe HbePLCappmletiheodd,ifimthpeuritteisetssuarbestaonfceminiosraimmipxorttuarneceo.f TchoempHoPuLnCdsmebtuthod
wishincohtraepapclticwaibtlhethteo setlruoenngt aorcidssurafnadceb-aascetsi,vemeatgaelntsc.omplexes, substances
GUIDELINES
Tghueidesltiundeys:procedure described in this report was based on the following GOurigdaenliiznaetiofnorfoTrestEicnognomoifcChCeom-iocpaelrsa,tiognuidaendlinDeevneol.opm1e17n:t (*OPEaCrDt)i,tioOnECD c(oHePLfCf)icimeenttho(dn-oc(atdaonpotle/dwaMtaerrc)h H30i,gh19P8e9r)formance Liquid Chromatography EA,uroMpeetahnodsEcofnoromitche Codmemtuenrimtiynat(iEoEnC),of EEphCy-sDiicroe-ccthievmeic9a2l/69proEpECe,rtiAensn,ex A.V,5: Part "Partition coefficient. EEC Publication no. L383, December 1992.
ARCHIVING
.
NOTOX B.V. will archive the following data protocol, report, test substance reference
for at sample
lanedastraw10dayteaa.rs:
- Page 6 -
000103
T-5869
NOTOX Project 121266
TEST SYSTEM AND RATIONALE
ATheHigshtaPteiornfaorrymanpcheaseLiqwuaisdbCohnrdoemdatsoiglriacpahCiwgi.thThaesmpoebcitlreophpohtasoenetwraisc75d/et2e5ctor. d(evs/vc)ribaecdetoinnittrhieles/eucattieorn. "BmoetthhodHPLoCf cihnesmtifcuamlenatnaatliyosnisan.d conditions are The test system was recognized by the international guidelines (OECD, EEC)
REFERENCE SUBSTANCES
Six chemicals for which Tog Poy has been reported were used to calibrate
-
tchoensiesltuetidonof:tine in units of 10g Poy. The mixture of reference substances
Reference substance
~~betnolzuyelnaelc(po.osl., (Mp.ear.c,k)Merck)
21.17
~~ 1F,i4u-odriacnhthleonreob(n9z8%e,neGC(,2.A5l.,driMcehrckC)heate)
3a.74
=Z d2i,b4e-n0z0y7l (9(99%9,%,WPGLCE,, AlRiderdieclh CdehenHtaee)n, Seelze, FRG)
a528
+ 10g Poy values according to the GEED guideline.
PERFORMANCE OF THE TEST
Preparation of the solutions
{
SLaoblsuctainonsLionfitetdheCor.e,ferDeunblcien,subIsretlaanncde)s waterea cproenpcaernetdratiinonmetohfan1o.l52(HgP/L1C.-grAade,
mSioxltuutrieonoftothaevroelfuemreetnrciec sFluabsskt.ancSeusbsewqausenptrleyp,aretdhisbyflaadsdkingwas125madule oupf eiatchh
mFoobriltehephdaesteertmoinaatifoinnalofvotolun(ereotfen2t5i.o0n atli.ne of the unretarded component), a
Satoluaticoonncoefntrfaotrimoanmidoef 1(.p7a)9,/1Mearncdk,theDraeramsfttaedrt,diFlRuGt)edin10mettihnaensolwitwhasmopbrielpeared
.
Rphassteo.ck solution of T-5869 was prepared by dissolving 287 mg test substance
diinlu5t0e.d0 m1l0 taicneetsoniwittrhilemob(i2leminpuhatsees,sorneiscualttiionng).inThtehesttoecskt ssoolluuttiioonn. vas
- Page 7 -
000104
T-5869
NOTOX Project 121286
Performance of the test Trheeferseonlcuetiosnusbstwaenrceesi,njmeocbteidleipnhatshee, fothlelowfionrgmamseiqdueenscoel:utitohne,mitxhteurteestof aSnodluttihoenfo(irnmamdiudpleicsaotleu)t,ionm.obile phase, the mixture of reference substances
Temperature of measurement nTheessutreemnpeenrtast.ure of the mobile phase was recorded several times during the
METHOD OF CHEMICAL ANALYSIS
aTrhee dceosncdriitbieodnsbeulsoewd: for the High Perforaance Liquid Chromatographic method
Analysts
Column
Mobile phase
FlDeotwection Injection volume
dLoieChr5osupnhe(rMer1c0k0,RPD-a1r6m;sta1d2t5,xF4RG)(.0.) wm; 7U8i1n2f5ted(viCvo).,acDuebtloinni,triIlreela(nHdP)L/CM-gir1a1die-,Q wLaatbesrcan 1(Mmill/lmipionre Corp., Bedford, HA, USA) 1U0Y walt Ae 210 nm
Instrumentation
AHuPtLoCsaPmupmpler Detector
1
Integrator
1Se5r5i-e2s0041(0PeLrCkin(PEelrmkeirn) Elmer, Norwalk, CT, USA) SBpeeaccthr,oMFiLo,niUtSoAr)3100 (LOC Analytical, Riviera 5p 4290 (Spectra Physics, San Jose, CA, USA)
:
DATA HANDLING
UvsailnugesHicgahn PbeerfaocrcmuarnacteelyLiqdueitdermChirnoemdaftroogrmapthhye, chersopemcaitaolglryaphliacrgeret10egntiPoony data. tThoethpiasrtientdi,onthceoefcfaipcaiceintty. faThcetorcap(akc')itywasfacusteodr,wassinccealciutlaitsedprofproorntitohneal to retention of the substance concerned (t) and the unretarded component (tg):
K = (tr = to)/to
From the resylts of the reference substances, a plot of log Poy (x-value) TvheersuTsogTko.g kv'alu(ey-voaflueea)chwacsompcoonnsetnrtucotfedt,heustiensgt sluibnseatrancreegwraesssicoonmpaarnealdyswiist.h the log k' values of the reference substances with known 10g Poy values.
- Pages -
000105
1-5869
NOTOX Project 121286
RESULTS
Rpehpasree)s,enttahteivmeixtHuPrLeC ocfhrormeafteorgernacnessoufbsttahencetsestandsoltuhteiofno,rmathmeidbelasnoklut(imoonbilaere shown in Figures 1 to 4.
Ianndt2hesmHaPlLlC tcehsrtomastuobgsrtaamnsceofpeaTk-5s86v9e,reusoibsnegrvdeedt.ectIinonaddaitti2o1n0,nmm,anyonesmallalrgetest sasusbusnteadncethapteaktshewelraergeobspeerakvedderbievtewdeenfraonpprtohxeimmaatjeolryco1mpaondnen6tmionfutteess.t It was substance whereas the small peaks derived from impurities.
mTehaesutorewmaesntsdet(eir.neine0d.89toanbde 00..9900 mmiinnuutteess).as a mean value of both
1Th0eg PmoeyananvdaluPeosy voaflutehse, arreetesnutmimoanritziemeds,ink'Tabvlaleue1s., Thleogplk'otvaolfue1s0,g Poy
F(ix-gvuarfell5e.) versls Tog k' (y-value) fron the reference substances is Shown in
Table 1 Results of the test.
[mm To[7[mv[mre[a]
tboelnuzeylnaelcohol
212164 || 0152073 || -00.157673 1271
1F,iv4o-rdaincthhleonreobenzene | 25..8697 || 25..323209 | | 00.732478 3a47
d2i,b4e-n0z0y7l
92.0172 || 39.514970| | 005.5903 a682
test substance
peak 1 (major comp.) | 7.75 7.659 0.884
pPeeaakk 23
6s.e9o6 | 6e.7s77 | 0.o8e3o1t
5.61 3.98x103
55.3411| 22..5010x010053
several small peaks | 1-6 [0.12/ 5.67|-0.93/0.75|-0.7/5.2 2[0.2/1.58x105
N$+ote : IMThneetaenrcpavolallcauuteleadtofiofnrtsohnevetrrheeetenrpteeicgofrnoersasteiidosnesusLiionnfge:bonytoth=csoh0ur.no3ds0ea0dtog+vraal0su.es7s30 (510.972, net)
The temperature of the mobile phase was 20.2-20.6C during the measurements
- Pages -
0001.06
T-5869
CHANNEL A
NOTOX Project 121286
INJECT 67-04-54 88:43:55 STORED TO BIN # Sa
2.5.2: 2.T1e5 i
. TATA SAVED TO BIN 4 sa
"
38196121286 WEL wETHOD 6
07-84-94 83:03:58 CH= "A" P= 1.
Rw 7 max 7
a1 so
PEAKE ARERZ
RT aren ee
2i 3
2@G.2a0s04s51 8GB.42s33 Sg13ai2ss1h a0a2ss
i5 3
3@142215 9251
n6s7es 102
1a3sz7i4e cei
o63n os
38S ea@l14a83ss5 1aall1sa 15a9s49s%%aaaeee
1i0 i
aisdiss alsss
11752 las
esreress dees
ooec or
pirs 3
LlTeeesszss F2Sl17e3 asachaeeisne aoonep
i128 $wna3is5st NUSlBEE aeiVeEsRaaEnx
;
1pr2sat mraaaa'nr saSfga E gRieAsAEbp
3
2EE 2o o 12.z0e7e6 2F6.861EE4E17S0L83EcGd2
Figure 1 HPLC chromatogram of the test solution of 574 mg/1 T-5869 in mobile phase.
CoHolbuimlne phase FlDeotwection
Injection volume
7LL5im/C2h/5rmois(npvn/ve)ra1c0e0toRnPi-t1r8;ile12M5ix141i(-10.D.v)atemrm; dpe un W, at \ = 210 nn
10'ul
HSSGooetpeers:axFitAiaLgaLutreetlhye31p3eaaTknhsdere2breotmrxieaneuntsess0wawsnadreaaspsapkusrreeodsiaauaamtts.eilvyahde1sIemninptuehtaeeksChaSin1ds0stsonopemteeonoesfo.ritvhoeef fbprereaoknsstthboeentwteeeant
- Page 10 - 0001.07
T-5869
NOTOX Project 121286
CHANNEL A
INJECT 67-84-94 A9:741A4 STORED TO BIN # 56 3
a TATA SAVED TO BIN # 5w6 o
38196121286
FILE 4. METHOD 8. FHALYST: Kei
Ks AREA
RT
12 a13s43 eaass
d3 ss3853 oa.t:ea
5: ?
7.87613 mmasrs 2503 412
8 alse 1A
TOTAL 108.
7-64-34 63:34:04 RUN 13 INDEX 11
AREA BC ag5ra7ev7ne 0aasp2 e4d41ss 6as2 zm1aaszze2e ammzs seeze
CH A PSs 1. BIN 6
Figure 2
HPLC chromatogram of a blank (mobile phase).
Column
FMloobwile phase DeIntjeeccttiioonn volume
LiChrospher
7L5m/2/5ni(nv/v)
100 RP-18; 125x4 (I.D.) mm; dp=5
acetonitrile/Mil1i-Q water
um
Uv10,'u1at x = 210 nm
- Page 11 -
0001.08
T-5869
CHANNEL A
NOTOX Project 121286
INJECT a7-a-as amismca? STORED TO BIN 4 S7 --_
:Tse
,
DATA SAVED TO BINx#o57
30196121286
a7-a4-9 asisarar Oe UA" PSs
FILE 1. METHOD a RUN 1s THIER 14
em 5
ANALYST: KRM
PERN ARERY wr awa ne
1%2 08EE.30525: a3s3HE 1m1sea2
i3: 3Ga.e18s:0 aoee3: sawGvarozriebosem
2iSo aSGt5n75E7 |0 1TB4Ei wssiSarcrieasnamo3
1Ho0 aaGssoy.: nBLE ah sFsumeadaoore
:
pB 3e0 EaeE E31E8 5SE58N0 aSTdahmeaaaar
.
RL se.
saesers
Figure 3 HPLC chromatogram of the mixture of reference substances in mobile
phase.
CMoolbuimlne phase
FDeltoewction
Injection volume
7L5i/C2h5ros(pvh/ev)r a10c0etoRPn-i1t8r;ile1/2M5ix4111(-IQ.D.w)atemrm; dp=5 um
U10,ml/atmixn = 210 mm
10'u1
bagez - 000109
T5869
NOTOK Project 121206
CHANEL A WEST B7-ad-94 7:W7:ad STORED TO BIN 8 49
Tak
:
S4e:s57 5.97
DATA SAVED TO BIN 8 49
"
38196/121206
o7-ne-d4 o7iiias He WROBEL
FIle 1. METHOD 6. RUN 6 INDEX 6
en 4s
ANLYSTE KRM
:
ene AREA: RT Ren ac
2zs 5T0..73i55 EeaFsDSf2i6e2 ama2e
5i8 sa1aa3i8s lel.a7ssa3 ereiaenn1ess:3 ao0e6n
is: $Sia53s5 L1w1aE87 eawieeraadnnz
1Hadsiae hIEE ceHwoEa A
ToL tee.
7sasen
5 <
Figure 4 RHoPbLiClechrphoansaet.ogran of a forsanide solution of 0.2 g/1 fn
CoNolbuimlne phase L75i/C2h5ros(pvh/ev)r 1a0c0etoRPn-i1t8r;ile1/2M5ix411i(-1Q.0.v)atemrn; dyes um
DFeltoewct on
ULYa,i7aatin = 210 na
Injection volume 10'u1
- Page 13 -
00014 0
T-5869
NOTOX Project 121286
13/04/94 TRI Pow
RE
! 0.800 [r Lr orpy
iii
0.600
':;
rv
HRY VE
Ca
fof ;
0-400
pp
0.200 [remem]
0.000
iiiiii
0.0 1.0 2.0 3.0 4.0 5.0 6.0
log Pow
*
Figure 5 PrleoftereofncelogsuPbos,tan(cxe-sv.alue) versus log k' (y-value) from the
- page 14 -
000111
