Document 2BMyX726vvD9kB64KEwqQvxb
i
RREEPPOORRTT
DETERMINATION
OF
THE
PARTITION
PARTITION
COEFFICIENT
COEFFICIENT
(N-OCTANOL/NATER)
(N-OCTANOL/BEATER)
OOFF
DETERMINATION OF THE
TT-55886699.
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BBYY HHIIGGHH PPEERRFFOORRMMAANNCCEE LLIIQQUUIIDD CCHHRROOMMAATTOOGGRRAAPPHHYY ((HHPPLLCC))
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RREECCEEIIVVEEDD
NNOOVV --99 11999944
33MM
TTOOXXIICCOOLLOOGGYY
' 2779944..0000011
EExhxihbibiitt 2794
State of Minnesota v. 3M Co., Court File No. 27-CV-10-28862
oT 33MM__MMNN0011663399887722
1-386
T-5869
NOTOX Project 121286
NOTOX Project 121286
SSTTAATTEENMEENNTT OOFF GGLLPP CCOOMMPPLLIIAANNCCEE
NOTOX
B.1.,,
*s--HHeerrttooggeannbbaosscchh,,
The
The
NNeetthheerrllaannddss
NOTOX B.V., 's
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most recent edition of:
The OECD Principles of Good Laboratory Practice
The OECD Principles of Good Laboratory Practice
which
are
essentially
fn
conforatty
conformity
wwiitthh::
which are essentially in
le:
TTRhehegeuUlUnantiiittoeenddsSStptaaarttteess56FF.oooodd aanndd DDrruugg AAddamiinniissttrraattiioonn.. TTiittllee 2211 CCooddee ooff FFeeddeerraall
Regulations Part 58.
oTTfhheeFeUUdnneiirttaeeldd SRStteaagttuelesastEiEnonnvvsiirroopnnammretenntt1aa6l0l.PPrrootteeccttiioonn AAggeennccyy ((FFIIFFRRAA)).. TTiittllee 4400 CCooddee
of Federal Regulations Part 160.
The
United
United
States
States
Environmental
Environmental
PPrrootteeccttiioonn
AAggeennccyy
((TTSSCCAA))..
TTiittllee
4400
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ooff
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t
SSttuuddyy DDiirreeccttoorr::
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Date: ue 3 aan
Date:
-- PPaaggee 2 --
2779944..00002
3aM__nMoN10e163399887733
= rox prsgect 12izee T-5869
NOTOX Project 121286
awn ASSURANCE STATENENT
QUALITY ASSURANCE STATEMENT
NNOOTTOOXX BB..VV..,, '*ss--HHeerrttooggeennbboosscchh,, TThhee NNeetthheerrllaannddss..
SLi) Sheciric processes dre tsb napecten at periodic hterals. SSttuuddyy pprroocceedduurreess wweerree ssuubbjjeecctt ttoo ppeerriiooddiicc iinnssppeeccttiioonnss aanndd ggeenneerraall nnoonn
study specific processes were also inspected at periodic intervals.
TeTohttihss orrseeppooarnrtdt
wwTaaesssuaTatuusdsittseecddeurbbayytettrhhyee
NNrOOeTTrOOiXXecQQuuaatllhiittyyFoAAssssdauutrraaa.nnccee
Unit
Unit
and
and
the
the
e
methods and results accurately reflect the raw data.
ons 07saoinsDeccan! DATES OF QAU INSPECTIONS/ AUDITS
ReroTING ones
REPORTING DATES
25 aren 1594 2250 Wren March 11959944
28 March 1994
2211 AApprriill 11999944
25 aren 1994 225 aren March 11959944
28 March 1994
2211 AApprriill 11999944
t
i
. aunty assurance anager Quality Assurance Manager
ea. witene a5. C.J. Mitchell B.Sc.
k
.T.a,/t~Ie,r/oZa.Tok au.
Date:COG - oL--9l,.
hea -- Page 3 --
2779944..00003
LL anore 3M_MN01639874
TT--55886699
REPORT APPROVAL
REPORT APPROVAL
STUDY
DIRECTOR: OR:
STUDY DIRECT
t
.
HANAGENENT::
MANAGEMENT
`
i
NNOOTTOOXX PPrroojjeecctt 112211228866
Drs. R. de Vries
Drs. R. de Vries
fe
oAe="--
vate: pr -., 9. aan
Date:
, ,tip`'`
J3S.e.AcA.tHMi.o.NnW..hveveaandn HHPheeyllsvviooctiorrttCheatstry
Section
~ head Physico
,n
Chemistry
P PP/-R)/
reoeJeefetler,eeees. TercY -h~noino caaCCl..Dn EiEnrnennciia tnnoggraa Technical Director
Dwaattee::o0g9 ll o6! o l 11(93b c9)4 +
-eage-d
- Page 4 -
27944..000004
oo a_notesss7s
3M_MN01639875
T-5869
T-5869
NNOOTTOOXX PPrroojjeecctt 112211228866
PPRREEFFAACCEE Ssppoonnssoorr
SSttuuddyy MMoonniittoorr TTeessttiinngg FFaacciilliittyy
SSttuuddyy DDiirreeccttoorr
SSttuuddyy ppllaann
3C3MaMnaBBdeeallsggitiurumnaa-t- CC1hh1eemmiiccaall EE8BCC B8CBe-a-l2n2g0a0i7d7u0a0msZtZWrWILaJIaNNtOO1RREE1CCHHTT
Belgium
MMrr.. RR.HH.. CCooxx HNNaOOsTTbOOaXXkeBBn..VwV.e.tering 3 5T5H22ah3m3eb11aNkeD0etDDnh'wesers--tlHHeaeernrridttnsooggge3ennbboosscchh
The Netherlands
DDrrss.. RR.. ddee VVrriieess SCStotamarprtlt:e:te33d00: MM0aar7rcchAhpr11i99l99441994
Completed: 07 April 1994
TTEESSTT SSUUBBSSTTAANNCCEE
IIddeennttiiffiiccaattiioonn
TT--55886699
DDeessccrriippttiioonn
CCrreeaanm ssoolliidd
:
BBaattcchh
22440088
PuPurriittyy
9955%%
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AAtt rroooomn tteemmppeerraattuurree iinn tthhee ddaarrkk
t
cosSnttadabbiiitlliiiottnyys.uunnddeerr ssttoorraaggee stable
conditions
Stable
i
EExxppiirryy ddaattee
JJaannuuaarryy 0011,, 11999966
<
k
-- pPaaggees5 -22779944..00000055
_ 33MM__MMNNO01166330988776.6
T-T-55886699
NNOOTTOOXX PPrroojjeecctt 112211228866
PPUURRPPOOSSEE AANNDD PPRRIINNCCIIPPLLEE
TTthheeestppuusrruppbosostseaencooeff btthehetewsesettnuuddyny-owwcaatssanttoool ddaeenttdeerrmwmiaitnneeer.tthhee ppaarrttiittiioonn ccooeeffffiicciieenntt ooff tthhee
test substance between n-octanol and water.
TooTnfhh-feoecttthphpaeaeanrroetetliqqituutiiiiaollonninidbbrrccwiaiootuueeeamffrPf.iccicoocinniecceneentnnttt(rr(naan-tt-oiiococonttnasasnnoioilnnl//waawaattttewweroor))pp(hh(PaaPsosoyewe)) ssyyi1ssssttededemneffiiccnnooeennddssiissaattssiinnttgghheeoo:ffrraattiioo
n-octanol and water.
?
TT1hhieqeuirrdeetteCenhntrtioiomonantottiginrmeaephooyff aa(HssPLuuCbb)ssttacanhncrceoemaiitnnogaararrpeehvvieecrrssesedyd-s-ptphehamasseeisHHiirggehhlatPPeeedrrffootrrosmaainntsccee
pTlpahiareqrtutiiiHtdPtiLioCConhnrmccoeootmheeaofftdfofigicrciisaiepenuhntsyte((f(Hnunl-P-oLocCcftot)arancnoho1llr0/g/owwmaaaPtttoeoeyrgr)r)V.a.aplhueisc
system is
between 0
related
and 6.
to
its
7
BUTUsuhsiseintngHg8P1Ltt5hCh0eemHbHeePPtLhLCoCsdpmpmelietisthehoduodsd,e,iffuiilmtmphpefuuorrriittteisiletoesgssPuaabrorsweetoavonffaclemumieinnsioosrrbeaitimmwmieppxeootnrrutt0aranenccaenoe.d.f 6TcT.hohemepHoHPuPLnLCdCsmmeebtutthhoodd
wimihssuiscnnthootatlrssaepopapcpltlbieicwcaiaabtpblhpleleithettedoo sesittlfrruotoennhngget oaatrcceiisddtsssusruaafbnnasddcte-abbanaacscseteesis,vi,esmmeaeattgaaemllnitxscct.ooummrppelleoexfxeescs,o,mspsuoububsnstdtaasnnccbeeusst
which react with the eluent or surface-active agents.
GGUUIIDDEELLIINNEESS
TgTuhhieedesslttiuunddeyys:pprroocceedduurree ddeessccrriibbeedd iinn tthhiiss rreeppoorrtt wwaass bbaasseedd oonn tthhee ffoolllloowwiinngg
guidelines:
OGOrurgigadanenilizizanatetiiofononrffToorerstEEiccnoognnoommoificcChCCeoom--ioocppaeelrrsaa,ttiioognnuiaadnendldinDDeeevvneeoll.ooppmm1e1e7nn:tt (("OPEEaCCrDDt))i,,tioOOnEECCDD
cGc(ouoHeiePLfdfCfef)ilicicimnieeeetnnhtftood(r(nn-T-oeo(cscatttdaiaonnnpogtolel/do/vfwaMataCterhercer)hm)iH3Hc0iia,gglhhs1,P9P6eeg9rru)ffi.oodrremmlaiannnceceenLoLi.iqq1uu1ii7dd:CC"hhPrraoormmtaaitttooiggorrnaapphhyy
(HPLC) method" (adopted March 30, 1989).
EAE,uurroMopepeteahanondsEEccoofnnoroonmfitchceCCoodmmemtmueunrninititynya(t(EiEEoECnC)),o,fEEEEpCCh--yDDsiiirrceeocc-tcthiievvmeeic99a22l//669p9roEEpEECeC,r,tiAAennsnn,eexxA.VV,8,: PPaarrtt
.
'A"P,PaarMrtetiittthiiooodnns ccfoooreefffftiihcceiiedenentttse".r.miEEnEECaCtPPiuoubnblliioccfaattpiihooynnsicnnooo.-.chLLe33m883i3,c,alDDeeccpeeramobbpeeerrrt1i199e99s22,..A.8:
:
AARRCCHHIIVVIINNGG
.
NpNrOOoTTtOOoXXcoBBl..,VV..rwweipilollrlt,aarrccthheiisvvteesuttbhhseetaffnoocllelloowwriiennfggerddeanatctaea ffsooarrmpaaltet llaeenadassttra1w100dayyteeaaa.rrss::
protocol, report, test substance reference sample and raw data.
- -
PPaaggees6
-
-
22779944..00000066
33MM__MMNNO011663399887777
T-5869
NOTOX Project 121286
TEST SYSTEM AND RATIONALE
THeighaptereforrmanece Letd Cramstegrac ith spectraphtonsirf deatreector. TTAhheeHisgshttaaPtteiiroonfnaoarrrymyapnphchaeasseeLiwqwauasisdbboConnhddreeoddmastsioilgliriaccpaahCCi1wg8i.t.hTThhaeespmmeoocbbtiirlloeephppohhtaaossmeeewtwarasisc7755d//e22t5e5ctor.
(v/v) acetonitrile/water. Both HPLC instrumentation and conditions are described in the section "method of chemical analysis'.
he tet systn vas recognized by the ternational ukdenes (OED, 60). The test system was recognized by the international guidelines (OECD, EEC).
REFERENCE SUBSTANCES
e ee a Se Ri So. he shes o reference sibstanes Six chemicals for which log P w has been reported were used to calibrate the elution time in units of ?og Pow. The mixture of reference substances consisted of:
Reference substance
apres ga Were) - benzylalcohol (p.a., Merck) Tee Gr) - toluene (p.a., Merck)
-~ 11,,44--ddiicchhlloorroobbeennzzeennee ((zz..ss..,, MMeerrcckk))
ee EE Dent - fluoranthene (98%, GC, Aldrich Chemie) = Ji eo, Siri - dibenzyl (99%, GC, Aldrich Chemie) Sibert G7 55 AUIS SER, seta, ny - 2,4-DOT (99%, HPLC, Riedel de Hadn, Seelze, FRG) FE -- log P., values according to the OECD guideline.
log Pow,
11.1 32.7
33..44
34.7 i4.8 26.2
PERFORMANCE OF THE TEST
Preparation of the solutions
3 Sotutons of tre reference upstnces vere prepared in sear) (PLE rac, Solutions of the reference substances were prepared in methanol (HPLC-grade, : RTL ah pier prices Rg UR Sr Labscan Limited Co., Dublin, Ireland) at a concentration of 1.5-2 g/1. A
mixture of the reference substances was prepared by adding 125 pl of each solution to a volumetric flask. Subsequently, this flask was made up with mobile phase to a final volume of 25.0 ml.
E eee ELateeo LEa He of ne retarded componaenrt,eaa For the determination of to (retention time of the unretarded component), a resem hocks 10 ss wi soe solution of formamide (p.a., Merck, Darmstadt, FRG) in methanol was prepared
at a concentration of 1.7 g/1 and thereafter diluted 10 times with mobile
, RB8s5 solution af 1-963 xs prepares by aissonving 27 mg ast substance phase. A stock solution of T-5869 was prepared by dissolving 287 mg test substance in 50.0 ml acetonitrile (2 minutes sonication). The stock solution was 8 5 denies smiction, Tie SESE Shetin. diluted 10 times with mobile phase, resulting in the test solution.
"rer- - Page 7 -
279944..00007
3M_MN01639878
1T--5508669
NNOOTTOOXX
Project
Project
121286
121286
pPereforrmfanoceroofmftathhneetcteesestt TTrhheefeersseoonllcuuettiioosnunsbsstwwaeenrrceeesii,nnjjseeccattbeelddeifpnnhattshheee, fftoohllelloowwfiionrngsganssieedqqeuueennsccoele:u:tittohhnee, mmiitxhxettuurrteeestooff
reference substances, mobile phase, the formamide solution, the test
sasonodlluutttiihoeonnf((oiirnnasddauiupdpleliicscaoatlteue)t),i,onmm.oobbiillee pphhaassee,, tthhee mmiixxttuurree ooff rreeffeerreennccee ssuubbssttaanncceess
and the formamide solution.
TTemepemraptureeoroffammeetaassuuurreermmeenentt
mTTehhaeesuttreeemmmppeeenrrtaastt.uurree ooff tthhee mmoobbiillee pphhaassee wwaass rreeccoorrddeedd sseevveerraall ttiimmeess dduurriinngg tthhee
measurements.
MMEETTHHOODD OOFF CCHHEEMMIICCAALL AANNAALLYYSSIISS
e
TaThrheee dccoeonsndcdirititibioeondnssbeuulssoeewdd: ffoorr tthhee HHiigghh PPeerrffoorramaannccee LLiiqquuiidd CChhrroosmaattooggrraapphhiicc mmeetthhoodd
are described below:
AAnnaallyysstiss coCloluummnn MMoobbiillee pphhaassee
FlIDDFneelojtotweeweccctttiiiooonnn volume Injection volume
LLiiCChhrroosspphheerr 110000 RRPP--1188;; 112255 xx 44 ((I1..00..)) mmmm;; L7d7dp=8i5p=7n/2t255t55e(duu(vmmvi/C(vov()M.M),eerraacccDckukee,btt,looinnDDniaia,rttrmrrmsiiTstllrtaeeeadldt(at(,Hn,HPdPL)FLFCR/CRG--MG)ggi)rr1a1ad1de-e,3, wLLaaatbbessrccaann (L1(MiWimwililNlt/iiemppdioonrrCeeo.CC,ooDrruppb..l,iBBnee,ddfIfororerdld,a,nHdMA)A,/,MiUUSlSKlA)i)-Q water 11UUVY0'msalmtt/mhiXen= 221100 mnam
10 ul
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Detector Autosampler
Detector
3
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Beach, FL, USA) SSPP 44229900 ((SSppeeccttrraa PPhhyyssiiccss,, SSaann JJoossee,, CCAA,, UUSSAA))
}
DDAATTAA HHAANNDDLLIINNGG
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'
Ttrthehoeteetnphptaaiirrsottniiettniidooof,nnttchhceooeeefcfsfafuipibcacsiciteieantnntcyt.e.faTcTchohteneocreccraa(nppkeaacdc'ii)tt(yywtra)fsfaaccuattsnooderrdt,vwhaseasisnucccneaarllecctiuuatllraaditteseedddpcrfoofrpmroopomnrotnitetohhnenetal(tto)o:
retention of the substance concerned (tr) and the unretarded component (to):
kK'os= ((ttrr - ttol)/tto VFFreroronsmustthheeTogrreekss'uylltt(ssy-ovoaffluttehh)ee wrraeesffeecrroeennnsccteerusscuutbbessdtt,aannccuesesis,n,gaalpipnlleooattrooffrelglorogegsPFsQoiwoyn((xax-n-vavlaayllsuuiees)). tTTvhhheeeersul1Toso0ggglKkok' ''g kvvv'aaalll(uuuyeees-vooofaffleeuaatecch)hhewccarosoemmfpcpeooornnneseenntcntretuocsofftubesttdthh,aeenucstteieesnssgttvsilsutiubhnbsesattkraannnocwcreneegvrw1ae0assgssciPcoooonmymppaavaarnrleeauddleyssww.iiistth.h
the log k values of the reference substances with known log Pow values.
-- Ppaaggees8 --
3SMM__MMNN0O1T663399887799
279944..00008
T-T-55886699
NNOOTTOOXX PPrroojjeecctt 112211228866
RESULTS
Representative HPLC chromatograms of the test solution, the blank (mobile phase), the mixture of reference substances and the formamide solution are
shown in Figures 1 to 4.
In the HPLC chromatograms of T-5869, using detection at 210 nm, one large and 2 small test substance peaks were observed. in addition, many small test substance peaks were observed between approximately 1 and 6 minutes. It was assumed that the large peak derived from the major component of test
substance whereas the small peaks derived from impurities.
The to was determined to be 0.90 minutes as a mean value of both measurements (i.e 0.89 and 0.90 minutes).
C
TThhee mmeeaann vvaalluueess ooff tthhee rreetteennttiioonn ttiimmeess,, kk'' vvaalluueess,, lloogg kk'' vvaalluueess,,
(l(xoxo-gvvaPaf?lwuiee)a)ndvveePrrosswuussvllaoolgguekks' a(r(yey--svvuaalmltmueae)r)izfferrdoonmIntthheTeabrrleeeffee1rr.eenncTceheessupublbsostttaaonnccfeeslsogi1ssPsoShwhoowwnn iinn
Figure 5.
[eee [ow [[mv [wm] a | Table 1 Results of the test.
Substance
trl
k'
log k' log Pow
Pow
benzylalcohol
1.14
0.274
-0.563
1.1
toluene
2.24
1.503
0.177
2.7
1,4-dichlorobenzene
2.89
2.229
0.348
3.4
fluoranthene
5.67
5.330
0.727
4.7
dibenzyl
4.07
3.547
0.550
4.8
2,4-DDT
9.12
9.190
0.963
6.2
. peak tteesstt peak
1ss1uu(bb(mssmattajaajononrcrceeccoommpp..))|
77..7755 |
77..665599| 00..888844
55..6602| 33..9588x010085
1
ppeeaakk 22
66..9966 66..777777
00..883311
55..4412 22..5511xx1100%5
:
pSpeeeavakekr3a3t smal peaks | 616.-.66600
[0.1662.7.337754.46
7|
-0
.009..388/0004.475
|-
0.
7515.5..33212
2[
0.222/..100.005xx611x010%05,% 1.58x105
75 -0.7/5.2 0.2/
several small peaks 1 - 6 0.12/ 5.67 -0.93/0.
2
Mean value of the retention times of both chromatograms. Interpolated from the regression line: y - 0.288x - 0.770 (r.0.972, n.6) Note : The calculations were performed using not rounded values.
The temperature of the mobile phase was 20.2-20.6C during the measurements.
- Page 9 -
27944..000009
3M_MN01639880
T-5869 T-5869
NNOOTTOOXX PPrroojjeecctt 112211228866
CCHHARNNNNEELL AA
INJECT
INJECT
0677--0944--9944 0028::4A33::5588 'SSTTOORREEDD TTOO BBIINN ##
So
50
4
2452.44R 4x.1]7
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47
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TARTTAR SSAAVVEEDD TTOO BIN & SB
BIN # 50
3831819966//112211228866
0077--0044--9944 0088::0033::5588 CH= "A" PS= 1.
fo
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NETHOD
METHOD
8.
RRUNN 77
i:H= "A" PS= 1.
INDEX 7
BIN so
=hi
INDEX 7
BIN 50
PPEERAKKN#
AREA
AREA%
RRTT
PARREEAA EBCC
12312
00886.....022864849091819
021.1335 0B.3245
151336223118 066222 63612528 0a22
:
345a
03B3..020442291558 006a..l79339s44 14039332218.37239429 AO8aR3m2
65787&
0068...412235248111 08..418958
01L1..6f70292 11.1129
183s303e8i917s314 00aa5cs6 15ge8s9s3 0a6c
18895 110
0088....2421525489 8A..482398
1111...44257379 16773099577348843 000ac666 11.75)28 1236977448 0ac6
11113212 1133
0030...88883_9937599 3B.e99927
1222....46708323 22s286a967e676r62949 00aae767 22.05438 92+973762 caacb
111111765465
011s11...i64061a526592257522
2333..1591553 2- a.l8d3
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00 aa3263 0032
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5 sG.6E5Le9 e822v888a331n89:11< 0 3ao3zz22 FE,S6?1 431k72A0e o<ar'2
2 S538 270 47nss a3 364
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FFiigguurree 11 THHP-PL5LC8C6c9chhrrioonmsamattooobggirrlaaemnpohoaffsett.hhee tteesstt ssoolluuttiioonn ooff 557744 mmgg//ll T-5869 in mobile phase.
t
CCHooollbuuimmlnne phase
L7Lii5CC1hh2rr5ooss(ppvhhIeevr)r 1a100c00etRRoPPn--i11t88r;;il11e22/55Mxxi4l4l({(I-1.q.DD..a))temmrmm;; ddpp==55 umm
DFelFMtlooobewwiclteiopnhase
17W1w5,/am21l//5atmm(iivxnn/=v)2a1c0etnoanitrile./Milli-Q water
IDInnejfteeeccctttiiiooonnn vvoolluusmee 1U10V0,uU11at a = 210 nm
.
NSNoopttpere:o:nAiALalLaltettlhhyee ppe'eaaaknksds b2beetatwiwereeuentneso0 vaaennrddeaapepppirrsooxcciihmnaaatsterelvlyeyd11 imnmiintnuhuteteecaahnniddcasssotoommgesreoonffsttohhfee ppsheaesakksSslebbneakttwweeesnn
(Gha Tiaure 2). approximately 1
(see Figure 2).
Thererore it vas assomed that there and 2 minutes were also observed in
Therefore it was assumed that these
peaks 18 not derive the chromatograms of
peaks did not derive
from the test the blank
from the test
= pam z = - substance.
-- Pano -in -
33MM__MMNN0O11663399883811
22779944..00001100
7T1--55886699
NNOOTTOOXX PPrroojjeecctt 112211228866
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5s6e8a3344
3
FFiigguurree 22 HHPPLLCC cchhrroommaattooggrraamm ooff aa bbllaannkk ((mmoobbiillee pphhaassee))..
coCHoollbuuimmlnen phase FlFMDloeoobtwwielcteiopnhase IDInenjtjeeeccctttiiiooonnn vvoolluusmee
LL7i5iC/C2hh5rrooss(ppvhh/eevrr) 11a0c0e00tRRoPnP--t11t88r;i;l1e12/2M55ixxT441(i(I-Id..DD.v.)a)temmarm;; ddpp=e55 uumm 17UL5Y,/mm2l/5/ammti(invnx/=v)21a0cetnomnitrile/Milli-Q water 1U10V0,'uul1at X = 210 nm
-- PPaaggee 1111 -22779944..00001111
33MM__MMNN0O11663309885822
T-T-55886699
CCHHAANNNEELL
A
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:
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121286
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0677--0044--9944 0099::5500::1177
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331961121266
FILE 1. METHOD
6.
RUN 6
INNDDEEXX 1144
BBIUN 57
FILE 1.
METHOD 0.
RUN 14
I
AANNAALLYYSSTT:: KKRRHH
PPEERAkKn# AARREERAZ1
PRTT
ReReFR
BC
RC
12125
00s0g..o1a21z4s42:553 00swa..aa12ass45 171ra10au,33mwi19ee00ezl22
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3
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1a01al..ls30a11es73 1105..35267
222g2..s.ea26g8r4e19 557s51s0a4rs"eF1mi4171ta13h1ee00eA:2ln23
i
12
15.524
BR 13
36.584
i5 a9m.3a36 14
0.316
564saS...is3069de1888
755334 01
emer 1877339 t+1 eiwsee eetn 15261 01
15
13.272
9.13 645770 01
o
TTOoTTeALL 110000..
4a8sFe,s5e611s3
FFiigguurree 33
HPLC chrosatagran phase. HPLC chromatogram
of
of
tthhee
mmiixxttuurree
ooff
rreeffeerreennccee
ssuubbssttaanncceess
iinn
mmoobbiillee
phase.
CHCooolbluiumlmnen phase FDelFMtloooebwwiclteiopnhase IIDnnejjteeeccctttiiiooonnn vvoolluurmee
LL7i5i/CC2hh5rrooss(ppvhhieevr)r 11a00c0e0tRRoPPn--i11t88r;i;l1e12/2M55ixx1441(i(I-1.Q.D0.w.)a)temmnrm;; ddpp-e55 uuma 71LU50a,/ml2l/a5/mmti(i)vnn/v= )21a0cet0aonitrile/Milli-Q water 1U1V00,uullat X - 210 nm
-- PPaaggee 1122 --
3SMM__M1NN0O1T663399888833
22779944..00001122
TT-55886699
NNOOTTOOXX PPrroojjeecctt 112211228866
CCHHAANNNNEELL
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TWJECT 9677--m044--9944 0077:113771:4444 ;STTOORREEDD TTOO BBIINN ## 4493
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651:8577 25.9977
3.65
DATA
DATA
SSAAVVEEDD
TTOO
BBIINN
##449
seas6/121z0886
0a77--0n4e--s9e4 0a7r2i1i7z:a4d4 ERE ERE PRSE= E1D.
3S196r1212
FILE 1. METHOD @
RUN 6
IINNDDEEXX 66
BeInN 44s9
FILE 1.
METHOD 0.
RUN 6
AANNAALLYYSSTT:: KKRRHH
EAka
PERK##
AREAL
ARER7.
RT
RT
AAmReEAn BBCC
12152
561D6....7331395859 00ee..a1a2s76LT 82Se2966ep22246me000ea222
345i 1a00V..i07s4t94e o.i5573:e5, 77i53ae93zi3e6ds03s 00a6e882
5672?6
55144...855424848
SG2i8 6.246
Ttair 008...788989
1.11
srosasn 4410249Q144343737 00@688 1.79 05
1I@r9s9 o003Tla...ois[418z4i229eas44 112N1z...o8E849r7727 a2os33xkp812me9R2ews94a00@aas5@21
11
20.915
3.65 15A9R9 01
TTOoTtL;L tloecei..
7255r0,559999
i FFiigguurree 44 HmHPPoLbLCiClecchhprrhooamnsaaett.ooggrraanm ooff aa ffoorrmmaammiiddee ssoolluuttiioonn ooff 00..22 gg//11 iinn
mobile phase.
CoHCoallbuulmmen phase L7L5ii/CC2hh5rrooss(ppVhIhVee)rr 1a1c00e00tRoRPnP--i11t88r;i;l1e1/22M55ixx1441(1(I-1Q..0D.v.)a)tesmarm;; ddyp=es5 #u,nm
`
Flow Mobile
Flow
phase
1715/mml2l//5mm(iivnn/v) acetonitrile/Milli-Q water
DeIDtneejteeccctttiiiooonnn voluse uU1wV0,,'u1aatt \X == 221100 mnmm
Injection volume 10 ul
- -
PPaaggee 1133
-
-
279944..00001133
3SMM__1MNNo011663309888844
1-586
T-5869
NoToK project 121266
NOTOX Project 121286
13/04/9944 TTRRIJ PPooww
1 Cor 1.000
1 8.800 frrmasnifonnmnenmeegng ofer fuss
0 0.800
Ir
in"
90.600[roi mi e |eoi fi hi e
9 0.600
i
CARO k 0.400
0.200
} TTT
00..000000
00..00
eed
11..00 22..00 33..00 44..00 55..00 66..00
lloogg PPooww
<
FFiigguurree
5.
5
PPelltooetrteonocffe:lloaggwaPPoofywe(r(xss--vv:aalluuee))
versus
versus
Tog
log
k' .
k'
(y-vaue)
(y-value)
fron
from
the
the
reference substances.
- pagers -
- Page 14 27944..00014
aw noressass 3M_MN01639885
