Document 821Geq3rgLedrvy7oqDKDjEpB
DR.U.NOACK-LABORATORIUMFUR ANGEWANDTE BIOLOGIE
1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroRespiration Inhibition Test with Activated Sludge
acc. to OECD Guideline No. 209 for Testingof Chemicals `adopted Apri4l, 1984
TelomerSRpeosnesarocrh Project Asan Gass Arora Cust
DAKNIOUSTRES LTD Dupont Author
Martina Noack Tost Facility 'DR.U.NOACK-LABORATORIUM FOR ANGEWANDTE BIOLOGIE Kathe-Paulus-Str. 1 0.31157 Sarsteat Laboratory Project ID. Project-No. 020109CK. Study-No. BBRE4111 `Study-No. of the Study Plan BBR8411 Page 10130 Study Completed September 26. 2002
Original 7 of 7 000083
FS--
Statement of GLP Compliance
Lars
custns
060 20 or Tsing of Chm to ri 4, 560
SEoR ar
Ia wssinanes
2009202
sLil PlinSSh
I.
vodOvibe e Sei
I
ban
000084
por
eS r+ 4+
Statement of the Quality Assurance Unit
inspection
date of inspection | daofrtepeort
20020008 | 2002-0806
ssom0z
lfpu.SEmUi 000085
DR.UNOACK-LABORATORIUM FUR ANGEWANDTE BIOLOGIE
Re1p-Doerctanol, 3.3.4.4,5.5,6,6.7.7,8,8,9.9,10,10,10-heptadecafluoro-
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Personnel Involved
Study Director
Martina Noack (Biologist)
Deputy
S(iElnkgeinFeieerb,igBiotechnologist)
Scientist
TR.esGpeofnfskiebl(eChfeomritceaslteintgeimnaenearl)ysis. Address see above
Technical Staff:
Jan Schwerdtfeger
Quality Assurance Unit: Deputy.
Gudrun Mohrmann-Kalabokidis: (Biologist) Susanne Becker (Biologist)
FDiarceicltorof the Test
(DBr.iolUodgoistN)oack
000086
DFU NOACK-LABORATUOMR FUR ANGEWANDTE BIOLOGIE
Re1p-Doerctanol, 3.3,4,4,5,5,6,6.7,7.8,8.9,9.10,10,10-heptadecafluoro-
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Table of Contents.
Page
Title Page.
1
Statement of GLP Compliance
2
Statement of Quality Assurance Unit
3
Personnel Involved `Table of Contents
45
List of Tables and Figures
5
1
Summary
7
2
Characterisation data of the test item
8
3 Method
" Results
"
a Solubility of the test item
1"
42 Volatisation of the test item
1
a3 Respiration rates and inhibition of the respiration
1"
as ECvalues
5
as
Biotic and abiotic factors
16
as
Reference test
16
5
Validity criteria
1
6
Literature / References
1
7
Raw data
"
8
Analytical method
18
81 Method
18
82 Method Validation
20
821 Linearity
20
822 Quanification Limit and Detection Limit
20
823 Precision (Repeatabilly)
2
824 Peak Symmetry
2
825 Accuracy
2
83 Results
2
84 Calibration Curves.
2
8s Chromatograms
2
9
Cortficate of tos item analysis
2
10
GLP-Cortficate of DF.U.NOACK-LABORATORIUM
30
000087
DR.U.NOAGK-LABORATORIUM FOR ANGEWANDTE BIOLOGIE
Re1p-Doerctanol, 3,3,4,4,5,5,6,6.7.7.8,8,9,9,10,10,10-heptadocafluoro-
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PSrtoujdeyc-tN:oN.o. 0BB2R08140181C1K
List of Tables and Figures
Tables:
Table 1: EC-values of 1-Decanol, 3.3.4.4.5.5,6.6.7.7.6,8,9.9.10,10.10-hepltadecafivoro- 7
Table 2: Respiration rates and inhibition of respiration of test and reference item
concentrations
15
Table 3: EC-values of 1-Decanol, 3.3.4,6.5,5,6,6.7.7,8,8.9..10.10,10 hopladecafiuoro- 15
Tablo4: Biotic andabiotic factors
1
Table 5: Raw data and respiration rates of test and reference item concentrations
"
Tabl6e: Repeoaf tinjeactibons oifTlestttyem
21
Tabl7e: Mean RecoveryRate of Fortified Samples.
2
Table 8: Concentrations of the Active Ingredient 1-Decanol,
3.3.4.45,5,6.6.7.7,8.8.9.9.10.10,10-heptadecafluoro- i the air trap
2
Figures:
Figure 1: Calibration Curve of Standard - concentration range 0.01 -0.06 mgil
2
Figure 2: Calibration Curve of Standard - concentration range 0.1 - 10 mgiL
2
Figure 3: Calibration Curve of Standard - concentration range 0.1 -0.6 mgiL
2
Figur4e: ChromatoofSgtarndaarmd
2
Figur5e: ChromatogramofTest item
2
000088
1 Summary
mg/L)
P=95(%)
Te ew
[mg/L]
Cee Tom |]
000089
_
'OR.UNOACK-LABORATORIUM FUR ANGEWANOTE BIOLOGIE
R1e-pDoerctanol, 3,3,6,6,5,5,6,6.7,7.8,8,9.9,10,10,10-heptadecafluoro-
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2 Characterisation data of the test item
TEST ITEM
1-Decanol, 3.3.4.4,6.5,6.6.7.7.8.8.9.9.10,10.10-heptadecalluoro-
Batch Number
Po0I001
cas RN
678.307
Chemical characterization 3(,E3I.N4E.C4S.5).5.6,6.7.7.8,8.9,9.10,10,10-hoptadecafluorodecane-1-o
Purity
Cs8u-mperpfelrufoiruooarlokayllkeytlheatnhoaln:ol999.39.9 %% ((aarlaa)).
Appearance
Yellowish sold wax
Watersolubiity
134 giL at12degreCe, Std 20ygiL, n=8 (DuPont, 2002) 137 ugiL at 25 degree C, SId 53 pglL, n=17 (DuPont, 2002)
Stability in water
Stable at test conditions
Density
Ca. 17 gem'
Expiry date Recommended storage Storage at esting facilly Retention Ientiication paramotor attesting facily
Unlimited if stored under the recommended conditions. Room temperature (20 C), protected from moisture. Room temperature, protected from moisture and light, Atleast 1.g has been retained
Name, batch number and colour.
The test tem and the information concerning the test item were provided by the sponsor.
000090
[DR.U.NOACK-LABORATORIUM FUR ANGEWANDTE BIOLOGIE
Re1p-Doerctanol, 3,3,4,4,5,5,6,6.7,7.8,8,9.9.10,10,10-heptadecafluoro-
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SPrtoujdeyc-tN:oN.o. 0B2B0R180491C1K1.
3 Method GUIDELINE
OECD Guideline 209
TYPE AND PURPOSE OF THE STUDY,
Respiration Inhibition Test with ECx-, ECs and ECy-values.
activated
sludge
to
determine
the
TEST SYSTEM Reason for the selection of study systom
origin Pre-treatment
Nutrient solution Ory siudge. concentration
Activated sludge Non adapted activated sludge from the sewage plant at Sarstedt is well suited as it comprises mosily household sewage and hardly Industrial waste water Municipal sewage treatment plant of D-31157 Sarstedt The sludge was washed with autoclaved tap water and diluted corresponding 10 a dry weight of 4.0 gL + 10 %. Synthetic waste water according to OECD 209
369g
TEST ITEM Stock solution Test concentrations. Pretreatment of the test tem
1-Decanol, 3,3,4,4,5,5,6,6,7.7.8,8.9.9,10,10,10-heptadecafluoroNone, directly weighing 100- 180 - 520 - 580 - 1000 mg/L "The test tem will be heated to 50 C. weighed directly into the Erlenmeyer flasks, filed with 250 mL autoclaved tap water and sired for 24 h
conTROL
2 control samples without test item were included in every test Series at the beginning and at the end of the test,
000091
DR. NOACK-LABORATORIUM FUR ANGEWANDTE BIOLOGIE
R1e-pDoerctanol, 3,3,4,4,5,5,6,6.7,7.8,8.9,8,10,10,10-heptadocafluoro-
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SPrtoujdeyc-tN-oN.o. B0B2R081A0191C1K
REFERENCE ITEM CAS No. Bateh-No Purity Expiry date Test concentrations Range of validity (EC) Tost date
Copper (I) sulphate pentahycrate p.a. Merck 7758-998 265990 999% 2005-11-30 58-100- 180 moll 54- 146 mglL 20020403
METHOD Tost duration Tost date Replcates
Tost vessels Volume of the study medium Application
Test temperature Ventiation
Static an 2002-04-03 One per concentration and two per control The highest concentration was tested in duplicates for analysis of airlow-outiet. 500 mL Erlenmeyer flasks, DIN 12440 500 mL
200 mL inoculum, 16 mL synthetic waste water 250 + 34 mL autoclaved water Test tom concentrations (directly weighing) 18-22C Permanent
TYPE AND FREQUENCY OF MEASUREMENT AND OBSERVATIONS
The pH value of the activated sludge was measured prior to testing and the temperature in the measuring cell once during the. measurement. The oxygen deplation of the control, reference and fost item was measured after 3 h incubation by means of oximeter and recorded for at least 3 minutes on a flat bed recorder. The room temperature during the test was recorded continuously by a hygrothermograph.
000092
DR.U NOACK-LABORATORIUM FOR ANGEWANOTE BIOLOGIE
R1e-pDoerctanol, 3,3,4,6,5,5,6,6.7,7.8,8,8.8.10,10.10-haptadocafluoro-
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Equipment
Adjustment of the recorder Calibration of the recorder
pH-meter, CORNING pH 240 Magnetic stirrer, IkawAG REO or RET Oximoter. Wrw Oxi 530 Flat bed recorder, Linse:s Membrane pump, BewR Tube pump, Biosens. Hygrothermograph, LuFFT
Voltage:
500 mv
Speed (y-direction): 1 cmimin
The recorder had been calibrated to the relation of mm (x-direction) and 0.1 mg/L oxygen reduction
DETERMINATION OF THE TEST ITEM IN AIR STREAM TEST DESCRIPTION
Possible losses of the test item via air outlet due to the aeration were analytically verified by gas chromatography with mass. spectromeric detection (m/z = 69, 385 and 463) from highest test concentration. For details see part 8
A range-finding test (NON-GLP-state) was carried out with three concentrations: 10- 10-0 1000 mg/L. A fresh sample of activated sludge taken from the sewage plant Sarstedt, washed twice with autoclaved tap water and diluted corresponding to a dry weight of 4.0 gL + 10 %, was used for the test procedure. 5 concentrations within the range 100- 1000 mi in a series with a dilution factor of 1.8 were tested. 2 controls without test item were included. Once every 7 days a reference test is carried out The reference item was tested in three concentrations within the concentration range 58 - 180 mg/L wilh a dilution factor of 1.8. The respiration rates of all samples were determined subsequent to.an incubation period of 3h Evaluation was carried out as described below.
000093
Dr. NOAGK-LABORATIOMR FUR AGEWANOTE BioLOGIE
TRRBoeaspcpaarnnaotlo,n 2A.n3.i4o,5n5,T6e6s.t7.w7i.h88A,c9i.a9i.e10d,1S0i.i1d0o-eheptadecafiuoro-
Page 120130 StudyNo. B8RE4111
acc. lo OECD-Guidaine No. 200
Projecto, 020100CK
EvaLUATION
tDroitnegr3miminnamroeahseurdoimsetanntceosrreeaccohrdteedtbvyeofi.at ed recordar 5Thmatmloeandshetortchoerfdaectrorar{e=e0qu.i0v2almegntO1La dcrease of 0.1 mg OL Twhaes epsetrifmoartmieodn obfytFhoerrmeuslpair(a1t).ion ate (R) according fo the aw data
Remar
mRd rmeosspisrrateidondaatencmeoomiimi +0002pmom0tmm
Tathescawlacsuapterofnoorfmerdesbpiyrastainodnarradtemse(Rt)haond inition of respiration
onion w(1e =|[1-5--22a2]_ 100
@
RRee, += RReseprastantattaeeofftosotlcnoncn 10 OL
caFlocrutlhaetecdonnt%ra.t the deviations of th respaton rates were
STATISTICAL ANALYSIS
TanhaelyEsCi-svuasliunegsosfoftthwearreefSeIrGeUnAcPeLfOTm(Wwienrdaocwasl)curlla.te6d.0w0,ih20p0r0ob,it $955 Corporarion PCornoftidveanlcueesinwteerrvealtsawkoenrefrcolmcuWaBtoEd a(c1c9o8r6)d,ing 1 a standard procedure (BRET& TOwSLG 1962)
000094
'DR.U.NOACK-LABORATORIUM FUR ANGEWANOTE BIOLOGIE
Report 1-Docanol,
3,3,4,4,5,5,6,6.7,7.8.8.9.9,10,10,10-heptadscafluoro-
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VALIDITY CRITERIA
The results are valg if. + The two control respiration rates differ not more than 15 % + Tho EC; of the reference item s in the range of 54 - 146 mg/L
DTEEVSITAGTUIIODNESLFIRNEOSM THE
In contrast to the guideline, it was decided o use copper (Il) sulphate pentahydrate instead of the prescribed 35dichiorophenol. The hance of Dichlorophenol is unsuitable for routine 1ab use.
DEVIATIONS FROM THE None STUDY PLAN
REPORTING
The final report is issued as paper copy (6 originals) and an electronic record (1 origina)
ARCHIVING
The following was retained in the archive of the test fail for the +peralilodraawsdsaptea,cified in the operative national GLP regulations: + study plan (orignal 1.12) + final report paper copy (orignal 1.1 6) + all records performed by the quality assurance programme
including master schedules + sample of test lem Microfims will be retained in a safe-deposit by Volksbank Sarstedt, D-31157 Sarstedt
000095
DR.U.NOACK-LABORATORIUM FUR ANGEWANDTE BIOLOGIE
Ro1p-Doerctanol, 3,3.4.4.5.5,6,6.7.7.8,8,9,9,10,10,10-heptadacafluoro-
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4 Results
4.1 Soluobftihelteistitteym
Due to the low water dissolved during the
tseoslt.ubility
of
the
test
item
(0.13
mg/L)
most
of
the
test
tom
was
not
42 Volatisation of the test item
| Testiom | Amount of tost| oid phase|
concentration| tem intest | exvacion |
solution | canrdge
Img
ims)
1000
00
cs
1000
00
ce
onc icationof crtridge ype see port 8.1
Testitem | adsorbed |
mg)
Testitem adsorbed
J)
Acration time (incubation): 3h
Aeration stream
>180Un
Oniy 1% negiigive.
of
the
test
tem
was
stripped
from
the
system,
therafore
losses
by
volatisation
were
4.3 Respiration rates and inhibition of the respiration
TFhreominthhiebiotixoyngoefntdheeplreetsipiornattihoenrreastpeisraftiroonm attheestewstoraendcarlecfuelraetnecdeinitmegm cOoncLentr(aTtaibolnes.2),
in % was calculated in comparison with the respiration listed in Table 2. The raw data are listed in Table 5.
rates from the control.
The
results
are
000096
1000 (1%)
28
9
1000 (2)
256
2
o=
o"e
::
=
-
=
"
a
:
CI ee[EoEmgw/L] CP RE
P=95[%] [mg/L]
||
000097
DR. NOACK-LABORATORIM FUR ANGEWANOTE BIOLOGE
R1e-pDoerctanol, 3,3,4,4,5.5,6,6.7.7.8,8,9.9,10.10.10-heptadecafluoro-
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SPrwoajoycNto-N.o. B0B2R0E140T91C1K
45 Biotic andabiotic factors The pHevalue of the activated sludge. the dy sludge concentration and the test temperature are documented in Table 4.
Table 4: Biotic and abiotic factors
Differenceof the contro respiration rates 1%] |__90 |
[psrivacteofthe voeas| us7g 0s e|
Ory sludge concentration [git]
EE
[restionpera|wewresr]
46 Reference tost
In the reference test the ECs -value was determined by probit analysis. The ECs value of the
roforence item i:
EC,= 104 mall
The ECas-value of the reference item copper(l-sulphate-pentahycrate is in the confidence range of 54-146 mglL.
5 Validity criteria
Vaidiy criteria were ulflec + The two control respiration rates differ not more than 15 %. + T5h4e-1E4C6smo(3llh.ours) of copper(jsuiphate pentahydrate i in the accepted range of
6 Literature / References (1) OECD-GuideliNnoe. 208 for Testing of Chemicals, adopedApril04. 1984 (2) ese,E. (1986): Grundrit der bilogischen Statistik, S. Auflage. (3) BVREEBTIGG.USGT.A.VTFOiMsPLcIHNEGR,VEWR.LA(eGd,itJoernsa,.1982): Methoden derWasseruntersiichungen 8.1. (4) 6D7u8P.o3n9t-.7,DeUtneprumbilniasthieodn roefsuplhtys,sicUop-dcahteemiFceabl. p1a5r,a2m0e0t2ers of Perfluoroociylethanol, CAS No.
000098
BRaaepecrame 23.4.4.5O5r6.6o77n.o0.L9A9s.o10R.a1r0o.m10unMepFtoRadAcsatEiAvNoDroT-E Bitoe Page 70130
eReemaiOoEnShH-Giutpminhe oNo.p300Acivaiod ge
SPruooeyeot.io B0o2R0s1a0r8n0y
7 Raw data
Toi 5 Raw dota and resiation tes af tt an erence em aoncenvations
Sonmeaamtrsaton|| con"acmororyyoaan]tyon||
maswarnecde | rosseaton ate mmm _| moun
| totam
T10o0000 (1%) sao
p7r2.508
5ow9
202366
|||
3102000
21T3e080e
6ao4r
a2205246
coTnvoEr2
2S6a1
27aa
wtoroncottm | T10o0
Torn
0wt
1T24e
ss
ss
106
Searsoi 5.S 1300.mlo Feoleon 35 11
000099
[DR.U NOACK-LABORATORIUM FUR ANGEMWANOTE BIOLOGIE
1Ro-pDoerctanol, 3.3.4.4,5,5,6,6,7,7.8,8,9,9.10,10,10-hoptadecafluoro-
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8 Analytical method
8.1 Method
METHOD OF DETERMINATION Equipment
Analyses the active
oifntghreedaiiernftlo1w--Doouctaenotlf,r3.o3m.4t.h4e.6h.i5g,h6e.s6t.7t.e7st.8c,o8n.9c.e9n,r1a0t,i10o,n
of
F1u0-sheedptSaidlieccaafClPu-oSrIoL- 8wacsapiclalrarriyedcoolutumvniaugsaisngcehxrtoemranatlogsrtaanpdhayrdosn. a
Detection was performed with a mass selective detector (MS).
Gas chromatograph: CP-3800, VARIAN
DeAtuetcotsaomrpler MCST,CSCaotmurbni2P0A0L0,, CVTaCRAANvALYTICS
Software.
Satur GCIMS Workstation 5.51, Varian
cSaorltirdipdgheasse extraction Reagents
HF Bond Elut C8, Varn HFBondElut C18, Varian fort-butyl methylether 99.8 %, Batch 42337011 31101, FLuka
CONDITIONS OF ANALYSIS
Column Injector Injector temperature Injection volume, Temperature programme.
CLhOrWomBpaLckEC/EMPSD,-8Fi(SlVmARItIhAiNcLk)n,es3s:0m0,.2i5..y:m0.25 mm.
Spiess 250C
(30
psi
pressure
pus)
for
1
min
iL
Hoating rate | Cimin)
Temperature | rc)
Holdimnign time
|
[T 0 1T "00 |
[Coe 10 |
so T2050
Carrier gas. Deltoneicstatoiron mode Run time Retention time
Helium Ms
1
mL
/
min
column
flow
E1l5e.c3t3romninionisation (1)
approx. 4.9 min
000100
DU NOACK-LABORATORIUM FOR ANGEWANOTE BIOLOGIE
R1e-pDoorctanol, 3,3,4,4,5,5,6,6.7.7.8,8.8,9.10,10.10-heptadecafluoro-
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STANDARD. PREPARATION OF STANDARDS, PREPARATION OF SAMPLES METHOD VALIDATION
Poak symmetry
Repeatability Accuracy
Test tom was used as standard.
Two stock solutions of he standard of 200 mg/L were prepared in tert-butyl methyl other, diluted (6 concentrations each) and used for calibration. For calibration range see part 8.2.1
The aiflow-outlet rom the test replicate was fillered through `Varian HF Bond Elut CB and VARIAN HF Bond Elut C18, respectively. Tho solid phase extraction cartridge was eluated with 5.0 mL tert-butyl methyl ether. The extract was injected directly into the GCIMS,
Quaniifcation of the test fem was calculated by peak area of the masses 69 + 395 + 463 (m/z) based on the extornal standards. "The calibration procedure and the principle for the determination of detection and quantiication limits were adapted from DIN 32645. The method was validated as described below:
Peak symmetries were calculated from chromatograms of analytical standards and test fem according to the following equation:
T= Wel
T= Wass =
PPeeaskkswiydmthmeat1y' % of poak height mm]
= fist socor of peak wiih ( cvidad by the perpendicular
line from the peak maximum) (mm)
5 sub-samplosofthe highest and lowest concentration prepared from a single homogenous sample were analysed. Mean values. standard deviations and variations of coefficients wore calculated
Three C, SPE-cartrdges were spiked with an amount of 5000 ug 1-Decanol, 3,3.4.4,5,5,6,6.7.7.8.8.9.9.10,10.10-heptadecafluoro(250 uL of 20000 mgIL). After spiking and romoving of excess of Solvent, air was sucked through the cartridges with approx. 150 Lin for 3h. Afterwards cartridges were eluted each with 5.0 mL for butyl methyl ether. The extracts were then cach dillod by factor 100 with tot. -butyl methy ether and injected into the GC/MS.
000101
DRLU.NOACK-LABORATORIUM FOR ANGEWANDTE BIOLOGIE
R1e-pDoerctanol, 3,3,4,6.5,5,6,67.7,8,8,9,9,10.10,10-heptadecafluoro-
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8.2 Method Validation The me~ tholdinweaarslyvalidated and tested with satisfactory results with respect to
precision (repeatability) -- pacecaukrsacyymmetry ~ determination imit and detection limit
8.2.1 Linearity The analytical system gave linear response in the range of 0.1 - 10 mg/L of 1-Decanol, o3b3t,6a.i4n,e6d.5f.o6r.s6t.a7n.7d,a8r,d8.a9n.d9.t1e0s.t10i,t1e0m-ahrepetgaidveecnafilnuofriog-u.resTh1e- c3.alFiborratdieotnercmuirnvaetiaonndacnhdrodmeatetcotgiroanms limits see part 8.3
5.2.2 Quantification Limit and Detection Limit
"The limit of quantification (LOG) and limit of detection (LOD) were calculated using the bind.
TvahleueLmOeDthwoads
ddeastcerrimbiendedintoDIbNe
32645 0.009
"Nachweis- und Bostimmungsgronze" mail and therefore the LOQ was 0.027
mgiL.
(ihreefold
the LOD).
000102
sat Pm
ry
ce
TT 20m [var|
[ T2 200 [ 1353
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DR. NOACK-LABORATORIUM FUR ANGEWANDTE BIOLOGE
R1e-pDoorctanol, 3.3.4.4,5.5,6.6.7.7,8,8,9.9.10,10,10-heptadacafluoro-
Page 24.0130
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Page 25 01 30
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R1e-pDoorctanol, 3,3,4,4,5,5,6,6.7,7.8,8,8.9.10,10,10-heptadscafluoro-
Page 26 of 30
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Page 27 01 30
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Page 29.01 30 StudyNo. BBREAT11
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