Document 1y9w1GYeGnOB6dGE7roVw5YX
fifi
3J0JI
Accession No. Study No.
C03-3620 33620
Study Report
Analysis of Residual Solvent (Ethanol) i: (non-GLP study)
3 3t
October 14, 2003
Chemicals Evaluation and Research Institute, Japan --Kurume Laboratory--
Company Sanitized. D oes not contain TSCA CB(
Table o f Contents
T i tle .........................................................................................................................................3
Commissioned by.................................................................................................................. 3
Testing Facility...................................................................................................................... 3
Purpose of Study.................................................................................................................... 3
Schedule.......................................................... .......................................................................3
Personnel................................................................................................................
3
Approval of Study R eport.....................................................................................................3
S u m m ary ..............................................................................
4
1. Test Substance....................................................................................................................... 5
2. Execution of Study.................................................................................................................5
3. Results of Study...................
7
Tables Table 1: Calculating the ethanol content from GC results.
Figures
Fig. 1: GC chromatogram for calibration curve, and calibration curve (ethanol). Fig. 2: GC chromatogram for ethanol analysis.
Study No. 33620
'Ceragany Sanitized. Does not contain TSCA CSI 2
Title:
Analysis of Residual Solvent (Ethanol) i (non-GLP study)
Commissioned by: DuPont KK 1-8-1 Shimo-meguro, Meguro-ku, Tokyo 153-0064
3
Testing Facility:
Kurume Laboratory Chemicals Evaluation and Research Institute, Japan (CERI) 19-14 Chuo-machi, Kurume-shi, Fukuoka Prefecture 830-0023
Purpose of Study: To determine the level of ethanol remaining in Forafac 1157.
Schedule:
Study began on: Test date: Study completed on:
July 29, 2003 July 29, 2003 October 14, 2003
Personnel:
Coordinator: Researcher:
Yasuko MATSUNOBE, Testing Section 1 Tomohiko YOSHDDA
Approval of Study Report:
[signed] Yasuko MATSUNOBE Study Coordinator October 14, 2003
Company Sanitized. Does not contain TSS. 531
*Translator's Note: Spellings o f personal names may need to be verified.
Study No. 33620
3
Summary
Title of Study Analysis of Residual Solvent (Ethanol) i:
jnon-GLP study)
Study Conditions
(1) Concentration of sample furnished:
1,000 mg/L
(2) Analysis: Analysis of ethanol by gas chromatography (GC)
Test Results Content of ethanol in sample furnished: 0%
Study No. 33620
Company Sanitized. Doe not eotrtn T*CA 0 4
1. Test Sil Name:
Lot No.:
f\
2. Execution of Study
Gas chromatography (GC) samples prepared as described in section 2.1 below were analyzed in accordance with section 2.2 on the next page, based upon which the ethanol contents of the samples furnished for testing were computed.
2.1 Preparation of Sample for Analysis Pretreatment was carried as shown in the flow scheme below so as to prepare a
GC sample for ethanol analysis.
Flow Scheme
Study No. 33620
Company Sanitized. Does not contain TSCA Clif 5
a
2.2 Ethanol Analysis by Gas Chromatography The GC sample prepared in section 2.1 above was analyzed for ethanol using the
quantitative determination conditions shown below. The ethanol concentration in the GC sample was determined by comparing the peak surface area on chromatograms for a 40.0 mg/L standard solution and for the GC sample, and calculating the ratio between the two (see Fig. 2).
(1) Quantitative Determination Conditions:
Apparatus:
Gas chromatograph
GC-17A (Shimadzu Corp.)
Detector:
hydrogen flame ionization detector (FID)
Column:
INNOWAX, film thickness 0.25 pm (Agilent Technologies)
Column temperature: 40C
Sample insertion port temperature:
200C
Carrier gas:
helium
column flow rate, 1.7 mL/min
Hydrogen:
60 kPa
Air: 50 kPa
Injection rate: 2 pL
Split ratio:
5:1
Detector
Temperature: 230C
Sensitivity: 10
(2) Preparation of Standard Solution: A standard solution for determining the ethanol concentration in analysis samples
was prepared as follows. One hundred milligrams of ethanol standard product (Nakalai Tesque, Inc.; grade
1 reagent) was precisely weighed out and dissolved in purified water to form a 1,000 mg/L ethanol solution. This solution was diluted with purified water to form a 40.0 mg/L standard solution.
(3) Preparation of Calibration Curve: Standard solutions having concentrations of 10.0, 20.0 and 40.0 mg/L were
prepared in the same way as described in (2) above. These were then analyzed under the quantitative determination conditions given in (1) above, following which a calibration curve was prepared from the peak areas on each of the chromatograms thus obtained and the respective solution concentrations (see Fig. 1).
Study No. 33620
Company Sanitized. D oes not contain TSCA CM 6
2.3 Calculation of Ethanol Content The ethanol content was calculated using the following formula.
Content (%) = ^ ^ x l O O A(A)
where A (D): A (A):
Amount of ethanol detected in GC sample (mg) Amount of furnished sample used to prepare GC sample (= 100 g)
3. Results o f Study
______ The results of analysis are given below.
Amount of sample
Amount of
furnished
ethanol detected
(ng) (mg)
GC sample
100
0
Ethanol content
(%) 0
Table Fig. 12
As is apparent from the above table, ethanol was not detected in the GC samples. Accordingly, it would appear that the sample furnished for testing was free of residual ethanol.
Study No. 33620
7
Sanitized. Does not contain IS C ACM Company
Sanrole descrintion
_A
Standardsolution40.0jg/L (ethanol)
57045
Solventblack
n.d.
Sample for GC analysis
n,cL
(1000 tns/Lsolution oftie iterosuppliedbythesponsor)
D 0
Study No, 33620
5F
00
Amountoffl itemsuppliedbythesponsoradded : 100(rog)
A: PeafeflMd((iV-sw) B: Ficaivolume : 10(mL) C: Ratioofportjonused foranalysis ; 10/100 D: Detectedamountofefljanol (mg)
D- G CA/ AOtaodurd}) * ( B/ C)f 1000
E: Percentagecontent ofethanol intheitemsuppliedbyti sponsor(%) ED /100 (rag) x 100
F : Averagepercentage contentofethanolintheitemsuppliedbythe sponsor(%)
G: Concentrationofethanol ofstandardsolution:40.0 (tag/L)
SeeFig, 2
October 8,2003
Name
Study No. 33620
8 Company Sanitized. D oes not contatici T$CA GSi
PKNQ
TIme (Win)
Total
Area
Height
fp.V-gecj tfeVi
0
Cent. (%i
o. 00
ltd.
....................
0,0
g,i0
" m "'11?o.,..o.
Slandard so lstio n 10,C ng/l
,
15.0
Opantar i Tonohtkia Voa^tda
:Operating ie t jui. 29.2003
PKW
Time (mini
1 3. 29
Total
Area (iiV'saet)
'4410
14410
Height Cone. (V) tfc) 1487 100.00
100. 00
i k ..... ........
o' 0 S O !0.'
Standard s o lu tio n 20.0 aig/L
l&O
Operator TomohiKo Yoshirfa
;Operating at Jui. 29, 2003
PKN3
?
Tima
(min)
3.29
Total
Aro* (wY'Soe)
28764
28764
Height Cone.
luV) (Taj
293) roa. 00
100. 00
i
1 IV 0 .0 S.'o
10.0
Standard solution 49. D sig/t
i l ii
i s ! o :Operator Tom'oh ifto Yoshlda
Operating Pat* : Jui. 29. 2003
PKNO l
Tine [wir) . 3.26
Total
Area (iiV-**c)
57611
5761!
Height Gone.
(*V)
(8.)
36S5 100. 00
100. 00
0.' 0
Fie 1 - 1
5. 0
10, 0
15 ,'q
Operator TomohDte Yoshida
C h r u s a t a g m f GC ace ly sis for cal { nation c a m <eibati.al).
Oat* : Jui. 23. 2003
W&roe
Study No. 33620
9 Sanitized, Poes not contaiBljgSftgik
SmdyNo. S3520
yl44Cx r-1.00
Comceatratfon (mg/L) 10.0 20.0 40.0
Peak area (fiV'Bce)
14410 28764 57611
Fig, I - 2 Calibration, curve o f e&sooJ.
October9,2003
Nan
/.
Study No. 33620
l o com pany Sanitized. D oes not contain TSCA CM
PKNO
!
niM
Aren
rwjEmi; m e .
(min) (aV'SOS) (yV)
(%)
3. Sfl 57S5
5776 1OS. 00
Total
S7Bil5
100.00
!
0.0 5.:0_._.___.._______*._._.10.ID
Sazple lor SC analysis
ftakpotiioB
7s] g(min) Operator i Toirwhiko ToshIda
Operating dato : Jul. 29, 2003
PlWO Tin Area Height Cone. Crain) CxiV'aae) (V) {%i
Total
0'
a 00
0. 0 B, 0 TO. 0 i&'ofein) Operator : Tomohlko YoshldO
Solvent 1>1auk
Operating data : Jwl. 29, 2003
PlWO Tima Are* Height Cone, (min) (tfV'see) (V) (X)
Total
0
5.00
fa ap w ittM
A
0,0S" " 11.............. Fig. 2
5,0-- y-- -- i
------ i
j i i ^ -- -- mu
)gp
i i i n ij
IB, pfaln)
Chroiatograa o 6C analysis lor ethanol.
Data t Jui. 29, 2003
Operator Warna i
Tomohlko Yoshirf* /,
Translation: Language Services F. Metreaud December 4, 2003
Study No. 33620
11 Company Sanitized. Does not contain TSCA CM|
