Document QkxnN29pg9wpDv4J6mZ7nyyk5
M M _ 3-
DuPont Haskell Laboratoiy for Health and Environmental Sciences
FROM: J. C. MASLANKA
August 5,2002 cc: G. A. Ladies
Medical Research Project Number: Haskell Sample Number: Analytical Test Code: Analytical Report Number:
Notebook References:
H2469 ~
CM 1 HA-2002-050
Attached is the analytical report, satisfy protocol requirements foj
identified above. This analysis was performed to out may also be used for other purposes.
Company Sanitized. Does not contain TSCA CBI
TEST SUBSTANCE STABILITY O
Medical Research Project Number: Haskell Sample Number: Analytical Report Number:
HA-2002-050
SUMMARY
A sample o |
[vas received February 12, 2002,
15, 2OO3
ge o f active ingredient (a.i.) was measured to b
range of
for replicate analyses (n = 3). The sponsor reported a purity
when sample was submitted.
SIGNATURES:
Analysis by:
jJl '(xplI /U f t *__n i l e d
Sheila A . R iley u
Chemistry A ssociate
Report by :
Senior Staff Chemist
SD ate
- cZt>0 z S D ate
Date issued:
tJLO oSU no!
C o m p a n y Does
on
HA-2002-050 page 2 o f 3
METHODS
Analysis for the percentage o f a.i. in a sample o: chromatography (GC). Sonication in methanol was require internal standard and analytical standard stock to ensure tha completely dissolved.
s performed by gas o f test subitanee:
as
SAMPLE PREPARATION & ANALYSIS
Aliquots (0.0294, 0.0318, 0.0317 grams) o | j j ^ B B B B B ^ | [ E J J w ere dissolved in methanol (100 mL) to give nominal concentrations oi294, 318, and 317 ppm rT he aliquots were further diluted to a nominal concentration o f 22.1, 23.9, 23.8 ppm, respectively, and analyzed according to the following method.
INSTRUMENT & CONDITIONS
Instrument:
Hewlett-Packard Model 6890 GC
Column:
J&W DB-1701, 30 M, 0.32 mm ID, 1.0 pm film thickness
Injector:
Split, 250C
Detector:
FID; 250C
Carrier Gas:
Helium (2.1 mL/min)
Split vent:
22.3 mL/min
Injection Volume:
2 microliter
Oven Program:
Gradient
Initial Temperature: 100C
Initial Time:
1.0 min.
Level 1 Rate:
20C/min.
Level 1 Temperature: 260C
Level 1 Time:
0.00 min.
Total run time:
9.00 min.
CALIBRATION & QUANTITATION c. C alibration and Q uantitation
An analytical standard 1H, 1H, 2H, 2H-Perfluorodecan-l-ol (H22703-171, purity 97.6%) was purchased from Fluorochem USA for the analysis. A stock solution w as prepared in m ethanol. This stock solution w as sonicated to assure that all m aterial w as in solution. Calibration solutions o f approximately 10.15 to 40.60 ppm were prepared in methanol. A stock solution o f internal standard (1H, 1H, 2H, 2H-perfluoro-9-m ethyldecan-l-ol, 98% pure) w as prepared in m ethanol and added to each calibration standard and le s t solution to give final concentration o f 41 ppm. The ratio o f the internal standard anc peak heights from replicate GC analysis o f these solutions were usedTo construct a calibration curve by least squares regression. M easured concentrations for each purity solution w ere determ ined by applying the peak height ratios from replicate injections o f each sample to the calibration curve.
Company Sanitized. Does not contain TSCA Cf
HA-2002-050 page 3 of 3
RESULTS
'approximately 3.5 mini submitted.
fluted from the GC column as res The sponsor reported a purity
Table 1. The percent of a.i. in th<
with a retention time o f hen the sample was
zed February 15, 2002,
1 22.1 2 23.9 3 23.8
Average Percent Nominal Standard Deviation Coefficient o f Variation
21.7 23.8 23.7
98.2 99.6 99.6
99.1 0 .8 1 0.8%
c o n t a in
sd, Oos n 0 `
