697
GCCHROMATOGRAMS |
PHARMACEUTICAL
Organic Volatile Impurities/Residual Solvents
GC_PH00951
ResidualSolventsClass1
Stabilwax® (G16)
Column:
Stabilwax
®
, 30m, 0.32mm ID, 0.25µm
(cat.# 10624)
Sample:
USP StockMixtureUSP<467>Residual
Solvents Class 1Mix (cat.# 36279) in
20mL headspace vial (cat.# 24685),
water diluent
Inj.:
headspace injection (split ratio 1:5),
2mm splitless liner IP deactivated
(cat.# 20712)
Inj. temp.:
140°C
Carrier gas:
helium, constant flow
Flow rate:
2.15mL/min., 35.2cm/sec.
Oven temp.:
50°C for 20min. to 165°C@ 6°C/min.
(hold for 20min.)
Det.:
FID@ 250°C
Headspace Conditions
Instrument:
Overbrook Scientific HT200H
Syringe temp.:
100°C
Sample temp.:
80°C
Sample equil. time.: 45min.
Injection vol.:
1.0mL
Injection speed:
setting 8
Injection dwell:
5 sec.
1. 1,1-dichloroethene
2. 1,1,1-trichloroethane
3. carbon tetrachloride
4. benzene
5. 1,2-dichloroethane
GC_PH00952
ResidualSolventsClass2MixA
Stabilwax® (G16)
Column:
Stabilwax
®
, 30m, 0.32mm ID, 0.25µm
(cat.# 10624)
Sample:
USP Stock Standard Residual Solvents
Class 2Mix A (cat.# 36271) in 20mL headspace
vial (cat.# 24685), water diluent
Inj.:
headspace injection (split ratio 1:5), 2mm
splitless liner IP deactivated (cat.# 20712)
Inj. temp.:
140°C
Carrier gas:
helium, constant flow
Flow rate:
2.15mL/min., 35.2cm/sec.
Oven temp.:
50°C for 20min. to 165°C@ 6°C/min.
(hold for 20min.)
Det.:
FID@ 250°C
Headspace Conditions
Instrument:
Overbrook Scientific HT200H
Syringe temp.:
100°C
Sample temp.:
80°C
Sample equil. time.: 45min.
Injection vol.:
1.0mL
Injection speed:
setting 8
Injection dwell:
5 sec.
1. cyclohexane
2. methylcyclohexane
3.
trans
-1,2-dichloroethene
4. tetrahydrofuran
5. methanol
6. dichloromethane
7.
cis
-1,2-dichloroethene
8. acetonitrile
9. toluene
10. 1,4-dioxane
11. ethyl benzene
12.
p
-xylene
13.
m
-xylene
14.
o
-xylene
15. chlorobenzene
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Mar 2011
