• 7 •
800-356-1688 •
2004vol. 3
Figure1
Stop-FlowGCprovides a rapid, sensitiveanalysis for ICHClass I andClass II residual solvents.
1. 2-methylpentane
2. hexane
3. 1,1-dichloroethene
4. methyl cyclopentane
5. methanol
6.
trans
-1,2-dichloroethene
7. carbon tetrachloride
8. methyl cyclohexane
9. methylene chloride
10. 1,1,1-trichloroethane
11. benzene
12. 1,2-dimethoxyethane
13.
cis
-1,2-dichloroethene
14. trichloroethene
15. acetonitrile
16. chloroform
17. 1,2-dichloroethane
18. toluene
19. 1,4-dioxane
20. nitromethane
21. 2-methoxyethanol
22. 2-hexanone (MBK)
23.
p
-xylene
24.
m
-xylene
25. pyridine
26. 2-ethoxyethanol
27.
o
-xylene
28. chlorobenzene
29. 1,1,2-trichloroethane
30. dimethyl formamide (DMF)
31. N,N-dimethylacetamide
32. 1,2,3,4-tetrahydronaphthalene
33. formamide
34. 1-methyl-2-pyrrolidinone
35. sulfolane
* impurities in solvent
Headspace Conditions
Instrument:
Teledyne Tekmar 7000HT high temperature static
headspace unit
Platen temp.:
140°C
Sample equilibration:
5min.
Mixing time:
10min.
Mixing power:
2
Mixture stabilization:
1min.
Pressure time:
0.2min.
Pressure equilibration:
0.3min.
Vial vol.:
22mL (high temperature vials)
Sample loop vol.:
1mL (standard size, Silcosteel
®
treated)
Loop/line temp.:
250°C
Loop fill time:
0.1min.
Loop equilibration:
0.05min.
Inj. time:
1.0min.
Static vial press.:
3.5psi helium
Vial press.:
8psi helium
Variable inj. press. (VIPR):
5psi helium
Interface:
plumbed through injection port, 1:20 split
GCConditions
Column #1:
Stabilwax
®
, 15m x 0.25mm x 0.5µm (cat. # 10635)
Column #2:
Rtx
®
-200, 30m x 0.25mm x 1.0µm (cat. # 15053)
Sample:
200ppm each component in 1,3-dimethyl-2-imidazolidinone (DMI)
Instrument:
Agilent 6890
Inj. port temp.:
250°C
Carrier gas:
helium, constant flow
Flow rate:
1.9mL/min., 25.6psi @ 40°C
Oven temp.:
40°C (hold 2min.) to 55°C@ 4°C/min., to 110°C@ 25°C/min.
(hold 2min.) to 250°C@ 25°C/min. (hold 5min.)
Det.:
FID #1 at column junction, FID #2 at sample outlet
(equal settings)
Det. temp.:
250°C
Reaction gas:
hydrogen, 40mL/min.
Air flow:
400mL/min.
Makeup:
helium, 40mL/min.
Data collection rate:
100Hz
Stop-FlowConditions
Instrument:
Restek Stop-FlowSystem for Agilent 6890GC
with cool on-column EPC (cat. #21168)
Inj. port connection:
cool on-column injector
Pressure:
31.0psi, constant pressure
Pulses:
valve opened 3.00 - 3.15min., 4.65 - 5.02min., 5.10 - 5.40min.
Total analysis time:
20.55min.
GC_PH00744
solvent (DMI)
