ADV01-05_1-298

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800-356-1688 •

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2004 vol. 3

Figure 1

Stop-Flow GC provides a rapid, sensitive analysis for ICH Class I and Class II residual solvents.

1. 2-methylpentane

2. hexane

3. 1,1-dichloroethene

4. methyl cyclopentane

5. methanol

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.

-xylene

24.

-xylene

25. pyridine

26. 2-ethoxyethanol

27.

-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:

5 min.

Mixing time:

10 min.

Mixing power:

Mixture stabilization:

1 min.

Pressure time:

0.2 min.

Pressure equilibration:

0.3 min.

Vial vol.:

22mL (high temperature vials)

Sample loop vol.:

1mL (standard size, Silcosteel

treated)

Loop/line temp.:

250°C

Loop fill time:

0.1 min.

Loop equilibration:

0.05 min.

Inj. time:

1.0 min.

Static vial press.:

3.5psi helium

Vial press.:

8psi helium

Variable inj. press. (VIPR):

5psi helium

Interface:

plumbed through injection port, 1:20 split

GC Conditions

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 2 min.) to 55°C @ 4°C/min., to 110°C @ 25°C/min.

(hold 2 min.) to 250°C @ 25°C/min. (hold 5 min.)

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-Flow Conditions

Instrument:

Restek Stop-Flow System for Agilent 6890 GC

with cool on-column EPC (cat. #21168)

Inj. port connection:

cool on-column injector

Pressure:

31.0psi, constant pressure

Pulses:

valve opened 3.00 - 3.15 min., 4.65 - 5.02 min., 5.10 - 5.40 min.

Total analysis time:

20.55 min.

GC_PH00744

solvent (DMI)