Assay residual process solvent

Chromatography Forum: GC Archives: Assay residual process solvent
Top of pagePrevious messageNext messageBottom of pageLink to this message  By gensun on Monday, September 9, 2002 - 11:26 am:

Need some expertise here: I need to assay the residual isobutanol (as process solvent) in an anthracenedione dye-base (b.p. >300C). People here suggested me for head space extraction. Any help will be grateful! Thanks


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Anonymous on Monday, September 9, 2002 - 12:16 pm:

Likely you could use anywhere from polar (Carbowax-type) to nonpolar methyl silicone-type capillary for this and be OK.


Top of pagePrevious messageNext messageBottom of pageLink to this message  By gensun on Monday, September 9, 2002 - 12:37 pm:

Thanks for the response. But is there a way to quantify the residual solvent? I'm thinking if I use head space extraction then I can only say if isobutanol is present or not right?


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Rod on Monday, September 9, 2002 - 01:44 pm:

I suspect that Dimethylacetamide will dissolve your dye, or DMSO.

Headspace will do a very good job of measuring the isobutanol down to the single digit ppm or less levels.

If you wish to measure 100ppm or more you may use manual methods as well using an internal std.

I have determined isobutanol in DMSO and DMAc solutions.

See the June Issue of Analytical Chemistry 1997 p 2221-p2223.

I would use n-propanol as an Int Std.

Be aware that dyes are not always homogeneous in amounts of residual solvent found. Use a large amount to dissolve to minimize this problem, or take small amounts from various locations of the drying tray or storage bottle.

Email me if you have any questions.

Rodney George
Senior Research Chemist
Gas Separations Research
Supelco
595 North Harrison Road
Bellefonte, PA 16823

814-359-5737 voice
814-359-5702 fax
rgeorge@sial.com


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