Help! I'm trying to develop a GC method for the purity of methanesulfonyl chloride. The problem is the degradent, methane sulfonic acid, is difficult to detect. I'm using a GC w/FID. I've tried using DB-WAX to separate the peaks. I have not been successful. I've also tried changing the split flow, temperature program, sample size, and column (to ZB-50). Still, I'm not getting the desired results. What are my other options? (Keep in mind, the GC w/FID is the only instrument available. I don't have another GC with a different detector.) I'm open for any other suggestions.
By Anonymous on Sunday, April 13, 2003 - 08:35 am:
The only thing that comes to mind is that both the DB-Wax and the ZB-50 are very polar columns. Have you tried a ZB-1 or ZB-5?
By maris on Wednesday, April 16, 2003 - 06:16 am:
It's not so easy to find a suitable method for quantification of Methansulfonic acid in methansulfonylchloride due to high sensitivity of the last to water and his high reactivity. I preffer to make derivatization of chloride with suitable reagent and than to determine the acid on FFAP or BP 21 columns (many other options available).
By Anonymous on Wednesday, April 16, 2003 - 12:11 pm:
If you derivatize the chloride in the sample, how would you be able to distinguish the free chloride from what is still attached to the Methansulfonylchloride?
By maris on Wednesday, April 16, 2003 - 11:20 pm:
If the derivatization was done properly, no residual methansulfonylchroride should remains (use the excess of derivatization reagent) - i.e. you analyze the mixture of methansulfonic acid and corresponding derivate of methansulfonyl chloride.