Residual solvents analysis of chloro compounds

Chromatography Forum: GC Archives: Residual solvents analysis of chloro compounds
Top of pagePrevious messageNext messageBottom of pageLink to this message  By bhaskar reddy.R on Tuesday, July 9, 2002 - 10:10 pm:

Dear All,

I am facing a ptoblem with chloro compounds(i.e.: 3-methyl-4-(2,2,2-trifluoroethoxy)-2-chloro methyl pyridine hydrochloride.)
When I am injecting the sample in to the injector, the compound is degrading and one of the fragments of the compound are eluting in the Residual solvents analysis. Can any one give the solution, how to overcome this problem.We identified the degradants by GC-MS also.


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Anonymous on Monday, July 15, 2002 - 06:48 am:

Hello Bhaskar,

My organic chemistry is really rusty but how about if you converted the hydrochloride to the free base before testing, you might not get any breakdown. I realize there is a dilution effect then, but you might be able to see the analytes.

Regards,
Mark


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Rod on Monday, July 15, 2002 - 08:44 am:

Several things can be tried.
Lower your injection temperature and find another volatile solvent instead of the (water??) solvent you are using now. Your solvent or temperature may be the primary cause of the reaction.
You may have a reactive injection liner, or the metal needle may be part of the problem.
Do the residual solvent analysis by headspace, preferably automated, or use Solid Phase Micro Extraction (SPME). (yes, I work for Supelco)
A cool on column sample injection may be a solution.
Good luck
Rodney George
Senior Research Chemist Gas Separations
Supelco


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