GC/MS analysis of tert. amine

Chromatography Forum: LC-MS & GC-MS Archives: GC/MS analysis of tert. amine
Top of pagePrevious messageNext messageBottom of pageLink to this message  By Anonymous on Sunday, February 27, 2000 - 02:55 pm:

We just received a new column for the analysis of diethanol alkylamines(Restek 5-amine). However, we are unable to reproduce results when the same sample is injected twice. The area counts are all over the place with no obvious trend. We also replaced the inlet liner, and we can't think of any other places where the compound might adsorb to.
Does anybody have any experience with this kind of column, this kind of analysis or any other suggestions of what could be going on here. I appreciate any help I can get.


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Ron S. on Monday, February 28, 2000 - 08:49 am:

Did the analysis give reproducible results before you changed the column? If it did, then either there is a problem with the column or with some other system component which was changed, adjusted, or removed and replaced when the column was changed. If this is the first time the analysis has been performed, then recheck all the basics: not just new liner, but properly deactivated, if using HP GC check the seal at the base of a split/splitless port, and through leak checking of the entire system. If you are using an autoinjector, check or replace the syringe in case it is worn.

The type of injection being used and the solvent used are not listed above. If a splitless injection is being performed using a solvent with a large expansion volume, verify you are not exceeding the capacity of the liner and having flashback. This is a problem with alcohols, acetone, and especially water. If exceeding the liner volume is your problem, reduce the injection volume and the problem should disappear.


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Anonymous on Sunday, May 9, 2004 - 06:40 am:

how do u reproduce results in gas chromatography


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