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Topic: GC and amines; problems with fronting and tailing  (Read 8323 times)

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Offline mir

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GC and amines; problems with fronting and tailing
« on: July 05, 2006, 01:26:47 PM »
I am running I really good synthesis of an nitroaryl with from an aminoprecursor. And to save time and money, I do it microscale. that means TLC is no good to detect the extent of the reaction and GC is only option (as far as I can see).

My chromatogram is showing extensive "fronting and tailing" on all peaks. The instrument have an unpolar column. Is this effect because of that amine is a base? May injection method (manually) cause fronting and tailing?
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Offline lemonoman

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Re: GC and amines; problems with fronting and tailing
« Reply #1 on: July 05, 2006, 10:38:44 PM »
Depending on what your nitroaryl is, it could definitely be an interaction with the column.

Most of the amine work I've seen done with GC...the amine compound has to be derivatized before you do GC work on it.

"Amines in general are difficult to analyze by Gas Chromatography (GC) due to their lack of volatility and their interaction with the GC column often leading to significant tailing and poor reproducibility."

- From Analysis of Biogenic Amines by GC/FID and GC/MS by Laura Nakovich (it's a thesis paper).  A good discussion of Amine Derivatization starts at the bottom of Page 3 of the thesis (which is page 15 of the PDF document)

Hope that helps...if you continue to encounter problems, let us know :D

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