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Abnormal peak shape

Posted: Wed Jun 24, 2020 6:39 pm
by BrieGalb
Hello everyone, I am currently using an Agilent 7890A GC System with a HP-5MS column to analyze acrylamide (2-propenamide as listed in the analysis library) in solution with predominately methanol and a very small amount of water. I used to run these samples (without methanol - just acrylamide and water) on an older GC-FID with a wax column and that worked great. However, I am getting a gradual build-up to my peak that lasts almost a minute. I found one protocol that was able to create peaks with this same setup and am using the same method. I was thinking the concentration is too high but it is a relatively short peak. I'm assuming it has something to do with my polar compound and this column, however this is the column I have to use (ah!).

I have a picture to post but am also struggling with how to do that. Oh me.

I have been trying to look online but am not finding any help as to what this not ideal peak shape is telling me about my runs. Anyone have any ideas?

Thank you so much in advance,
Brie

Re: Abnormal peak shape

Posted: Wed Jun 24, 2020 9:33 pm
by Gizmo
I recall when looking into acrylamide analysis via GCMS that either derivitization was necessary with a non-polar column or that a more polar column was needed. Maybe look into derivatizing with bromine?

Re: Abnormal peak shape

Posted: Wed Jul 01, 2020 1:57 pm
by BrieGalb
I will look into that.

I had found an agilent experiment/protocol where they were able to analyze acrylamide without derivitization using a 5ms column. The retention times varied (by very small amounts) but they were able to get picture perfect peaks. I am using the same method so wondered if something was "off" with the GCMS.

Thank you for your thoughts!