Hi,

I'm have problems with analyzing epichlorohydrine by GC-MS. I currently use the following equipment/method:

Matrix: diisopropylether
Column: Macherey-Nagel Optima 5MS (95% DMPS, 5% DVB) (almost non-polar), 60m/0,25µm/0,25mm
Inj.-Temperature: isothermal 40 °C for 20 min., then 10°C/min to 250°C
Carriergas: Helium
Flow: about 25 cm/s
Split-ration: 1:10

I already tried by variing the temperature program but don't get good results. Next I removed the glass-wool of the liner - no effect. I finally managed to get a peak of epichlorohydrine, but it is very poor (about 70000 detector counts with 10 µm/ml), too poor to be satisfied.

Has anybody an idea what's possibly going wrong? Do I use the wrong column or is it too long?
Thanx for any hints!

- Christian (chemie@cschad.de)

epichlorohydrin is of course very reactive. You may need a completely deactivated column, no glass wool or things like this.

Something that sometimes works is to inject a ton of epichlorohydrin. Hopefully, it will react with all active sites, and then you can run your analysis without trouble for a reasonable time.

Please do not ask, what "a ton of epichlorohydrin" means or wherefrom you can get a ton! :-))

I suggest you try a column from a different vendor after making certain your ether does not contain peroxides.

I think epichlorohydrine should better be analysed using a more polar column like Optima 624 (cyanopropyl-phenyl-dimethylpolysiloxane). You can find applications on different vendor`s pages (M&N, Agilent.......).Furthermore You could try to do a purge and trap step.