Chromatography Forum

Hello everyone,

I have recentlly been asked to start reporting Epichlorohydrin by EPA method 524.2. The detection limit we are trying to hit is 0.4 ug/L running on a 6890/5973 GC/MS system using an RTX-VMS 20m x 0.18 column and purging 25ml sample volume. I am so far having no luck getting even close to that detection limit and was wondering if anyone has had any success with this analyte and what kind of set up they are using or if there is any guidance anyone may can provide to achieve a lower limit. I am about at my wits end with this so far so any help would be appreciated.

Thanks

Hi

Not really familiar with this EPA method but is it really supposed to be used for Epichlorohydrin? As I recall one adjust pH to like <2 with HCl which potentially is a great way to split up the target molecule into 2 alcohols (ie reversing the synthesis of epichlorohydrin).

Have work with trace analysis a long time ago, might be able to dig something up when back at work.

Have you worked only with diluted standards (prepared how?) or are you refering to spiked samples (how is sample prepared)?

524.2 is basically a purge and trap volatiles by gc/ms, it isn't really the best method for this analyte but it is how I am being asked to report it so trying to see what I can do and I am not sure if I am just spinning my wheels at this point.

With that said, so far I am only working at a standards level. Starting with a stock standard of 2000 ug/ml in MeOH, diluting that down to 100ug/m in MeOH, and making a work standard at a concentration of 50ppb in Di H2O. From there I am purging 25 ml on the instrument. I have tried to run concentrations up to 100 ppb and have not had any luck seeing anything.

I have not run any end user samples yet, as I am just in the research stage at this point.

Hi Jinxwolf

Sorry, when back at work it turned out I had worked with trace analysis of a reaction product originating from epichlorohydrine and another reactant plus a biproduct.

So I do not think I can help you further.