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Xylenes/TEOF coelution problem

Posted: Mon Mar 26, 2012 8:28 pm
by cawarhur
Greetings everyone.

I'm looking at a reaction mixture with xylenes and TEOF (triethyl orthoformate) in solution. We're looking for TEOF in our samples, but the reaction solvent (xylenes) coelutes with TEOF.

Is there a way to derivatize an ether for analysis? Any other suggestions?

Thanks!

EDIT:

Boiling Points:

Xylenes (C8H10): 138.5C
o-Xylene: 144C
m-Xylene: 139C
p-Xylene: 138C

TEOF (C7H16O3): 146C


EDIT: Problem solved. It took a very little bit of method tweaking to get good separation....the method that was previously being used was just awful and I didn't bother checking it before I ran my samples. Yay! :D

Re: Xylenes/TEOF coelution problem

Posted: Tue Mar 27, 2012 12:47 am
by chromatographer1
Change the column you are using. If you using a Methyl Silicone, try a Wax or a 1301 phase.

TEOF is itself a reagent for derivatization.

Use care.

Rod

Re: Xylenes/TEOF coelution problem

Posted: Thu Mar 29, 2012 9:50 pm
by chromatographer1
I would also look at freezing the solution and see if you can effect a physical separation in that manner.

best wishes

Rod