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Chemistry Forums for Students => Analytical Chemistry Forum => Topic started by: sparky on February 07, 2005, 02:22:44 PM

Title: Assay fo 1,3,5 Trioxane
Post by: sparky on February 07, 2005, 02:22:44 PM

I'm trying to develop a method to analyze 1,3,5 trioxane for assay.  I have considered dissolving the trioxane in chloroform and analyzing by gc but I have a few concerns.  My first concern is that there may be high boilers that don't elute on the method.  My second concern is that the trioxane may break down to formaldehyde.  Another idea I had was to dissolve the trioxane in water, add ammonium nitrate which will react with any free formaldehyde and form nitric acid which will in turn force the trioxane to formaldehyde which will again react with ammonium nitrate to form nitric acid.  I will then titrate the acid with a base solution.  Any ideas?

Title: Re:Assay fo 1,3,5 Trioxane
Post by: movies on February 07, 2005, 03:51:18 PM

How about just taking an NMR?

Title: Re:Assay fo 1,3,5 Trioxane
Post by: sparky on February 09, 2005, 11:35:57 AM

Thanks for the suggestion, but I don't have access to a NMR.  I could send the sample out for NMR but that wouldn't help because I need a routine test method.

Title: Re:Assay fo 1,3,5 Trioxane
Post by: Mitch on February 09, 2005, 12:21:16 PM

Just run a known standard of trioxane and formaldehyde through a GC, a GC-MS preferably.

Title: Re:Assay fo 1,3,5 Trioxane
Post by: sparky on February 10, 2005, 08:15:33 AM

I have tried this an it seems to work if I dissolve the trioxane in acetone.  Since trioxane is a solid, I was concerned that there may be high boiling impurities that don't elute by GC.

Title: Re:Assay fo 1,3,5 Trioxane
Post by: Mitch on February 10, 2005, 11:53:23 AM

You would only have to worry abot column clogging if the MW gets above 1000 or so.