Chromatography Forum

So our team has recently begun doing reactions in TOA. (Tri-n-octylamine, just in case.) This stuff is an absolute nightmare for me as it just sticks to anything and everything it comes into contact with. We have several analytes in the samples that all need to be quantitatively analyzed and I need to complete a standard procedure for doing so. Extracting into a better background medium is not really an option and the idea of running these samples through any of our instruments keeps me up night. Does anyone have any tips on dealing with TOA using GC/FID analysis?

Is this a trace analysis? I've never handled TOA so I am a little surprised that it's so misbehaved. Usually, it's the primary and secondary amines that are the biggest headaches. I have never been troubled by tertiary amines. What are your other analytes? Have you given SPME a try? C24 is a little heavy for headspace analysis but perhaps you could simply dissolve your sample in some water and immerse the fiber in the aqueous sample to pull out your analytes?

If it was trace, I think it would be quite easy to deal with. Problem is that it makes up about 90% of the background matrix, so a majority of my sample is TOA. This is what makes it so difficult. In small amounts I'm sure it would be easy to quantify. Trace would be very easy as well, seeing as it is big and fragments well under mass spec.

Thank you for the suggestions, as well. If it was in a trace amount, I would imagine that SPME would be a great choice. I don't think it would fly too well with headspace analysis, TOA is pretty heavy.

For now I guess I will just have to forego quantification of the TOA for GC, it does run fairly nice through the LC, might be able to pull the data using DAD if it absorbs in a good area. Anyone know if there is wavelength for TOA in UV/Vis?

Yep. Too bad. Why is it that you can't simply "dilute and shoot"? I think you'll have a hard time coming up with a single procedure that can give you low concentrations of things as well as the TOA. Good luck!