Triethanolamine analysis

[g-star]

Hi,

I am attempting to do quantitative analysis of triethanolamine (extracted from industrial fluids by ion exchange SPE) by split injection GC/FID on an RTX-35 amine column.

Reproducibility of standards is very bad. I have eliminated injection as a source of error, and other ethanolamines don't seem to behave so badly. My calibration curve is poor, and area counts jump for a single standard by a great deal.

This just doesn't make any sense to me....does anybody have ideas or suggestions????

Thanks!!

[Consumer Products Guy]

Amines can be tough under any conditions, and triethanolamine is very polar. Dissolve the sample in DMF, filter if cloudy. Mix a portion with equal amount of BSTFA derivatizing agent. Use split injection, DB-1 or DB-5 type capillary column, program from somewhere about 80C up to like 240C at 10C/minute; do this way or determine what temperature you need for isothermal GC. I've done this assay this way for years, the three hydroxy groups will derivatize.

[dpr]

Not sure what concentrations your looking at but I've succesful
used CP Sil 8CB capillary column with the following conditions
90°C for 10 mins then 8°C/minute to 240°C for solutions of Mono, Di and Tri ethanolamine.

A 25 times dilution in MeOH and an area % method gave good repeatability.