Consumer Products Guy wrote:
I used trimethylsilylation a lot for GC and GCMS of hydroxy groups. Typically I used DMF or pyridine as solvents, and added BSTFA as the silylation agent to the autosampler vial. Silylation was practically instantaneous.
When I had to silylate an amine, I used pyridine, BSTFA, and heated in a sealed autosampler vial 10 minutes.
Sorry to resurrect this old thread.
I am working on a general large chain and nonvolatile, and hydroxy acids method using BSTFA or BSTFA+TMCS.
I have done silylation in the past using pyridine dried with NaOH. I saw some issues with calibration linearity when operating from 10-1000ppm that improved when I reduced it from 1-100ppm instead. I have been reviewing the literature and found one that recommends using DMF
https://www.lmaleidykla.lt/ojs/index.ph ... /4100/2989 and reviewing the literature and Daniel Knapp's book of Analytical Derivatization Reactions I see there is conflict in the literature about whether pyridine helps or actually inhibits the reaction. There is also conflict as to whether a base is necessary (which pyridine is) like triethylamine or not in other solvents.
Did you see major differences between DMF and Pyridine?