AbstractFatty acids can be conveniently derivatized in less than one minute with (chloro)alkyl chloroformates such as methyl chloroformate, 2‐chloroethyl chloroformate and 2,2,2‐trichloroethyl chloroformate. 2,2,2‐Trichloroethyl chloroformate is the most reactive reagent, and yields a reaction product which can be sensitively detected by GC ECD (detection limit 50 ng/ml,i.e.25 pg/injection, for C8, C10, and C12acids).In non‐aqueous media 3‐picoline,N‐methylpiperidine, and dimethylaminopyridine show catalytic activity comparable with that of pyridine and can, therefore, replace it.N‐methylpiperidine is the best basic catalyst in aqueous media (i.e.media containing up t