Trimethyl phosphate, dimethylbutyl phosphate, methyldibutyl phosphate and tributyl phosphate were determined by use of an FID and a 10 ft × ¼ in. stainless steel column containing 60/80 mesh siliconized glass beads coated with 0.15 wt % Carbowax 20M. Samples were obtained by methylation of the degradation products of tributyl phosphate resulting from attack by nitric acid and/or 60Co irradiation.