A gas chromatographic system employing a Flame Photometric Detector (GC/FPD) was used to develop a method for the determination of Dimethyl methylphosphonate (DMMP), Diisorpropyl methylphosphonate (DIMP) and Trimethyl phosphate (TMP) in aqueous samples under Task R902.35.14. The precision and accuracy of the developed method was determined from the analysis of aqueous samples spiked with 4.92 to 98.40 micron g/L of DIMP in the presence of 10 mg/L each of DMMP and TMP. The detection limit at the 90% confidence level, calculated by the method of Hubaux and Vos, is 9.05 micron g/L of DIMP in the presence of 10 mg/L each of DMMP and TMP. (Author)