A gas-liquid chromatographic technique has been developed to separate and detect, simultaneously, some organophosphate pesticides, their oxons, and hydrolysis products. Reoplex-400 (polypropylene glycol adipate), a polyester liquid phase, was used to separate the organophosphate systems of Diazinon, Baytex, parathion, and malathion. Two detection systems were used-flame ionization and electron-capture. Isothermal separations at 180°C. are described for individual systems of Diazinon. Baytex, and parathion. Also chromatograms and relative retention times indicate multiple analyses of these three pesticides, their hydrolysis products, malathion, and the oxons of parathion and Diazinon. Data are given under isothermal conditions which indicate the generally greater sensitivity of the electron-capture system except for the hydrolysis products of Diazinon and Baytex. The malathion system was examined with the flame ionization detector by techniques of dual isothermal analysis or programmed temperature.At present, there is an incomplete picture of the persistence l_ and fate of organophosphate pesticides in natural water environments. These pesticides have the potential of causing changes in water quality which may affect human and aquatic life. Their toxicity to fish and wildlife is well known. Breidenbach (1965) has outlined other water quality problems caused by organic pesticides.