Abstract: This paper reported Gas Chromatographic procedure for. separating, and determining 12 organophosphorus pesticide residues in Water, soil, rice, beverage and vegetables. The detector FPD Was equipped with 526 nm filter. A glass column (φ>3.2mm×2.1m) filled with statiaary phase OV-17 1.5%+QF-1 1098% coated onchromasorb W.AW.DMCS with 80-100 meshes was used. A two-step temperature prpgram, of column Was conducted. This model offered excellent presicion and high sensitivity. Typical MDQ. ranged from 10^-12 to 10^-13 g, resolution ranged from 0..8 to 3.5.A method of simultansously extracting 12 OP pesticide residues from any sample of Water, soil, rice, beverage or vegetable Was also introduced. Average recoveries were greater than 90% and sensitivities over 0.020 ppm. This method proved to be quick and economical.