Abstract: Electrochemical behavior of phoxim was studied by single sweeping polargraphy. It was found that the adsorptive wave of complex of titan yellow and Tween-80 was inhibited by phoxim in a PBS of pH 6.7. Based on this reaction, a single sweeping polargraphic determination of phoxim was proposed. Linear relationship between values of peak current and mass concentration of phoxim was obtained in the range of 0.009 4-28.22 mg·L-1, with detection limit (3s/k) of 0.008 6 mg·L-1. The proposed method was applied to analysis of samples of grain and soil, giving values of recovery in the range of 94.6%-105%.