Abstract: In a B-R buffer solution of pH 2.21,with 0.1 mol·L-1 KCl solution as supporting electrolyte,a sensitive reductive wave of phoxim was found at the potential of -0.72 V (vs.Ag/AgCl electrode).Linear relationship between the peak current (Ip) and concentration of phoxim was obtained in the range of 4×10-5-8×10-4mol·L-1,with the scanning rate of 100 mV·s-1.In analyzing a sample of phoxim for 6 times,an average value of 3.42% was obtained with its value RSD 1.7%.Test for recovery was made by the standard addition method,and values of recovery obtained were in the range of 98.6%-103.6%.The mechanism of the electrochemical reduction of phoxim at the glassy carbon electrode was proved to be an irreversible process.