Abstract: Single-sweeping oscillopolarography was applied to the determination of chlordiazepoxide. A polarographic reductive wave of chlordiazepoxide was observed at -1.25 V in an ammoniacal buffer medium of pH 10.2±0.1. Linearity was kept between the 2nd derivative of peak current (I″p) and the concentration of chlordiazepoxide and in the range of 1.6×10-7-2.4×10-5mol·L-1 (r=0.999 3,n=8),with a detection limit of 2.0×10-8mol·L-1. In its application to the analysis of chlordiazepoxide tablets,results obtained were in consistency with the results found by HPLC. Value of RSD′s (n=8) of this method was found to be 0.56%. Recovery test was performed and results obtained were in the range of 96.4%-102.1%. A study on the electrochemical behavior of chlordiazepoxide was also made and a brief discussion was given.