Poly (m-toluidine) (PMT) was formed by successive cyclic voltammetry in a monomer solution containing Triton X-100 (TX-100) at the surface of carbon paste electrode (CPE). Nickel was then incorporated into the polymer by electrodeposition of Ni(II) from NiSO4 acidic solution. The electrochemical behavior of this modified electrode (Ni/PMT(TX-100)/MCPE) was investigated in the electrooxidation of ethylene glycol (EG) using cyclic voltammetry and chronoamperometry techniques. Among the electrodes [Ni/PMT(TX-100)/MCPE, Ni/PMT/MCPE, Ni/MCPE, PMT(TX-100)/MCPE, and CPE] used in this study, Ni/PMT(TX-100)/MCPE showed the most effective catalytic activity. The effects of various parameters such as film thickness, electrodepositing time, TX-100 concentration, MT concentration, and EG concentration were investigated on the electrocatalytic oxidation of EG at the surface of Ni/PMT(TX-100)/MCPE. The catalytic rate constant (k) for EG oxidation was also calculated to be 2.1 x 10(6) cm(3) mol(-1) s(-1) using a chronoamperometric method.