The advantageous features of polymer modification and dispersion of metallic particles into the organic polymer was studied by construction of poly ortho-anisidine (POA) film and Ni(ΙΙ) were used in combination with POA films by immersion of the glassy carbon modified electrode in Nickel ions solution. This modified electrode exhibits good electrocatalytic activity toward the electrooxidation of hydrazine and has been studied by cyclic voltammetry (CV) and chronoamperometry techniques. The oxidation of hydrazine is occur at a potential about 140 mV less positive than that at unmodified electrode. The electron transfer coefficient (α) was determined and the electrocatalytic oxidation peak current of hydrazine showed a linear dependent on the hydrazine concentration and a linear calibration plot were obtained in the range of 5×10 -5 M-1.4×10 -2 M with cyclic voltammetry method. The detection limit (2σ) were determined as 3.9×10 -5 M.