A novel method for the determination of palladium in synthetic nuclear waste samples has been developed using a computerized voltammetric analyzer. The electrode system consists of hanging mercury drop electrode (HMDE)/glassy carbon/Ag–AgCl electrode. Various experimental conditions including electrolyte type, pH and concentration have been optimized, leading to a detection limit of 40ng/ml. The mixture of 4.10^–3M citric acid + 2.10^–2 M ammonia-ammonium chloride buffer + 4.10^–3 M EDTA was used as a supporting electrolyte at pH 9.0. Standard addition method was employed to determine the concentration of palladium present in the nuclear waste sample. The relative standard deviation of the proposed method was found to be 8% at 40ng/ml of palladium content. The method is direct, simple, rapid and free from any possible interference.