An amorphous Pd33Ni60P7 alloy was prepared by electrodeposition in a bath containing 0.02 mol L-1 PdCl2, 0.04 mol L-1 NiSO4 center dot 6H(2)O, 0.24 mol L-1 H3PO3, 0.32 mol L-1 H3BO3, and 0.08 mol L-1 ethylenediamine (C2H8N2), under conditions of pH 4.0, 50 degrees C and 25 mA cm(-2). The amorphous structure of the Pd33Ni60P7 deposit was confirmed with X-ray diffraction (XRD) analysis. The activity of electrocatalytic reduction of nitrate on the amorphous Pd33Ni60P7 deposit was studied with cyclic voltammetric (CV) technique in a neutral 0.1 mol L-1 KClO4 solution with or without KNO3. The results indicate that the Pd33Ni60P7 alloy deposit exhibits a higher activity for the reduction of the nitrate in comparison with the electrodeposited films of Pd, Ni and Pd-Ni, which could be owing to its amorphous structure. The reduction reaction of NO3-; on the electrode is a totally irreversible process. (C) 2008 Elsevier B.V. All rights reserved.