This is a first report on the synthesis of nickel phosphate nanoparticles (N-NiPh) from its precursors using a reflux-based route at 90 degrees C and its use for destruction and conversion of urea (a biochemical species) to useful fuel (H-2 gas). The prepared particles are characterized by different techniques including: X-ray diffraction (XRD), scanning electron microscopy (SEM), FTIR spectroscopy and BET surface area determination. The particle size is found to have an average value of similar to 70 nm with surface area of 22.3 m(2)/g. According to the XRD pattern and FTIR spectrum, the obtained phase structure of the NiPh nanoparticles is Ni-3(PO4)(2)center dot 8H(2)O with a monoclinic crystallographic form. Using cyclic voltammetry (CV) (and also EIS), the N-NiPh modified glassy carbon electrode (GC/N-NiPh) is activated upon potential cycling in 0.5 M KOH for 75 cycles. This is obtained at the maximum attainable enrichment of the N-NiPh surface by Ni(II)/Ni(III) species. The GC/N-NiPh shows superior electrocatalytic activity towards urea oxidation from alkaline solution compared to the corresponding Ni(OH)(2)-based electrodes. The oxidation process is analyzed in the light of the measured and collected electrochemical data. (C) 2016 Elsevier B.V. All rights reserved.