The study of the electrochemical oxidation (ECO) of ammonia (NH3) is becoming increasingly an important issue in environmental electrochemistry. For this investigation of platinum-containing electrode material was synthesized by coprecipitating H2PtCl6, Pd(NO3)(3) and Rh(NO3)(3) and employed as a typical electrocatalytic reaction such as NH3-ECO for fuel cell application. In this study, ECO ability immersed in a 0.5 M H2SO4 solution, where the electrolyte was measured using an electrochemical cyclic voltammetry (CV) technique. Furthermore, the electrocatalytic materials were analyzed by UV-Vis absorption spectra, excitation emission fluorescent matrix (EEFM) spectroscopy, and zeta potential. Preliminary experimental results showed that the activity of the PtPdRh alloy catalysts using a high potential scan rate; the maximum current density reached for the NH3-ECO in the voltage range of 0.2 V. Additionally, EEFM was applied to evaluate the freshly prepared catalyst yields for the fluorescent peak at 300/400 nm is associated with the Pt clusters, and UV-Vis absorption spectra revealed that the platinum (IV) species were observed at about 350 nm. Copyright (C) 2012, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.