Plating bath concentrations of Pt(IV) and Ir(III) have been optimized as well as the total catalytic loading of bimetallic Pt-Ir alloy for the electro-oxidation of ammonia in alkaline media at standard conditions. This was accomplished using cyclic voltammetry, scanning electron microscopy (SEM). energy dispersive X-ray (EDX), and statistical optimization tools. Concentrations of Pt(IV) and Ir(III) of the plating bath strongly influence electrode surface atomic compositions of the Pt-Ir alloy directly affecting the electro-oxidation behavior of ammonia. Several anode materials were studied using cyclic voltammetry, which demonstrated that Pt-Ir was the most active catalyst for the electro-oxidation of ammonia. Criteria for optimization were minimizing the climatic oxidation overpotential for ammonia and maximizing the exchange current density. Optimized bath composition was found to be 8.844 +/- 0.001 g L-1 Pt(IV) and 4.112 +/-0.001 g L-1 Ir(III) based on electrochemical techniques. Physical characterization of the electrodes by SEM indicates that the plating bath concentrations of Pt and Ir influence the growth and deposition behavior of the alloy. (C) 2010 Elsevier Ltd. All rights reserved.