Cu and Ni based catalysts were synthesized using solution combustion synthesis method. The catalytic activity and hydrogen selectivity were investigated for ethanol decomposition reaction. The amount of fuel content in the combustion solution was found to greatly affect the phase and the microstructure of the synthesized catalyst. In situ X-ray absorption spectroscopy (XAS) studies were carried out to study the reduction of the catalyst containing mixed oxides of copper and nickel. The reduced catalyst was further subjected to an oxidizing environment to collect the in situ XAS data during the oxidation of the catalyst. These investigations show that the catalyst oxidation state changes rapidly in the first few minutes of the pretreatment process and then gradually slows downs. (C) 2015 Elsevier B.V. All rights reserved.