This work describes the preparation and the characterization of a catalytic system for the production of hydrogen by oxidative steam reforming of methanol (OSRM), prepared by deposition of palladium acetate on an organized mesoporous alumina, followed by pre-reduction at room temperature with a zinc borohydride solution. This procedure allows one to obtain intimately interacting Pd-Zn species that easily generate the 1:1 Pd/Zn alloy, as a result of thermal treatment in reducing conditions at 500 degrees C. The alloy formation was clearly proven by X-ray diffraction measurements. The samples were also characterized by N-2 adsorption-desorption, atomic absorption spectroscopy (AAS), X-ray photoelectron spectroscopy (XPS), infrared spectroscopy (FT-IR). This type of material was found to be active in the oxidative steam reforming of methanol, in the temperature range between 100 and 400 degrees C, producing a hydrogen/CO2 mixture with low concentrations of CO. (C) 2006 Elsevier B.V. All rights reserved.