Iron and/or ruthenium supported activated carbon (AC) materials, prepared by different preparation methods are studied by X-ray diffraction (XRD), Mossbauer spectroscopy (MS) and X-ray Photoelectron Spectroscopy (XPS) techniques. Their catalytic behavior in methanol decomposition to CO and methane is tested. A well defined effect of the metal loading sequence on the catalytic properties of iron-ruthenium samples is established. The relation between the catalysts' phase composition and the reaction mechanism is discussed. (C) 2004 Elsevier B.V. All rights reserved.