A fundamental step for a sustainable industrial development based on "H-2 Economy" is the implementation of fuel cell technology, in terms of new devices, materials and convenient processes for their production. Rare earth doped ceria oxides are suitable materials for the new generations of cells and their cost effective production becomes fundamental as the price of rare earths is increasing. In this view, our study investigates a modified method of co-precipitation of Ce0.8Sm0.2O1.9-x. (SDC) evaluating the effects of adding of H2O2 in the process. The parameters controlled were the molar ratio [H2O2]/[M3+], (M3+ = Ce3+, Sm3+ present in starting nitrate salts solutions) and the pH of precipitation; in some cases the precipitates were also treated under reflux at 373 K overnight. The powder catalysts, both as fresh precipitates and calcined oxides were analyzed via N-2 adsorption (BET), X-Ray diffraction (XRD) and temperature programmed reduction (TPR) techniques and their morphological, structural and redox properties were correlated with the synthesis parameters used. The electrical conductivity properties of these materials have also been investigated via electrochemical impedance spectroscopy (EIS) and the results compared with those of a commercial oxide. The synthesis approach was shown to be very versatile in the development of materials with properties exploitable for applications in catalysis and in intermediate temperature Solid Oxide Fuel Cell (IT-SOFC) systems. Copyright (C) 2011, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.