The preparation and characterization of a CuO-CeO2 sorbent-catalyst was performed by an inorganic/organic synthesis route and the materials were tested in de-SOx type reactions. The preparation of mesostructured CeO2 was made using hexadecylamine surfactant and cerium acetate as the inorganic precursor. This procedure was modified by inclusion of the CuO precursor during the synthesis. These sorbent-catalysts were characterized by transmission electronic microscopy (TEM), N-2 physisorption, X-ray diffraction (XRD) and temperature-programmed reduction (TPR). The adsorbent-catalysts were tested by means of sulfurization from room temperature to 760 degrees C using a combined SO2/N-2 gas mixture (3600 ppm) and the gain of weight was recorded in a thermo-balance. The materials prepared with those surfactants showed high surface area due to mesopores and small CuO particles dispersed on the ceria support. The catalytic performance in the de-SOx reaction was higher than conventional sorbent-catalysts prepared by impregnation of commercial ceria. The improved SO2 adsorption capacity of these materials is attributed to a better distribution and interaction of the copper species with the ceria support. (c) 2005 Elsevier B.V. All rights reserved.