Anew synthesis route driving redox-precipitation reactions among Mn-VII, Ce-III and Mn-II precursors in basic aqueous solution yields MnCeOx catalysts (Mn loading, 9-33 wt%) with improved textural and structural properties in comparison to the conventional co-precipitation technique. Irrespective of the Mn loading, BET, X-ray diffraction (XRD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS) findings prove that the new method ensures a very high reproducibility in all the main physicochemical properties of MnCeOx catalysts. Enabling a monolayer dispersion of the active phase, the "redox-precipitation" method greatly promotes the reducibility and the surface affinity of the MnCeOx system towards gas-phase oxygen. (C) 2007 Elsevier Ltd. All rights reserved.