The application of NOx storage and reduction (NSR) catalysts for the cleanup of diesel engine exhaust gases requires unequivocally a structured support. In this paper, a cordierite monolithic substrate on which Al2O3 was washcoated and then the active phases, namely Pt and Ba, were incorporated by adsorption from solution and impregnation, respectively, is innovatively characterized. Alternatively to the standard characterization techniques, which often are not applicable for structured catalysts, we used a FIB-SEM with the aim of determining Pt and Ba dispersion and distribution in the alumina washcoat. First, using the imaging ability of the FIB-SEM, it was observed that barium was evenly distributed along the washcoat surface. Secondly, with the cutting ability of the equipment, a thin washcoat film was lifted out from the washcoat in order to be observed by TEM. Pt and Ba were found to be well distributed all over the washcoat depth with an excellent platinum dispersion with particles around 1-2 nm. The NOx storage and reduction experiments showed an excellent storage capacity (74%) and nitrogen selectivity (87%) which was related to the adequate contact between the active phases, Pt and Ba. (C) 2013 Elsevier B.V. All rights reserved.