This paper presents the preparation of a completely new Pt/Rh/Pt multilayer. This material was characterized by means of X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (where the change in the electroactive area in the material during the deposition of the bilayer was discarded). The material was further tested for the oxidation of small organic molecules (methanol, ethanol, formaldehyde and formic acid) with the aid of cyclic voltammetry and chronoamperometry. In this study, increases of 295%, 266%, 140% and 380% in the voltammetric peak current density for methanol, ethanol, formaldehyde, and formic acid oxidation at the Pt/Rh/Pt bilayer, respectively, are presented. (C) 2004 Elsevier B.V. All rights reserved.