Automotive catalyst deactivation can be promoted by thermal and poisoning mechanisms. Catalyst efficiency is reduced by thermal degradation resulting in the agglomeration of precious metals and the reduction of the wash-coat surface area. In this paper, the temperature influence on the commercial Pd/Rh-based automotive catalyst performance was studied. Textural and physicochemical characterisation techniques were employed, such as X-ray fluorescence (XRF), atomic absorption spectrometry (AAS), N(2) physisorption, X-ray diffraction (XRD), temperature programmed reduction (TPR) and scanning electron microscopy coupled with energy-dispersive X-ray analysis (SEM-EDX). The catalysts were evaluated for CO and propane oxidation with a stoichiometric gas mixture similar to engine exhaust gas. The results indicated the transformation of alumina into high temperature phases and the formation of new mixed oxide phases. Evidence of sintered particles and several spots of palladium agglomerates was seen by SEM-EDX analysis. The activity results showed the effects of thermal deactivation on the conversion of the pollutants. In spite of exposure to extreme temperature conditions (72 h at 1200 degrees C), significant activity was still observed for carbon monoxide and propane oxidation reactions. (c) 2009 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.