This work focalizes on a nanosized La0.6Sr0.4Co0.8Fe0.2O3-delta (LSCF) perovskite and Fe2O3/LSCF nanocomposites. The nanosized LSCF perovskite is obtained by Pechini method and treated at 1173 K; nanocomposite Fe2O3/LSCF powder samples (Fe2O3/LSCF = 1:9 and 1:1 wt.) are obtained by wet impregnation. The reactivity of the obtained samples with respect to pure methanol and to a 1 M aqueous solution of methanol, is investigated by means of IR Spectroscopy and Quadrupole Mass Spectrometry (QMS). In presence of pure methanol the main reaction is methanol decomposition with the formation of CO and H-2. The activity with respect to this reaction starts to be observed at 573 K both for the LSCF perovskite and for the Fe2O3/LSCF nanocomposites and shows an irregular trend as a function of temperature. Steam-reforming reaction is evident at T >= 623 K when a 1 M solution of methanol is used. The reactivity with respect to methanol and to the 1 M solution of methanol was also investigated as a function of time: only at 673 K the methanol decomposition starts immediately; the waiting time changes as a function of temperature, sample composition and reactive mixture. The steam reforming reaction, in contrast, begins immediately. (C) 2007 Elsevier B.V. All rights reserved.