Gel-combustion synthesis (M) in self-sustaining mode was used for preparation of mixed oxide with spinel structure AB(2)O(4) (where A = Co, Cu and B = Cr, Co). To support these mixed oxides on CeO2 and ZrO2 powders, the GCS technique in self-propagating mode was developed. The synthesized materials were characterized by IR-spectroscopy, X-ray diffraction and transmission electron microscopy. The GCS preparation leads to the formation of nanocrystalline, single-phase spinel catalysts. which showed high activity in VOCs (hexane) elimination. The best catalytic performance was obtained over copper cobaltite catalyst prepared by GCS from glycerin-chelated precursor. (c) 2008 Elsevier B.V. All rights reserved.