Titania supported vanadia catalysts (2.5, 5, and 11 wt.% V2O5) were prepared by a wet impregnation technique and their thermal behavior, morphology as well as redox properties were examined by thermal analysis methods thermogravimetry (TGA), differential scanning calorimetry (DSC), temperature programmed-evolved gas analysis with mass spectroscopy, (EGA-MS), scanning electron microscopy (SEM), and temperature programmed reduction (TPR). The two Eurocat samples EL10V1 and EL10V8 containing 1 and 8 wt. % V2O5 were also characterized using the same techniques. Thermal decomposition of vanadium oxide precursors (ammonium vanadyl oxalate) supported on TiO2 as evidenced by thermal analysis, occurs in three successive steps, which are influenced by the surrounding atmosphere (oxidative, reductive, and inert). The presence of tower-like vanadia crystals in the sample with the highest vanadia loading (11 wt.% V2O5) was identified by SEM. The H-2-TPR experiments revealed that the reduction temperature is a factor of the vanadia loading and the type of support. Vanadia species supported on Norton titania are more reducible that those supported on Eurocat titania. (C) 2004 Elsevier B.V. All rights reserved.