Platinum doped TiO2 materials were studied for the gas phase photocatalytic degradation of toluene. Platinum deposition was achieved by photodeposition method over TiO2 prepared by means of a sol-gel route. The effect of sulphuric acid pretreatment on the further platinisation process has been extensively studied. From the wide structural and surface analysis of the catalysts an interesting synergetic effect has been demonstrated. The previous sulphate treatment over TiO2 leads to improved dispersion of the Pt which presents a lower aggregation and homogeneous cluster size. This fact, together with the adequate control of anatase structural and surface parameter due to the sulphate treatment, renders a good photocatalytic performance for toluene oxidation reaction. The highest reaction rates and CO2 selectivities have been obtained for Pt-S-TiO2 samples. (c) 2010 Elsevier B.V. All rights reserved.