Nanocrystalline mesoporous TiO2 photocatalyst with narrow pore size distribution was synthesized by a surfactant-assisted templating sol-gel technique and used as a support for Pt towards photocatalytic H-2 evolution. Single-step sol-gel (SSSG) method, in which Pt precursor was introduced into the completely hydrolyzed TiO2 sol prepared with a mesopore-directing surfactant template, was utilized to load the Pt cocatalyst onto the synthesized mesoporous TiO2. In comparison, the conventional loading methods namely incipient wetness impregnation (IWI) and photochemical deposition (PCD) were also performed. The mesoporous Pt/TiO2 photocatalyst prepared by the SSSG method showed higher photocatalytic activity for H-2 evolution over entire range of Pt loading content (optimum loading of 0.6 wt%) as well as broader photocatalytic activity window with respect to the amount of loaded Pt than those prepared by the other two methods and Pt/Degussa P-25 TiO2. Hence, the SSSG method has been postulated as a beneficial alternative for synthesis of effective metal-loaded mesoporous photocatalyst. (c) 2005 International Association for Hydrogen Energy. Published by Elsevier Ltd. All rights reserved.