Nanocrystalline mesoporous titania was synthesized via a combined sol-gel process with surfactant-assisted templating route and evaluated for photocatalytic activity of hydrogen evolution from an aqueous methanol solution. In this proposed method, applied surfactant template molecules advantageously behaved as both mesopore-forming and gel formation-assisting agent. The activity of the mesoporous titania thermally treated under appropriate conditions, i.e., at calcination temperature of 600 degreesC for 4 h, was considerably higher than that of commercial titania powders, Ishihara ST-01 and Degussa P-25. It is clearly revealed that introducing mesoporous framework into TiO2 by this synthetic system provided much better photocatalytic performance. (C) 2004 Elsevier B.V. All rights reserved.