Well-defined nanoparticles of rutile (with the size of 5 nm) were successfully prepared by the unusual solid-state transformation of an amorphous precursor in well-defined nanospace of a mesoporous silica template (SBA-15) at room temperature. An aqueous colloidal suspension of the rutile nanoparticles was successfully obtained by dissolution of SBA-15 and subsequent pH adjustment. The isolated rutile nanoparticles were used for H-2 evolution from an aqueous methanol solution by UV irradiation.