Titanium-containing mesoporous molecular sieves including periodic mesoporous silicas (SBA-15-type) and organosilicas (PMO-type) can be assembled by using mixed inorganic acid-base pairs (TiCl4 and tetrabutyl titanate) or a single inorganic TiCl3 as the titanium sources and tetraethoxysilane and/or 1,2-bis(triethoxysilyl)ethane as the silica sources and triblock copolymer as the structure-directing agent in acidic media through the hydrothermal method. Characterization using XRD, nitrogen sorption isotherms, UV-vis, FT-IR and NMR techniques reveals that the Ti-containing mesoporous materials possess ordered 2D hexagonal mesostructures, high surface areas (421-1070 m(2)/g), uniform pore sizes (5.1-8.0 nm), large pore volumes (0.5-1.3 cm(3)/g), and tetrahedrally incorporated titanium (IV) species in the silica network. The maximum incorporated Ti content is about 0.34 wt% for the ordered mesostructure regardless of the titania and silica sources and the initial Si/Ti ratio. (C) 2009 Elsevier B.V. All rights reserved.