A highly photoactive Ti-containing Cr-modified MCM-48 photocatalyst (Si/Ti = 3.4, Si/Cr = 50) was prepared by a facile one-step method at room temperature. A combination of various physicochemical techniques such as X-ray diffraction (XRD), N-2 physisorption, diffuse reflectance UV-vis spectra (DRS) and X-ray photoelectron spectra (XPS) were used to characterize the properties of the synthetic catalysts. The characterization and experimental results indicated that tetrahedral Ti oxide moieties as dominant Ti oxide were loaded into the mesoporous structure and there was a synergistic interaction between the Ti species anchored on the walls and the Cr ions presented in the MCM-48 framework, which was considered to be directly correlated to the photoactivity. The Ti-Cr-MCM-48 sample can remove H2S with the efficiency of 92% under visible light, being the Cr6+ species primarily responsible for this photoactivity. A deactivation was observed as a consequence of sulfate accumulation on the surface of the catalyst and reduction of Cr6+. (C) 2012 Elsevier B.V. All rights reserved.