Transparent anatase mesoporous TiO2 (MTiO2) and TiO2 nanometer thin films were prepared on soda-lime glass and fused quartz via the reverse micellar method and sol-gel method, respectively. The as-prepared MTiO2 and TiO2 films were then treated by dipping them in a H2SO4 solution. The MTiO2 and TiO2 films before and after surface acid treatment were characterized by X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), transmission electron microscopy (TEM), X-ray diffraction (XRD), BET surface area and UV-VIS spectrophotometry. The photocatalytic activity of the samples was evaluated by photocatalytic oxidation of acetone in air. It was found that MTiO2 thin films showed higher photocatalytic activity than that of the TiO2 thin films. This was attributed to the fact that MTiO2 thin films were composed of smaller monodisperse spherical particles about 15 nm and had higher specific surface areas. Furthermore, the monodispersity of TiO2 Particles was beneficial to transfer and separation of photo-generated electrons and holes in the inner of and on the surface of TiO2 Particle and reduced the recombination of photo-generated electrons and holes. The films deposited on quartz showed the highest photocatalytic activity because films deposited on quartz exhibited a better crystallization and had no sodium contaminant. The photocatalytic activity of MTiO2 and TiO2 thin films deposited on different substrates after treated with H2SO4 Solution was significantly enhanced. Acid treatment was particularly effective for MTiO2/glass and TiO2/glass, which showed activity enhancement of four and over two times, respectively. This increase in activity has been correlated with the reduction of sodium ions and the increase in the adsorbed hydroxyl content on the surface of TiO2 films.