Nanocrystalline mesoporous titania was synthesized via a combined sol-gel process with surfactant-assisted templating method using cetyltrimethyl ammonium bromide (CTAB) as the structure-directing agent. The process was catalyzed by different acid (hydrochloric acid, nitric acid, sulfuric acid, or phosphoric acid). The prepared samples were characterized by XRD, TEM, BET and FT-IR. The photocatalytic activity of the samples was determined by degradation of phenol in aqueous solution. Results showed that different acid had different effect on the structure and crystal phase of the samples. The sample adjusted by phosphoric acid showed highest surface area and photocatalytic activity. The formation mechanism of the samples catalyzed by different acid was also discussed. (C) 2009 Elsevier B.V. All rights reserved.