Carbon-TiO2 sulfated composites were obtained from TiOSO4 center dot xH(2)O and glycerol as the TiO2 and carbon sources, respectively. The precursor xerogels were prepared in a one-step ultrasonic-assisted sol-gel reaction, followed by thermal treatment at 400 degrees C under a nitrogen atmosphere to produce carbon-TiO2 sulfated composites. XRD, micro-Raman, SEM, and TEM studies showed that the composites consisted of nanocrystalline clusters of TiO2 and carbon. Ultrasonication in glycerol promoted the crystallinity of the xerogel precursors prior to thermal treatment. X-ray powder diffraction and Raman spectroscopy studies confirmed that glycerol also facilitated the formation of small crystallites. The band gaps of carbon-TiO2 composites with two different carbon loadings were found to be 3.06 eV and 2.69 eV. By contrast, the band gap of TiO2 prepared by our method was 3.53 eV. Calcination of the precursors led to an unusual increase in the specific surface and porosity of the composites compared to TiO2. The photocatalytic activities of the prepared composites were tested in a decomposition assay of Acid Orange 7. The reaction was monitored by UV-vis spectrophotometry and by LC-ESI-(Qq)-TOF-MS-DAD. Some intermediate species were identified by LC-ESI-QTOF-MS. (C) 2013 Elsevier B.V. All rights reserved.