Cellulose/TiO2 microsphere composites were made by a one-step phase separation method using cellulose xantate aqueous solution and sodium polyacrylate aqueous solution. The distribution of TiO2 particles is easily adjusted by adding polyethylene glycol as a diluent. As a result, we succeeded in preparing cellulose/TiO2 microsphere composites with the surface covered with dense arrangement of TiO2 by this technique. In addition, carbon/TiO2 microsphere composites, prepared by carbonization of the cellulose/TiO2 microsphere composites, were also developed and used as a photocatalyst. The TiO2 crystal phase in the cellulose/TiO2 microsphere composites and the microsphere composites, carbonized in a stream of nitrogen at 600 degreesC, were both found to have the anatase-form as revealed by X-ray diffraction. The process of carbonization proceeded TiO2 particles appeared more on the surface. The TiO2 content in the adsorbent was found to be much more than that in commercially activated carbon/TiO2 composites, as confirmed by elemental analysis. As a result, the carbon surface worked well as the effective to concentrate organic pollutant around the TiO2 anchored on the composite surface. 9 2002 Elsevier Science B.V. All rights reserved.