TiO2 nanoparticles were synthesized by a sol-gel method and the effect of ball milling of dried gel on the particle size has been investigated. The results show that the ball milling has a crucial role in preparation of nanosized TiO2 powder. Also thermal treatment at different temperatures can control the size of prepared nanoparticles. The photocatalytic activities of TiO2 nanoparticles with different sizes were studied by photocatalytic degradation of Congo red dye using a homemade photoreactor. The photo degradation of Congo red dye was monitored by UV-Vis absorption measurements. It was found that the nanopowders which were synthesized at 550 degrees C with average particle size of 55 nm show the maximum photocatalytic activities. These nanopowders which were a mixture of anatase and rutile phases did not show the same photocatalytic effect on Eriochrome black, Bromocresol green, Methyl orange and Rose Bengal dyes. (C) 2011 Elsevier B.V. All rights reserved.