In this paper, the preparation of nanosized synthetic rutile by reductive hydrochloric acid leaching of mechanically activated ilmenite concentrate (FeTiO(3)) is discussed. X-ray fluorescence analysis of the nanosized rutile which forms by rapid hydrolysis of dissolved titanium indicates that the powder contains 91.1% TiO(2), 1.3% Fe(2)O(3), 6.3% SiO(2). The presence of the rutile phase is confirmed by X-ray diffractometry and the sizes of particles are measured by transmission electron microscopy to be less than 100 nm. The photocatalytic activity of nanosized rutile is observed by the decomposition of methylene blue. (C) 2010 Elsevier Ltd. All rights reserved.