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Nanosizedwas prepared using the sol-gel procedure. The prepared powder was thermally treated up to TiO 2 1000 ÄC. X-ray di †raction (XRD) measurements showed that the starting powder and the samples obtained after heating this powder up to 500 ÄC were mixtures of anatase, as the dominant phase, and brookite. The crystallite sizes of the samples were estimated using the Scherrer equation. A new approach to the size determination of nanosized by low-wavenumber Raman scattering, was also applied. The particle sizes, determined by lowTiO 2 , wavenumber Raman scattering, were in agreement with the crystallite sizes measured by XRD. Rutile was produced by heat treatment of the starting powder at 850 ÄC and higher temperatures.