The synthesis of nanostructured TiO 2 particles in this work was carried out using the hydrothermal method. Titanium (IV) isopropoxide (TTIP) was used as a precursor for the synthesis, while methanol was used as a solvent. The prepared mixture was transferred to a three-necked flask and TiO 2 synthesis was carried out with the addition of water and reflux for 3 hours at temperatures of 80°C, 82°C and 85°C. After crystallization, the solid phase was separated and the obtained product was dried and calcined at temperatures of 500°C and 840°C. The structural characterization of the prepared TiO 2 was carried out using powder X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR). The size and size distribution of TiO 2 particles were measured over the sample, while the morphology was determined using a transmission electron microscope (TEM). The measurement results indicate that the process of synthesis of nanostructured TiO 2 was carried out successfully with the crystallization of two polymorphic structural forms, anatase and brookite. On TEM images, it was observed that TiO 2 particles with a size of 50-70 nm are agglomerated into particles whose dimensions are greater than 280 nm. The dimensions of the agglomerates are indicated by measurements obtained by the laser diffraction method, where the sizes range up to micrometer dimensions.