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Synthesis and characterization of spherulite-like nanocrystalline titania with rutile structure (r-TiO2) are described herein. The r-TiO2 particles were synthesized via the convenient and low-cost hydrothermal treatment of TiO(C6H6O7) titanyl citrate. The r-TiO2 spherulites are micron-sized agglomerates of rod-shaped nanocrystals with characteristic sizes of 7(±2) × 43(±10) nm, oriented along (101) crystallographic direction, and separated by micropores, as revealed by SEM and TEM. PXRD and Raman spectroscopy confirmed the nanocrystalline nature of r-TiO2 crystallites. BET analysis showed a high specific surface area of 102.6 m2/g and a pore volume of 6.22 mm3/g. Photocatalytic performances of the r-TiO2 spherulites were investigated for the processes of methyl violet (MV) degradation in water and hydrogen evolution reaction (HER) in aqueous solutions of ethanol. The (MV) degradation kinetics was found to be first-order and the degradation rate coefficient is 2.38 × 10−2 min−1. The HER was performed using pure r-TiO2 spherulites and nanocomposite r-TiO2 spherulites with platinum deposited on the surface (r-TiO2/Pt). It was discovered that the r-TiO2/Pt nanocomposite has a 15-fold higher hydrogen evolution rate than pure r-TiO2; their rates are 161 and 11 nmol/min, respectively. Thus, the facile synthesis route and the high photocatalytic performances of the obtained nanomaterials make them promising for commercial use in such photocatalytic processes as organic contamination degradation and hydrogen evolution. [ABSTRACT FROM AUTHOR]