Abstract. Mesoporous pure TiO 2 (M-TiO 2 ) and mesoporous-vanadium-doped TiO 2 (M-V-doped TiO 2 ) were successfully synthesized via a facile and simple reflux technique. The purpose of this research was to study the effect of vanadium dopant on the physicochemical properties of all materials obtained. Characterization of the prepared materials was carried out using X-ray diffraction (XRD), scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS) and N 2 -adsorptiondesorption analysis. The presence of Ti and O elements in M-TiO 2 and of Ti, V and O elements in M-V doped TiO 2 could be detected by SEM-EDS, while the patterns of X-ray diffraction of all the prepared samples had a well-crystalline surface of anatase type. All mesoporous vanadium-doped TiO 2 (M-V-doped TiO 2 ) materials performed in a highly transparent mode in the visible region at 554 nm (E g = 2.24 eV) and 588 nm (E g = 2.12 eV) for 3.3 and 4.9 wt% V doped TiO 2, respectively. The Rietveld refinement method was applied to extract the structural parameters of the M-TiO 2 and M-V-doped TiO 2 using the Fullprof program in the WinPlotr package. The prepared materials were refined in the crystal system and space group of anatase (tetragonal, I4 1 /amd (141)). The vanadium ion was successfully doped into TiO 2 . The isotherm type of M-TiO 2 and 2.3 wt% V doped TiO 2 were of type IV, with a profile of type H2 hysteresis loops, while the 3.3 and 4.9 wt% vanadium-doped TiO 2 reflected isotherm type III. The Brunauer-Emmett-Teller (BET) results showed a significant reduction in surface area due to increased concentrations of vanadium. The highest values of BET-specific surface area, pore volume and average pore size of M-TiO 2 were 46 m 2 /g, 18.45 nm and 0.2572 cm 3 /g respectively.