Nanocrystalline TiO2 powders were prepared by the sol-gel method and evaluated in the NO photocatalytic oxidation. Samples annealed at 200 and 500°C (TiO2-P-200, TiO2-P-500) were characterized by nitrogen adsorption, XRD-Rietveld refinements, TEM, FTIR and UV-vis spectroscopies. The photocatalytic test of the sol-gel TiO2 samples was carried out in an insulated chamber with 10 ppm of NO, using a 365-nm UV light lamp; the test results were compared with those obtained with a commercial catalyst (P25). Improved photoactivity (89 % of NO oxidized in 60 min) was obtained with the TiO2-P-200 solid which showed high surface area, small crystallite size, higher amount of OH and highly abundant brookite phase (37.2 %) coexisting with the anatase phase (62.8 %). The photo-oxidation activity of the sol-gel catalyst annealed at 500 °C (TiO2-P-500) showed changes in its textural and morphologic properties and therefore, less photoactivity. Sol-gel photocatalysts could be a good option for abating pollution in both indoor and outdoor environments at room temperature.