The surface of a TiO2 material was modified by loading NiOx in 10 wt% by impregnation with nickel nitrate followed by calcination in air at different temperatures. The TiO2 and NiOx/TiO2 samples prepared were applied for photocatalytic H2 production from glycerol and water at 50 ºC. The H2 evolution was enhanced by NiOx loading and was dependent on calcination temperature. A maximum H2 evolution was observed with 450 ºC calcined NiOx/TiO2 sample. The properties of those TiO2 and NiOx/TiO2 samples were characterized by nitrogen adsorption, XRD, UV/Vis, and XPS measurements to examine factors responsible for the enhancement of photocatalytic H2 evolution with NiOx loaded and calcined TiO2 samples.