The adsorption of basic dye methylene blue (MB) onto titanium dioxide (titania) powder that were prepared by coprecipitation method of TiCl3 and NH4OH as iniatial material with different calcination temperature was studied to examine the photocatalytic activity. Synthesis process carried out by the solution pH was adjusted to be 8. Effect of calcination temperature on the titania powder were characterized with Differential Scanning Calorimetry/Thermogravimetry (DSC/TG), X-ray diffraction (XRD), and Scanning Electron Microscopy (SEM). The result of TG and XRD showed that the NH4Cl decomposed between 235-372°C. The XRD result showed that the anatase TiO2 only contained a single phase when the calcination temperature of the precursor at 800°C, and over which it began to grow rutile phase. The influence of synthesis condition on the photocatalytic activity of TiO2 powder was determined by the photodegradation of MB dye under UV light.