Various preparations of nanostructured TiO2 Starting from Ti(iSO-OC3H7)(4) or TiCl4 are reported. The samples were characterized by X-ray diffractometry, specific surface area and porosity determinations, scanning and transmission electron microscopy, and diffuse reflectance spectroscopy. 4-Nitrophenol photodegradation in aqueous medium was employed as a probe reaction to test the photoactivity of the catalysts. The photoactivity of some samples derived from Ti(iso-OC3H7)(4) was found comparable with that of commercial powders. Calcination after the hydrolysis process was necessary to achieve crystallization of the particles before using them as photocatalysts for the reaction studied. The samples deriving from TiCl4 were the most photoactive among the home-prepared catalysts, and neither filtration nor calcination was needed to obtain a highly photoactive anatase phase.