TiO2 nanoparticles have been prepared by amine assisted sol-gel precipitation of Ti4+ aqueous solutions and further hydrothermal treatment. The effect of different starting acidic solution (nitric, chlorhydric and acetic acids) as well as the addition of triethylamine (TEA) at different pH has been widely investigated. It has been stated that different amounts of TEA could have interesting effects upon hydrothermal treatment. Surface and morphological features significantly differ from TiO2 prepared using different synthetic route. In all cases, amine precipitated TiO2 obtained exhibit high conversion values for phenol photo-oxidation reaction, being in certain conditions higher than that exhibited by TiO2 Degussa P25. The precipitation of the acetic acidified solution leads to high surface area values and well crystallized anatase with small crystallite size. In addition, this set of catalysts show the cleanest surface after the hydrothermal treatment. The conjunction of these features would be the characteristic features responsible of the best photocatalytic activity observed. (C) 2007 Published by Elsevier B.V.