Nanoporous titania was prepared from non-ionic surfactant reverse micelles (e.g. Triton-X) and the effects of the chain length of the surfactants and calcination temperature of the precursor gels on the surface properties of the product (mesoporous titania) were investigated. The studies included sample characterization of the precursor gels from the titania samples characterized by UV-Vis, ATR-FTIR, XRD, TGA/DSC and the titania samples by N 2 -adsorption BET, XRD, FT-IR, UV-Vis diffuse reflectance and SEM measurements after calcination at 400 C, 500 C, 600 C, 700 C and 800 C. According to the experimental results, generally increasing the length of the polar tail of Triton-X results in an increased specific surface area and volume, and an average pore diameter of the solids. Moreover, increasing the length of the polar tail is associated with a smaller crystallite size and higher thermal stability of the materials. Finally, a nucleation mechanism of the titania particles within the aqueous centre of the reversed micelles is proposed.