Studied was the effect surfactant removal and titanium content have on the structure and textural properties of Ti-MCM-41 mesoporous materials. The synthesized solids were characterized by N2 adsorption, X-ray fluorescence (FRX), X-ray diffraction (DRX), electronic microscopy of high resolution(HREM), and FT-Raman and UV-vis diffuse reflectance spectroscopy (DRS). Between the two methods of surfactant removal studied, the application of a polar solvent (solution of 0.05 M H2SO4 in ethanol) was to be more effective in removing the surfactant and diminishing the destruction of mesoporous material during calcination. The samples treated by this method showed a more ordered hexagonal pore arrangement (HREM, XRD) and larger surface area. The effect of an increase in TiO2 content in synthesized solids translates itself into a significant decrease of the peak intensity characteristic of Ti- MCM-41 (2È = 2.2-2.5o) and textural properties (SBET pore volume), which indicates that during the synthesis it is not possible to incorporate more than 10 mol. % of TiO2 into the MCM-41 framework.