Titanium dioxide nanoparticles can be synthesized using different techniques; among these, the sol-gel spin coating is fast and economical and guarantees excellent results. This work reports the results of the characterization of TiO2 films, prepared with the sol-gel spin coating method on glass and silicon, with the Rutherford Backscattering Spectrometry (RBS). The influence of rotation speed and sol-gel volume deposited on the film thickness was investigated. Furthermore, the effect of heat treatment was evaluated. The results showed that as the speed increases, the thickness of the film decreases with an exponential trend. The volume of sol-gel deposited does not affect the thickness instead. Heat treatments induce a decrease in the film thickness and an elimination of the solvents present in the sol-gel.