Cubic Pm3n mesoporous silica films have been prepared on silicon wafers and quartz crystal microbalance (QCM) devices covered with gold electrodes by a spin-coating process from preformed silica/CTABr/ethanol/water assemblies under acidic conditions. Post-synthesis functionalization of mesoporous films with amino- and thiol-containing organosilanes is performed in order to modify the mesoporous surface for further confinement of nanoscale structures. The type of mesophase structure and the functionalization process was followed with surface sensitive techniques such as grazing incidence diffraction (GID), reflection-absorption FT-IR spectroscopy and gravimetric measurements by applying QCMs technique. Nitrogen sorption data using QCM devices were obtained for the calcined and functionalized mesoporous films.