High-resolution thermogravimetry (HR TGA) was successfully used to study thermodesorption of n-butanol from ordered mesoporous materials. The current study was performed for lanthanum and cerium incorporated MCM-41 samples, which were synthesized via liquid crystal templating mechanism. Due to highly ordered structure of mesopores in these materials it was possible to distinguish the characteristic features on the DTG curves, which reflect the starting points for thermodesorption of n-butanol from the interior of primary mesopores as well as from their surface. It was demonstrated that n-butanol thermodesorption data obtained by HR TGA provide accurate values of the volume of primary mesopores and their specific surface area, which are in a good agreement with those obtained from nitrogen adsorption isotherms. In addition, this study showed that a simple evaluation of the specific surface area and pore volume of nanoporous materials is possible by HR TGA.