Benzene and ethanol adsorption in pure silicate MCM-41 samples of differing pore diameters was studied. The adsorption was used as a tool for characterizing the pore structure and study the thermal effects on capillary condensation process. Adsorption isotherms of benzene was observed to increase as the pore diameter increase while ethanol exhibited a higher affinity toward the MCM-41 surface due to the polarity of the ethanol molecules.