Thermoporosimetry, i.e., DSC measurements of melting point depression of water and heptane confined in mesopores, has been used for determination the pore size distribution of several mesoporous silicas synthesized with the use of micelle templates. Porosity of these materials was additionally characterized by low-temperature nitro- gen adsorption and quasi-equilibrated thermodesorption of nonane. The pore size distributions obtained using the water thermoporosimetry were similar to those determined using the other methods, but the pore size values found for the narrow pore materials were underestimated by ca 1 nm. Too large pore sizes obtained for the wide pore silica from heptane thermoporosimetry were attributed to nonlinear dependence of the melting point depression on the reci- procal of the pore size.