Thermoporometry, a calorimetric procedure, is applied for measuring the pore size distribution, pore volume and surface area of mesoporous MCM-41 molecular sieves using water as the adsorbate. A series of MCM-41 materials with various pore diameters was synthesized and subjected to the new method. The results are compared with nitrogen physisorption. Both methods are complementary, whereby the former provides also information about the pore shape. MCM-41 materials with pores wider than 50 Angstrom also allow the use of benzene as the adsorbate in thermoporometry.