A new method of measurement of pore volume distribution in a porous material by adsorption of gases is proposed. In the newly proposed method the use of spherical molecules with relatively large molecular weight as adsorbates is strongly recommended to eliminate the troubles caused by stereospecificity and low boiling point of widely used $N_2$. It is also claimed that the universal t-curves that have been widely used since proposed by de Boer et al. must be replaced by the flat-surface isotherms that can be derived from the theory proposed by Chang et al. The results of analysis of pore volume distribution based on the method described in this paper are found to be reasonable and satisfactory.