A new method to study the pore connectivity of meso- and macrporous ma
terials was proposed. The dependence of the melting temperature of a f
rozen liquid in a pore on its size was used to single out the pores of
a given size in a sample and to estimate the pore size. The sample wa
s heated after preliminary freezing of a liquid (adsorbate) that was i
ntroduced into sample pores. Adsorbate melts in pores with smaller (th
an definite) sizes. The state of adsorbate was controlled by the data
on NMR relaxation; the pore connectivity was determined by the data on
self-diffusion of liquid molecules in selected pores studied by the p
ulse field gradient (PFG) NMR method. The applicability of the method
of the estimation of pore sizes was considered using the mesoporous ca
rbonaceous adsorbent-cyclohexane system, and that of the method of stu
dying pore connectivity using the anhydrous cement-cyclohexane system
as examples.