Cryogenic NMR and NMR spin−lattice relaxation time (NMRT) measurements of pore-confined water (D 2 O) have been performed using deuterium NMR to probe the pore size distribution (PSD) of silica materials and porous membranes. NMRT measurements were performed at a temperature slightly below the normal freezing point (277 K) of bulk water (D 2 O) to ensure that all interparticle water was frozen out. PSD derived from cryogenic NMR was in excellent agreement with PSD obtained from N 2 -adsorption measurements. Also, PSD obtained by NMRT revealed approximately the same average pore dimension as obtained by N 2 adsorption. However, the former experimental technique resulted in somewhat narrower PSD than obtained by cryogenic NMR and N 2 adsorption and is discussed in the text. An attempt to determine the PSD of a TiO 2 membrane on a silica support by NMRT will also be discussed. The main results obtained in this work suggest that a combined use of cryogenic NMR and NMRT may give information on both PSD and pore-connectivity.
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Hansen et al. (2002) studied this question.
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