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Interactions between the hierarchical structure of Japanese cypress and small hydroxylic solvents with high polarity were studied using variable-temperature  13 C cross-polarization and magic-angle spinning nuclear magnetic resonance (CP/MAS) NMR spectroscopy, including low-temperature measurements.  13 C CP/MAS NMR spectra were enhanced by dipolar interactions closely related to  1 H– 13 C magnetization transfer, providing information about the interaction between woody materials and small hydroxyl molecules. The change in interaction was particularly near the melting point of the hydroxylic solvent, where a decrease in the intensity of the cypress carbohydrate signal and the appearance of the signal of solvent molecules were observed. The trend of signal intensity in the variable-temperature  13 C CP/MAS NMR spectra of cypress and cellulose fibers in the presence of hydroxylic solvents indicated that the decrease in the carbohydrate signal intensity due to the transfer of magnetization near the melting point of the hydroxyl molecule is greater when the size of the hydroxyl molecule is smaller. Furthermore, molecular association in the nanopores of the hierarchical structure allowed the hydroxyl molecular signals of the impregnated cypress to appear above the melting point.

Variable-temperature solid-state NMR analysis of woody materials in the presence of small hydroxyl molecules