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The adsorption of water in the mesoporous silica material with cylindrical pores of uniform diameter, Controlled Pore Glass 10-75 (CPG), was studied by  1 H-MAS solid state NMR spectroscopy. From the NMR spectra it is evident that inside the mesopores of the silica different water environments exist, which are characterized by their individual chemical shift. All observed hydrogen atoms are either surface –SiOH groups or hydrogen bonded water molecules. It is found that there exist some stronger bound water molecules on the surface which are not removable even by heating at a vacuum pump. As a tentative assignment these water molecules are attributed to surface defects or inaccessible cavities in the CPG 10-75. At intermediate water filling levels, the principal signal is a single NMR line with continuously varying chemical shift. This finding is interpreted as the result of a radial water filling mechanism. That is, the filling of the pore grows from the pore surface towards the pore axis. Finally it is shown that water is a sensor for surface and structural inhomogeneity and that a coexistence of inner pore and outer bulk water exists in the system.

Hydrogen Bonding of Water Confined in Controlled-Pore Glass 10-75 Studied by 1 H-Solid State NMR