Abstract
1H magic angle spinning NMR spectroscopy was used to study xerogels containing the 3-mercaptopropyl group. These xerogels were synthesized using tetraethoxysilane, 1,2-bis(triethoxysilyl)ethane, and 1,4-bis(triethoxysilyl)benzene as structuring agents. The assignment of the NMR signals observed showed the presence of thiol groups introduced during syntheses and organic bridges in the frame of polysilsesquioxane samples. An analysis of the 1H magic angle spinning NMR spectra also showed the presence of small amounts of alcohols, water participating in H-bonding, and nonhydrolyzed alkoxyl groups in the xerogels. In several instances, the structural units of Tn and Qm types present in the xerogels were identified. The 1H magic angle spinning NMR spectroscopy combined with 13C and 29Si solid-state NMR spectroscopy allows the composition of xerogels and the nature of the structural units they contain to be identified more thoroughly and reliably.
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Original Russian Text © N.V. Stolyarchuk, I.V. Mel’nik, G.I. Dobryanskaya, Yu.L. Zub, B. Alonso, 2007, published in Zhurnal Fizicheskoi Khimii, 2007, Vol. 81, No. 6, pp. 1070–1075.
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Stolyarchuk, N.V., Mel’nik, I.V., Dobryanskaya, G.I. et al. A magic angle spinning NMR study of xerogels functionalized by 3-mercaptopropyl groups. Russ. J. Phys. Chem. 81, 935–940 (2007). https://doi.org/10.1134/S0036024407060179
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DOI: https://doi.org/10.1134/S0036024407060179