Abstract
Multiple-quantum magic-angle spinning (MQMAS) and double rotation (DOR) techniques were applied in the fields of 17.6 T and 11.7 T to the study the 17O NMR of oxygen-17 enriched zeolites A, LSX and sodalite. In addition, some 29Si and 1H MAS NMR experiments were performed. Zeolites with the ratio Si/Al = 1 were chosen, in order to have an alternating distribution of silicon and aluminum atoms. A linear correlation between the isotropic value of the chemical shift and the Si–O–Al bond angle α (taken from X-ray data) could be found for the zeolites A and LSX, but not for sodalites. Hydration of the zeolites causes a downfield 17O NMR chemical shift of about 8 ppm with respect to the dehydrated zeolites. Ion exchange of the hydrated zeolites generates stronger chemical shift effects. The increase of the basicity of the oxygen framework of the zeolite LSX is reflected by a downfield shift of ca. 10 ppm going from the lithium to the cesium form, and the substitution of sodium by thallium in the zeolite A causes a shift of 34 ppm for the O3 site. 17O DOR NMR spectra are superior to 17O 3QMAS NMR spectra, featuring a resolution increase by a factor of two and are about equal with respect to the sensitivity. The residual linewidths of the signals in the 17O DOR and 17O 5QMAS NMR spectra can be explained by a distribution of the Si-O-Al angles in the zeolites.
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Freude, D., Loeser, T. 17O NMR Studies of Zeolites. In: Haberlandt, R., Michel, D., Pöppl, A., Stannarius, R. (eds) Molecules in Interaction with Surfaces and Interfaces. Lecture Notes in Physics, vol 634. Springer, Berlin, Heidelberg. https://doi.org/10.1007/978-3-540-40024-0_4
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DOI: https://doi.org/10.1007/978-3-540-40024-0_4
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