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Title: High-resolution multinuclear magnetic resonance of inorganic solids. Oxygen-17 nuclear magnetic resonance studies of inorganic oxides, oxyanions, and silicates

Thesis/Dissertation ·
OSTI ID:6716435

High resolution (8.45 and 11.7 Tesla) oxygen-17 NMR spectra have been obtained for a variety of oxides, oxyanions, carbonyls and for crystals and glasses in the system CaO-MgO-SiO/sub 2/ using magic-angle sample spinning (MASS) and variable-angle sample spinning (VASS) techniques. The results indicate that a very wide range of oxygen-17 quadrupole coupling constants and linewidths are to be anticipated in solid state oxygen-17 NMR studies. The linewidth of solid Mg/sup 17/O (0.3 ppm) is narrower than that of liquid water, due to the high symmetry of the oxygen site. In the SiO/sub 4//sup 2 -/ unit of forsterite, each nonequivalent oxygen is partially resolved, and split by a large second-order quadrupole interaction, permitting determination of the isotropic chemical shifts, quadrupole coupling constants, and electric field gradient tensor asymmetry parameters for each of the three types of oxygen present. The oxygen-17 spectra of many glasses contain multiple peaks due to non-bridging oxygens, bridging oxygens coordinated to non-Q/sup 4/ silicons, and bridging oxygens coordinated to Q/sup 4/ silicons. The oxygen-17 quadrupole coupling constant decreases as the percent ionic character of the cation oxygen bond increases. For metasilicate crystals and glasses, the oxygen-17 chemical shift of the non-bridging oxygen becomes progressively deshielded as the ionic potential of the cation present increases.

Research Organization:
Illinois Univ., Urbana (USA)
OSTI ID:
6716435
Resource Relation:
Other Information: Thesis (Ph. D.)
Country of Publication:
United States
Language:
English