Development and application of techniques in solid-state NMR

Abstract

The purpose of this thesis is to describe research into the extension and development of methods in solid state NMR, and their application to chemical systems where, for various reasons, analysis was difficult, incomplete, or impossible by other spectroscopic techniques. In particular silicon-29, sodium-23, fluorine-19 and proton nuclei have been used as molecular probes in inorganic silicates, macrocyclic polyether crown complexes and fluoropolymer chemical systems. The sodium-23 chemical shift and lineshape have been shown to be sensitive to coordination and local symmetry. The cross-polarization experiment has also been applied to the sodium-23 nucleus, and shown to exhibit the same steric selectivity which has been observed in carbon-13 andsilicon-29 experiments. A probe has been configured at 4.7 Tesla to perform proton and fluorlne-19 CRAMPS experiments. Multiple pulse sequences and CRAMPS experiments have been used to investigate the molecular motions and chemical environments of the systems investigated. Conclusions are drawn upon the results which support the utility of these methods in application to difficult solid state systems.