I. Optical pumping and magic angle spinning surface NMR spectroscopy. II. Multiplex NMR

In Part I of this thesis a new approach to the study of surfaces using solid-state NMR is described. The technique combines the enhanced surface sensitivity and selectivity afforded by optically polarized Xe with magic angle spinning in order to provide high-resolution spectra. The optically polarized Xe is adsorbed onto a surface and a portion of its hyperpolarization is transferred to nearby surface spins. The polarization transfer takes place via the so called spin polarization induced nuclear Overhauser effect (SPINOE). A summary of the theoretical aspects of optical pumping theory and SPINOE is presented. Experiments to explore the utility of the approach as well as a detailed analysis of the kinetics of the polarization transfer process are presented. In Part II, Multiplex NMR is introduced as a new approach to increasing the throughput of NMR measurements by recording NMR signal from several samples simultaneously. The use of a linear magnetic field gradient is shown to allow the signal from four sample coils to be obtained concurrently. The signals are subsequently assigned to their respective coils by a software algorithm. It is also shown that the Multiplex methodology is fully compatible with two-dimensional NMR methods.