High-resolution NMR of solids (Reprinted from NMR Spectroscopy Techniques, Second Edition, Revised and Expanded, pg 417-485, 1996)

摘要

This chapter is intended to provide a bridge between the principles of NMR spectroscopy of solids and the practical execution of these experiments in the laboratory. The point of view is one of physical concepts, rather than of mathematical rigor. Interwoven with the fundamentals of solid-state NMR are practical tips garnered from laboratory experience. The presentation of material is intended to apply generally to both superconducting and electromagnet geometries. Standard experiments are emphasized, rather than the more exotic and instrument-demanding techniques. The introduction contrasts the nuclear-spin interactions (Zeeman, dipole-dipole, scalar, chemical shift) in solution and in the solid state. The section on magic-angle spinning examines the effects of mechanical specimen rotation on these nuclear-spin interactions. The concept of dipolar decoupling is introduced next, followed by a section on cross-polarization. Some of the more standard solid-state NMR experiments are described in the section on advanced techniques. Finally, the section on instrumental considerations presents spectrometer and probe requirements for solid-state NMR operation. [References: 80]