Many problems in chemistry cannot be tackled with solution NMR, either because the material cannot be dissolved or because special interactions only present in the solid state are to be investigated. These are especially the study of the anisotropy of the NMR parameters such as the chemical shift or the spin-spin coupling.

The scope of solid-state NMR is extremely wide, from solid-state physics and materials science to structural biology. Corresponding to this there exist a multitude of methods that are currently in use or still being developed. Similarly, there is a very large variety in the available instrumentation, reaching from hybrid instruments designed to perform high-resolution measurements in both the liquid and the solid states to very specialized solid-state instruments, which are specially designed to cover wideline NMR applications of quadrupolar nuclei or even NMR microscopy of solid materials.

Whereas in high-resolution NMR of the liquid state, as described in the first 13 chapters of this book, one can hardly cause serious damage to the instrument by choosing wrong parameters, this can easily happen at the high power levels typically used in solid-state NMR. Thus, for instance, in solid-state NMR one uses high-power continuous-wave decoupling instead of low-power composite-pulse decoupling. The novice in this field should therefore be extremely careful and always double-check on all set- tings of both hardware connections and software parameters before starting up an ex- periment. Probe-head coils, preamplifiers, and other parts of the instrument can easily be destroyed by wrong settings. For instance, it is advisable to remove the proton preamplifier when using high-power decoupling.

In this chapter we provide descriptions for shimming a solid-state probe-head, set- ting the magic angle, finding the Hartmann–Hahn matching condition, and performing the basic CP/MAS experiment. We also introduce some side-band suppressing meth- ods (TOSS and SELTICS) and editing experiments such as NQS. The newly added REDOR experiment makes use of the recently developed technique of TPPM decoup- ling. An HR-MAS example for soft solids concludes the chapter.

[1] C. A. Fyfe, Solid State NMR for Chemists, C.F .C. Press, Guelph, 1983.

[2] R. Voelkel, Angew. Chem. Int. Ed. Engl. 1988, 27, 1468-1483.

[3] C. P. Slichter, Principles of Magnetic Resonance, 3rd Edition, Springer, Berlin,

[4] B. Bliimich (ed.), NMR-Basic Principles and Progress 1994, Volumes 30-33.

[5] K. Schmidt-Rohr, H. W. Spiess, Multidimensional Solid-State NMR and Polymers, Academic Press, London, 1994.

[6] E. O. Stejskal, J. D. Memory, High-Resolution NMR in the Solid State, Oxford University Press, New York, 1994.

[7] D. D. Laws, H.-M. L. Bitter, A. Jerschow, Angew. Chem. Int. Ed. 2002, 41,