Setting up 13 C CP/MAS experiments

The 13 C cross‐polarization (CP) technique combined with magic angle spinning (MAS) has become one of the more commonly performed solid‐state nuclear magnetic resonance (NMR) experiments. The basics of initially setting up the experiment are given and used to illustrate such NMR phenomena as rotational echoes, homogeneous and inhomogeneous interactions, continuous wave 1 H decoupling, and coupling of quadrupolar 14 N nuclei to 13 C nuclei. The polarization transfer from the protons to the carbons is described briefly with the usual thermodynamic and quantum mechanical models. The setup and use of the experiment for routine analyses are discussed. © 2004 Wiley Periodicals, Inc. Concepts Magn Reson 22A: 37–49, 2004.