The experimental concepts of high resolution solid state13C cross-polarization magic angle spinning (CP-MAS) NMR spectroscopy are examined and contrasted with those used for obtaining NMR spectra in the liquid state. The setting of the critical experimental parameters necessary for obtaining quantitative responses in the solid state experiment are discussed in terms of the relative magnitudes of relaxation processes that are essential for the successful implementation of the technique. Methods for evaluating morphological changes and identifying resonances of the spectra with regard to chemical and/or physical diversity are also described and illustrated with spectral studies of different carbohydrates.