QUANTITATION IN C-13 NMR-SPECTROSCOPY OF CARBONACEOUS SOLIDS

This chapter provides an overview of the fundamental issues concerning quantitation in C-13 NMR spectroscopy of carbonaceous solids. General factors governing quantitation in solid-state C-13 NMR spectroscopy (such as sample heterogeneity, the presence of unpaired electron spins, interference of proton decoupling by molecular motion, magic-angle spinning (MAS) effects, and implementation of the proper recycle-delay time) are discussed together with those factors that play a major role in cross-polarization (CP) experiments (Hartmann-Hahn match, proton spin-locking, cross-polarization spin dynamics, and interference of cross-polarization from MAS). Technical aspects and requirements of the solid-state C-13 NMR experiment are outlined, and effective strategies to obtain the most reliable results are presented.