13C NMR studies of organic matter in whole soils: I. Quantitation possibilities

A detailed discussion of the quantitative nature of ¹³C CPMAS NMR spectra as applied to solid samples, such as soil, is given. In particular, the influence of the cross-polarization (CP) time constant (T_CH), the relaxation time constant of protons in the rotating frame (T_1pH) and the contact time (t_c) in the CPMAS experiment are considered. Three distinct quantitation regimes are numerically identified according to sample parameters t_CH and T_1PH > and the experimental choice of t_c: (i) quantitation obtainable from a single CPMAS spectrum; (ii) quantitation obtainable from a series of CPMAS spectra; and (iii) quantitation not possible using CPMAS. Strategies for the measurement of sample parameters T_CH and Ti_pH are reviewed. When quantitation is not possible using CPMAS it is necessary to regress to the direct polarization (DP) of ¹³C nuclei. The sensitivity problems of DPMAS are discussed, as too are general factors that affect the quantitation of ¹³C data such as spinning sidebands. More specifically in relation to soil samples, the effects on quantitation arising from the presence of paramagnetics and the actual methods for the measurement of signal intensities are covered.