ATTEMPTS TO IMPROVE SOLID STATE 13C NMR SPECTRA OF WHOLE MINERAL SOILS

Abstract

This study describes a number of different preparation techniques for recording solid state 13C NMR spectra of whole mineral soils. Removal of paramagnetic Fe3+ improves the quality of 13C NMR spectra of whole soils and of particle size fractions. The C:Fe ratio appears to be an important indicator for obtaining satisfactory 13C NMR spectra of whole soils and fractions separated from them. If the C:Fe ratio is >> 1, the quality of the spectrum will be good; if the ratio is > 1, a reasonable spectrum will be obtained, but if the ratio is < 1, the spectrum will be poor. Organic-matter-rich soil and particle size fractions separated by a flotation technique produce well-defined 13C NMR spectra, typical of humic materials. Reduction of C-enriched fractions with sodium dithionite and stannous chloride improves the spectral resolution. The data presented herein show that satisfactory solid state 13C NMR spectra can be run on untreated soil particle size fractions, non-magnetic portions of whole soils, and fractions enriched in soil organic matter by flotation, especially after chemical reduction. Key words: 13C NMR spectroscopy, paramagnetic mineral separation