Separating subspectra from cross-polarization magic-angle spinning nuclear magnetic resonance spectra by proton spin relaxation editing

Abstract

Differences in proton spin relaxation time constants can be exploited to edit cross-polarization magic-angle spinning nuclear magnetic resonance (CP-MAS NMR) spectra of heterogeneous mixtures of different types of organic matter. This paper describes an extension of the editing procedure from two-component to three-component mixtures. Clean separation of 13C NMR subspectra was achieved for three synthetic polymers mixed as powders. Applying the procedure to both 13C and 31P CP-MAS NMR spectra of solid dairy pond sludge provided clues to the location of the phosphorus relative to different types of organic matter, and provided estimates of the proportions of organic matter in categories labeled “plant fragments”, “partly degraded residues” and “recalcitrant structures”. The editing procedure increased noise levels by factors between 2 and 11 in these worked examples, depending on the degree of difficulty involved in distinguishing differences in proton spin relaxation time constants.