Two-dimensional spin-exchange solid-state NMR studies of 13 C-enriched wood

Abstract

Two-dimensional high-resolution solid-state NMR has been used to study 13C-enriched wood. Wood is a complex material containing three major polymers: cellulose, hemicelluloses and lignin. The use of an enriched 13C-compound allows the observation of intra-molecular spin-diffusion driven by dipolar couplings. Correlations between spins at progressively longer distances have been obtained as the mixing time is increased, corresponding, for each of the separate polymer chains, to intra-unit and then to inter-unit interactions, and in the case of cellulose to inter-chain interactions. A straightforward qualitative analysis of the spin diffusion spectra is shown to yield the assignment of the carbon-13 spectrum. The cellulose resonances can all be sequentially assigned using the spin diffusion experiment. Using the experiments it is shown that, at least on a distance scale of several nanometres explored by the spin diffusion process, the three main components of wood occur in separate phases. Also, a question concerning the structure of the hemicellulose units is resolved by locating the O-acetyl group at the 2-position of the xylan chains.