13C NMR analysis of cellulose samples from different preparation methods

Abstract

Alpha-cellulose is a part of the wooden material that preserves isotopic composition during tree-growth, and therefore provides important indirect data for paleoclimatological studies. For this reason, it is exceptionally important to extract the alpha-cellulose component from plants, e.g. from tree rings of wood. Since the cell wall of plant cells consists of multicomponent polysaccharides, the extraction of cellulose from wood is not an obvious task. In this paper, we describe, evaluate and compare nine methods, based on the literature and experimental observations, for obtaining cellulose from tree rings of wood. We show that the distortionless enhancement by polarization transfer (DEPT-135) variant of liquid-state 13C NMR spectroscopy is a powerful analytical method for monitoring the preparation process. Trifluoroacetic acid was applied as solvent for the NMR analysis. We proved that all the preparation methods give pure cellulose samples without hemicellulose and lignin content, and we propose methods resulting in non-fragmented cellulose. 13C and 18O isotope ratio measurements have shown that all the applied extraction methods result in similar isotope ratios, thus they are suitable for paleoclimatological studies.