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A Study on Water Adsorption onto Microcrystalline Cellulose by Near-Infrared Spectroscopy with Two-Dimensional Correlation Spectroscopy and Principal Component Analysis

Volume 60, Number 9 (Sept. 2006) Page 1054-1061

Watanabe, Akihiko; Morita, Shigeaki; Ozaki, Yukihiro


Water adsorption onto microcrystalline cellulose (MCC) in the moisture content (Mc) range of 0.2-13.4 wt % was investigated by near-infrared (NIR) spectroscopy. In order to distinguish heavily overlapping O-H stretching bands in the NIR region due to MCC and water, principal component analysis (PCA) and generalized two-dimensional correlation spectroscopy (2DCOS) were applied to the obtained spectra. The NIR spectra in four adsorption stages separated by PCA were analyzed by 2DCOS. For the low Mc range of 0.2-3.1 wt %, a decrease in the free or weakly hydrogen-bonded (H-bonded) MCC OH band, increases in the H-bonded MCC OH bands, and increases in the adsorbed water OH bands are observed. These results suggest that the inter- and intrachain H-bonds of MCC are formed by monomeric water molecule adsorption. In the Mc range of 3.8-7.1 wt %, spectral changes in the NIR spectra reveal that the aggregation of water molecules starts at the surface of MCC. For the high Mc range of 8.1-13.4 wt %, the NIR results suggest that the formation of bulk water occurs. It is revealed from the present study that approximately 3-7 wt % of adsorbed water is responsible for the stabilization of the H-bond network in MCC at the cellulose-water surface.