4.7 Article

Hydration properties of regioselectively etherified celluloses monitored by 2H and 13C solid-state MAS NMR spectroscopy

Journal

CARBOHYDRATE POLYMERS
Volume 89, Issue 2, Pages 640-647

Publisher

ELSEVIER SCI LTD
DOI: 10.1016/j.carbpol.2012.03.067

Keywords

2,3-O-hydroxypropylcellulose; 2,3-O-hydroxyethylcellulose; Solid-state; NMR; Hydration; Regioselective

Funding

  1. Danish Council for Strategic Research [2108-08-0068]

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The hydration properties of 2,3-O-hydroxypropylcellulose (HPC) and 2,3-O-hydroxyethylcellulose (HEC) were analyzed by multi-nuclear solid-state MAS NMR spectroscopy. By C-13 single-pulse (SP) MAS and cross-polarization (CP) MAS NMR, differences between the immobile regions and all parts of the polysaccharides were detected as a function of hydration. Complementary information about the water environments was observed by H-2 MAS NMR. By this approach it was demonstrated that side chains in 2,3-O-HPC and 2,3-O-HEC were easier to hydrate than the cellulose backbone. Furthermore the motion of water was more restricted (slower) in 2,3-O-HPC than in 2,3-O-HEC. For both polysaccharides the hydration could be explained by a two-step process: in step one increased ordering of the immobile regions occurs after which the entire polymer is hydrated in step two. (C) 2012 Elsevier Ltd. All rights reserved.

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