Solid-state C-13 CP/MAS NMR for Alkyl-O-Aryl bond determination in lignin preparations

A1 Journal article (refereed)


Internal Authors/Editors


Publication Details

List of Authors: Edward I. Evstigneyev, Anton S. Mazur, Aleksandra V. Kalugina, Andrey V. Pranovich, Aleksander V. Vasilyev
Publisher: Taylor & Francis, Inc.
Publication year: 2018
Journal: Journal of Wood Chemistry and Technology
Journal acronym: J. Wood Chem. Technol.
Volume number: 38
Issue number: 2
Start page: 137
End page: 148
Number of pages: 12
ISSN: 0277-3813
eISSN: 1532-2319


Abstract

Several lignin preparations (Freudenberg lignin, Björkman lignin, and Pepper lignin), technical lignins (soda, soda-AQ, Kraft, Kraft-AQ, and hydrolysis), dimeric lignin model compounds, and different polysaccharides (galactoglucomannan, arabinogalactan, xylan, and arabinan) were analyzed by means of solid-state 13C CP/MAS NMR. Signals assignment in solid-state NMR lignin spectra was performed on the basis of the conducted studies and earlier published data. It was established that there exists strong linear correlation (r = 0.985) between Alkyl-O-Aryl inter-unit bond content in lignin and integral signals intensity in NMR spectra in the range of chemical shifts of 96–68 ppm. The integral signals intensity was measured in correlation with the reference integral signals in the range of chemical shifts of 162–102 ppm, typical for aromatic carbon atoms. To eliminate the effect, caused by carbohydrates contained in lignin, the correction factor of 0.67% of the area of integration per 1% of carbohydrates was determined. It was shown that the solid-state 13C CP/MAS NMR method allowed to determine Alkyl-O-Aryl bond content in both soluble and insoluble lignin preparations, and also to determine methoxyl groups content in soluble preparations.


Keywords

Alkyl-O-Aryl bonds, lignins, MAS NMR, methoxyl groups, Solid-state C-13 CP


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