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Elucidating Structural Characteristics of Biomass using Solution‐State 2 D NMR with a Mixture of Deuterated Dimethylsulfoxide and Hexamethylphosphoramide
Author(s) -
Yoo Chang Geun,
Pu Yunqiao,
Li Mi,
Ragauskas Arthur J.
Publication year - 2016
Publication title -
chemsuschem
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 2.412
H-Index - 157
eISSN - 1864-564X
pISSN - 1864-5631
DOI - 10.1002/cssc.201600135
Subject(s) - hexamethylphosphoramide , chemistry , biomass (ecology) , lignocellulosic biomass , solvent , carbon 13 nmr , derivatization , green chemistry , proton nmr , organic chemistry , reaction mechanism , catalysis , hydrolysis , oceanography , high performance liquid chromatography , geology
Recent developments of NMR methods for characterization of lignocellulosic biomass allow improved understanding of plant cell‐wall structures with minimal deconstruction and modification of biomass. This study introduces a new NMR solvent system composed of dimethylsulfoxide (DMSO‐ d 6 ) and hexamethylphosphoramide (HMPA‐ d 18 ). HMPA as a co‐solvent enhanced swelling and mobility of the biomass samples; thereby it allowed enhancing signals of NMR spectra. The structural information of biomass was successfully analyzed by the proposed NMR solvent system (DMSO‐ d 6 /HMPA‐ d 18 ; 4:1, v / v ) with different biomass. The proposed bi‐solvent system does not require derivatization or isolation of biomass, facilitating a facile sample preparation and involving with no signals overlapping with biomass peaks. It also allows analyzing biomass with a room‐temperature NMR probe instead of cryo‐probes, which are traditionally used for enhancing signal intensities.