skip to main content
OSTI.GOV title logo U.S. Department of Energy
Office of Scientific and Technical Information

Title: Elucidating structural characteristics of biomass using solution-state 2 D NMR with a mixture of deuterated dimethylsulfoxide and hexamethylphosphoramide

Journal Article · · ChemSusChem
 [1];  [2];  [1];  [1]
  1. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
  2. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Univ. of Tennessee, Knoxville, TN (United States)
+ Show Author Affiliations

Abstract 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.

Research Organization:
Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States). BioEnergy Science Center (BESC)
Sponsoring Organization:
USDOE Office of Science (SC)
Grant/Contract Number:
AC05-00OR22725
OSTI ID:
1261570
Alternate ID(s):
OSTI ID: 1401664
Journal Information:
ChemSusChem, Vol. 9, Issue 10; ISSN 1864-5631
Publisher:
ChemPubSoc EuropeCopyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 52 works
Citation information provided by
Web of Science

References (33)

Lignin degradation in wood-feeding insects journal August 2008
Cellulose I crystallinity determination using FT–Raman spectroscopy: univariate and multivariate methods journal May 2010
Analysis of biomass sugars using a novel HPLC method journal March 2007
Assessing the molecular structure basis for biomass recalcitrance during dilute acid and hydrothermal pretreatments journal January 2013
NMR characterization of lignins in Arabidopsis altered in the activity of ferulate 5-hydroxylase journal October 1999
High-resolution Thermogravimetric Analysis For Rapid Characterization of Biomass Composition and Selection of Shrub Willow Varieties journal October 2007
Non-degradative dissolution and acetylation of ball-milled plant cell walls: high-resolution solution-state NMR journal August 2003
Bt corn has a higher lignin content than non- Bt corn journal September 2001
Whole plant cell wall characterization using solution-state 2D NMR journal August 2012
2D-NMR (HSQC) difference spectra between specifically 13C-enriched and unenriched protolignin of Ginkgo biloba obtained in the solution state of whole cell wall material journal July 2009
Hexamethylphosphoramide. An Aprotic Solvent for Active Metals journal March 1965
Evaluation of FT-IR and Nile Red methods for microalgal lipid characterization and biomass composition determination journal January 2013
Cyanoethylated cellulose prepared by homogeneous reaction in paraformaldehyde-DMSO system journal August 1986
Effect of acetyl groups on enzymatic hydrolysis of cellulosic substrates journal July 2006
Effect of reduced ferulate-mediated lignin/arabinoxylan cross-linking in corn silage on feed intake, digestibility, and milk production journal October 2011
Determination of Arylglycerol−β-Aryl Ether Linkages in Enzymatic Mild Acidolysis Lignins (EMAL): Comparison of DFRC/ 31 P NMR with Thioacidolysis ⊥ journal May 2008
High Resolution Solid State 2D NMR Analysis of Biomass and Biochar journal December 2014
Solution-state 2D NMR of ball-milled plant cell wall gels in DMSO-d6/pyridine-d5 journal January 2010
Quantifying Biomass Composition by Gas Chromatography/Mass Spectrometry journal September 2014
HSQC (heteronuclear single quantum coherence) 13C–1H correlation spectra of whole biomass in perdeuterated pyridinium chloride–DMSO system: An effective tool for evaluating pretreatment journal September 2011
Dissolution and Gelation of Cellulose in TBAF/DMSO Solutions: The Roles of Fluoride Ions and Water journal September 2009
Physical and chemical characterizations of corn stover and poplar solids resulting from leading pretreatment technologies journal September 2009
133Cs NMR study of Cs+ ion complexes with dibenzo-21-crown-7 and dibenzo-24-crown-8 in some mixed solvents journal January 1986
Solution-state 2D NMR of Ball-milled Plant Cell Wall Gels in DMSO-d 6 journal March 2008
Perdeuterated pyridinium molten salt (ionic liquid) for direct dissolution and NMR analysis of plant cell walls journal January 2009
Individual Contribution of Grain Outer Layers and Their Cell Wall Structure to the Mechanical Properties of Wheat Bran journal March 2003
Isolation and Structural Characterization of the Milled Wood Lignin, Dioxane Lignin, and Cellulolytic Lignin Preparations from Brewer’s Spent Grain journal January 2015
Swelling of Wood. Part II. Swelling in Organic Liquids journal January 1994
Differences in the chemical structure of the lignins from sugarcane bagasse and straw journal October 2015
Solvents applied in the field of cellulose chemistry: a mini review journal June 2005
Variations in Cellulosic Ultrastructure of Poplar journal October 2009
Thermodynamic properties of binary mixtures: Hexamethylphosphoric triamide + a polar liquid at 25�C journal February 1994
A gel-state 2D-NMR method for plant cell wall profiling and analysis: a model study with the amorphous cellulose and xylan from ball-milled cotton linters journal January 2014

Cited By (13)

The effect of liquid hot water pretreatment on the chemical–structural alteration and the reduced recalcitrance in poplar journal November 2017
Determination of hydroxyl groups in biorefinery resources via quantitative 31P NMR spectroscopy journal August 2019
PdWND3A, a wood-associated NAC domain-containing protein, affects lignin biosynthesis and composition in Populus journal November 2019
Fractionation and characterization of lignin streams from unique high-lignin content endocarp feedstocks journal November 2018
Cellulolytic enzyme-aided extraction of hemicellulose from switchgrass and its characteristics journal January 2019
Impact of Dilute Sulfuric Acid, Ammonium Hydroxide, and Ionic Liquid Pretreatments on the Fractionation and Characterization of Engineered Switchgrass journal August 2017
Integration of renewable deep eutectic solvents with engineered biomass to achieve a closed-loop biorefinery journal June 2019
Current Understanding of the Correlation of Lignin Structure with Biomass Recalcitrance journal November 2016
Ethanol: A Promising Green Solvent for the Deconstruction of Lignocellulose journal September 2018
Downregulation of pectin biosynthesis gene GAUT4 leads to reduced ferulate and lignin-carbohydrate cross-linking in switchgrass journal January 2019
Overexpression of a Domain of Unknown Function 231-containing protein increases O-xylan acetylation and cellulose biosynthesis in Populus journal December 2017
Adding tetrahydrofuran to dilute acid pretreatment provides new insights into substrate changes that greatly enhance biomass deconstruction by Clostridium thermocellum and fungal enzymes journal November 2017
The effect of liquid hot water pretreatment on the chemical–structural alteration and the reduced recalcitrance in poplar text January 2017

Similar Records

Direct hydrogen-1 and phosphorus-31 nuclear magnetic resonance cation solvation study of Al(ClO$sub 4$)$sub 3$, Ga(ClO$sub 4$)$sub 3$, In(ClO$sub 4$)$sub 3$, UO$sub 2$(ClO$sub 4$)$sub 2$, and UO$sub 2$(NO$sub 3$)$sub 2$ in water-acetone-dimethylsulfoxide and water-acetone-hexamethylphosphoramide mixtures
Journal Article · Wed Nov 01 00:00:00 EST 1972 · J. Solution Chem., v. 1, no. 5, pp. 433-444 · OSTI ID:1261570
+1 more
Coal extraction by supersolvents, November 1, 1982-January 31, 1983. [Tetramethyl urea; hexamethylphosphoramide]
Technical Report · Sat Jan 01 00:00:00 EST 1983 · OSTI ID:1261570
Proton magnetic resonance study of ligand exchange on tetrakis (hexamethylphosphoramide) dioxouranium(VI)
Journal Article · Sat Jul 01 00:00:00 EDT 1978 · Inorg. Chem.; (United States) · OSTI ID:1261570

Related Subjects

09 BIOMASS FUELS