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

doi:10.1002/cssc.201600135

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

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In 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. Moreover, 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. Furthermore, it also allows analyzing biomass with a room-temperature NMR probe instead of cryo-probes, which are traditionally used for enhancing signal intensities.

Authors:

Pu, Yunqiao ^[1] ; Ragauskas, Arthur J. ^[2] ; Yoo, Chang Geun ^[1] ; Li, Mi ^[1]

Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Univ. of Tennessee, Knoxville, TN (United States)

Publication Date:: 2016-04-26

Grant/Contract Number:: AC05-00OR22725

Type:: Accepted Manuscript

Journal Name:: ChemSusChem

Additional Journal Information:: Journal Volume: 9; Journal Issue: 10; Journal ID: ISSN 1864-5631

Publisher:: ChemPubSoc Europe

Research Org:: Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). BioEnergy Science Center (BESC)

Sponsoring Org:: USDOE Office of Science (SC)

Country of Publication:: United States

Language:: English

Subject:: 09 BIOMASS FUELS

OSTI Identifier:: 1261570

Alternate Identifier(s):: OSTI ID: 1401664


                    Pu, Yunqiao, Ragauskas, Arthur J., Yoo, Chang Geun, and Li, Mi. Elucidating structural characteristics of biomass using solution-state 2 D NMR with a mixture of deuterated dimethylsulfoxide and hexamethylphosphoramide.  United States: N. p.,  
        Web.  doi:10.1002/cssc.201600135.

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                    Pu, Yunqiao, Ragauskas, Arthur J., Yoo, Chang Geun, & Li, Mi. Elucidating structural characteristics of biomass using solution-state 2 D NMR with a mixture of deuterated dimethylsulfoxide and hexamethylphosphoramide.  United States.  doi:10.1002/cssc.201600135.

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                    Pu, Yunqiao, Ragauskas, Arthur J., Yoo, Chang Geun, and Li, Mi. 2016.  
        "Elucidating structural characteristics of biomass using solution-state 2 D NMR with a mixture of deuterated dimethylsulfoxide and hexamethylphosphoramide".  United States.  
        doi:10.1002/cssc.201600135.  https://www.osti.gov/servlets/purl/1261570.

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@article{osti_1261570,

  title        = {Elucidating structural characteristics of biomass using solution-state 2 D NMR with a mixture of deuterated dimethylsulfoxide and hexamethylphosphoramide},

  author       = {Pu, Yunqiao and Ragauskas, Arthur J. and Yoo, Chang Geun and Li, Mi},

  abstractNote = {In 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-d6) and hexamethylphosphoramide (HMPA-d18). HMPA as a co-solvent enhanced swelling and mobility of the biomass samples; thereby it allowed enhancing signals of NMR spectra. Moreover, the structural information of biomass was successfully analyzed by the proposed NMR solvent system (DMSO-d6/HMPA-d18; 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. Furthermore, it also allows analyzing biomass with a room-temperature NMR probe instead of cryo-probes, which are traditionally used for enhancing signal intensities.},

  doi          = {10.1002/cssc.201600135},

  journal      = {ChemSusChem},

  number       = 10,

  volume       = 9,

  place        = {United States},

  year         = {2016},

  month        = {4}

}

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

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