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Vibrational spectral signatures of crystalline cellulose using high resolution broadband sum frequency generation vibrational spectroscopy (HR-BB-SFG-VS)

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Abstract

Both the C–H and O–H region spectra of crystalline cellulose were studied using the sub-wavenumber high-resolution broadband sum frequency generation vibrational spectroscopy (HR-BB-SFG-VS) for the first time. The resolution of HR-BB-SFG-VS is about 10-times better than conventional scanning SFG-VS and has the capability of measuring the intrinsic spectral lineshape and revealing many more spectral details. With HR-BB-SFG-VS, we found that in cellulose samples from different sources, including Avicel and cellulose crystals isolated from algae Valonia (Iα) and tunicates (Iβ), the spectral signatures in the O–H region were unique for the two allomorphs, i.e. Iα and Iβ, while the spectral signatures in the C–H regions varied in all samples examined. Even though the origin of the different spectral signatures of the crystalline cellulose in the O–H and C–H vibrational frequency regions are yet to be correlated to the structure of cellulose, these results lead to new spectroscopic methods and opportunities to classify and to understand the basic crystalline structures, as well as variations in polymorphism of the crystalline cellulose.

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Acknowledgments

This work was made possible through the support of the DARPA Young Faculty Award Contract # N66001-11-1-414. Authors also acknowledge the support of Bioproducts, Sciences and Engineering Laboratory, Department of Biosystems Engineering at Washington State University. L. Zhang was partially supported by the grant from the Chinese Scholarship Council (CSC). S.Y. Ding was supported by the BioEnergy Science Center, a DOE Bioenergy Research Center, and the Genomic Science Program (ER65258), both supported by the Office of Biological and Environmental Research in the DOE Office of Science. Part of this work was conducted at the William R. Wiley Environmental Molecular Sciences Laboratory (EMSL), a national scientific user facility located at the Pacific Northwest National Laboratory (PNNL) and sponsored by the Department of Energy’s Office of Biological and Environmental Research (BER). We also thank Dr. Seong Kim (Penn State University) for insightful discussions.

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Author notes

  1. Zhou Lu

    Present address: Beijing National Laboratory for Molecular Sciences, Institute of Chemistry, The Chinese Academy of Sciences, Beijing, 100190, China

  2. Luis Velarde

    Present address: Department of Chemistry, University at Buffalo, The State University of New York, Buffalo, NY, 14260, USA

  3. Yunqiao Pu & Arthur J. Ragauskas

    Present address: Department of Chemical and Biomolecular Engineering, The University of Tennessee, Knoxville, TN, 37996-2200, USA

  4. Shi-You Ding

    Present address: Department of Plant Biology, Michigan State University, East Lansing, MI, 48824-1312, USA

Authors and Affiliations

  1. Bioproduct Sciences and Engineering Laboratory, Department of Biological Systems Engineering, Washington State University, Richland, WA, 99354, USA

    Libing Zhang & Bin Yang

  2. William R. Wiley Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, Richland, WA, 99354, USA

    Zhou Lu, Luis Velarde, Li Fu & Hong-Fei Wang

  3. School of Chemistry and Biochemistry, Georgia Institute of Technology, Atlanta, GA, 30332, USA

    Yunqiao Pu & Arthur J. Ragauskas

  4. Biosciences Center, National Renewable Energy Laboratory, Golden, CO, 80401, USA

    Shi-You Ding

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10570_2015_588_MOESM1_ESM.docx

Table S1 Peak position and relative peak intensity parameters from curve fitting using Lorentzian lineshape profiles (as in Eq. 3 in the main text) of (a) Avicel, (b) cellulose Iα from alga Valonia ventricosa (Glaucocystis (nostochinearum)), and (c) cellulose Iβs from red reef tunicate and (d) Halocynthiaroretzi tunicate within wavelength of 2700–3050 cm−1 and 3200 cm−1–3450 cm−1. (DOCX 156 kb)

10570_2015_588_MOESM2_ESM.docx

Figure S1 (a) Raman spectra of cellulose Iα from alga Valonia ventricosa (Glaucocystis (nostochinearum)) and (b) cellulose Iβ from Halocynthiaroretzi tunicate in the frequency regions of 300 to 1600 cm−1 and 2500 to 3700 cm−1. (DOCX 277 kb)

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Zhang, L., Lu, Z., Velarde, L. et al. Vibrational spectral signatures of crystalline cellulose using high resolution broadband sum frequency generation vibrational spectroscopy (HR-BB-SFG-VS). Cellulose 22, 1469–1484 (2015). https://doi.org/10.1007/s10570-015-0588-0

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