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Characterization of lignin using multi-angle laser light scattering and atomic force microscopy
Authors:Aarti V. Gidh  Stephen R. Decker
Affiliation:a National Bioenergy Center, National Renewable Energy Laboratory, Golden, CO 80401, USA
b Department of Chemical Engineering, University of Mississippi, 134, Anderson Hall, P.O. Box 8304, MS 38677, USA
Abstract:Small differences in the isolation techniques of lignin can result in significant changes in its molecular structure and configuration. Light scattering (evaluated at 18 different angles in a plane), Atomic Force Microscopy (AFM) and Near Infrared Spectroscopy (NIR) proved very effective for evaluating the characteristics of lignin. Zimm plots were generated using Zimm, Debye and Berry formalisms to evaluate the weight average molecular weight (MW), radius of gyration (rg), hydrodynamic radius (rh) and second virial coefficient (A2). Two types of lignin and nine different solvents were used for the study, to analyze the conformation of lignin molecules in different solvents expected to be used in lignin degradation and subsequent analysis. Absolute MW and rg decreased and the dn/dc increased when the solvent used for lignin was changed from water to sodium hydroxide. The two types of lignin also exhibited different values for all the above estimated parameters. This study also highlighted the differences between the unlyophilized and lyophilized lignin in terms of aggregation, pH dependence and stability over time. This aggregation has never been seen on a ultraviolet (UV) or refractive index (RI) detector that has been used so far for liquid chromatography (LC) reducing the reliability of lignin depolymerization data obtained without light scattering.
Keywords:NL, NREL lyophilized lignin   NREL, second batch of NREL lyophilized lignin   LL, NREL unlyophilized lignin   pH 12, lignin dissolved in 0.1   N NaOH titrated down to pH 12   pH 14, untitrated 0.1   N NaOH
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