Advancing Molecular Weight Determination of Lignin by Multi-Angle Light Scattering

Clobes, Mason L.; Kozliak, Evguenii I.; Kubátová, Alena

doi:10.3390/polym16040477

Title: Advancing Molecular Weight Determination of Lignin by Multi-Angle Light Scattering

Journal Article · 01 February 2024 · Polymers

DOI: https://doi.org/10.3390/polym16040477 · OSTI ID:2293611

Clobes, Mason L. ^[1]; Kozliak, Evguenii I. ^[1];

^[1]

Univ. of North Dakota, Grand Forks, ND (United States)

Due to the complexity and recalcitrance of lignin, its chemical characterization is a key factor preventing the valorization of this abundant material. Multi-angle light scattering (MALS) is becoming a sought-after technique for absolute molecular weight (MW) determination of polymers and proteins. Lignin is a suitable candidate for MW determination via MALS, yet further investigation is required to confirm its absolute MW values and molecular size. Studies aiming to break down lignin into a variety of renewable products will benefit greatly from a simple and reliable determination method like MALS. Recent pioneering studies, discussed in this review, addressed several key challenges in lignin’s MW characterization. Nevertheless, some lignin-specific issues still need to be considered for in-depth characterization. This study explores how MALS instrumentation manages the complexities of determining lignin’s MW, e.g., with simultaneous fractionation and fluorescence interference mitigation. Additionally, we rationalize the importance of a more detailed light scattering analysis for lignin characterization, including aspects like the second virial coefficient and radius of gyration.

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Research Organization:: Univ. of North Dakota, Grand Forks, ND (United States)

Sponsoring Organization:: USDOE Office of Energy Efficiency and Renewable Energy (EERE); USDOE

Grant/Contract Number:: EE0009257

OSTI ID:: 2293611

Alternate ID(s):: OSTI ID: 2472305

Journal Information:: Polymers, Vol. 16, Issue 4; ISSN 2073-4360

Publisher:: MDPICopyright Statement

Country of Publication:: United States

Language:: English

References (62)

A review on the catalytic hydrodeoxygenation of lignin-derived phenolic compounds and the conversion of raw lignin to hydrocarbon liquid fuels Shu, Riyang; Li, Rongxuan; Lin, Biqin Biomass and Bioenergy, Vol. 132 https://doi.org/10.1016/j.biombioe.2019.105432	journal	January 2020
A review for lignin valorization: Challenges and perspectives in catalytic hydrogenolysis Ye, Ke; Liu, Ying; Wu, Shubin Industrial Crops and Products, Vol. 172 https://doi.org/10.1016/j.indcrop.2021.114008	journal	November 2021
The full-length cytochrome P450 enzyme CYP102A1 dimerizes at its reductase domains and has flexible heme domains for efficient catalysis Zhang, Haoming; Yokom, Adam L.; Cheng, Shen Journal of Biological Chemistry, Vol. 293, Issue 20 https://doi.org/10.1074/jbc.RA117.000600	journal	May 2018
SEC-MALS method for the determination of long-chain branching and long-chain branching distribution in polyethylene Yu, Youlu; DesLauriers, Paul J.; Rohlfing, David C. Polymer, Vol. 46, Issue 14 https://doi.org/10.1016/j.polymer.2005.04.036	journal	June 2005
The Effect of the Kraft Pulping Process, Wood Species, and pH on Lignin Recovery from Black Liquor Jardim, Juliana M.; Hart, Peter W.; Lucia, Lucian A. Fibers, Vol. 10, Issue 2 https://doi.org/10.3390/fib10020016	journal	February 2022
Hydrothermal Decomposition of a Lignin Dimer under Neutral and Basic Conditions: A Mechanism Study Nagel, Eric; Zhang, Cheng Industrial & Engineering Chemistry Research, Vol. 58, Issue 40 https://doi.org/10.1021/acs.iecr.9b00400	journal	September 2019
Method for Improved Fluorescence Corrections for Molar Mass Characterization by Multiangle Light Scattering Pittman, Zachariah A.; McCarthy, Madeline E.; Birtwistle, Marc R. Biomacromolecules, Vol. 23, Issue 9 https://doi.org/10.1021/acs.biomac.2c00600	journal	August 2022
Catalytic lignin valorisation by depolymerisation, hydrogenation, demethylation and hydrodeoxygenation: Mechanism, chemical reaction kinetics and transport phenomena Ročnik, Tina; Likozar, Blaž; Jasiukaitytė-Grojzdek, Edita Chemical Engineering Journal, Vol. 448 https://doi.org/10.1016/j.cej.2022.137309	journal	November 2022
Thermal Liquefaction of Lignin to Aromatics: Efficiency, Selectivity, and Product Analysis Kozliak, Evguenii I.; Kubátová, Alena; Artemyeva, Anastasia A. ACS Sustainable Chemistry & Engineering, Vol. 4, Issue 10 https://doi.org/10.1021/acssuschemeng.6b01046	journal	August 2016
Silver and gold nanoparticles characterization by SP-ICP-MS and AF4-FFF-MALS-UV-ICP-MS in human samples used for biomonitoring Bocca, Beatrice; Battistini, Beatrice; Petrucci, Francesco Talanta, Vol. 220 https://doi.org/10.1016/j.talanta.2020.121404	journal	December 2020
Asymmetric Flow Field-Flow Fractionation: Current Status, Possibilities, Analytical Limitations and Future Trends Podzimek, Stepan; Johann, Christoph Chromatographia, Vol. 84, Issue 6 https://doi.org/10.1007/s10337-021-04035-w	journal	March 2021
Biomass-derived lignin to jet fuel range hydrocarbons via aqueous phase hydrodeoxygenation Wang, Hongliang; Ruan, Hao; Pei, Haisheng Green Chemistry, Vol. 17, Issue 12 https://doi.org/10.1039/C5GC01534K	journal	January 2015
Green and sustainable route for oxidative depolymerization of lignin: New platform for fine chemicals and fuels Kumaravel, Sangeetha; Thiruvengetam, Prabaharan; Karthick, Kannimuthu Biotechnology Progress, Vol. 37, Issue 2 https://doi.org/10.1002/btpr.3111	journal	December 2020
An insight into the OPAHs and SPAHs formation mechanisms during alkaline lignin pyrolysis at different temperatures Xiao, Lingfeng; Hu, Song; Han, Hengda Journal of Analytical and Applied Pyrolysis, Vol. 156 https://doi.org/10.1016/j.jaap.2021.105104	journal	June 2021
Microbial lignin valorization through depolymerization to aromatics conversion Li, Fei; Zhao, Yiquan; Xue, Le Trends in Biotechnology, Vol. 40, Issue 12 https://doi.org/10.1016/j.tibtech.2022.09.009	journal	December 2022
Size exclusion chromatography of lignin: The mechanistic aspects and elimination of undesired secondary interactions Andrianova, Anastasia A.; Yeudakimenka, Natallia A.; Lilak, Samuel L. Journal of Chromatography A, Vol. 1534 https://doi.org/10.1016/j.chroma.2017.12.051	journal	January 2018
Light Scattering, Size Exclusion Chromatography and Asymmetric Flow Field Flow Fractionation Podzimek, Stepan Wiley https://doi.org/10.1002/9780470877975	journal	February 2011
Applications of Mass Spectrometry in the Onset of Amyloid Fibril Formation: Focus on the Analysis of Early-Stage Oligomers Hu, Jiaojiao; Zheng, Qiuling Frontiers in Chemistry, Vol. 8 https://doi.org/10.3389/fchem.2020.00324	journal	May 2020
Off-line comprehensive size exclusion chromatography × reversed-phase liquid chromatography coupled to high resolution mass spectrometry for the analysis of lignocellulosic biomass products Dubuis, Alexis; Le Masle, Agnès; Chahen, Ludovic Journal of Chromatography A, Vol. 1609 https://doi.org/10.1016/j.chroma.2019.460505	journal	January 2020
Catalytic C–O bond cleavage in a β-O-4 lignin model through intermolecular hydrogen transfer Ahsan Usman, Muhammad; Naeem, Maham; Saeed, Muhammad Inorganica Chimica Acta, Vol. 521 https://doi.org/10.1016/j.ica.2021.120305	journal	June 2021
Rapid quantification and characterization of the pyrolytic lignin fraction of bio-oils by size exclusion chromatography coupled with multi-angle laser light scattering detector (SEC-MALS) Ruiz, Miguel; Valette, Jeremy; Broust, Francois Journal of Analytical and Applied Pyrolysis, Vol. 142 https://doi.org/10.1016/j.jaap.2019.104662	journal	September 2019
Influence of nonrubber components on properties of unvulcanized natural rubber Nun‐anan, Phattarawadee; Wisunthorn, Suwaluk; Pichaiyut, Skulrat Polymers for Advanced Technologies, Vol. 31, Issue 1 https://doi.org/10.1002/pat.4746	journal	August 2019
Characterisation of selenium and tellurium nanoparticles produced by Aureobasidium pullulans using a multi-method approach Nwoko, Kenneth C.; Liang, Xinjin; Perez, Magali AMJ Journal of Chromatography A, Vol. 1642 https://doi.org/10.1016/j.chroma.2021.462022	journal	April 2021
Physical Properties of Sodium Poly(styrene sulfonate): Comparison to Incompletely Sulfonated Polystyrene Balding, Paul; Borrelli, Rachel; Volkovinsky, Ron Macromolecules, Vol. 55, Issue 5 https://doi.org/10.1021/acs.macromol.1c01065	journal	February 2022
Molar mass determination of lignins and characterization of their polymeric structures by multi-detector gel permeation chromatography Gaugler, Evamaria C.; Radke, Wolfgang; Vogt, Andrew P. Journal of Analytical Science and Technology, Vol. 12, Issue 1 https://doi.org/10.1186/s40543-021-00283-5	journal	July 2021
Aptamer–Target–Gold Nanoparticle Conjugates for the Quantification of Fumonisin B1 Mirón-Mérida, Vicente Antonio; González-Espinosa, Yadira; Collado-González, Mar Biosensors, Vol. 11, Issue 1 https://doi.org/10.3390/bios11010018	journal	January 2021
How is the z‐Average Molar Mass Related to the Sedimentation Data? Ye, Xiaodong; Chen, Yonggang; Wu, Chi Macromolecular Chemistry and Physics, Vol. 224, Issue 3 https://doi.org/10.1002/macp.202200331	journal	November 2022
Hydrogenolysis of Lignin-Derived Aromatic Ethers over Heterogeneous Catalysts Shivhare, Atal; Jampaiah, Deshetti; Bhargava, Suresh K. ACS Sustainable Chemistry & Engineering, Vol. 9, Issue 9 https://doi.org/10.1021/acssuschemeng.0c06715	journal	February 2021
Perspective on Technical Lignin Fractionation Sadeghifar, Hasan; Ragauskas, Arthur ACS Sustainable Chemistry & Engineering, Vol. 8, Issue 22 https://doi.org/10.1021/acssuschemeng.0c01348	journal	May 2020
Modification of Poly(lactic acid) by the Plasticization for Application in the Packaging Industry Gzyra-Jagieła, Karolina; Sulak, Konrad; Draczyński, Zbigniew Polymers, Vol. 13, Issue 21 https://doi.org/10.3390/polym13213651	journal	October 2021
Comparative study of the microstructure of solid rubber from Ficus carica and Hevea brasiliensis Yokota‐Imai, Saki; Chida, Shinsuke; Suzuki, Takehiro Polymers for Advanced Technologies, Vol. 32, Issue 11 https://doi.org/10.1002/pat.5441	journal	July 2021
Milled Wood Lignin: A Linear Oligomer Crestini, Claudia; Melone, Federica; Sette, Marco Biomacromolecules, Vol. 12, Issue 11 https://doi.org/10.1021/bm200948r	journal	November 2011
High-Resolution Profiling of the Functional Heterogeneity of Technical Lignins Musl, Oliver; Galler, Samira; Wurzer, Gerhild Biomacromolecules, Vol. 23, Issue 3 https://doi.org/10.1021/acs.biomac.1c01630	journal	February 2022
Size distribution and chain conformation of six different fucoidans using size-exclusion chromatography with multiple detection Neupane, Sandesh; Bittkau, Kaya Saskia; Alban, Susanne Journal of Chromatography A, Vol. 1612 https://doi.org/10.1016/j.chroma.2019.460658	journal	February 2020
Hydrothermal Liquefaction of Lignin to Aromatic Chemicals: Impact of Lignin Structure Cao, Yang; Zhang, Cheng; Tsang, Daniel C. W. Industrial & Engineering Chemistry Research, Vol. 59, Issue 39 https://doi.org/10.1021/acs.iecr.0c01617	journal	May 2020
Formic-acid-induced depolymerization of oxidized lignin to aromatics Rahimi, Alireza; Ulbrich, Arne; Coon, Joshua J. Nature, Vol. 515, Issue 7526, p. 249-252 https://doi.org/10.1038/nature13867	journal	November 2014
Benchtop versus high field NMR: Comparable performance found for the molecular weight determination of lignin Burger, René; Lindner, Simon; Rumpf, Jessica Journal of Pharmaceutical and Biomedical Analysis, Vol. 212 https://doi.org/10.1016/j.jpba.2022.114649	journal	April 2022
Base promoted hydrogenolysis of lignin model compounds and organosolv lignin over metal catalysts in water Konnerth, Hannelore; Zhang, Jiaguang; Ma, Ding Chemical Engineering Science, Vol. 123 https://doi.org/10.1016/j.ces.2014.10.045	journal	February 2015
Depolymerization and conversion of lignin to value-added bioproducts by microbial and enzymatic catalysis Weng, Caihong; Peng, Xiaowei; Han, Yejun Biotechnology for Biofuels, Vol. 14, Issue 1 https://doi.org/10.1186/s13068-021-01934-w	journal	April 2021
Economical concerns of lignin in the energy sector Sharma, Archita; Kaur, Pritam; Singh, Gursharan Cleaner Engineering and Technology, Vol. 4 https://doi.org/10.1016/j.clet.2021.100258	journal	October 2021
Ni-Catalyzed Cleavage of Aryl Ethers in the Aqueous Phase He, Jiayue; Zhao, Chen; Lercher, Johannes A. Journal of the American Chemical Society, Vol. 134, Issue 51, p. 20768-20775 https://doi.org/10.1021/ja309915e	journal	December 2012
Fractionation of Lignin with Decreased Heterogeneity: Based on a Detailed Characteristics Study of Sequentially Extracted Softwood Kraft Lignin Liu, Rui; Smeds, Annika; Wang, Luyao ACS Sustainable Chemistry & Engineering, Vol. 9, Issue 41 https://doi.org/10.1021/acssuschemeng.1c04725	journal	October 2021
Characterization of Polymer Molecular Weight Distribution by NMR Diffusometry: Experimental Criteria and Findings Hou, Jianbo; Pearce, Eric Analytical Chemistry, Vol. 93, Issue 22 https://doi.org/10.1021/acs.analchem.1c00793	journal	May 2021
Measurement of Special Nanoparticle Structures by Light Scattering Wyatt, Philip J. Analytical Chemistry, Vol. 86, Issue 15 https://doi.org/10.1021/ac500185w	journal	July 2014
Revisiting the Molar Mass and Conformation of Derivatized Fractionated Softwood Kraft Lignin Ji, Lun; Liu, Li-Yang; Cho, Mijung Biomacromolecules, Vol. 23, Issue 3 https://doi.org/10.1021/acs.biomac.1c01101	journal	December 2021
Characterization of Lignin Compounds at the Molecular Level: Mass Spectrometry Analysis and Raw Data Processing Zhang, Ruochun; Qi, Yulin; Ma, Chao Molecules, Vol. 26, Issue 1 https://doi.org/10.3390/molecules26010178	journal	January 2021
Reductive or oxidative catalytic lignin depolymerization: An overview of recent advances Bourbiaux, Dolorès; Pu, Junjie; Rataboul, Franck Catalysis Today, Vol. 373 https://doi.org/10.1016/j.cattod.2021.03.027	journal	August 2021
Improving liquid chromatography-mass spectrometry sensitivity for characterization of lignin oligomers and phenolic compounds using acetic acid as a mobile phase additive Song, Woo-Young; Park, Hyejin; Kim, Tae-Young Journal of Chromatography A, Vol. 1685 https://doi.org/10.1016/j.chroma.2022.463598	journal	December 2022
Electrospray Ionization with High-Resolution Mass Spectrometry as a Tool for Lignomics: Lignin Mass Spectrum Deconvolution Andrianova, Anastasia A.; DiProspero, Thomas; Geib, Clayton Journal of The American Society for Mass Spectrometry, Vol. 29, Issue 5 https://doi.org/10.1007/s13361-018-1916-z	journal	March 2018
Characterization of lignin using multi-angle laser light scattering and atomic force microscopy Gidh, Aarti V.; Decker, Stephen R.; See, Chun H. Analytica Chimica Acta, Vol. 555, Issue 2 https://doi.org/10.1016/j.aca.2005.09.023	journal	January 2006
Is NMR Combined with Multivariate Regression Applicable for the Molecular Weight Determination of Randomly Cross-Linked Polymers Such as Lignin? Burger, René; Rumpf, Jessica; Do, Xuan Tung ACS Omega, Vol. 6, Issue 44 https://doi.org/10.1021/acsomega.1c03574	journal	October 2021
New Insights into Green Protocols for Oxidative Depolymerization of Lignin and Lignin Model Compounds Scimmi, Cecilia; Sancineto, Luca; Drabowicz, Jozef International Journal of Molecular Sciences, Vol. 23, Issue 8 https://doi.org/10.3390/ijms23084378	journal	April 2022
Absolute molar mass determination in mixed solvents. 2. SEC/MALS/DRI in a mix of two “nearly-isovirial” solvents Striegel, André M. Analytica Chimica Acta, Vol. 1231 https://doi.org/10.1016/j.aca.2022.340369	journal	October 2022
Reactivity of lignin model compounds through hydrogen transfer catalysis in ethanol/water mixtures Besse, Xavier; Schuurman, Yves; Guilhaume, Nolven Applied Catalysis B: Environmental, Vol. 209 https://doi.org/10.1016/j.apcatb.2017.03.013	journal	July 2017
Fractionation and Absolute Molecular Weight Determination of Organosolv Lignin and Its Fractions: Analysis by a Novel Acetone-Based SEC─MALS Method Ponnudurai, Arulselvan; Schulze, Peter; Seidel-Morgenstern, Andreas ACS Sustainable Chemistry & Engineering, Vol. 11, Issue 2 https://doi.org/10.1021/acssuschemeng.2c06309	journal	December 2022
A concise review of current lignin production, applications, products and their environmental impact Bajwa, D. S.; Pourhashem, G.; Ullah, A. H. Industrial Crops and Products, Vol. 139 https://doi.org/10.1016/j.indcrop.2019.111526	journal	November 2019
Molar Mass Characterization of Crude Lignosulfonates by Asymmetric Flow Field-Flow Fractionation Sulaeva, Irina; Vejdovszky, Philipp; Henniges, Ute ACS Sustainable Chemistry & Engineering, Vol. 7, Issue 1 https://doi.org/10.1021/acssuschemeng.8b02856	journal	November 2018
Characteristics and evolution of heavy components in bio-oil from the pyrolysis of cellulose, hemicellulose and lignin Zhong, Dian; Zeng, Kuo; Li, Jun Renewable and Sustainable Energy Reviews, Vol. 157 https://doi.org/10.1016/j.rser.2021.111989	journal	April 2022
Getting Closer to Absolute Molar Masses of Technical Lignins Zinovyev, Grigory; Sulaeva, Irina; Podzimek, Stepan ChemSusChem, Vol. 11, Issue 18 https://doi.org/10.1002/cssc.201801177	journal	August 2018
Hydrothermal conversion of lignin: A review Kang, Shimin; Li, Xianglan; Fan, Juan Renewable and Sustainable Energy Reviews, Vol. 27 https://doi.org/10.1016/j.rser.2013.07.013	journal	November 2013
Challenges in industrial applications of technical lignins Vishtal, Alexey; Kraslawski, Andrzej BioResources, Vol. 6, Issue 3 https://doi.org/10.15376/biores.6.3.3547-3568	journal	June 2011
Unfolding of Lignin Structure Using Size-Exclusion Fractionation LaVallie, Audrey; Andrianova, Anastasia A.; Schumaker, Joshua Polymers, Vol. 15, Issue 19 https://doi.org/10.3390/polym15193956	journal	September 2023

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36 MATERIALS SCIENCE
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
multi-angle light scattering
technical lignin
radius of gyration
second virial coefficient
differential refractive index increment
Rayleigh–Gans approximation

Title: Advancing Molecular Weight Determination of Lignin by Multi-Angle Light Scattering

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