Plant Biomass Characterization: Application of Solution‐ and Solid‐State NMR Spectroscopy

Pu, Yunqiao; Hallac, Bassem B.; Ragauskas, Arthur J.

doi:10.1002/9780470975831.ch18

Cited by 32 publications

(36 citation statements)

References 68 publications

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“…22 Among these are milled wood lignin (MWL), 23,24 cellulolytic enzymatic lignin (CEL), 24 kraft lignin, soda lignin, and organosolv lignin, 23 with MWL and CEL considered to retain the native lignin structure. Isolated lignin has been characterized using numerous methods such as solution-and solid-state NMR, [25][26][27] SEC, 28 GC-MS n , LC-MS n , UV-Vis, 29 FTIR, 30,31 Raman, 32 SEM/TEM, and EPR. NMR, especially solution-state NMR, which is a non-destructive method, has provided analytical breakthroughs for insights into the interunit linkages of whole lignin.…”

Section: Lignin Structurementioning

confidence: 99%

Chapter 1. A Brief Introduction to Lignin Structure

Kathahira¹,

Elder²,

Beckham³

2018

Energy and Environment Series

102

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Section: Lignin Structurementioning

confidence: 99%

Chapter 1. A Brief Introduction to Lignin Structure

Kathahira¹,

Elder²,

Beckham³

2018

Energy and Environment Series

102

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“…The deconvolution of the C4 region of the 13 C CP-MAS NMR spectrum, from 80 to 92 ppm, was carried out with the Topspin software (Bruker). It followed the approach presented by Pu et al (2013) with crystalline signals at 89. 5, 89.0, 88.8, 88.1 ppm and amorphous signals at 83.2, 84.7, 83.0 ppm (see Fig.…”

Section: Solid-state Nmr Spectroscopymentioning

confidence: 99%

“…The ratio of bands intensities at 380 cm -1 and 1096 cm -1 should represent the crystallinity index; however, without any certitude on the orientation of the fibers spotted by the laser it seemed difficult to follow the method proposed by Agarwal et al [5]. [6] S-17 Comparison of XRD and solid-state NMR spectroscopy Cellulose has a complex hierarchical structure. Stating that there are only two types of domains, crystalline and amorphous domains, may be a misconception.…”

Section: Raman Spectroscopymentioning

confidence: 99%

Cellulose consolidation under high-pressure and high-temperature uniaxial compression

et al. 2019

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A hstrac t Materials based on cellulose cannot be obtained from thermoplastic processes. Our aim is to prepare all-cellulose materials by uniaxial high pres sure thermocompression of cellulose. The effect of moisture content (0 8 w/w%) and temperature (175 250 °C) was characterized through the mechan ical properties (bending and tensile), morphology (scanning electron rnicroscopy, X-ray tomography) and microstructure (viscometric degree of polymer ization, Raman spectroscopy, X-ray diffraction, solid state NMR) of the specimens. The specimens were mechanically stronger in bending than in tension. They exhibited a more porous heart, a dense but very thin skin on the faces (orthogonal to the compression axis) and thick and extremely dense sides. During thermocompression severe friction between fibers caused a decrease in molecular weight while heating

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“…Adjacent microfibrils are laterally aligned and bundled to form macrofibrils or lamellae in plant cell walls. By virtue of its less ordered structure, the amorphous phase of cellulose microfibrils is more accessible to cellulase enzymes . In a recent stochastic modeling study by Kumar and Murthy, the amorphous and crystalline regions experience differing EG I activity and do not have differing accessibility.…”

Section: Introductionmentioning

confidence: 99%

“…By virtue of its less ordered structure, the amorphous phase of cellulose microfibrils is more accessible to cellulase enzymes. 9,[45][46][47] In a recent stochastic modeling study by Kumar and Murthy, 14 the amorphous and crystalline regions experience differing EG I activity and do not have differing accessibility. None of the aforementioned modeling studies involved any examination of the variation of crystallinity with the extent of cellulose conversion.…”

Section: Introductionmentioning

confidence: 99%

Parameter determination and validation for a mechanistic model of the enzymatic saccharification of cellulose-I_β

Nag

Sprague

Griggs

et al. 2015

Biotechnol Progress

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Cost-effective production of fuels and chemicals from lignocellulosic biomass often involves enzymatic saccharification, which has been the subject of intense research and development. Recently, a mechanistic model for the enzymatic saccharification of cellulose has been developed that accounts for distribution of cellulose chain lengths, the accessibility of insoluble cellulose to enzymes, and the distinct modes of action of the component cellulases [Griggs et al. (2012) Biotechnol. Bioeng., 109(3):665-675; Griggs et al. (2012) Biotechnol. Bioeng., 109(3):676-685]. However, determining appropriate values for the adsorption, inhibition, and rate parameters required further experimental investigation. In this work, we performed several sets of experiments to aid in parameter estimation and to quantitatively validate the model. Cellulosic materials differing in degrees of polymerization and crystallinity (α-cellulose-Iβ and highly crystalline cellulose-Iβ ) were digested by component enzymes (EGI/CBHI/βG) and by mixtures of these enzymes. Based on information from the literature and the results from these experiments, a single set of model parameters was determined, and the model simulation results using this set of parameters were compared with the experimental data of total glucan conversion, chain-length distribution, and crystallinity. Model simulations show significant agreement with the experimentally derived glucan conversion and chain-length distribution curves and provide interesting insights into multiple complex and interacting physico-chemical phenomena involved in enzymatic hydrolysis, including enzyme synergism, substrate accessibility, cellulose chain length distribution and crystallinity, and inhibition of cellulases by soluble sugars.

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Plant Biomass Characterization: Application of Solution‐ and Solid‐State NMR Spectroscopy

Cited by 32 publications

References 68 publications

Chapter 1. A Brief Introduction to Lignin Structure

Chapter 1. A Brief Introduction to Lignin Structure

Cellulose consolidation under high-pressure and high-temperature uniaxial compression

Parameter determination and validation for a mechanistic model of the enzymatic saccharification of cellulose-I_β

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Plant Biomass Characterization: Application of Solution‐ and Solid‐State NMR Spectroscopy

Cited by 32 publications

References 68 publications

Chapter 1. A Brief Introduction to Lignin Structure

Chapter 1. A Brief Introduction to Lignin Structure

Cellulose consolidation under high-pressure and high-temperature uniaxial compression

Parameter determination and validation for a mechanistic model of the enzymatic saccharification of cellulose-Iβ

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Product

Resources

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Parameter determination and validation for a mechanistic model of the enzymatic saccharification of cellulose-I_β