Characterization of lignin using multi-angle laser light scattering and atomic force microscopy

Gidh, Aarti; Decker, Stephen R.; See, Chun Hwa; Himmel, Michael E.; Williford, Clint

doi:10.1016/j.aca.2005.09.023

Cited by 56 publications

(79 citation statements)

References 22 publications

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“…Ultimately, reproducible, in situ measurements of lignin structure have been coveted for decades. Lignin structure Functionality specific reactions [40][41][42][43][44][47][48][49][50] CZE [52] APPI-MS [67] CRS Microscopy [116,117] AFM [178] GC [44] DFT [88,180] GCMS [171] DE-MS [62] Dispersive Raman [92][93][94][95][96] DSC [60] ClO 2 [45] GLC-FID [54] ESI/MS [77] Potentiometry [44] Modified oximation [46] GLC-MS [54] MALDI-MSI [68] Ellipsometry [179] Headspace GC [55] SEM [71,75] MALDI/TOF [73] Fluorescence [102,103,120,131,176,177] TEM [103] RP-HPLC [53] MBMS [75] FTIR [13,44,…”

Section: Wet Chemistrymentioning

confidence: 99%

Recent innovations in analytical methods for the qualitative and quantitative assessment of lignin

Lupoi

Singh

Parthasarathi

et al. 2015

Renewable and Sustainable Energy Reviews

296

188

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a b s t r a c tAs the attraction of creating biofuels and bio-based chemicals from lignocellulosic biomass has increased, researchers have been challenged with developing a better understanding of lignin structure, quantity and potential uses. Lignin has frequently been considered a waste-product from the deconstruction of plant cell walls, in attempts to isolate polysaccharides that can be hydrolyzed and fermented into fuel or other valuable commodities. In order to develop useful applications for lignin, accurate analytical instrumentation and methodologies are required to qualitatively and quantitatively assess, for example, what the structure of lignin looks like or how much lignin comprises a specific feedstock's cellular composition. During the past decade, various diverse strategies have been employed to elucidate the structure and composition of lignin. These techniques include using two-dimensional nuclear magnetic resonance to resolve overlapping spectral data, measuring biomass with vibrational spectroscopy to enable modeling of lignin content or monomeric ratios, methods to probe and quantify the linkages between lignin and polysaccharides, or refinements of established methods to provide higher throughput analyses, less use of consumables, etc. This review seeks to provide a comprehensive overview of many of the advancements achieved in evaluating key lignin attributes. Emphasis is placed on research endeavored in the last decade.

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Section: Wet Chemistrymentioning

confidence: 99%

Recent innovations in analytical methods for the qualitative and quantitative assessment of lignin

Lupoi

Singh

Parthasarathi

et al. 2015

Renewable and Sustainable Energy Reviews

296

188

View full text Add to dashboard Cite

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“…Creation of high molecular mass aggregates was partially eliminated by increase of pH above 8.5. Gidh et al [23] explained the phenomena in terms of the results of LC studies. By use of a light scattering detector they observed very high peaks with negligible corresponding peaks detected by a UV photometric detector or refractometric detector.…”

Section: Introductionmentioning

confidence: 97%

“…Gidh et al [23] characterized lignin by use of a SEC run in an aqueous mobile phase and multi-angle laser light scattering. Additionally, they used atomic force microscopy for the study.…”

Section: Introductionmentioning

confidence: 99%

Characterization of Klason lignins by reversed-phase high-performance liquid chromatography using wide-pore octadecylsilica and stepwise gradients of dimethylformamide in water

et al. 2006

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RP-HPLC using stepwise gradients of N,N-dimethylformamide (DMF) in a phosphate-buffered (pH 3.00) aqueous mobile phase and a wide-pore (30 nm) octadecylsilica column has been applied to the analysis of a variety of lignins--organocell lignin, dioxane lignin, Björkman lignin, and Klason lignins from both softwoods and hardwoods, respectively, in order to demonstrate the usefulness of the approach for their characterization. Tandem combination of spectrophotometric diode array detection and fluorimetric detection was used to acquire more detailed information about the chromatographic behavior of lignins. The results show that a ten-step gradient can reveal distinct features of lignins and humic substances. Combination of good solvating properties of DMF for lignins together with a wide-pore RP sorbent improves surface interactions of the analytes and suppresses the influence of size exclusion effects. Thus it provides reproducibility of characterization profiles and robustness of the method. The calculated repeatability of the retention time of selected peaks was +/- 0.46% RSD. The reproducibility of the data within one week (set of seven data) was +/- 1.1% RSD. These data are also representative of the other well-shaped peaks of analyzed substances.

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“…11,12,16,17,20 Studies have also been carried out with light scattering [21][22][23][24][25][26] and have concluded that MALLS (multiangle laser light scattering) can be used for the determination of the molecular weight and the molecular weight distribution of lignins. MALLS is an absolute molecular weight technique that is based on the intensity of the light that is scattered when a laser passes through a sample.…”

Section: Introductionmentioning

confidence: 99%

“…Therefore, light scattering is a good technique for indirectly studying interaction forces characterized by apparent molecular weight changes that are induced by lignin association phenomena. Gidh et al 26 have therefore concluded that light scattering techniques offer great insight into lignin aggregate characterization.…”

Section: Introductionmentioning

confidence: 99%

Propensity of Lignin to Associate: Light Scattering Photometry Study with Native Lignins

et al. 2008

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Many studies of lignins in solution invoke association and aggregation phenomena to explain their solution behavior (e.g., reprecipitation onto pulp fibers, condensation, etc.). Following their colloidal (apparent) molecular weights in solution as a function of time allows us to explore observable dissociation phenomena. These measurements were carried out using multiple angle laser light scattering (MALLS) photometry in the static mode. The challenges and opportunities of measuring the specific refractive index increment (dn/dC) of lignin solutions and determining the kinetics of the dissociation process were thus investigated. Hardwood and softwood representative lignins were isolated, and method for their full dissolution in THF was further developed, which then lead to accurate dn/dC values being obtained as a function of time. When coupled to additional work using light scattering static measurements and Zimm plots for the same solutions, this effort offers insight into the aggregation and ensuing dissociative events that operate within the lignin macromolecules.

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Characterization of lignin using multi-angle laser light scattering and atomic force microscopy

Cited by 56 publications

References 22 publications

Recent innovations in analytical methods for the qualitative and quantitative assessment of lignin

Recent innovations in analytical methods for the qualitative and quantitative assessment of lignin

Characterization of Klason lignins by reversed-phase high-performance liquid chromatography using wide-pore octadecylsilica and stepwise gradients of dimethylformamide in water

Propensity of Lignin to Associate: Light Scattering Photometry Study with Native Lignins

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