2017
DOI: 10.1002/cssc.201601517
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Fast Track to Molar‐Mass Distributions of Technical Lignins

Abstract: Technical lignins (waste products obtained from wood pulping or biorefinery processes) have so far required lengthy analysis procedures and different eluents for molar-mass analysis by gel permeation chromatography (GPC). This challenge has become more pressing recently since attempts to utilize lignins have increased, leading to skyrocketing numbers of samples to be analyzed. A new approach, which uses the eluent DMSO/LiBr (0.5 % w/v) and converts lignosulfonate salts into their acidic form before analysis, o… Show more

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Cited by 43 publications
(58 citation statements)
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“…The columns were calibrated using polystyrene sulfonate standards (Na‐PSS) of narrow molecular weight distribution ( Ð ≤ 1.20; M w 1100, 1920, 3610, 6520, 14,900, 29,100, 63,900, 148,000 g mol −1 ). Solubilization of PSS standards in DMSO was achieved by pretreatment with acidic cation‐exchange resin as described elsewhere . Data evaluation was performed using Empower 3 Chromatography Data Software.…”
Section: Methodsmentioning
confidence: 99%
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“…The columns were calibrated using polystyrene sulfonate standards (Na‐PSS) of narrow molecular weight distribution ( Ð ≤ 1.20; M w 1100, 1920, 3610, 6520, 14,900, 29,100, 63,900, 148,000 g mol −1 ). Solubilization of PSS standards in DMSO was achieved by pretreatment with acidic cation‐exchange resin as described elsewhere . Data evaluation was performed using Empower 3 Chromatography Data Software.…”
Section: Methodsmentioning
confidence: 99%
“…Solubilization of PSS standards in DMSO was achieved by pretreatment with acidic cationexchange resin as described elsewhere. 10 Data evaluation was performed using Empower 3 Chromatography Data Software. 31 P NMR analysis was performed as described elsewhere 11,12 using TMDP as phosphitylation reagent to label all free hydroxyl groups present in the respective lignins and the solvent mixture M (CDCl 3 /pyridine, 1:1.6, v/v) to prepare the following solutions: (A) analyte solution containing 35 mg mL 21 lignin; (B) standard stock solution containing 50 mg mL 21 cholesterol and 30 mg mL 21 N-hydroxy-5-norbornene-2,3-dicarboxylic acid imide; (C) relaxation reagent solution containing 5 mg mL 21 of chromium (lll) acetylacetonate.…”
Section: Methodsmentioning
confidence: 99%
“…Recently,asimple protocol employing aN a-PSS protonation procedure has been proposed allowing for the complete dissolution of protonated PSS in DMSO. [21] Considering that DMSO is au niversal solvent system capable of dissolving almosta ll lignin types, the SEC setup with DMSO as the eluent and PSSbased calibrationr epresents ar easonable approach to lignosulfonate characterization. However,t he errors in lignin molar mass calculations, as ar esult of the structural dissimilarities between calibranta nd analyte, remainq uite large.…”
Section: Shortcomings and Limitations Of Conventional Approaches To Mmentioning
confidence: 99%
“…Because no lignin SEC standards are available, the molar mass is assessed based on narrow polystyrene (PS) standards or PS sulfonate (PSS) standards in the case of lignosulfonates. To avoid any confusion, we would like to point out that polystyrene is insoluble in DMSO, but PSS can be dissolved 21. Our point assumes that, among the suitable standard compounds commercially available, these polymers structurally resemble the lignin molecules most closely.…”
Section: Introductionmentioning
confidence: 99%
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