Rapid determination of gamma-value and xanthate group distribution on viscose by liquid-state 1H NMR spectroscopy

Kateryna Wöss; Hansjörg Weber; Peter Grundnig; Thomas Röder; Hedda Weber

doi:10.1016/j.carbpol.2016.01.004

Rapid determination of gamma-value and xanthate group distribution on viscose by liquid-state 1H NMR spectroscopy

Kateryna Wöss, Hansjörg Weber, Peter Grundnig, Thomas Röder, Hedda Weber^*

^*Corresponding author for this work

Institute of Organic Chemistry (6410)

Research output: Contribution to journal › Article › peer-review

Abstract

A method for the determination of the γ-value and more importantly the distribution of xanthate groups on cellulose xanthate produced during the viscose process is presented. The method is based upon stabilization of xanthate groups attached to the cellulose chain by reaction with 4-methylbenzyl bromide and analysis of the resulting product by liquid-state 1H NMR. Careful analysis of the proton-spectrum using deconvolution gave a very fast method for the measurement of the γ-value which compared well with the data obtained by IR spectroscopy. In addition it could be shown that the distribution of the xanthate groups on the anhydroglucose monomeric unit (xanthation at position 2, 3 or 6) changes significantly during ripening. The method gave useful results even for viscose with low γ-values of about 25.

Original language	English
Pages (from-to)	184-189
Journal	Carbohydrate Polymers
Volume	141
DOIs	https://doi.org/10.1016/j.carbpol.2016.01.004
Publication status	Published - 2016

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Human- & Biotechnology

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10.1016/j.carbpol.2016.01.004

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@article{074373fa365c4acb9d4ce948ef1a1675,

title = "Rapid determination of gamma-value and xanthate group distribution on viscose by liquid-state 1H NMR spectroscopy",

abstract = "A method for the determination of the γ-value and more importantly the distribution of xanthate groups on cellulose xanthate produced during the viscose process is presented. The method is based upon stabilization of xanthate groups attached to the cellulose chain by reaction with 4-methylbenzyl bromide and analysis of the resulting product by liquid-state 1H NMR. Careful analysis of the proton-spectrum using deconvolution gave a very fast method for the measurement of the γ-value which compared well with the data obtained by IR spectroscopy. In addition it could be shown that the distribution of the xanthate groups on the anhydroglucose monomeric unit (xanthation at position 2, 3 or 6) changes significantly during ripening. The method gave useful results even for viscose with low γ-values of about 25.",

author = "Kateryna W{\"o}ss and Hansj{\"o}rg Weber and Peter Grundnig and Thomas R{\"o}der and Hedda Weber",

year = "2016",

doi = "10.1016/j.carbpol.2016.01.004",

language = "English",

volume = "141",

pages = "184--189",

journal = "Carbohydrate Polymers",

issn = "1879-1344",

publisher = "Elsevier Limited",

}

TY - JOUR

T1 - Rapid determination of gamma-value and xanthate group distribution on viscose by liquid-state 1H NMR spectroscopy

AU - Wöss, Kateryna

AU - Weber, Hansjörg

AU - Grundnig, Peter

AU - Röder, Thomas

AU - Weber, Hedda

PY - 2016

Y1 - 2016

N2 - A method for the determination of the γ-value and more importantly the distribution of xanthate groups on cellulose xanthate produced during the viscose process is presented. The method is based upon stabilization of xanthate groups attached to the cellulose chain by reaction with 4-methylbenzyl bromide and analysis of the resulting product by liquid-state 1H NMR. Careful analysis of the proton-spectrum using deconvolution gave a very fast method for the measurement of the γ-value which compared well with the data obtained by IR spectroscopy. In addition it could be shown that the distribution of the xanthate groups on the anhydroglucose monomeric unit (xanthation at position 2, 3 or 6) changes significantly during ripening. The method gave useful results even for viscose with low γ-values of about 25.

AB - A method for the determination of the γ-value and more importantly the distribution of xanthate groups on cellulose xanthate produced during the viscose process is presented. The method is based upon stabilization of xanthate groups attached to the cellulose chain by reaction with 4-methylbenzyl bromide and analysis of the resulting product by liquid-state 1H NMR. Careful analysis of the proton-spectrum using deconvolution gave a very fast method for the measurement of the γ-value which compared well with the data obtained by IR spectroscopy. In addition it could be shown that the distribution of the xanthate groups on the anhydroglucose monomeric unit (xanthation at position 2, 3 or 6) changes significantly during ripening. The method gave useful results even for viscose with low γ-values of about 25.

U2 - 10.1016/j.carbpol.2016.01.004

DO - 10.1016/j.carbpol.2016.01.004

M3 - Article

SN - 1879-1344

VL - 141

SP - 184

EP - 189

JO - Carbohydrate Polymers

JF - Carbohydrate Polymers

ER -

Rapid determination of gamma-value and xanthate group distribution on viscose by liquid-state 1H NMR spectroscopy

Abstract

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