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Wood Research and Technology

Holzforschung

Cellulose – Hemicelluloses – Lignin – Wood Extractives

Editor-in-Chief: Salmén, Lennart

Editorial Board: Daniel, Geoffrey / Militz, Holger / Rosenau, Thomas / Sixta, Herbert / Vuorinen, Tapani / Argyropoulos, Dimitris S. / Balakshin, Yu / Barnett, J. R. / Burgert, Ingo / Rio, Jose C. / Evans, Robert / Evtuguin, Dmitry V. / Frazier, Charles E. / Fukushima, Kazuhiko / Gindl-Altmutter, Wolfgang / Glasser, W. G. / Holmbom, Bjarne / Isogai, Akira / Kadla, John F. / Koch, Gerald / Lachenal, Dominique / Laine, Christiane / Mansfield, Shawn D. / Morrell, J.J. / Niemz, Peter / Potthast, Antje / Ragauskas, Arthur J. / Ralph, John / Rice, Robert W. / Salin, Jarl-Gunnar / Schmitt, Uwe / Schultz, Tor P. / Sipilä, Jussi / Takano, Toshiyuki / Tamminen, Tarja / Theliander, Hans / Welling, Johannes / Willför, Stefan / Yoshihara, Hiroshi


IMPACT FACTOR 2017: 2.079

CiteScore 2018: 2.43

SCImago Journal Rank (SJR) 2018: 0.829
Source Normalized Impact per Paper (SNIP) 2018: 1.082

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1437-434X
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Volume 59, Issue 2

Issues

Quantitative 1H NMR analysis of alkaline polysulfide solutions

Dimitris S. Argyropoulos
  • Department of Wood and Paper Science, North Carolina State University, Raleigh, NC 27695-8005, USA and Department of Chemistry, McGill University, Montreal, Quebec H3A 2A7, Canada
  • Other articles by this author:
  • De Gruyter OnlineGoogle Scholar
/ Yihua Hou / Ramana Ganesaratnam / David N. Harpp / Keiichi Koda
  • Department of Wood and Paper Science, North Carolina State University, Raleigh, NC 27695-8005, USA and Graduate School of Agriculture, Hokkaido University, Sapporo, Hokkaido 060-8589, Japan
  • Other articles by this author:
  • De Gruyter OnlineGoogle Scholar
Published Online: 2005-06-01 | DOI: https://doi.org/10.1515/HF.2005.019

Abstract

A novel analytical protocol for the absolute determination of the various polysulfide species present in alkaline aqueous media was developed. The method is comprised of alkylating polysulfide ions with dimethyl sulfate, followed by quantitative proton NMR spectroscopy using 1,3,5-tributyl benzene as the internal standard. In order to arrive at a quantitative acquisition protocol, a number of variables were examined in detail for their effect on the alkylation reaction, including the presence of oxygen, the amount of dimethyl sulfate and sodium hydroxide, and the various modes of adding the alkylating reagent to the reaction mixture. Most of these variables were found to play a role in determining the quantitative reliability of the procedure. Consequently, a method is described that can be used for the efficient and reliable quantitative detection of polysulfide ions. The protocol developed could be particularly useful in promoting our understanding of the intricate and delicate chemistry of polysulfide equilibria in aqueous alkaline media.

Keywords: alkylation; dimethyl sulfate; nuclear magnetic resonance (NMR); polysulfide; pulping liquor

About the article

Corresponding author. Phone: +1-919-515-7708; Fax: +1-919-515-6302


Received: March 18, 2004

Accepted: June 21, 2004

Published Online: 2005-06-01

Published in Print: 2005-02-01


Citation Information: Holzforschung, Volume 59, Issue 2, Pages 124–131, ISSN (Online) 1437-434X, ISSN (Print) 0018-3830, DOI: https://doi.org/10.1515/HF.2005.019.

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