2D Assignment and quantitative analysis of cellulose and oxidized celluloses using solution-state NMR spectroscopy
Artikel i vetenskaplig tidskrift, 2020

The limited access to fast and facile general analytical methods for cellulosic and/or biocomposite materials currently stands as one of the main barriers for the progress of these disciplines. To that end, a diverse set of narrow analytical techniques are typically employed that often are time-consuming, costly, and/or not necessarily available on a daily basis for practitioners. Herein, we rigorously demonstrate a general quantitative NMR spectroscopic method for structural determination of crystalline cellulose samples. Our method relies on the use of a readily accessible ionic liquid electrolyte, tetrabutylphosphonium acetate ([P-4444][OAc]):DMSO-d(6), for the direct dissolution of biopolymeric samples. We utilize a series of model compounds and apply now classical (nitroxyl-radical and periodate) oxidation reactions to cellulose samples, to allow for accurate resonance assignment, using 2D NMR. Quantitative heteronuclear single quantum correlation (HSQC) was applied in the analysis of key samples to assess its applicability as a high-resolution technique for following cellulose surface modification. Quantitation using HSQC was possible, but only after applying T(2)correction to integral values. The comprehensive signal assignment of the diverse set of cellulosic species in this study constitutes a blueprint for the direct quantitative structural elucidation of crystalline lignocellulosic, in general, readily available solution-state NMR spectroscopy. [GRAPHICS] .

Nitroxyl radical

Ionic liquid

Cellulose dissolution

Quantitative HSQC

TEMPO

Periodate

Författare

Tetyana Koso

Helsingin Yliopisto

Daniel Rico del Cerro

Helsingin Yliopisto

Sami Heikkinen

Helsingin Yliopisto

Tiina Nypelö

Chalmers, Kemi och kemiteknik, Tillämpad kemi

Jean Buffiere

Aalto-Yliopisto

Jesus E. Perea-Buceta

Helsingin Yliopisto

Antje Potthast

Univ Nat Resources & Life Sci Vienna BOKU

Thomas Rosenau

Univ Nat Resources & Life Sci Vienna BOKU

Harri Heikkinen

VERIFIN Kemiallisen aseen kieltosopimuksen instituutti

Hannu Maaheimo

VTT Tech Res Ctr Finland Ltd

Akira Isogai

University of Tokyo

Ilkka Kilpelainen

Helsingin Yliopisto

Alistair W. T. King

Helsingin Yliopisto

Cellulose

0969-0239 (ISSN)

Vol. 27 14 7929-7953

Ämneskategorier

Analytisk kemi

Polymerteknologi

Annan kemi

DOI

10.1007/s10570-020-03317-0

Mer information

Senast uppdaterat

2020-10-01