Related Experiment Video
Updated: Mar 23, 2026

Preparation of Fungal and Plant Materials for Structural Elucidation Using Dynamic Nuclear Polarization Solid-State NMR
Published on: February 12, 2019
Solution-State One- and Two-Dimensional NMR Spectroscopy of High-Molecular-Weight Cellulose
Ashley J Holding1, Valtteri Mäkelä1, Lasse Tolonen2
1Laboratory of Organic Chemistry, Department of Chemistry, University of Helsinki, A.I. Virtasen aukio 1 (Chemicum), PL 55, 00014 University of, Helsinki, Finland.
Abstract:
High-molecular-weight celluloses (which even include bacterial cellulose) can be dissolved fully in methyltrioctylphosphonium acetate/[D6 ]DMSO solutions to allow the measurement of resonance-overlap-free 1 D and 2 D NMR spectra. This is achieved by a simple and non-destructive dissolution method, without solvent suppression, pre-treatment or deuteration of the ionic component. We studied a range of cellulose samples by using various NMR experiments to make an a priori assignment of the cellulose resonances. Chain-end resonances are also visible in the (1) H NMR spectrum. This allows the rough determination of the degree of polymerisation (DP) of a sample for low-DP celluloses by the integration of non-reducing chain ends C1 versus polymeric cellobiose C1. Low-DP celluloses show a good agreement with the gel-permeation chromatography (GPC) values, but high-DP pulps show more deviation. For high-purity pulps (pre-hydrolysis kraft and sulfite), residual xyloses and mannoses can also be identified from the (1) H-(13) C heteronuclear single-quantum coherence (HSQC) spectra. Resonances are thus assigned for the common polymeric polysaccharides found in chemical pulps.
More Related Videos
11:32Highly Stable, Functional Hairy Nanoparticles and Biopolymers from Wood Fibers: Towards Sustainable Nanotechnology
Published on: July 20, 2016
09:27High Resolution Quantification of Crystalline Cellulose Accumulation in Arabidopsis Roots to Monitor Tissue-specific Cell Wall Modifications
Published on: May 10, 2016
Related Concept Videos
¹H NMR of Conformationally Flexible Molecules: Temporal Resolution
Two-Dimensional (2D) NMR: Overview
The first step is the preparation period, during which nucleus A is excited with a radiofrequency pulse....
2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)
2D NMR: Homonuclear Correlation Spectroscopy (COSY)
¹H NMR of Conformationally Flexible Molecules: Variable-Temperature NMR
Cellulose and Pectic Polysaccharides
As a cell matures, its cell wall specializes according to its type. For example, the...