13C NMR assignments of regenerated cellulose from solid-state 2D NMR spectroscopy
Journal article, 2016

From the assignment of the solid-state 13C NMR signals in the C4 region, distinct types of crystalline cellulose, cellulose at crystalline surfaces, and disordered cellulose can be identified and quantified. For regenerated cellulose, complete 13C assignments of the other carbon regions have not previously been attainable, due to signal overlap. In this study, two-dimensional (2D) NMR correlation methods were used to resolve and assign 13C signals for all carbon atoms in regenerated cellulose. 13C-enriched bacterial nanocellulose was biosynthesized, dissolved, and coagulated as highly crystalline cellulose II. Specifically, four distinct 13C signals were observed corresponding to conformationally different anhydroglucose units: two signals assigned to crystalline moieties and two signals assigned to non-crystalline species. The C1, C4 and C6 regions for cellulose II were fully examined by global spectral deconvolution, which yielded qualitative trends of the relative populations of the different cellulose moieties, as a function of wetting and drying treatments.

13C CP/MAS NMR

2D correlation NMR

Mercerized cellulose

Deconvolution

Assignment

Regenerated cellulose

Author

Alexander Idström

Chalmers, Chemistry and Chemical Engineering, Applied Chemistry, Applied Surface Chemistry

Staffan Schantz

AstraZeneca AB

Johan Sundberg

Chalmers, Chemistry and Chemical Engineering, Applied Chemistry, Polymer Technology

B. F. Chmelka

University of California

Paul Gatenholm

Wallenberg Wood Science Center (WWSC)

Chalmers, Chemistry and Chemical Engineering, Applied Chemistry, Polymer Technology

Lars Nordstierna

Chalmers, Chemistry and Chemical Engineering, Applied Chemistry, Applied Surface Chemistry

Carbohydrate Polymers

0144-8617 (ISSN)

Vol. 151 480-487

Subject Categories

Chemical Engineering

DOI

10.1016/j.carbpol.2016.05.107

PubMed

27474592

More information

Latest update

8/24/2018