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A revised solid-state NMR method to assess the crystallinity of cellulose

Artikel i vetenskaplig tidskrift
Författare T. Sparrman
L. Svenningsson
K. Sahlin-Sjovold
L. Nordstierna
G. Westman
Diana Bernin
Publicerad i Cellulose
Volym 26
Nummer/häfte 17
Sidor 8993-9003
ISSN 0969-0239
Publiceringsår 2019
Publicerad vid Svenskt NMR-centrum vid Göteborgs universitet
Sidor 8993-9003
Språk en
Länkar dx.doi.org/10.1007/s10570-019-02718...
Ämnesord Crystallinity, Cellulose, MAS, C-13 NMR, C-13 T-1, Cross-polarization, cell-wall polysaccharides, x-ray-diffraction, regenerated cellulose, c-13-nmr
Ämneskategorier Kemi

Sammanfattning

The crystallinity of cellulose has a strong impact on various material properties. Over the years, many methods have become available to estimate the crystallinity. The purpose of this work was to revise existing NMR-based methods and to introduce a complementary NMR method related to the C-13 T-1 relaxation time. The C-13 T-1 differs by an order of magnitude for amorphous and crystalline polymers among them cellulose. We have utilized the signal boost of H-1-C-13 cross polarization and the difference in C-13 T-1 as a filter to calculate the degree of crystallinity. The evaluation of the method is based on the difference in peak integrals, which is fed into a simple equation. The method was applied to five cellulosic samples of different nature and compared the obtained degree of crystallinity with the degree estimated from deconvoluted X-ray scattering patterns. Furthermore, an attempt has been made to give a basic understanding on the origin of CP enhancement in order to validate various proposed NMR methods. With the recent progress of NMR equipment, the presented method can be automatized and applied to a series of samples using a sample changer.

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