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Cellulose

, Volume 19, Issue 6, pp 1837–1854 | Cite as

Ultrastructure of cellulose crystallites in flax textile fibres

  • Benoît Duchemin
  • Anthony Thuault
  • Aurélie Vicente
  • Baptiste Rigaud
  • Christian Fernandez
  • Sophie Eve
Original Paper

Abstract

Seven varieties of flax (Linum usitatissimum) fibres were analyzed in order to gain a deeper insight into the morphological features of the crystalline assembly. Different spectroscopic techniques and a chemical bleaching process were used to provide an accurate description of the lateral arrangement of the polysaccharide chains within the fibre cell wall. The flax fibres were analyzed in their natural state and after an extraction treatment of the non-crystalline components such as hemicelluloses, pectins and phenolics. The chemical bleaching process consisted of a Soxhlet extraction in toluene, a sodium chlorite treatment and an alkaline extraction of the residual hemicelluloses. Solid-state 13C nuclear magnetic resonance (NMR) confirmed the sequential removal of the non-cellulosic components from the flax cell wall. Both wide-angle X-ray diffraction (WAXD) and solid-state 13C NMR provided measures of the crystallite thicknesses and overall crystallinities before and after treatment. The existence of non-cellulosic highly ordered paracrystalline domains was also evidenced by proton spin relaxation time calculation. Whereas the overall crystallinity determined by WAXD decreased after treatment, the cellulose crystallinity calculated with the help of the solid-state 13C NMR slightly increased. This is explained by the difference in chemical selectivity between these two techniques and by the paracrystalline state of both hemicelluloses and pectins. Strong adhesion between cellulose crystallites, hemicelluloses and pectins in the fibres was evidenced by low spin–spin relaxation times and by an increase in crystallite thickness after bleaching. A simple model is proposed that describes the rearrangement of the macromolecules during the bleaching process.

Keywords

WAXD 13C solid-state NMR Peak-fitting PCA Flax fibres 

Notes

Acknowledgments

We would like to thank Mr. Cyril Jouannic and Abdellatif Chachdi for their assistance with the extraction work. Mr. Franck Gascoin and Philippe Bazin are acknowledged for their help with, respectively, the amorphous cellulose preparation and the FTIR spectroscopy.

Supplementary material

10570_2012_9786_MOESM1_ESM.jpeg (342 kb)
Supplementary material 1 (JPEG 341 kb)

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Copyright information

© Springer Science+Business Media Dordrecht 2012

Authors and Affiliations

  • Benoît Duchemin
    • 1
  • Anthony Thuault
    • 1
  • Aurélie Vicente
    • 2
  • Baptiste Rigaud
    • 2
  • Christian Fernandez
    • 2
  • Sophie Eve
    • 3
  1. 1.LOMC, UMR 6294, CNRS-Université du HavreLe HavreFrance
  2. 2.Laboratoire Catalyse et Spectrochimie (LCS)ENSICAEN, Université de Caen, CNRSCaenFrance
  3. 3.Laboratoire de Cristallographie et de Sciences des MatériauxENSICAEN, Université de Caen, CNRSCaenFrance

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