Skip to main content
SpringerLink
Log in

Determination of the 13C chemical shift anisotropies of cellulose I and cellulose II

  • Published:
Cellulose Aims and scope Submit manuscript

Abstract

The chemical shift anisotropies (CSAs) of cellulose Iα and Iβ, the two crystalline constituents of bacterial cellulose produced by Acetobacter xylinum (DSM 14666), and regenerated cellulose II are reported for each of the spectroscopically resolved carbon resonances using the phase adjusted spinning sideband (PASS) experiment. The data are compared with experimental results using the recoupling of anisotropy information (RAI) technique and with theoretical calculations of the structure of cellulose, including the hydrogen bonding systems.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Similar content being viewed by others

References

  1. D.W. Alderman G. McGeorge J.Z. Hu R.J. Pugmire D.M. Grant (1998) ArticleTitleA sensitivehigh resolution magic angle turning experiment for measuring chemical shift tensor principal values Mol. Phys. 95 IssueID6 1113–1126

    Google Scholar 

  2. O.N. Antzutkin S.C. Shekar M.H. Levitt (1995) ArticleTitleTwo-dimensional sideband separation in magic-angle-spinning NMR J. Magn. Reson. A 115 7–19

    Google Scholar 

  3. R.H. Atalla J.C. Gast (1980) ArticleTitle13C NMR spectra of cellulose polymorphs J. Am. Chem. Soc. 102 IssueID9 3249–3251

    Google Scholar 

  4. R.H. Atalla D.L. VanderHart (1984) ArticleTitleNative cellulose: a composite of two distinct crystalline forms Science 223 283–284

    Google Scholar 

  5. A. Bax N.M. Szeverenyi G.E. Maciel (1983a) ArticleTitleCorrelation of isotropic shifts and chemical shift anisotropies by two-dimensional Fourier-transform magic-angle hopping NMR spectroscopy J. Magn. Reson. 52 147–152

    Google Scholar 

  6. A. Bax N.M. Szeverenyi G.E. Maciel (1983b) ArticleTitleChemical shift anisotropy in powdered solids studied by 2D FT NMR with flipping of the spinning axis J. Magn. Reson. 55 494–497

    Google Scholar 

  7. R.L. Dudley C.A. Fyfe P.J. Stephenson Y. Deslandes G.K. Hamer R.H. Marchessault (1983) ArticleTitleHigh-resolution 13C CP/MAS NMR spectra of solid cellulose oligomers and the structure of cellulose II J. Am. Chem. Soc. 105 IssueID8 2469–2472

    Google Scholar 

  8. W.L. Earl D.L. VanderHart (1980) ArticleTitleHigh resolution magic angle sample spinning 13C NMR of solid cellulose I J. Am. Chem. Soc. 102 3251–3252

    Google Scholar 

  9. W.L. Earl D.L. VanderHart (1982) ArticleTitleMeasurement of 13C chemical shifts in solids J. Magn. Reson. 48 35–54

    Google Scholar 

  10. T. Erata T. Shikano S. Yunoki M. Takai (1997) ArticleTitleThe complete assignment of the 13C CP/MAS NMR spectrum of native cellulose by using 13C labeled glucose Cellulose Commun. 4 128–131

    Google Scholar 

  11. D. Gagnaire D. Mancier M. Vincendon (1980) ArticleTitleCellulose organic solutions: a nuclear magnetic resonance investigation J. Polym. Sci. Polym. Chem. Ed. 18 IssueID1 13–25

    Google Scholar 

  12. Z. Gan (1994) ArticleTitleSpinning-sideband suppression using a pseudo-two-dimensional experiment J. Magn. Reson. 109 253–255

    Google Scholar 

  13. J.C. Gast R.H. Atalla R.D. McKelvey (1980) ArticleTitleThe Carbon-13 NMR spectra of the xylo- and cellooligosaccharides Carbohydr. Res. 84 IssueID1 137–146

    Google Scholar 

  14. J. Herzfeld A.E. Berger (1980) ArticleTitleSideband intensities in NMR spectra of samples spinning at the magic angle J. Chem. Phys. 73 IssueID12 6021–6030

    Google Scholar 

  15. St. Hesse (1998) NMR-Untersuchungen von Cellulosen und Biopolymeren Diploma Thesis IOQ/HF FSU JenaGermany

    Google Scholar 

  16. F. Horii A. Hirai R. Kitamaru (1983) ArticleTitleSolid-state 13C-NMR study of conformations of oligosaccharides and cellulose: conformation of CH2OH group about the exo-cyclic C–C bond Polym. Bull. 10 357–361

    Google Scholar 

  17. J.Z. Hu W. Wang F. Liu M.S. Solum D.W. Alderman R.J. Pugmire D.M. Grant (1995) ArticleTitleMagic-angle-turning experiments for measuring chemical-shift-tensor principal values in powdered solids J. Magn. Reson. A 133 210–222

    Google Scholar 

  18. Y. Inoue R. Chujo (1978) ArticleTitleThe carbon-13 NMR spectra of (1→4)-linked β-d-gluco-oligosaccharides Carbohydr. Res. 60 IssueID2 367–370

    Google Scholar 

  19. C.Jaeger, J.Pauli, H.-P. Schmauder 2004 Observation of the glycosidic bond and complete ring assignment of the carbons in uniformly 13C labeled bacterial cellulose Macromolecules submitted

  20. F.-Th. Koch W. Priess R. Witter U. Sternberg (2000) ArticleTitleCalculation of solid-state 13C NMR spectra of cellulose IαIβ and II using a semi-empirical approach and molecular dynamics Macromol. Chem. Phys. 201 1930–1939

    Google Scholar 

  21. F.J. Kolpak J. Blackwell (1976) ArticleTitleDetermination of the structure of cellulose II Macromolecules 9 273–278

    Google Scholar 

  22. H. Kono S. Yunoki T. Shikano M. Fujiwara T. Erata M. Takai (2002) ArticleTitleCP/MAS 13C NMR study of cellulose and cellulose derivatives. 1. Complete assignment of the CP/MAS 13C NMR spectrum of the native cellulose J. Am. Chem. Soc. 124 7506–7511

    Google Scholar 

  23. H. Kono T. Erata M. Takai (2003) ArticleTitleDetermination of the through-bond carbon–carbon and carbon–proton connectivities of the native celluloses in the solid state Macromolecules 36 5131–5138

    Google Scholar 

  24. P. Langan Y. Nishiyama H. Chanzy (1999) ArticleTitleA revised structure and hydrogen-bonding system in cellulose II from a neutron fiber diffraction analysis J. Am. Chem. Soc. 121 9940–9946

    Google Scholar 

  25. A. Lesage M. Bardet L. Emsley (1999) ArticleTitleThrough-bond carbon–carbon connectivities in disordered solids by NMR J. Am. Chem. Soc. 121 10987–10993

    Google Scholar 

  26. G.E. Maciel N.M. Szeverenyi M. Sardashti (1985) ArticleTitleChemical-shift-anisotropy powder patterns by the two-dimensional angle-flipping approach. Effects of crystallite packing J. Magn. Reson. 64 365–374

    Google Scholar 

  27. J. Mason (1993) ArticleTitleConvention for the reporting of nuclear magnetic shielding (or shifts) tensors suggested by participants in the NATO ARW on NMR shielding constants at the University of MarylandCollege Park, July 1992 Solid State Nucl. Magn. Res. 2 285–288

    Google Scholar 

  28. Y. Nishiyama P. Langan H.J. Chanzy (2002) ArticleTitleCrystal structure and hydrogen-bonding system in cellulose Iβ from synchrotron X-ray and neutron fiber diffraction J. Am. Chem. Soc. 124 9074–9082

    Google Scholar 

  29. Y. Nishiyama J. Sugiyama H. Chanzy P. Langan (2003) ArticleTitleCrystal structure and hydrogen bonding system in cellulose Iα from synchrotron X-ray and neutron fiber diffraction J. Am. Chem. Soc. 125 14300–14306

    Google Scholar 

  30. S. Raymond A. Kvick H. Chanzy (1995) ArticleTitleThe structure of cellulose II: a revisit Macromolecules 28 8422–8425

    Google Scholar 

  31. M. Schramm S. Hestrin (1954) ArticleTitleFactors affecting production of cellulose at the air/liquid interface of a culture of Acetobacter xylinum J. Gen. Microbiol. 11 123–129

    Google Scholar 

  32. U. Sternberg M. Möllhoff (2001) ArticleTitleMolecular mechanics with fluctuating atomic charges – a new force field with a semi-empirical charge calculation J. Mol. Model. 7 90–102

    Google Scholar 

  33. U. Sternberg F.-Th. Koch W. Priess R. Witter (2003) ArticleTitleCrystal structure refinements of cellulose polymorphs using solid-state 13C chemical shifts Cellulose 10 189–199

    Google Scholar 

  34. J. Sugiyama J. Persson H. Chanzy (1991a) ArticleTitleCombined infrared and electron diffraction study of the polymorphism of native celluloses Macromolecules 24 2461–2466

    Google Scholar 

  35. J. Sugiyama R. Vuong H. Chanzy (1991b) ArticleTitleElectron diffraction study on the two crystalline phases occurring in native cellulose from an algal cell wall Macromolecules 24 4168–4175

    Google Scholar 

  36. N.M. Szeverenyi A. Bax G.E. Maciel (1985) ArticleTitleMagic-angle hopping as an alternative to magic-angle spinning for solid state NMR J. Magn. Reson. 61 440–447

    Google Scholar 

  37. R. Tycko G. Dabbagh P.A. Mirau (1989) ArticleTitleDetermination of chemical-shift-anisotropy lineshapes in a two-dimensional magic-angle-spinning NMR experiment J. Magn. Reson. 85 265–274

    Google Scholar 

  38. D.L. VanderHart R.H. Atalla (1984) ArticleTitleStudies of microstructure in native cellulose using solid-state 13C NMR Macromolecules 17 1465–1472

    Google Scholar 

  39. D.L. VanderHart R.H. Atalla (1987) Further carbon-13 NMR evidence for the coexistence of two crystalline forms in native celluloses R.H. Atalla (Eds) The Structures of Celluloses. ACS Symp. Ser., 340 American Chemical Society Washington, DC 88–118

    Google Scholar 

  40. K. Wickholm E.-L. Hult P.T. Larsson T. Iversen H. Lennholm (2001) ArticleTitleQuantification of cellulose forms in complex cellulose materials: a chemometric model Cellulose 8 139–148

    Google Scholar 

  41. R. Witter St. Hesse U. Sternberg (2003) ArticleTitleNew powder pattern recoupling at 10 kHz spinning speed applied to cellulose J. Magn. Reson. 161 35–42

    Google Scholar 

  42. C. Zollfrank (1999) Darstellung von Cellulose-II-Einkristallen und Untersuchung ihrer Kristallstruktur Dissertation HFM TU München, Germany

    Google Scholar 

Download references

Author information

Author notes

  1. Stephanie Hesse

    Present address: Centre of Excellence for Polysaccharide Research, Friedrich-Schiller-Universität Jena, Lessingstrasse 8, D-07743, Jena, Germany

Authors and Affiliations

  1. Institute of Optics and Quantum Electronics, Friedrich-Schiller-Universität Jena, Max-Wien-Platz 1, D-07743, Jena, Germany

    Stephanie Hesse

  2. Federal Institute for Materials Research and Testing, Project Group I.3903, Richard Willstaetter Strasse 11, D-12489, Berlin, Germany

    Christian Jäger

Authors
  1. Stephanie Hesse
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Christian Jäger
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Stephanie Hesse.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Hesse, S., Jäger, C. Determination of the 13C chemical shift anisotropies of cellulose I and cellulose II. Cellulose 12, 5–14 (2005). https://doi.org/10.1007/s10570-004-0211-2

Download citation

  • Received:

  • Accepted:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10570-004-0211-2

Keywords

Search

Navigation