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A solid-state NMR study of cellulose degradation

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Abstract

A series of laboratory-aged transformer insulating papers were investigated using solid-state NMR spectroscopy. Carbon-13 CPMAS, and proton MAS experiments were carried out along with static proton relaxation (T1, and T) and free induction decay (FID) measurements. Some proton CRAMPS and proton-carbon-13 correlation (WISE) experiments were also undertaken. A change in the proton T1 and FID with ageing was detected. No detectable change was found in the proton T. Some amorphous cellulose was detected in the carbon-13 spectrum. There was, however, no evidence for a substantial change in the nature of the cellulose with ageing. The carbon-13 spectra from some aged samples showed signals not present in the spectrum from an unaged sample. This was taken to be evidence of chemical degradation. Proton MAS and the WISE exeriment gave some information about the nature of the water in the sample.

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References

  • Burum, D. P. and Rhim, W. K. (1979) Analysis of multiple pulse NMR solids,J. Chem. Phys. 71, 944.

    Google Scholar 

  • Emsley, A. M. and Stevens, G. C. (1994a) Review of chemical indicators of degradation of cellulosic electrical paper insulation in oil-filled transformers,IEE Proc., Sci. Measure. Technol. 141 (5), 324–333.

    Google Scholar 

  • Emsley, A. M. and Stevens, G. C. (1994b) Kinetics and mechanisms of the low-temperature degradation of cellulose,Cellulose 1, 26–56.

    Google Scholar 

  • Horii, F., Hirai, A. and Kitamaru, R. (1984) CPMAS carbon-13 NMR study of spin relaxation phenomena of cellulose containing crystalline and noncrystalline components,J. Carbohydr. Chemi. 3 (4), 641–662.

    Google Scholar 

  • Kenwright, A. M. and Say, B. J. (1993) Solid-state proton NMR studies of polymers, inNMR Spectroscopy of Polymers, (R. N. Ibbett, ed.) Glasgow: Blackie Academic and Professional.

    Google Scholar 

  • Mansfield, P. (1965) Multiple-pulse NMR transients in solids,Phys. Rev. 137 (3A), 961–974.

    Google Scholar 

  • McBrierty, V. J. (1974) NMR of solid polymers: a review,Polymer 15, 503–520.

    Google Scholar 

  • McBrierty, V. J. and Douglass, D. C. (1981) Recent advances in the NMR of solid polymers,J. Polym. Sci.: Macromol. Rev. 16, 295–366.

    Google Scholar 

  • Schaefer, J. and Stejskal, E. O. (1976) Carbon-13 NMR of polymers spinning at the magic-angle.J. Am. Chem. Soc. 98, 1031–1033.

    Google Scholar 

  • Schmidt-Rohr, K., Clauss, J. and Spiess, H. W. (1992) Correlation of structure, mobility and morphological information in heterogeneous polymer materials by two-dimensional wideline separation NMR spectroscopy,Macromolecules 25, 3273–3277.

    Google Scholar 

  • VanderHart, D. L. and Atalla, R. H. (1984) Studies of microstructure in native celluloses using solid-state13C NMR,Macromolecules 17 (8), 1465–1472.

    Google Scholar 

  • Wehrli, F. W. and Wirthlin, T. (1976)Interpretation of Carbon-13 Spectra, London: Heyden.

    Google Scholar 

Download references

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Ali, M., Apperley, D.C., Eley, C.D. et al. A solid-state NMR study of cellulose degradation. Cellulose 3, 77–90 (1996). https://doi.org/10.1007/BF02228792

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