Quantitative Aspects of Structural Resolution Methods in CP. MAS 13C NMR

  • J. M. Dereppe
Chapter
Part of the NATO ASI Series book series (ASIC, volume 124)

Abstract

Solid state 13C NMR studies of materials such as coals, kerogens, asphaltenes are usually made in order to characterize and quantify chemical identities of the various constituents. Unfortunately these spectra do not exhibit a high level of resolution. They usually consist of two broad bands corresponding to aromatic/olefinic carbons and to aliphatic carbons. These aromatic and aliphatic bands sometimes show shoulders suggesting the presence of certain structure moeities. It has been shown (1) that the line width is primarily due to the heterogeneous nature of the sample, e.g. due to a multitude of similar but slightly different chemical shifts. Resolution enhancing methods, based on differential relaxation behavior, are therfore useful for distinguishing structural differences that would not appear in the usual CP. MAS spectra. The general problem of the analytical reliability of the results obtained by the CP. MAS method has been studied in various ways (2,3). The purpose of this work is to explore the quantitative aspects of the results obtained by some structural resolution methods. The approach used here is to compare these results with data obtained by the more classical methods of high resolution on liquids.

Keywords

Magnetization Curve Aromatic Carbon Methyl Carbon Aliphatic Carbon Saturated Carbon 
These keywords were added by machine and not by the authors. This process is experimental and the keywords may be updated as the learning algorithm improves.
This is a preview of subscription content, log in to check access.

Preview

Unable to display preview. Download preview PDF.

Unable to display preview. Download preview PDF.

References

  1. (1).
    A.R. Palmer and G.E. Maciel, 1982. Anal. Chem., 54, p. 2194CrossRefGoogle Scholar
  2. (2).
    G.E. Maciel, V.J. Bartuska, F.P. Miknis, 1979. Fuel, 58, p. 391CrossRefGoogle Scholar
  3. (3).
    P. Du Bois Murphy, T.J. Cassady and B.C. Gerstein, 1982, Fuel, 61, p. 1233CrossRefGoogle Scholar
  4. (4).
    D.J. Cookson and B.E. Smith, 1981. Org.Magn.Reson., 16, p. 111CrossRefGoogle Scholar
  5. (5).
    A. Pines, M.G. Gibby and J.S. Waugh, 1973. J.Chem.Phys., 59, p. 582CrossRefGoogle Scholar
  6. (6).
    M.T. Sullivan and G.E. Maciel, 1982. Anal. Chem., 54, p. 1606CrossRefGoogle Scholar
  7. (7).
    P. Du Bois Murphy and B.C. Gerstein, 1982. Anal.Chem., 54, p. 522CrossRefGoogle Scholar
  8. (8).
    S. Gillet and J.J. Delpuech, 1980. J.Magn.Res., 38, p. 433Google Scholar
  9. (9).
    M.A. Wilson, P.J. Collin, R.J. Pugmire and D.M. Grant, 1982. Fuel, 61, p. 959CrossRefGoogle Scholar
  10. (10).
    D.J. Cookson and B.E. Smith, 1982. Fuel, 61, p. 1007CrossRefGoogle Scholar
  11. (11).
    T. Suzuki, 1982. Fuel, 61, p. 402CrossRefGoogle Scholar
  12. (12).
    J. Schaefer and E.O. Stejskal, 1976. J.Am.Chem.Soc., 98, p. 1031CrossRefGoogle Scholar
  13. (13).
    A.N. Garroway, W.B. Moniz and H.A. Resing in “Carbon-13 NMR in Polymer Science”, Ed W. M. Baska. Am.Chem.Soc.Symp.Ser.103Google Scholar
  14. (14).
    A.R. Palmer and G.E. Maciel, 1982. Anal.Chem., 54, p. 2194CrossRefGoogle Scholar
  15. (15).
    D. L. Vander Hart and A.N. Garroway, 1979. J. Chem. Phys., 71, p. 2773CrossRefGoogle Scholar
  16. (16).
    J. Schaefer, E.O. Stejskal and R. Buchdal, 1977. Macromolecules, 10, p. 384CrossRefGoogle Scholar

Copyright information

© D. Reidel Publishing Company 1984

Authors and Affiliations

  • J. M. Dereppe
    • 1
  1. 1.University of LouvainLouvain-la-NeuveBelgique

Personalised recommendations