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Solid-State 13C NMR in Oil Shale Research: An Introduction with Selected Applications

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Composition, Geochemistry and Conversion of Oil Shales

Part of the book series: NATO ASI Series ((ASIC,volume 455))

Abstract

An introduction to solid-state 13C NMR techniques and their applications to oil shale research are discussed. Techniques include cross polarization and magic-angle spinning with high-power decoupling, single pulse excitation, dipolar dephasing, and sideband suppression at high magnetic fields. The quantitative reliability of solid-state 13C NMR measurements is discussed also. Results from recent studies on coals show that single pulse methods give more reliable carbon aromaticities than those obtained using cross polarization. This is because a greater percentage of the total carbons are observed in the single pulse experiment than in the cross polarization experiment. Similar comparisons for oil shales have not been made. However, because oil shales generally are more aliphatic than coals, differences in measured carbon aromaticities and percentages of carbons observed may not be as serious a problem for oil shales. Selected applications of solid-state 13C NMR techniques to oil shale resource evaluation, oil shale conversion, and structure are presented.

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7. References

  1. Yen T.F. and G. V. Chilingarian eds., Oil Shale, Elsevier, New York, 1976.

    Google Scholar 

  2. Breger I.A., Organic Geochemistry. Pergamon Press, London, 1963.

    Google Scholar 

  3. Durand B., ed, Kerogen, Editions Technip, Paris, 1980.

    Google Scholar 

  4. Eglinton G. and M.T.J. Murphy, Organic Geochemistry, Springer-Verlag, New York, 1969.

    Google Scholar 

  5. Tissot B.P. and D.H. Welte, Petroleum Formation and Occurrence, Springer-Verlag,New York, 1978.

    Book  Google Scholar 

  6. Pelet R. in Petrakis L. and J.P. Fraissard, eds, Magnetic Resonance, Introduction, Advanced Methods, and Applications to Fossil Energy, NATO ASI Series C, 124, D. Reidel Pub. Co., Dordrecht, Netherlands, 1984, pp 219–233.

    Google Scholar 

  7. 6a Miknis F.P. and J.F. McKay, eds, Geochemistry and Chemistry of Oil Shales, ACS Symp. Series 230, Am. Chem. Soc. Washington, DC, 1983 .

    Google Scholar 

  8. VanderHart D.L. and H.L. Retcofsky, Fuel, 55, 202, (1976).

    Article  Google Scholar 

  9. Bartuska V.J., G.E. Maciel, J. Schaefer, and E.O. Stejskal, Fuel, 56, 354,(1977).

    Article  Google Scholar 

  10. Resing H.A., A.N. Garroway, and R.N. Hazlett, Fuel, 57, 450, (1978).

    Article  Google Scholar 

  11. Miknis F.P., and D.A. Netzel, in Magnetic Resonance in Colloid and Interface Science, H.A. Resing and C.G. Wade, eds., ACS Symp.Ser.34, Am. Chem. Soc., Washington, DC, 1976, Ch. 16.

    Google Scholar 

  12. Axelson D.E, Solid State Nuclear Magnetic Resonance of Solid Fossil Fuels, Multiscience Publications Ltd., CANMET and Canadian Government Publishing Centre, 1985.

    Google Scholar 

  13. Fyfe C.A., Solid State NMR For Chemists, CFC Press, Guelph, Ontario, Canada, 1983.

    Google Scholar 

  14. Wilson M.A., NMR Techniques and Applications in Geochemistry and Soil Chemistry, Pregamon Press, New York, 1987.

    Google Scholar 

  15. Petrakis L. and J.P. Fraissard, eds, Magnetic Resonance, Introduction, Advanced Methods, and Applications to Fossil Energy, NATO ASI Series C, 124, D. Reidel Pub. Co., Dordrecht, Netherlands, 1984.

    Google Scholar 

  16. Wershaw R.L. and M.A. Mikita, eds., NMR of Humic Substances and Coal, Lewis Publishers, Chelsea, MI, 1987.

    Google Scholar 

  17. R.E. Botto and Y.Sanada, eds., Magnetic Resonance of Carbonaceous Solids, Adv. Chem. Ser. 229, Am. Chem. Soc., Washington, DC, 1993.

    Google Scholar 

  18. Miknis F.P., Magn. Reson. Rev., 7, 87, (1982)

    Google Scholar 

  19. Miknis F.P., in Y. Yurum, ed., New Trends in Coal Science, NATO ASI Series C, V244, Kluwer Academic Publishers, Boston, 1988, pp117–158.

    Chapter  Google Scholar 

  20. Davidson R.M., Nuclear Magnetic Resonance Studies of Coal, IEA COal Research, London, 1986, Report No. ICTIS/TR32

    Google Scholar 

  21. Pines A., M.G. Gibby, and J.S. Waugh, J. Chem. Phys., 54,569 (1973)

    Article  Google Scholar 

  22. Schaefer J.and E.O. Stejskal, J. Am. Chem. Soc., 98, 569, (1976).

    Google Scholar 

  23. Wind R.A., G.E. Maciel, and R.E. Botto, in Magnetic Resonance of Carbonaceous Solids, R.E. Botto and Y.Sanada, eds, Adv. Chem. Ser. 229, Am. Chem. Soc., Washington, DC, 1993, Ch1

    Google Scholar 

  24. Sullivan M.J. and G.E. Maciel, Anal. Chem., 54, 1615, (1982).

    Article  Google Scholar 

  25. Dixon W.T., J. Magn. Reson., 44, 220, (1981).

    Article  Google Scholar 

  26. Adachi Y. and M. Nakamizo, in, Magnetic Resonance of Carbonaceous Solids, Adv. Chem. Series 229, Botto R.E. and Y. Sanada eds., Am. Chem.Soc. Washington, DC, 1993, Ch 13.

    Google Scholar 

  27. Sullivan M.J. in Petrakis L. and J.P. Fraissard, eds, Magnetic Resonance, Introduction, Advanced Methods, andApplications to Fossil Energy, NATO ASI Series C, 124, D. Reidel Pub. Co., Dordrecht, Netherlands, 1984. pp 525–533.

    Google Scholar 

  28. Zhang and Maciel, J. Magn. Reson., 25, 156, (1989).

    Google Scholar 

  29. Miknis F.P., J.Jhou, D.B. MacGowan, and R.C. Surdam, Org. Geochem., 20, 339,(1993).

    Article  Google Scholar 

  30. Franz J.A., and J.C. Linehan, in R.E. Botto and Y.Sanada, eds., Magnetic Resonance of Carbonaceous Solids, Adv. Chem. Ser. 229, Am. Chem. Soc., Washington, DC, 1993. Ch20.

    Google Scholar 

  31. Love G.D., R.V. Law, and C.E. Snape, Energy and Fuels, 7,639 (1993).

    Google Scholar 

  32. Sullivan M.J. and G.E. Maciel, Anal. Chem. 54, 1606, (1982).

    Article  Google Scholar 

  33. Yurum Y., ed., New Trends in Coal Science, NATO ASI Series C, V244, Kluwer Academic Publishers, Boston, 1988.

    Google Scholar 

  34. Murphy P.D.,T.J. Cassady,and B.C. Gerstein, Fuel, 61, 1233, (1982).

    Article  Google Scholar 

  35. Opella S.J., and M.H. Frey, J. Am. Chem. Soc., 101, 5854 (1979)

    Article  Google Scholar 

  36. Wilson MA, Vassallo A.M., and N.J. Russell, Org. Geochem., 5, 35, (1983).

    Article  Google Scholar 

  37. Botto R.E., R. Wilson, and R.E. Winans, Energy and Fuels, 1, 173, (1987).

    Article  Google Scholar 

  38. Zhang M. and G.E. Maciel, Fuel, 69, 557, (1990).

    Article  Google Scholar 

  39. Maciel G.E., C.E. Bronnimann, A. Jurkiewicz, R.A. Wind, and V.H. Pan, Fuel, 70, 925, (1991).

    Article  Google Scholar 

  40. Miknis F.P., M.J. Sullivan, V.J.Bartuska, and G.E. Maciel, Org. Geochem., 3, 19, (1981)

    Article  Google Scholar 

  41. Dudley R.L. and C. A. Fyfe, Fuel, 61, 651, (1983).

    Article  Google Scholar 

  42. Packer K.J., R.K. Harris, A.M. Kenwright, and C.E. Snape, Fuel, 62, 999, (1983).

    Article  Google Scholar 

  43. Wilson M.A., P.J. Collin, R.J. Pugmire, and D.M. Grant, Fuel, 61, 959,(1982).

    Article  Google Scholar 

  44. Wilson M.A., A.M. Vassallo, P.J. Collin, and H. Rottendorf, Anal. Chem., 56, 433, (1984).

    Article  Google Scholar 

  45. Snape C.E., D.E. Axelson, R.E. Botto, J.J. Delpeuch, P.Tekely, B.C.Gerstein, M. Pruski, G.E. Maciel, and M.A. Wilson, Fuel, 68, 547,

    Google Scholar 

  46. Wilson M.A., A.M. Vassalo, D. Gizachew, and E. Lafargue, Org.Geochem., 17, 107,(1991).

    Article  Google Scholar 

  47. Stock L.M., J.V. Muntean, and R.E. Botto, in Yurum Y., ed., New Trends in Coal Science, NATO ASI Series C, V244, Kluwer Academic Publishers, Boston, 1988, ppl59–167.

    Google Scholar 

  48. Muntean J.V., L.M. Stock, and R.E. Botto, J. Magn. Reson., 76, 540, (1988).

    Article  Google Scholar 

  49. Muntean J.V., L.M. Stock, and R.E. Botto, Energy Fuels, 2, 108, (1988).

    Article  Google Scholar 

  50. Maciel G.E, V.J. Bartuska, and F.P. Miknis, Fuel, 58, 391, (1979).

    Article  Google Scholar 

  51. Miknis F.P., G.E. Maciel, and V.J. Bartuska, Org. Geochem., 1, 169,(1979)47.

    Article  Google Scholar 

  52. Maciel G.E, V.J. Bartuska, and F.P. Miknis, Fuel, 57, 505, (1978).

    Article  Google Scholar 

  53. Hagaman E.W., F.M. Schell, and D.C. Cronauer, Fuel,, 63, 915, (1984).

    Article  Google Scholar 

  54. Evans E., B. Batts, and N. Cant, Fuel, 66, 326, (1987).

    Article  Google Scholar 

  55. Miknis F.P. and P.J. Conn, Fuel, 65, 248, (1986).

    Article  Google Scholar 

  56. Miknis F.P., Fuel. 71, 731, (1993).

    Article  Google Scholar 

  57. Sato S., M. Enomoto, and S. Takahashi, Fuel Proc. Technol, 18, 305 (1988).

    Article  Google Scholar 

  58. Miknis F.P., D.A. Netzel, J.W. Smith, M.A. Mast, and G.E.Maciel, Geochim. Cosmochim. Acta, 46, 977, (1982).

    Article  Google Scholar 

  59. Miknis F.P., N.M. Severenyi, and G.E. Maciel, Fuel, 61, (1982).

    Google Scholar 

  60. Qin K., D. Chen, and Z. Li, Org. Geochem. 17, 856 (1991).

    Google Scholar 

  61. Hershkowitz F., W.N. Olmstead, R.P. Rhodes, and K.D. Rose, in Geochemistry and Chemistry of Oil Shales, F.P. Miknis and J.F. McKay, eds, ACS Symp. Series 230,Am. Chem. Soc., Washington, DC, 1983, Ch. 15.58.

    Google Scholar 

  62. Burhnam A.K., and J.A. Happe, Fuel, 63, 1353, (1984).

    Article  Google Scholar 

  63. Miknis F.P., T.F. Turner, L.W. Ennen, and D.A. Netzel, Fuel, 67, 1568, (1988).

    Article  Google Scholar 

  64. Schmitt K.D., and E.W. Sheppard, Fuel, 63, 1241 (1984).

    Article  Google Scholar 

  65. Trewhella M.J., I.J. F. Poplet, and A. Grint, Fuel, 65, 541, (1986).

    Article  Google Scholar 

  66. Solum M.S., R.J. Pugmire, and D.M. Grant, Energy and Fuels, 3, 187, (1989).

    Article  Google Scholar 

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Miknis, F.P. (1995). Solid-State 13C NMR in Oil Shale Research: An Introduction with Selected Applications. In: Snape, C. (eds) Composition, Geochemistry and Conversion of Oil Shales. NATO ASI Series, vol 455. Springer, Dordrecht. https://doi.org/10.1007/978-94-011-0317-6_5

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  • DOI: https://doi.org/10.1007/978-94-011-0317-6_5

  • Publisher Name: Springer, Dordrecht

  • Print ISBN: 978-94-010-4140-9

  • Online ISBN: 978-94-011-0317-6

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