Abstract
Solid state 13C nmr spectroscopy employing the experimental techniques of dipolar decoupling,2,3 magic angle spinning4,5 and 1H-13C cross polarization3 (CP/MAS-13C nmr spectroscopy) yields spectra which approach solution 13C-FT-nmr spectra in resolution and sensitivity. Resonance linewidths of 10–50 Hz in discrete organic substances are typical. Those in amorphous solids and glassy polymers generally are degraded to 50–150 Hz (2–6 ppm at 2.35T) by chemical shift dispersion and/or residual dipolar broadening.5–10 In homogeneous systems, this level of resolution permits the measurement of isotropic chemical shift and relaxation time parameters in solids.
Access this chapter
Tax calculation will be finalised at checkout
Purchases are for personal use only
Preview
Unable to display preview. Download preview PDF.
References
Research sponsored by the Division of Chemical Sciences, Office of Basic Energy Sciences, U. S. Department of Energy, under contract W-7405-eng-26 with the Union Carbide Corporation.
L. R. Sarles and R. M. Cotts, Double Nuclear Magnetic Resonance and the Dipole Interaction in Solids, Phys. Rev. 111: 853 (1958).
A. Pines, M. G. Gibby, and J. S. Waugh, Proton-enhanced NMR of Dilute Spins in Solids, J. Chem. Phys. 59: 569 (1973).
E. R. Andrew, The Narrowing of NMR Spectra of Solids by High-Speed Specimen Rotation and the Resolution of Chemical Shifts and Spin Multiplet Structures for Solids, in “Progress in Nuclear Magnetic Resonance Spectroscopy,” J. W. Ensley, J. Feeney, and L. H. Sutcliffe, eds., Pergamon Press, Oxford (1972).
J. Schaefer, E. O. Stejskal and R. Buchdahl, High-Resolution Carbon-13 Nuclear Magnetic Resonance Study of Some Solid Glassy Polymers, Macromolecules 8: 291 (1975).
J. Schaefer and E. O. Stejskal, Carbon-13 Nuclear Magnetic Resonance of Polymers Spinning at the Magic Angle, J. Am. Chem. Soc. 98: 1031 (1976).
J. Schaefer, E. O. Stejskal, and R. Buchdahl, Magic-Angle 13C NMR Analysis of Motion in Solid Glassy Polymers, Macromolecules 10: 384 (1977).
C. A. Fyfe, J. R. Lyerla, W. Volksen, and C. S. Yannoni, High-Resolution Carbon-13 Nuclear Magnetic Resonance Studies of Polymers in the Solid State. Aromatic Polyesters, Macromolecules 12: 757 (1979).
W. L. Earl and D. L. Vanderhart, Observations in Solid Polyethylenes by Carbon-13 Nuclear Magnetic Resonance with Magic Angle Sample Spinning, Macromolecules 12: 762 (1979).
W. S. Veeman, E. M. Menger, W. Ritchey, and E. deBoer, High-Resolution Carbon-13 Nuclear Magnetic Resonance of Solid Poly(oxymethylene), Macromolecules 12: 924 (1979).
D. L. Vanderhart and H. L. Retcofsky, Estimation of Coal Aromaticities by Proton-decoupled Carbon-13 Magnetic Resonance Spectra of Whole Coals, Fuel 55: 202 (1976).
V. J. Bartuska, G. E. Maciel, J. Schaefer, and E. O. Stejskal, Prospects for Carbon-13 Nuclear Magnetic Resonance Analysis of Solid Fossil Fuel Materials, Fuel 56: 354 (1977).
H. L. Retcofsky and D. L. “Vanderhart” 13C-1H Cross-polarization Nuclear Magnetic Resonance Spectra of Macérais from Coal, Fuel 57: 421 (1978).
K. W. Zilm, R. J. Pugmire, D. M. Grant, R. E. Wood, and W. H. Wiser, A Comparison of the Carbon-13 NMR Spectra of Solid Coals and their Liquids Obtained by Catalytic Hydrogénation, Fuel 58: 11 (1979).
G. E. Maciel, V. J. Bartuska, and F. P. Miknis, Characterization of Organic Material in Coal by Proton-decoupled 13C Nuclear Magnetic Resonance with Magic Angle Spinning, Fuel 58: 391 (1979).
H. A. Resing, A. N. Garroway, and R. N. Hazlett, Determination of Aromatic Hydrocarbon Fraction in Oil Shale by 13C N.M.R. with Magic-Angle Spinning, Fuel 57: 450 (1978).
F. P. Miknis, G. E. Maciel, and V. J. Bartuska, Cross Polarization Magic-Angle Spinning 13C N.M.R. Spectra of Oil Shales, Org. Geochem. 1: 169 (1979).
I. D. Campbell, C. M. Dobson, R. J. P. Williams, and A. V. Xavier, Resolution Enhancement of Protein PMR Spectra Using the Difference Between a Broadened and a Normal Spectrum, J. Magn. Res. 11: 172 (1973).
R. R. Ernst, Sensitivity Enhancement in Magnetic Resonance, in “Advances in Magnetic Resonance,” J. S. Waugh, ed., Academic Press, New York (1966).
Cf. C. H. A. Seiter, G. W. Feigenson, S. I. Chan, and M.-C. Hsu, Delayed Fourier Transform Proton Magnetic Resonance Spectroscopy, J. Am. Chem. Soc. 94: 2535 (1972).
S. R. Hartmann and E. L. Hahn, Nuclear Double Resonance in the Rotating Frame, Phys. Rev. 128: 2042 (1962).
K. Niemann and H.-P. Hombach, Studies in the Chemical Characterization of Coal: Reduction Via Solvated Electrons, Fuel 58: 853 (1979).
C. J. Collins, H.-P. Hombach, B. Maxwell, M. C. Woody, and B. M. Benjamin, Carbon-Carbon Cleavage during Birch-Hlickel-Type Reductions, J. Am. Chem. Soc. 102: 851 (1980).
Author information
Authors and Affiliations
Editor information
Editors and Affiliations
Rights and permissions
Copyright information
© 1982 Plenum Press, New York
About this chapter
Cite this chapter
Hagaman, E.W., Woody, M.C. (1982). Structure Analysis of Coals by Resolution Enhanced Solid State 13C NMR Spectroscopy. In: Filby, R.H., Carpenter, B.S., Ragaini, R.C. (eds) Atomic and Nuclear Methods in Fossil Energy Research. Springer, Boston, MA. https://doi.org/10.1007/978-1-4684-4133-8_24
Download citation
DOI: https://doi.org/10.1007/978-1-4684-4133-8_24
Publisher Name: Springer, Boston, MA
Print ISBN: 978-1-4684-4135-2
Online ISBN: 978-1-4684-4133-8
eBook Packages: Springer Book Archive