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Related Experiment Videos

High-resolution solid-state NMR of quadrupolar nuclei.

M D Meadows1, K A Smith, R A Kinsey

  • 1School of Chemical Sciences, University of Illinois at Urbana-Champaign, 505 South Mathews Avenue, Urbana, Illinois 61801.

Proceedings of the National Academy of Sciences of the United States of America
|February 1, 1982
PubMed
Summary

High-resolution solid-state NMR spectra are now achievable for quadrupolar nuclei, even with large quadrupole coupling constants. This breakthrough expands the range of accessible nuclei for solid-state NMR analysis in inorganic systems.

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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy
  • Inorganic materials characterization
  • Quadrupolar nuclei spectroscopy

Background:

  • Solid-state NMR of quadrupolar nuclei (e.g., Sodium-23, Aluminum-27, Vanadium-51) is often limited by large electric quadrupole coupling constants (e²qQ/h).
  • These large couplings typically lead to broad spectral lines, hindering high-resolution analysis and limiting the study of many inorganic systems.
  • Previous research suggested that nuclei with quadrupole coupling constants in the megahertz range were largely inaccessible for high-resolution solid-state NMR.

Purpose of the Study:

  • To demonstrate the feasibility of obtaining high-resolution solid-state NMR spectra from quadrupolar nuclei with significant quadrupole coupling constants.
  • To investigate the applicability of observing the ((1/2), -(1/2)) spin transition for high-resolution NMR in challenging inorganic systems.

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  • To expand the scope of nuclei amenable to detailed solid-state NMR analysis.

    • Main Methods:

    • Observation of the ((1/2), -(1/2)) spin transition in solid-state NMR experiments.
    • Application of fast magic-angle sample rotation (MAS) to average out broadening effects.
    • Acquisition of high-resolution spectra for Sodium-23, Aluminum-27, and Vanadium-51 in various inorganic compounds.

    Main Results:

    • Achieved relatively high-resolution spectra (approx. 10 ppm linewidth) for quadrupolar nuclei with e²qQ/h in the 1-5 MHz range.
    • Successfully obtained high-resolution spectra for Sodium-23 in NaNO₃ and Aluminum-27 in α-Al₂O₃.
    • Observed rotational echo decays for Vanadium-51 in V₂O₅ due to chemical shift anisotropy, while still demonstrating spectral information.
    • Preliminary results for Niobium-93 (I = 9/2) with a very large e²qQ/h (approx. 19.5 MHz) were also reported.

    Conclusions:

    • High-resolution solid-state NMR is achievable for quadrupolar nuclei with quadrupole coupling constants up to several megahertz by focusing on the ((1/2), -(1/2)) transition.
    • This technique significantly broadens the applicability of solid-state NMR, making approximately two-thirds of all nuclei accessible for study.
    • The findings overcome previous limitations, opening new avenues for detailed structural and electronic investigations of inorganic materials.