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- W2513303488 abstract "We report the observation of high-resolution solid-state NMR spectra of 23Na (I = 3/2), 27AI (I = 5/2) and 51V (I = 7/2) in various inorganic systems. We show that, contrary to popular belief, relatively high-resolution (-10 ppm linewidth) spectra may be obtained from quadrupolar systems, in which elec- tric quadrupole coupling constants (e2qQ/h) are in the range -1-5 MHz, by means of observation of the (1/2, - 1/2) spin transition. The (1/2, -1/2) transition for all nonintegral spin quadrupolar nuclei (I = 3/2, 5/2, 7/2, or 9/2) is only normally broadened by dipolar, chemical shift (or Knight shift) anisotropy or second-order quadrupolar effects, all of which are to a greater or lesser extent averaged under fast magic-angle sample rotation. In the case of 23Na and 27AM, high-resolution spectra of 23NaNO3 (e2qQ/h =300 kHz) and a-27A1203 (e2qQ/h -2-3 MHz) are presented; in the case of 51V205 (e2qQ/h :800 kHz), rotational echo decays are observed due to the presence of a 103-ppm chemical shift ani- sotropy. The observation of high-resolution solid-state spectra of systems having spins I = 3/2, 5/2, and 7/2 in asymmetric en- vironments opens up the possibility of examining about two out of three nuclei by solid-state NMR that were previously thought of as inaccessible due to the presence of large (a few megahertz) quadrupole coupling constants. Preliminary results for an I = 9/2 system, 93Nb, having e2qQ/h =19.5 MHz, are also reported. technical reason outlined above but also because of the increas- ing importance of second-order quadrupole effects which in- crease as (e2qQ/h)2 (15, 16). In this paper, we indicate that such problems may be cir- cumvented to a large extent by operation at very high magnetic field strength and observation solely of the (1/2, - 1/2) spin transitions of nonintegral spin quadrupolar nuclei, under con- ditions of magic-angle sample spinning. Because heteronuclear (e.g., 'H) decoupling and enhancement also may be used in such systems, and because second-order effects in many cases may be averaged to very small values, our observations open new areas of application of the magic-angle sample-spinning technique to high-resolution NMR of solids of chemical and biological interest. Independently of this work, Muiller et al. (17) have reported high-resolution NMR spectra of some alu- minum oxide compounds, some of which exhibit broad lines in the solid state (18)." @default.
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- W2513303488 date "2016-01-01" @default.
- W2513303488 modified "2023-09-27" @default.
- W2513303488 title "High-resolution solid-state NMR of quadrupolar nuclei (magic-angle spinning/nonintegral spins/second-order quadrupole interaction/rotational echoes/catalysts)" @default.
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