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Low-power broadband solid-state MAS NMR of 14 N

Pell, Andrew J ; Sanders, Kevin J ; Wegner, Sebastian ; Pintacuda, Guido ; Grey, Clare P

The Journal of chemical physics, 2017-05, Vol.146 (19), p.194202 [Periódico revisado por pares]

United States: American Institute of Physics

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  • Título:
    Low-power broadband solid-state MAS NMR of 14 N
  • Autor: Pell, Andrew J ; Sanders, Kevin J ; Wegner, Sebastian ; Pintacuda, Guido ; Grey, Clare P
  • Assuntos: Analytical chemistry ; Chemical Sciences
  • É parte de: The Journal of chemical physics, 2017-05, Vol.146 (19), p.194202
  • Notas: USDOE
    AC02-05CH11231
  • Descrição: We propose two broadband pulse schemes for N solid-state magic-angle-spinning (MAS) nuclear magnetic resonance (NMR) that achieves (i) complete population inversion and (ii) efficient excitation of the double-quantum spectrum using low-power single-sideband-selective pulses. We give a comprehensive theoretical description of both schemes using a common framework that is based on the jolting-frame formalism of Caravatti et al. [J. Magn. Reson. 55, 88 (1983)]. This formalism is used to determine for the first time that we can obtain complete population inversion of N under low-power conditions, which we do here using single-sideband-selective adiabatic pulses. It is then used to predict that double-quantum coherences can be excited using low-power single-sideband-selective pulses. We then proceed to design a new experimental scheme for double-quantum excitation. The final double-quantum excitation pulse scheme is easily incorporated into other NMR experiments, as demonstrated here for double quantum-single quantum N correlation spectroscopy, and H- N dipolar heteronuclear multiple-quantum correlation experiments. These pulses and irradiation schemes are evaluated numerically using simulations on single crystals and full powders, as well as experimentally on ammonium oxalate ((NH ) C O ) at moderate MAS and glycine at ultra-fast MAS. The performance of these new NMR methods is found to be very high, with population inversion efficiencies of 100% and double-quantum excitation efficiencies of 30%-50%, which are hitherto unprecedented for the low radiofrequency field amplitudes, up to the spinning frequency, that are used here.
  • Editor: United States: American Institute of Physics
  • Idioma: Inglês

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