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Updated: Jul 16, 2026

High-Temperature and High-Pressure In situ Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy
Published on: October 9, 2020
Observation of satellite signals due to scalar coupling to spin-1/2 isotopes in solid-state nuclear magnetic
Adriana Iuga1, Dinu Iuga, Albert R Cross
1Department of Chemistry and Biochemistry, University of Lethbridge, 4401 University Drive, Lethbridge, Alberta T1K 3M4, Canada.
Abstract:
A method is introduced to select the signal from a spin-1/2 nucleus I specifically bound to another spin-1/2 nucleus S for solid-state magic angle spinning nuclear magnetic resonance (NMR) spectroscopy via correlation through the heteronuclear J coupling. This experiment is analogous to the bilinear rotation decoupling (BIRD) sequence in liquid-state NMR spectroscopy which selects for signals from 1H directly bound to 13C. The spin dynamics of this modified BIRD experiment is described using the product-operator formalism, where experimental considerations such as rotor synchronization and the effect of large chemical shielding anisotropies on I and S are discussed. Two experiments are proposed that accommodate large chemical shielding anisotropies on S: (1) by stepping the inversion pulse frequency through the entire S spectral range or (2) by adiabatically inverting the S spins. Both these experiments are shown to successfully select the signal of 19F bound to 129Xe in XeF+ salts, removing the contributions from isotopomers containing non-spin-1/2 Xe isotopes. The feasibility in obtaining isotope-selective 19F spectra of inorganic fluoride compounds is discussed, and further modifications are proposed to expand the application to other chemical systems.
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