Improvements in Resolution of ¹H NMR of solids

Authors

  • Bruno Simões de Almeida Institut des Sciences et Ingénierie Chimiques, Ecole Polytechnique Fédérale de Lausanne (EPFL), CH-1015 Lausanne
  • Lyndon Emsley Institut des Sciences et Ingénierie Chimiques, Ecole Polytechnique Fédérale de Lausanne (EPFL), CH-1015 Lausanne

DOI:

https://doi.org/10.2533/chimia.2023.212

PMID:

38047798

Keywords:

Magic angle spinning anti-z COSY, PIP, Solid-state NMR

Abstract

Magic angle spinning (MAS) in 1H NMR has allowed progress from featureless spectra in static samples to linewidths of a few hundreds of Hertz for powdered solids at the fastest spinning rates available today (100-150 kHz). While this is a remarkable improvement, this level of resolution is still limiting to the widespread use of 1H NMR for complex systems. This review will discuss two recent alternative strategies that have significantly improved 1H resolution, when combined with fast MAS. The first is based on anti-z-COSY, a 2D experiment originally used for J decoupling in liquids, which removes residual broadening due to splittings caused by imperfect coherent averaging of MAS. The second strategy is to obtain pure isotropic proton (PIP) spectra in solids, by parametrically mapping any residual broadening due to imperfect averaging into a second dimension of a multidimensional correlation spectrum.  

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Published

2023-04-26