Improvements in Resolution of 1H NMR of solids

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 li...

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Main Authors: Bruno Simões de Almeida, Lyndon Emsley
Format: Article
Language:deu
Published: Swiss Chemical Society 2023-04-01
Series:CHIMIA
Subjects:
Online Access:https://www.chimia.ch/chimia/article/view/6950
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author Bruno Simões de Almeida
Lyndon Emsley
author_facet Bruno Simões de Almeida
Lyndon Emsley
author_sort Bruno Simões de Almeida
collection DOAJ
description 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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spelling doaj.art-0dafe9dc08084ea2b858d88b4d78acf02023-05-16T00:10:58ZdeuSwiss Chemical SocietyCHIMIA0009-42932673-24242023-04-0177410.2533/chimia.2023.212Improvements in Resolution of 1H NMR of solidsBruno Simões de Almeida0Lyndon Emsley1Institut des Sciences et Ingénierie Chimiques, Ecole Polytechnique Fédérale de Lausanne (EPFL), CH-1015 LausanneInstitut des Sciences et Ingénierie Chimiques, Ecole Polytechnique Fédérale de Lausanne (EPFL), CH-1015 Lausanne 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.   https://www.chimia.ch/chimia/article/view/6950Magic angle spinning anti-z COSYPIPSolid-state NMR
spellingShingle Bruno Simões de Almeida
Lyndon Emsley
Improvements in Resolution of 1H NMR of solids
CHIMIA
Magic angle spinning anti-z COSY
PIP
Solid-state NMR
title Improvements in Resolution of 1H NMR of solids
title_full Improvements in Resolution of 1H NMR of solids
title_fullStr Improvements in Resolution of 1H NMR of solids
title_full_unstemmed Improvements in Resolution of 1H NMR of solids
title_short Improvements in Resolution of 1H NMR of solids
title_sort improvements in resolution of 1h nmr of solids
topic Magic angle spinning anti-z COSY
PIP
Solid-state NMR
url https://www.chimia.ch/chimia/article/view/6950
work_keys_str_mv AT brunosimoesdealmeida improvementsinresolutionof1hnmrofsolids
AT lyndonemsley improvementsinresolutionof1hnmrofsolids