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research article

High-resolution H-1 NMR of powdered solids by homonuclear dipolar decoupling

Paruzzo, Federico M.  
•
Emsley, Lyndon  
December 1, 2019
Journal of Magnetic Resonance

The development of homonuclear dipolar decoupling sequences to obtain high-resolution H-1 NMR spectra from solids has recently celebrated its 50th birthday. Over the years, a series of different decoupling schemes have been developed, starting with the pioneering Lee-Goldburg and WAHUHA sequences up to the most recent generation of experimentally optimized phase-modulated schemes such as eDUMBO-1(22) and LG4. These schemes can all yield over an order of magnitude reduction in H-1 NMR linewidths in solids. Here we provide an overview and a broad experimental comparison of the performance of the main sequences, which has so far been absent in the literature, especially between the newest and the oldest decoupling schemes. We compare experimental results obtained using eight different decoupling schemes (LG, WHH-4, MREV-8, BR-24, FSLG/PMLG, DUMBO-1, eDUMBO-1(22) and LG4) on three different microcrystalline powdered samples (alanine, glycine and beta-AspAla) and at three different MAS rates (3.0, 12.5 and 22.0 kHz). Finally, since these sequences can be technically demanding, we describe the experimental protocol we have used to optimize these schemes with the aim to provide simple guidelines for the optimization of CRAMPS experiments for all NMR users. (C) 2019 The Authors. Published by Elsevier Inc.

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Type
research article
DOI
10.1016/j.jmr.2019.106598
Web of Science ID

WOS:000497799500006

Author(s)
Paruzzo, Federico M.  
Emsley, Lyndon  
Date Issued

2019-12-01

Publisher

Academic Press Inc - Elsevier Science

Published in
Journal of Magnetic Resonance
Volume

309

Article Number

106598

Subjects

Biochemical Research Methods

•

Physics, Atomic, Molecular & Chemical

•

Spectroscopy

•

Biochemistry & Molecular Biology

•

Physics

•

Spectroscopy

•

solid-state nmr

•

high-resolution

•

homonuclear dipolar decoupling

•

cramps

•

h-1 nmr

•

pulse sequences optimization

•

multiple-pulse nmr

•

nuclear-magnetic-resonance

•

state nmr

•

high-order

•

low-power

•

spectroscopy

•

proton

•

sequences

•

mas

•

rotation

Note

This is an open access article under the terms of the Creative Commons Attribution License

Editorial or Peer reviewed

REVIEWED

Written at

EPFL

EPFL units
LRM  
FunderGrant Number

FNS

200020_178860

Available on Infoscience
December 5, 2019
Use this identifier to reference this record
https://infoscience.epfl.ch/handle/20.500.14299/163554
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