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  4. High-Resolution H-1 Solid-State NMR Spectroscopy Using Windowed LG4 Homonuclear Dipolar Decoupling
 
research article

High-Resolution H-1 Solid-State NMR Spectroscopy Using Windowed LG4 Homonuclear Dipolar Decoupling

Halse, Meghan E.
•
Schlagnitweit, Judith
•
Emsley, Lyndon  
2014
ISRAEL JOURNAL OF CHEMISTRY

We investigate the optimal implementation of windowed LG4 decoupling for the direct acquisition of high-resolution H-1 solid-state NMR spectra in the moderate magic-angle spinning regime ((r)<2 x 35kHz). We determine how the optimal value of the azimuth of the LG rotation axis, , is affected by the choice of windowing parameters. We find that for both the windowless and windowed implementation of LG4, the optimal value of is that for which the chemical-shift scaling factor is approximately 0.43. We then provide an analytical expression for estimating the chemical-shift scaling factor as a function of both and the windowed decoupling parameters, which allows the optimal value of to be easily determined for any implementation of LG4. We also introduce a simple and general method for improving the performance of any phase-modulated homonuclear dipolar decoupling sequence by compensating for pulse imperfection errors that accumulate in windowed spectra due to the repeated switching of the RF irradiation. This method involves the introduction of short (<0.5 mu s) compensation pulses at the start and end of each decoupling pulse, the duration and phase of which are chosen to cancel the effects of the amplitude and phase transients that arise as a result of the RF switching. We demonstrate how this method can be implemented for homonuclear dipolar decoupling sequences such as wPMLG and wLG4 to reduce the chemical-shift scaling factor distortions generated by phase transients such that high-quality, high-resolution H-1 NMR spectra can be acquired at arbitrary RF offsets.

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Type
research article
DOI
10.1002/ijch.201300101
Web of Science ID

WOS:000332009500014

Author(s)
Halse, Meghan E.
Schlagnitweit, Judith
Emsley, Lyndon  
Date Issued

2014

Publisher

WILEY-V C H VERLAG GMBH

Published in
ISRAEL JOURNAL OF CHEMISTRY
Volume

54

Issue

1-2, SI

Start page

136

End page

146

Subjects

Lee-Goldburg decoupling

•

magic-angle spinning

•

NMR spectroscopy

•

RF pulse imperfections

•

solid-state NMR

Editorial or Peer reviewed

REVIEWED

Written at

OTHER

EPFL units
LRM  
Available on Infoscience
January 8, 2015
Use this identifier to reference this record
https://infoscience.epfl.ch/handle/20.500.14299/109953
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