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Improving the sensitivity of J coupling measurements in solids with application to disordered materials

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Guerry, Paul, Brown, Steven P. and Smith, Mark E. (2016) Improving the sensitivity of J coupling measurements in solids with application to disordered materials. AIP Advances, 6 (5). 055008. doi:10.1063/1.4948965

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Official URL: http://dx.doi.org/10.1063/1.4948965

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Abstract

It has been shown previously that for magic angle spinning (MAS) solid state NMR the refocused INADEQUATE spin-echo (REINE) experiment can usefully quantify scalar (J) couplings in disordered solids. This paper focuses on the two z filter components in the original REINE pulse sequence, and investigates by means of a product operator analysis and fits to density matrix simulations the effects that their removal has on the sensitivity of the experiment and on the accuracy of the extracted J couplings. The first z filter proves unnecessary in all the cases investigated here and removing it increases the sensitivity of the experiment by a factor ∼1.1–2.0. Furthermore, for systems with broad isotropic chemical shift distributions (namely whose full widths at half maximum are greater than 30 times the mean J coupling strength), the second z filter can also be removed, thus allowing whole-echo acquisition and providing an additional √2 gain in sensitivity. Considering both random and systematic errors in the values obtained, J couplings determined by fitting the intensity modulations of REINE experiments carry an uncertainty of 0.2–1.0 Hz (∼1−10 %).

Item Type: Journal Article
Subjects: Q Science > QC Physics
Divisions: Faculty of Science > Physics
Library of Congress Subject Headings (LCSH): Particles (Nuclear physics), Solids, Nuclear magnetic resonance spectroscopy
Journal or Publication Title: AIP Advances
Publisher: American Institute of Physics
ISSN: 2158-3226
Official Date: 4 May 2016
Dates:
DateEvent
4 May 2016Published
26 April 2016Accepted
26 November 2015Submitted
Volume: 6
Number: 5
Article Number: 055008
DOI: 10.1063/1.4948965
Status: Peer Reviewed
Publication Status: Published
Access rights to Published version: Restricted or Subscription Access
Funder: Engineering and Physical Sciences Research Council (EPSRC), University of Lancaster
Grant number: EP/C000633/1

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