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

Paul Guerry | Zendy; Steven P. Brown | Zendy; Mark E. Smith | Zendy

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

Author(s) -

Paul Guerry,

Steven P. Brown,

Mark E. Smith

Publication year - 2016

Publication title -

aip advances

Language(s) - English

Resource type - Journals

SCImago Journal Rank - 0.421

H-Index - 58

ISSN - 2158-3226

DOI - 10.1063/1.4948965

Subject(s) - sensitivity (control systems) , isotropy , pulse sequence , scalar (mathematics) , spinning , magic angle spinning , coupling (piping) , filter (signal processing) , spin echo , materials science , product (mathematics) , physics , computational physics , nuclear magnetic resonance , statistical physics , analytical chemistry (journal) , chemistry , nuclear magnetic resonance spectroscopy , mathematics , optics , computer science , electronic engineering , engineering , medicine , geometry , chromatography , magnetic resonance imaging , composite material , computer vision , radiology , metallurgy

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 %)

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