Improved sensitivity and quantification ...
Document type :
Article dans une revue scientifique: Article original
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Title :
Improved sensitivity and quantification for 29Si NMR experiments on solids using UDEFT (Uniform Driven Equilibrium Fourier Transform)
Author(s) :
Duong, Nghia Tuan [Auteur]
Trebosc, Julien [Auteur]
Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Lafon, Olivier [Auteur]
Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Amoureux, Jean-Paul [Auteur]
Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Trebosc, Julien [Auteur]
Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Lafon, Olivier [Auteur]

Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Amoureux, Jean-Paul [Auteur]

Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Journal title :
Solid State Nuclear Magnetic Resonance
Abbreviated title :
Solid State Nuclear Magnetic Resonance
Volume number :
100
Pages :
52-62
Publication date :
2019-08
ISSN :
09262040
English abstract : [en]
We demonstrate the possibility to use UDEFT (Uniform Driven Equilibrium Fourier Transform) technique in order to improve the sensitivity and the quantification of one-dimensional 29Si NMR experiments under magic-angle ...
Show more >We demonstrate the possibility to use UDEFT (Uniform Driven Equilibrium Fourier Transform) technique in order to improve the sensitivity and the quantification of one-dimensional 29Si NMR experiments under magic-angle spinning (MAS). We derive an analytical expression of the signal-to-noise ratios of UDEFT and single-pulse (SP) experiments subsuming the contributions of transient and steady-state regimes. Using numerical spin dynamics simulations and experiments on 29Si-enriched amorphous silica and borosilicate glass, we show that 59180298059180 refocusing composite π-pulse and the adiabatic inversion using tanh/tan modulation improve the robustness of UDEFT technique to rf-inhomogeneity, offset, and chemical shift anisotropy. These pulses combined with a two-step phase cycle limit the pulse imperfections and the artifacts produced by stimulated echoes. The sensitivity of SP, UDEFT and CPMG (Carr-Purcell-Meiboom-Gill) techniques are experimentally compared on functionalized and non-functionalized mesoporous silica. Furthermore, experiments on a flame retardant material prove that UDEFT technique provides a better quantification of 29Si sites with higher sensitivity than SP method.Show less >
Show more >We demonstrate the possibility to use UDEFT (Uniform Driven Equilibrium Fourier Transform) technique in order to improve the sensitivity and the quantification of one-dimensional 29Si NMR experiments under magic-angle spinning (MAS). We derive an analytical expression of the signal-to-noise ratios of UDEFT and single-pulse (SP) experiments subsuming the contributions of transient and steady-state regimes. Using numerical spin dynamics simulations and experiments on 29Si-enriched amorphous silica and borosilicate glass, we show that 59180298059180 refocusing composite π-pulse and the adiabatic inversion using tanh/tan modulation improve the robustness of UDEFT technique to rf-inhomogeneity, offset, and chemical shift anisotropy. These pulses combined with a two-step phase cycle limit the pulse imperfections and the artifacts produced by stimulated echoes. The sensitivity of SP, UDEFT and CPMG (Carr-Purcell-Meiboom-Gill) techniques are experimentally compared on functionalized and non-functionalized mesoporous silica. Furthermore, experiments on a flame retardant material prove that UDEFT technique provides a better quantification of 29Si sites with higher sensitivity than SP method.Show less >
Language :
Anglais
Peer reviewed article :
Oui
Audience :
Internationale
Popular science :
Non
Administrative institution(s) :
CNRS
Centrale Lille
ENSCL
Univ. Artois
Université de Lille
Centrale Lille
ENSCL
Univ. Artois
Université de Lille
Collections :
Research team(s) :
RMN et matériaux inorganiques (RM2I)
Submission date :
2021-12-08T09:52:47Z
2022-02-28T15:18:01Z
2022-03-01T09:48:55Z
2022-02-28T15:18:01Z
2022-03-01T09:48:55Z
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