Improved sensitivity and quantification ...
Type de document :
Article dans une revue scientifique: Article original
URL permanente :
Titre :
Improved sensitivity and quantification for 29Si NMR experiments on solids using UDEFT (Uniform Driven Equilibrium Fourier Transform)
Auteur(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
Titre de la revue :
Solid State Nuclear Magnetic Resonance
Nom court de la revue :
Solid State Nuclear Magnetic Resonance
Numéro :
100
Pagination :
52-62
Date de publication :
2019-08
ISSN :
09262040
Résumé en anglais : [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 ...
Lire la suite >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.Lire moins >
Lire la suite >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.Lire moins >
Langue :
Anglais
Comité de lecture :
Oui
Audience :
Internationale
Vulgarisation :
Non
Établissement(s) :
CNRS
Centrale Lille
ENSCL
Univ. Artois
Université de Lille
Centrale Lille
ENSCL
Univ. Artois
Université de Lille
Collections :
Équipe(s) de recherche :
RMN et matériaux inorganiques (RM2I)
Date de dépôt :
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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