Solid-state NMR covariance of homonuclear correlation spectra

Hu, B.; Amoureux, Jean-Paul; Trebosc, Julien; Deschamps, M.; Tricot, G.

Type de document :

Article dans une revue scientifique: Article original

DOI :

10.1063/1.2884341

PMID :

18397072

URL permanente :

http://hdl.handle.net/20.500.12210/83737

Titre :

Solid-state NMR covariance of homonuclear correlation spectra

Auteur(s) :

Hu, B. [Auteur]
Amoureux, Jean-Paul [Auteur]

Trebosc, Julien [Auteur]

Deschamps, M. [Auteur]
Tricot, G. [Auteur]

Titre de la revue :

J. Chem. Phys.

Nom court de la revue :

J. Chem. Phys.

Date de publication :

2008-04-07

ISSN :

0021-9606

Discipline(s) HAL :

Chimie

Résumé en anglais : [en]

Direct covariance NMR spectroscopy, which does not involve a Fourier transformation along the indirect dimension, is demonstrated to obtain homonuclear correlation two-dimensional (2D) spectra in the solid state. In contrast ...
Lire la suite >Direct covariance NMR spectroscopy, which does not involve a Fourier transformation along the indirect dimension, is demonstrated to obtain homonuclear correlation two-dimensional (2D) spectra in the solid state. In contrast to the usual 2D Fourier transform (2D-FT) NMR, in a 2D covariance (2D-Cov) spectrum the spectral resolution in the indirect dimension is determined by the resolution along the detection dimension, thereby largely reducing the time-consuming indirect sampling requirement. The covariance method does not need any separate phase correction or apodization along the indirect dimension because it uses those applied in the detection dimension. We compare in detail the specifications obtained with 2D-FT and 2D-Cov, for narrow and broad resonances. The efficiency of the covariance data treatment is demonstrated in organic and inorganic samples that are both well crystallized and amorphous, for spin nuclei with ⁠, ⁠, and through-space or through-bond homonuclear 2D correlation spectra. In all cases, the experimental time has been reduced by at least a factor of 10, without any loss of resolution and signal to noise ratio, with respect to what is necessary with the 2D-FT NMR. According to this method, we have been able to study the silicate network of glasses by 2D NMR within reasonable experimental time despite the very long relaxation time of the nucleus. The main limitation of the 2D-Cov data treatment is related to the introduction of autocorrelated peaks onto the diagonal, which does not represent any actual connectivity.Lire moins >

Langue :

Anglais

Établissement(s) :

Université de Lille
CNRS
Centrale Lille
ENSCL
Univ. Artois

Collections :

Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181

Équipe(s) de recherche :

RMN et matériaux inorganiques (RM2I)

Date de dépôt :

2023-05-30T18:15:31Z

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