Titre :

Accelerating high-resolution NMR of half-integer quadrupolar nuclei in solids: SPAM-MQMAS and SPAM-STMAS

Auteur(s) :

Sasaki, Akiko [Auteur]
Tsutsumi, Yu [Auteur]
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 :

108

Pagination :

101668

Date de publication :

2020-08

ISSN :

09262040

Discipline(s) HAL :

Chimie/Chimie inorganique

Résumé en anglais : [en]

In solid-state NMR, multiple-quantum MAS (MQMAS) and satellite-transition MAS (STMAS) experiments are well-established techniques to obtain high-resolution spectra of half-integer quadrupolar nuclei. In 2004 and 2005, a ...
Lire la suite >In solid-state NMR, multiple-quantum MAS (MQMAS) and satellite-transition MAS (STMAS) experiments are well-established techniques to obtain high-resolution spectra of half-integer quadrupolar nuclei. In 2004 and 2005, a soft-pulse-added-mixing (SPAM) concept was introduced by Gan and Amoureux to enhance the S/N ratio of MQMAS and STMAS experiments. Despite their robustness and simplicity, SPAM approaches have not yet been widely applied. Here, we further exploit SPAM concepts for sensitivity enhancement upon acquisition of two-dimensional MQMAS and STMAS spectra and also establish a general procedure upon implementation of SPAM-MQMAS and SPAM-STMAS NMR. Its effectiveness and ease in experimental setup are demonstrated using simulations and experiments performed on I ​= ​3/2 (23Na, 87Rb), 5/2 (27Al, 85Rb) and 9/2 (93Nb) nuclei with a variety of quadrupolar coupling constants (CQ). Compared to the conventional z-filter methods, sensitivity enhancements in between 2 and 4 are achievable with SPAM. We recommend to use SPAM with a ratio of 4:1 for the number of echoes and antiechoes to safely maximize the sensitivity and resolution simultaneously. In addition, a comparison of the experimental approaches is made in the context of SPAM-MQMAS and SPAM-STMAS NMR with respect to repetition delay and spinning frequency, aiming to discuss the precautions upon making a judicious choice of high-resolution NMR methods of half-integer quadrupolar nuclei.Lire moins >

Langue :

Anglais

Comité de lecture :

Oui

Audience :

Internationale

Vulgarisation :

Non

Établissement(s) :

CNRS
Centrale Lille
ENSCL
Univ. Artois
Université de Lille

Collections :

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

Équipe(s) de recherche :

RMN et matériaux inorganiques (RM2I)

Date de dépôt :

2021-12-08T09:51:28Z
2022-03-01T15:38:15Z
2023-12-05T10:02:29Z