Title :

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

Author(s) :

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

108

Pages :

101668

Publication date :

2020-08

ISSN :

09262040

HAL domain(s) :

Chimie/Chimie inorganique

English abstract : [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 ...
Show more >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.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

Collections :

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

Research team(s) :

RMN et matériaux inorganiques (RM2I)

Submission date :

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