Improved resolution for spin-3/2 isotopes ...
Document type :
Article dans une revue scientifique: Article original
PMID :
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Title :
Improved resolution for spin-3/2 isotopes in solids via the indirect NMR detection of triple-quantum coherences using the T-HMQC sequence
Author(s) :
Bayzou, Racha [Auteur]
Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
Trebosc, Julien [Auteur]
Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Hung, Ivan [Auteur]
National High Magnetic Field Laboratory [NHMFL]
Gan, Zhehong [Auteur]
National High Magnetic Field Laboratory [NHMFL]
Rankin, Andrew [Auteur]
Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
Lafon, Olivier [Auteur]
UCCS Équipe RMN et matériaux inorganiques
Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Amoureux, Jean-Paul [Auteur]
UCCS Équipe RMN et matériaux inorganiques
Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
Trebosc, Julien [Auteur]
Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Hung, Ivan [Auteur]
National High Magnetic Field Laboratory [NHMFL]
Gan, Zhehong [Auteur]
National High Magnetic Field Laboratory [NHMFL]
Rankin, Andrew [Auteur]
Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
Lafon, Olivier [Auteur]
UCCS Équipe RMN et matériaux inorganiques
Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Amoureux, Jean-Paul [Auteur]
UCCS Équipe RMN et matériaux inorganiques
Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Journal title :
Solid State Nuclear Magnetic Resonance
Abbreviated title :
Solid State Nucl Magn Reson
Volume number :
122
Pages :
101835
Publisher :
Elsevier
Publication date :
2022-11-03
ISSN :
1527-3326
HAL domain(s) :
Chimie/Chimie inorganique
English abstract : [en]
The indirect NMR detection of quadrupolar nuclei in solids under magic-angle spinning (MAS) is possible with the through-space HMQC (heteronuclear multiple-quantum coherence) scheme incorporating the TRAPDOR (transfer of ...
Show more >The indirect NMR detection of quadrupolar nuclei in solids under magic-angle spinning (MAS) is possible with the through-space HMQC (heteronuclear multiple-quantum coherence) scheme incorporating the TRAPDOR (transfer of population in double-resonance) dipolar recoupling. This sequence, called T-HMQC, exhibits limited t1-noise. In this contribution, with the help of numerical simulations of spin dynamics, we show that most of the time, the fastest coherence transfer in the T-HMQC scheme is achieved when TRAPDOR recoupling employs the highest radiofrequency (rf) field compatible with the probe specifications. We also demonstrate how the indirect detection of the triple-quantum (3Q) coherences of spin-3/2 quadrupolar nuclei in solids improves the spectral resolution for these isotopes. The sequence is then called T-HMQC3. We demonstrate the gain in resolution provided by this sequence for the indirect proton detection of 35Cl nuclei in l-histidine∙HCl and l-cysteine∙HCl, as well as that of 23Na isotope in NaH2PO4. These experiments indicate that the gain in resolution depends on the relative values of the chemical and quadrupolar-induced shifts (QIS) for the different spin-3/2 species. In the case of NaH2PO4, we show that the transfer efficiency of the T-HMQC3 sequence employing an rf-field of 80 kHz with a MAS frequency of 62.5 kHz reaches 75% of that of the t1-noise eliminated (TONE) dipolar-mediated HMQC (D-HMQC) scheme.Show less >
Show more >The indirect NMR detection of quadrupolar nuclei in solids under magic-angle spinning (MAS) is possible with the through-space HMQC (heteronuclear multiple-quantum coherence) scheme incorporating the TRAPDOR (transfer of population in double-resonance) dipolar recoupling. This sequence, called T-HMQC, exhibits limited t1-noise. In this contribution, with the help of numerical simulations of spin dynamics, we show that most of the time, the fastest coherence transfer in the T-HMQC scheme is achieved when TRAPDOR recoupling employs the highest radiofrequency (rf) field compatible with the probe specifications. We also demonstrate how the indirect detection of the triple-quantum (3Q) coherences of spin-3/2 quadrupolar nuclei in solids improves the spectral resolution for these isotopes. The sequence is then called T-HMQC3. We demonstrate the gain in resolution provided by this sequence for the indirect proton detection of 35Cl nuclei in l-histidine∙HCl and l-cysteine∙HCl, as well as that of 23Na isotope in NaH2PO4. These experiments indicate that the gain in resolution depends on the relative values of the chemical and quadrupolar-induced shifts (QIS) for the different spin-3/2 species. In the case of NaH2PO4, we show that the transfer efficiency of the T-HMQC3 sequence employing an rf-field of 80 kHz with a MAS frequency of 62.5 kHz reaches 75% of that of the t1-noise eliminated (TONE) dipolar-mediated HMQC (D-HMQC) scheme.Show less >
Language :
Anglais
Audience :
Internationale
Popular science :
Non
ANR Project :
Other project(s) or funding source(s) :
Chevreul Institute (FR 2638)
Ministère de l’Enseignement Supérieur de la Recherche et de l’Innovation
Région Hauts de France
FEDER
R-RMN-THC FR-3050 CNRS
T-UEPEARL-20-005-LAFON-HAMDOUNA (NMR-MECA-DRUG)
National Science Foundation through NSF/DMR-1644779
State of Florida to the National High Magnetic Field Laboratory
Ministère de l’Enseignement Supérieur de la Recherche et de l’Innovation
Région Hauts de France
FEDER
R-RMN-THC FR-3050 CNRS
T-UEPEARL-20-005-LAFON-HAMDOUNA (NMR-MECA-DRUG)
National Science Foundation through NSF/DMR-1644779
State of Florida to the National High Magnetic Field Laboratory
Administrative institution(s) :
Université de Lille
CNRS
Centrale Lille
ENSCL
Univ. Artois
CNRS
Centrale Lille
ENSCL
Univ. Artois
Collections :
Research team(s) :
RMN et matériaux inorganiques (RM2I)
Submission date :
2023-05-03T00:19:15Z
2023-05-10T08:58:54Z
2023-11-24T09:32:42Z
2023-05-10T08:58:54Z
2023-11-24T09:32:42Z
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