Evaluation of excitation schemes for ...
Document type :
Article dans une revue scientifique: Article original
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Title :
Evaluation of excitation schemes for indirect detection of 14N via solid-state HMQC NMR experiments
Author(s) :
Rankin, Andrew G.M. [Auteur]
Trebosc, Julien [Auteur]
Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Paluch, Piotr [Auteur]
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
Paluch, Piotr [Auteur]
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
Journal title :
Journal of Magnetic Resonance
Abbreviated title :
Journal of Magnetic Resonance
Volume number :
303
Pages :
28-41
Publication date :
2019-06
ISSN :
10907807
English abstract : [en]
It has previously been shown that 14N NMR spectra can be reliably obtained through indirect detection via HMQC experiments. This method exploits the transfer of coherence between single-(SQ) or double-quantum (DQ) 14N ...
Show more >It has previously been shown that 14N NMR spectra can be reliably obtained through indirect detection via HMQC experiments. This method exploits the transfer of coherence between single-(SQ) or double-quantum (DQ) 14N coherences, and SQ coherences of a suitable spin-1/2 ‘spy’ nucleus, e.g., 1H. It must be noted that SQ-SQ methods require a carefully optimized setup to minimize the broadening related to the first-order quadrupole interaction (i.e., an extremely well-adjusted magic angle and a highly stable spinning speed), whereas DQ-SQ ones do not. In this work, the efficiencies of four 14N excitation schemes (DANTE, XiX, Hard Pulse (HP), and Selective Long Pulse (SLP)) are compared using J-HMQC based numerical simulations and either SQ-SQ or DQ-SQ 1H-{14N} D-HMQC experiments on l-histidine HCl and N-acetyl-l-valine at 18.8 T and 62.5 kHz MAS. The results demonstrate that both DANTE and SLP provide a more efficient 14N excitation profile than XiX and HP. Furthermore, it is shown that the SLP scheme: (i) is efficient over a large range of quadrupole interaction, (ii) is highly robust to offset and rf-pulse length and amplitude, and (iii) is very simple to set up. These factors make SLP ideally suited to widespread, non-specialist use in solid-state NMR analyses of nitrogen-containing materials.Show less >
Show more >It has previously been shown that 14N NMR spectra can be reliably obtained through indirect detection via HMQC experiments. This method exploits the transfer of coherence between single-(SQ) or double-quantum (DQ) 14N coherences, and SQ coherences of a suitable spin-1/2 ‘spy’ nucleus, e.g., 1H. It must be noted that SQ-SQ methods require a carefully optimized setup to minimize the broadening related to the first-order quadrupole interaction (i.e., an extremely well-adjusted magic angle and a highly stable spinning speed), whereas DQ-SQ ones do not. In this work, the efficiencies of four 14N excitation schemes (DANTE, XiX, Hard Pulse (HP), and Selective Long Pulse (SLP)) are compared using J-HMQC based numerical simulations and either SQ-SQ or DQ-SQ 1H-{14N} D-HMQC experiments on l-histidine HCl and N-acetyl-l-valine at 18.8 T and 62.5 kHz MAS. The results demonstrate that both DANTE and SLP provide a more efficient 14N excitation profile than XiX and HP. Furthermore, it is shown that the SLP scheme: (i) is efficient over a large range of quadrupole interaction, (ii) is highly robust to offset and rf-pulse length and amplitude, and (iii) is very simple to set up. These factors make SLP ideally suited to widespread, non-specialist use in solid-state NMR analyses of nitrogen-containing materials.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
Centrale Lille
ENSCL
Univ. Artois
Université de Lille
Collections :
Research team(s) :
RMN et matériaux inorganiques (RM2I)
Submission date :
2021-12-08T09:52:34Z
2022-02-28T15:19:55Z
2022-03-01T09:57:55Z
2022-02-28T15:19:55Z
2022-03-01T09:57:55Z
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