Efficient transfer of dnp-enhanced ...
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Article dans une revue scientifique: Article original
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Title :
Efficient transfer of dnp-enhanced <sup>1</sup> h magnetization to half-integer quadrupolar nuclei in solids at moderate spinning rate
Author(s) :
Nagashima, Hiroki [Auteur]
Trebosc, Julien [Auteur]
Kon, Yoshihiro [Auteur]
Lafon, Olivier [Auteur]
Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
Amoureux, Jean-Paul [Auteur]
Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
Trebosc, Julien [Auteur]

Kon, Yoshihiro [Auteur]
Lafon, Olivier [Auteur]

Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
Amoureux, Jean-Paul [Auteur]

Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
Journal title :
Magnetic resonance in chemistry . MRC
Abbreviated title :
Magn Reson Chem
Publication date :
2020-12-10
ISSN :
1097-458X
English keyword(s) :
half-integer quadrupolar nuclei
adiabatic pulse
DNP
solid-state NMR
adiabatic pulse
DNP
solid-state NMR
HAL domain(s) :
Chimie/Catalyse
English abstract : [en]
We show herein how the proton magnetization enhanced by dynamic nuclear polarization (DNP) can be efficiently transferred at moderate magic-angle spinning (MAS) frequencies to half-integer quadrupolar nuclei, S ≥ 3/2, using ...
Show more >We show herein how the proton magnetization enhanced by dynamic nuclear polarization (DNP) can be efficiently transferred at moderate magic-angle spinning (MAS) frequencies to half-integer quadrupolar nuclei, S ≥ 3/2, using the Dipolar-mediated Refocused Insensitive Nuclei Enhanced by Polarization Transfer (D-RINEPT) technique, in which a symmetry-based SR 4 2 1 recoupling scheme built from adiabatic inversion 1 H pulses reintroduces the 1 H-S dipolar couplings, while suppressing the 1 H-1 H ones. The use of adiabatic pulses also improves the robustness to offsets and radiofrequency (rf)-field inhomogeneity. Furthermore, the efficiency of the polarization transfer is further improved by using 1 H composite pulses and continuous-wave irradiations between the recoupling blocks, as well as by manipulating the S satellite transitions during the first recoupling block. Furthermore, in the case of large 1 H-S dipolar couplings, the D-RINEPT variant with two pulses on the quadrupolar channel results in an improved transfer efficiency. We compare here the performances of this new adiabatic scheme with those of its parent version with single π pulses, as well as with those of PRESTO and CPMAS transfers. This comparison is performed using simulations as well as DNP-enhanced 27 Al, 95 Mo, and 17 O NMR experiments on isotopically unmodified γ-alumina, hydrated titania-supported MoO3 , Mg(OH)2 , and l-histidine·HCl·H2 O. The introduced RINEPT method outperforms the existing methods, both in terms of efficiency and robustness to rf-field inhomogeneity and offset.Show less >
Show more >We show herein how the proton magnetization enhanced by dynamic nuclear polarization (DNP) can be efficiently transferred at moderate magic-angle spinning (MAS) frequencies to half-integer quadrupolar nuclei, S ≥ 3/2, using the Dipolar-mediated Refocused Insensitive Nuclei Enhanced by Polarization Transfer (D-RINEPT) technique, in which a symmetry-based SR 4 2 1 recoupling scheme built from adiabatic inversion 1 H pulses reintroduces the 1 H-S dipolar couplings, while suppressing the 1 H-1 H ones. The use of adiabatic pulses also improves the robustness to offsets and radiofrequency (rf)-field inhomogeneity. Furthermore, the efficiency of the polarization transfer is further improved by using 1 H composite pulses and continuous-wave irradiations between the recoupling blocks, as well as by manipulating the S satellite transitions during the first recoupling block. Furthermore, in the case of large 1 H-S dipolar couplings, the D-RINEPT variant with two pulses on the quadrupolar channel results in an improved transfer efficiency. We compare here the performances of this new adiabatic scheme with those of its parent version with single π pulses, as well as with those of PRESTO and CPMAS transfers. This comparison is performed using simulations as well as DNP-enhanced 27 Al, 95 Mo, and 17 O NMR experiments on isotopically unmodified γ-alumina, hydrated titania-supported MoO3 , Mg(OH)2 , and l-histidine·HCl·H2 O. The introduced RINEPT method outperforms the existing methods, both in terms of efficiency and robustness to rf-field inhomogeneity and offset.Show less >
Language :
Anglais
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 :
2022-03-02T07:15:23Z
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