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Oxygen-17 dynamic nuclear polarisation enhanced solid-state NMR spectroscopy at 18.8 T

Authors :
Brownbill, Nick J
Gajan, David
Lesage, Anne
Emsley, Lyndon
Blanc, Frédéric
Dept Chem
University of Liverpool
Solid-State NMR Methods for Materials - Méthodes de RMN à l'état solide pour les matériaux
Institut des Sciences Analytiques (ISA)
Université Claude Bernard Lyon 1 (UCBL)
Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL)
Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)
Ecole Polytechnique Fédérale de Lausanne (EPFL)
Department of Chemistry and Stephenson Institute for Renewable Energy
Financial support from the EPSRC for a DTA studentship for N. J. B. and grant EP/M00869X/1 to F. B., ERC Advanced Grant No. 320860 for L. E. and EQUIPEX contract ANR-10-EQPX-47-01 for A. L. and L. E. is acknowledged.
ANR-10-EQPX-0047,SENS,RMN de Surface Exalté par Polarisation Dynamique Nucléaire(2010)
European Project: 320860,EC:FP7:ERC,ERC-2012-ADG_20120216,HI-SENS(2013)
Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL)
Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL)
Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)
Source :
CHEMICAL COMMUNICATIONS, Chemical Communications, Chemical Communications, 2017, 53 (17), pp.2563-2566. ⟨10.1039/c6cc09743j⟩, Chemical Communications, Royal Society of Chemistry, 2017, 53 (17), pp.2563-2566. ⟨10.1039/c6cc09743j⟩
Publication Year :
2017

Abstract

We thank Dr Sachin R. Chaudhari (CRMN Lyon), Kenneth K. Inglis (University of Liverpool), and Dr O. Ouari and Prof. P. Tordo (Aix-Marseille Universite, CNRS) for valuable technical assistance, sample preparation, and radicals, respectively. F. B. thanks the TGIR-RMN-THC Fr3050 CNRS for access to the 18.8 T DNP NMR facility at the CRMN. The experimental data are provided as a supporting dataset from the University of Liverpool Data Catalogue portal at https://datacat.liverpool.ac.uk/245/.; International audience; We report (17)O dynamic nuclear polarisation (DNP) enhanced solid-state NMR experiments at 18.8 T. Several formulations were investigated on the Mg(OH)2 compound. A signal enhancement factor of 17 could be obtained when the solid particles were incorporated into a glassy o-terphenyl matrix doped with BDPA using the Overhauser polarisation transfer scheme whilst the cross effect mechanism enabled by TEKPol yielded a slightly lower enhancement but more time efficient data acquisition.

Subjects

Subjects :
[CHIM]Chemical Sciences

Details

Language :
English
ISSN :
13597345 and 1364548X
Database :
OpenAIRE
Journal :
CHEMICAL COMMUNICATIONS, Chemical Communications, Chemical Communications, 2017, 53 (17), pp.2563-2566. ⟨10.1039/c6cc09743j⟩, Chemical Communications, Royal Society of Chemistry, 2017, 53 (17), pp.2563-2566. ⟨10.1039/c6cc09743j⟩
Accession number :
edsair.pmid.dedup....c9d4a1885a1d13ba6dcf39f29a4f7ba5
Full Text :
https://doi.org/10.1039/c6cc09743j⟩