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Pushing NMR sensitivity limits using dynamic nuclear polarization with closed-loop cryogenic helium sample spinning

Eric Bouleau 1 Pierre Saint-Bonnet 2 Frederic Mentink-Vigier 3 H. Takahashi 3 Jean-François Jacquot 4 Michel Bardet 3 F. Aussenac 5 A. Purea 6 F. Engelke 6 Sabine Hediger 3 Daniel Lee 3 Gaël de Paëpe 3 
1 L3C - Laboratoire de Calculs et Conception Cryogénique
SBT - Service des Basses Températures : DRF/IRIG/SBT
2 LCF - Laboratoire de Cryogénie pour la Fusion
SBT - Service des Basses Températures : DRF/IRIG/SBT
3 RM - Magnetic Resonance
MEM - Modélisation et Exploration des Matériaux : DRF/IRIG/MEM
4 RICC - Reconnaissance Ionique et Chimie de Coordination
SYMMES - SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé : DRF/INAC/SYMMES
Abstract : We report a strategy to push the limits of solid-state NMR sensitivity far beyond its current state-of-the-art. The approach relies on the use of dynamic nuclear polarization and demonstrates unprecedented DNP enhancement factors for experiments performed at sample temperatures much lower than 100 K, and can translate into 6 orders of magnitude of experimental time-savings. This leap-forward was made possible thanks to the employment of cryogenic helium as the gas to power magic angle sample spinning (MAS) for dynamic nuclear polarization (DNP) enhanced NMR experiments. These experimental conditions far exceed what is currently possible and allows currently reaching sample temperatures down to 30 K while conducting experiments with improved resolution (thanks to faster spinning frequencies, up to 25 kHz) and highly polarized nuclear spins. The impressive associated gains were used to hyperpolarize the surface of an industrial catalyst as well as to hyperpolarize organic nano-assemblies (self-assembling peptides in our case), for whom structures cannot be solved using diffraction techniques. Sustainable cryogenic helium sample spinning significantly enlarges the realm and possibilities of the MAS-DNP technique and is the route to transform NMR into a versatile but also sensitive atomic-level characterization tool.
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Submitted on : Thursday, September 14, 2017 - 12:15:38 PM
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Eric Bouleau, Pierre Saint-Bonnet, Frederic Mentink-Vigier, H. Takahashi, Jean-François Jacquot, et al.. Pushing NMR sensitivity limits using dynamic nuclear polarization with closed-loop cryogenic helium sample spinning. Chemical Science , The Royal Society of Chemistry, 2015, 6 (12), pp.6806-6812. ⟨10.1039/c5sc02819a⟩. ⟨hal-01587521⟩



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