6-12 avr. 2021 En ligne (France)
Dynamic Nuclear Polarization at 21.15 T and 65 kHz MAS
Pierrick Berruyer  1@  , Snædís Björgvinsdóttir  1@  , Andrea Bertarello  1@  , Gabriele Stevanato  1@  , Yu Rao  1@  , Ganesan Karthikeyan  2@  , Gilles Casano  2@  , Olivier Ouari  2@  , Moreno Lelli  3@  , Christian Reiter  4@  , Frank Engelke  4@  , Lyndon Emsley  1@  
1 : Institut des Sciences et Ingénierie Chimiques, École Polytechnique Fédérale de Lausanne  (ISIC EPFL)
Av Forel 2, CH-1015 Lausanne -  Suisse
2 : Institut de Chimie Radicalaire  (ICR)  -  Site web
Aix Marseille Université : UMR7273, Centre National de la Recherche Scientifique : UMR7273
Avenue Escadrille Normandie-Niemen Service D42 13397 Marseille cedex 20 -  France
3 : Magnetic Resonance Center (CERM) and Department of Chemistry  -  Site web
Dipartimento di Chimica "Ugo Schiff" Polo Scientifico e Tecnologico, Università di Firenze Via della Lastruccia 13, I-50019 Sesto Fiorentino (Firenze) -  Italie
4 : Bruker BioSpin
76287 Rheinstetten -  Allemagne

We present the first DNP MAS experiments using 0.7 mm rotors, allowing us to reach spinning frequencies of 65 kHz at 100 K and 21.1 T (900 MHz), the highest magnetic field available for DNP today.(1)

 

We show that the mixed radical HyTEK2 allows us to reach DNP enhancements as high as 200 at a MAS rate of 65 kHz, and the carbon-centered radical BDPA in an ortho-terphenyl glass yields an enhancement of 106. For the two systems, we observe the 1H DNP enhancements increasing with increasing MAS frequency, this behaviour has been interpretated using a spin diffusion model.

 

Faster MAS spinning frequencies enable exceptional 1H resolution in MAS DNP and stimulate the use of 1H detected spectra. We obtained resolved DNP enhanced 1H detected 1H−13C and 1H−15N correlation spectra of microcrystalline histidine·HCl·H2O.

 

(1) P. Berruyer, S. Björgvinsdóttir, A. Bertarello, G. Stevanato, Y. Rao, G. Karthikeyan, G. Casano, O. Ouari, M. Lelli, C: Reiter, F. Engelke, L. Emsley, Dynamic Nuclear Polarization Enhancement of 200 at 21.15 T Enabled by 65 kHz Magic Angle Spinning. J. Phys. Chem. Lett. 11, 8386-8391 (2020).


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