Dynamic nuclear polarization (DNP) has recently emerged as a tool to enhance the sensitivity of solid-state NMR experiments. However, so far high enhancements (>100) are limited to relatively low magnetic fields, and DNP at fields higher than 9.4 T significantly drops in efficiency. Here we report solid-state Overhauser effect DNP enhancements of over 100 at 18.8 T. This is achieved through the unexpected discovery that enhancements increase rapidly with increasing magic angle spinning (MAS) rates. The measurements are made using 1,3-bisdiphenylene-2-phenylallyl dissolved in o-terphenyl at 40 kHz MAS. We introduce a source−sink diffusion model for polarization transfer which is capable of explaining the experimental observations. The advantage of this approach is demonstrated on mesoporous alumina with the acquisition of well-resolved DNP surface- enhanced 27Al cross-polarization spectra.
Dynamic Nuclear Polarization Efficiency Increased by Very Fast Magic Angle Spinning / Chaudhari, Sachin R.; Wisser, Dorothea; Pinon, Arthur C.; Berruyer, Pierrick; Gajan, David; Tordo, Paul; Ouari, Olivier; Reiter, Christian; Engelke, Frank; Copéret, Christophe; Lelli, Moreno*; Lesage, Anne; Emsley, Lyndon. - In: JOURNAL OF THE AMERICAN CHEMICAL SOCIETY. - ISSN 0002-7863. - STAMPA. - 139:(2017), pp. 10609-10612. [10.1021/jacs.7b05194]
Dynamic Nuclear Polarization Efficiency Increased by Very Fast Magic Angle Spinning
Lelli, Moreno
Writing – Review & Editing
;
2017
Abstract
Dynamic nuclear polarization (DNP) has recently emerged as a tool to enhance the sensitivity of solid-state NMR experiments. However, so far high enhancements (>100) are limited to relatively low magnetic fields, and DNP at fields higher than 9.4 T significantly drops in efficiency. Here we report solid-state Overhauser effect DNP enhancements of over 100 at 18.8 T. This is achieved through the unexpected discovery that enhancements increase rapidly with increasing magic angle spinning (MAS) rates. The measurements are made using 1,3-bisdiphenylene-2-phenylallyl dissolved in o-terphenyl at 40 kHz MAS. We introduce a source−sink diffusion model for polarization transfer which is capable of explaining the experimental observations. The advantage of this approach is demonstrated on mesoporous alumina with the acquisition of well-resolved DNP surface- enhanced 27Al cross-polarization spectra.File | Dimensione | Formato | |
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