Issue 15, 2016

Dynamic nuclear polarization at 40 kHz magic angle spinning


DNP-enhanced solid-state NMR spectroscopy under magic angle spinning (MAS) is rapidly developing into a powerful analytical tool to investigate the structure of a wide range of solid materials, because it provides unsurpassed sensitivity gains. Most developments and applications of DNP MAS NMR were so far reported at moderate spinning frequencies (up to 14 kHz using 3.2 mm rotors). Here, using a 1.3 mm MAS DNP probe operating at 18.8 T and ∼100 K, we show that signal amplification factors can be increased by up to a factor two when using smaller volume rotors as compared to 3.2 mm rotors, and report enhancements of around 60 over a range of sample spinning rates from 10 to 40 kHz. Spinning at 40 kHz is also shown to increase 29Si coherence lifetimes by a factor three as compared to 10 kHz, substantially increasing sensitivity in CPMG type experiments. The contribution of quenching effects to the overall sensitivity gain at very fast MAS is evaluated, and applications are reported on a functionalised mesostructured organic–inorganic material.

Graphical abstract: Dynamic nuclear polarization at 40 kHz magic angle spinning

Supplementary files

Article information

Article type
05 Feb 2016
11 Mar 2016
First published
14 Mar 2016
This article is Open Access
Creative Commons BY license

Phys. Chem. Chem. Phys., 2016,18, 10616-10622

Author version available

Dynamic nuclear polarization at 40 kHz magic angle spinning

S. R. Chaudhari, P. Berruyer, D. Gajan, C. Reiter, F. Engelke, D. L. Silverio, C. Copéret, M. Lelli, A. Lesage and L. Emsley, Phys. Chem. Chem. Phys., 2016, 18, 10616 DOI: 10.1039/C6CP00839A

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