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research article

Dynamic Nuclear Polarization NMR Spectroscopy of Microcrystalline Solids

Rossini, Aaron J.  
•
Zagdoun, Alexandre
•
Hegner, Franziska
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2012
Journal of the American Chemical Society

Dynamic nuclear polarization (DNP) solid-state NMR has been applied to powdered microcrystalline solids to obtain sensitivity enhancements on the order of 100. Glucose, sulfathiazole, and paracetamol were impregnated with bis-nitroxide biradical (bis-cyclohexyl-TEMPO-bisketal, bCTbK) solutions of organic solvents. The organic solvents were carefully chosen to be nonsolvents for the compounds, so that DNP-enhanced solid-state NMR spectra of the unaltered solids could be acquired. A theoretical model is presented that illustrates that for externally doped organic solids characterized by long spin-lattice relaxation times (T-1(H-1) > 200 s), H-1-H-1 spin diffusion can relay enhanced polarization over micrometer length scales yielding substantial DNP enhancements (epsilon). epsilon on the order of 60 are obtained for microcrystalline glucose and sulfathiazole at 9.4 T and with temperatures of ca. 105 K. The large gain in sensitivity enables the rapid acquisition of C-13-C-13 correlation spectra at natural isotopic abundance. It is anticipated that this will be a general method for enhancing the sensitivity of solid-state NMR experiments of organic solids.

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Type
research article
DOI
10.1021/ja308135r
Web of Science ID

WOS:000309566400066

Author(s)
Rossini, Aaron J.  
Zagdoun, Alexandre
Hegner, Franziska
Schwarzwalder, Martin
Gajan, David
Coperet, Christophe
Lesage, Anne
Emsley, Lyndon  
Date Issued

2012

Publisher

AMER CHEMICAL SOC

Published in
Journal of the American Chemical Society
Volume

134

Issue

40

Start page

16899

End page

16908

Editorial or Peer reviewed

REVIEWED

Written at

OTHER

EPFL units
LRM  
Available on Infoscience
January 8, 2015
Use this identifier to reference this record
https://infoscience.epfl.ch/handle/20.500.14299/109984
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