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Solid-State Dynamic Nuclear Polarization at 9.4 and 18.8 T from 100 K to Room Temperature.
Journal article

Solid-State Dynamic Nuclear Polarization at 9.4 and 18.8 T from 100 K to Room Temperature.

  • Lelli M Institut de Sciences Analytiques, Centre de RMN à Très Hauts Champs, Université de Lyon (CNRS/ENS Lyon/UCB Lyon 1) , 69100 Villeurbanne, France.
  • Chaudhari SR Institut de Sciences Analytiques, Centre de RMN à Très Hauts Champs, Université de Lyon (CNRS/ENS Lyon/UCB Lyon 1) , 69100 Villeurbanne, France.
  • Gajan D Institut de Sciences Analytiques, Centre de RMN à Très Hauts Champs, Université de Lyon (CNRS/ENS Lyon/UCB Lyon 1) , 69100 Villeurbanne, France.
  • Casano G Aix-Marseille Université, CNRS, ICR UMR 7273 , 13397 Marseille, France.
  • Rossini AJ Institut des Sciences et Ingénierie Chimiques, Ecole Polytechnique Fédérale de Lausanne (EPFL) , CH-1015 Lausanne, Switzerland.
  • Ouari O Aix-Marseille Université, CNRS, ICR UMR 7273 , 13397 Marseille, France.
  • Tordo P Aix-Marseille Université, CNRS, ICR UMR 7273 , 13397 Marseille, France.
  • Lesage A Institut de Sciences Analytiques, Centre de RMN à Très Hauts Champs, Université de Lyon (CNRS/ENS Lyon/UCB Lyon 1) , 69100 Villeurbanne, France.
  • Emsley L Institut des Sciences et Ingénierie Chimiques, Ecole Polytechnique Fédérale de Lausanne (EPFL) , CH-1015 Lausanne, Switzerland.
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  • 2015-11-12
Published in:
  • Journal of the American Chemical Society. - 2015
Colloid and Surface Chemistry
Biochemistry
General Chemistry
Catalysis
English Efficient dynamic nuclear polarization (DNP) in solids, which enables very high sensitivity NMR experiments, is currently limited to temperatures of around 100 K and below. Here we show how by choosing an adequate solvent, (1)H cross effect DNP enhancements of over 80 can be obtained at 240 K. To achieve this we use the biradical TEKPol dissolved in a glassy phase of ortho-terphenyl (OTP). We study the solvent DNP enhancement of both TEKPol and BDPA in OTP in the range from 100 to 300 K at 9.4 and 18.8 T. Surprisingly, we find that the DNP enhancement decreases only relatively slowly for temperatures below the glass transition of OTP (Tg = 243 K), and (1)H enhancements around 15-20 at ambient temperature can be observed. We use this to monitor molecular dynamic transitions in the pharmaceutically relevant solids Ambroxol and Ibuprofen.
Language
  • English
Open access status
hybrid
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Persistent URL
https://sonar.ch/global/documents/256133
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