4.3 Article

Is solid-state NMR enhanced by dynamic nuclear polarization?

期刊

SOLID STATE NUCLEAR MAGNETIC RESONANCE
卷 66-67, 期 -, 页码 6-20

出版社

ACADEMIC PRESS INC ELSEVIER SCIENCE
DOI: 10.1016/j.ssnmr.2015.01.003

关键词

Dynamic nuclear polarization; Magic angle spinning; Solid-state NMR

资金

  1. French National Research Agency (through the Labex ARCANE [ANR-11-LABX-0003-01]
  2. programme chaire d'excellence [ANR08-CEXC-003-01]
  3. programme blanc [ANR-12-BS08-0016-01]
  4. RTB
  5. CEA-EUROTALENTS [PCO-FUND-GA-2008- 228664]

向作者/读者索取更多资源

The recent trend of high-held (similar to 5-20 T), low-temperature (similar to 100 K) ssNMR combined with dynamic nuclear polarization (DNP) under magic angle spinning (MAS) conditions is analyzed. A brief overview of the current theory of hyperpolarization for so-called MAS-DNP experiments is given, along with various reasons why the DNP-enhancement, the ratio of the NMR signal intensities obtained in the presence and absence of microwave irradiation suitable for hyperpolarization, should not be used alone to gauge the value of performing MAS-DNP experiments relative to conventional ssNMR. This is demonstrated through a dissection of the current conditions required for MAS-DNP with particular attention to resulting absolute sensitivities and spectral resolution. Consequently, sample preparation methods specifically avoiding the surplus of glass-forming solvents so as to improve the absolute sensitivity and resolution are discussed, as are samples that are intrinsically pertinent for MAS-DNP studies (high surface area, amorphous, and porous). Owing to their pertinence, examples of recent applications on these types of samples where chemically-relevant information has been obtained that would have been impossible without the sensitivity increases bestowed by MAS-DNP are also detailed. Additionally, a promising further implementation for MAS-DNP is exampled, whereby the sensitivity improvements shown for (correlation) spectroscopy of nuclei at low natural isotopic abundance, facilitate internuclear distance measurements, especially for long distances (absence of dipolar truncation). Finally, we give some speculative perspectives for MAS-DNP. (C) 2015 Elsevier Inc. All rights reserved.

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