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Solid Effect DNP in a Rapid-melt setup.

P J M van Bentum1, M Sharma1, S G J van Meerten1

  • 1Institute for Molecules and Materials, Solid State NMR, Radboud University, Heyendaalseweg 135, 6525 AJ Nijmegen, The Netherlands.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|January 23, 2016
PubMed
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This study introduces a rapid melt method for Dynamic Nuclear Polarization (DNP) enhanced liquid-state NMR, achieving high proton enhancements. The technique allows detailed investigation of DNP mechanisms in solid phases.

Area of Science:

  • Nuclear Magnetic Resonance Spectroscopy
  • Hyperpolarization Techniques

Background:

  • Dynamic Nuclear Polarization (DNP) is crucial for enhancing Nuclear Magnetic Resonance (NMR) sensitivity.
  • A novel rapid melt approach combines solid-state hyperpolarization with in situ liquid-state NMR detection.

Purpose of the Study:

  • To investigate Solid Effect DNP mechanisms using a rapid melt DNP method.
  • To analyze the role of specific radicals (BDPA, TEMPOL) and proton concentration in Solid Effect DNP.

Main Methods:

  • Development of a rapid melting technique for solid hyperpolarized samples.
  • Utilizing 'in situ' liquid-state NMR detection with fast cycling for signal averaging.
  • Employing BDPA and TEMPOL radicals in nonpolar and aqueous frozen samples.
Keywords:
DNPDynamic Nuclear PolarizationLow temperatureNMRNuclear magnetic resonanceRapid meltSolid Effect

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Main Results:

  • Achieved proton enhancement factors up to 400 in nonpolar solvents with BDPA radicals.
  • Observed Solid Effect DNP with both narrow-line (BDPA) and wide-line (TEMPOL) radicals.
  • A simplified spin diffusion model semi-quantitatively described DNP enhancements with BDPA.

Conclusions:

  • The rapid melt DNP method is effective for studying solid-phase DNP mechanisms.
  • BDPA protons significantly contribute to Solid Effect DNP with BDPA radicals.
  • The simplified spin diffusion model provides a useful framework for analyzing Solid Effect DNP.