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Characterization of strongly hyperfine-split protons by DNP.

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Dynamic nuclear polarization (DNP) experiments enhance NMR signals. This study reveals how electron spins polarize nearby nuclear spins and quantifies the spin diffusion barrier around radicals.

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Area of Science:

  • Magnetic Resonance
  • Physical Chemistry
  • Spectroscopy

Background:

  • Dynamic nuclear polarization (DNP) enhances nuclear magnetic resonance (NMR) sensitivity by transferring electron polarization to nuclear spins.
  • The precise mechanisms of polarization transfer and the extent of nuclear spin involvement in bulk magnetization via spin diffusion remain incompletely understood.

Purpose of the Study:

  • To investigate the mechanisms of polarization transfer from electron spins to nuclear spins in DNP.
  • To determine the spin-diffusion barrier around electron radicals and understand its impact on bulk magnetization.
  • To elucidate the role of electron-electron spin diffusion in DNP experiments.

Main Methods:

  • Utilized reverse DNP and band-selective inversion pulses on nuclear spins.
  • Acquired electron-detected NMR spectra of proton spins in Oxo63 trityl samples with varying solvents and radical concentrations.
  • Employed hole-burning spectroscopy to probe spin diffusion processes.

Main Results:

  • Characterized the electron-detected NMR spectrum of protons directly involved in DNP.
  • Quantified the spin-diffusion barrier, finding proton spin diffusion is quenched beyond ~250 kHz hyperfine coupling, corresponding to a radius of 5.4–6.8 Å.
  • Observed and explained electron-electron spin diffusion imprinted on the proton NMR spectrum using a three-spin model.

Conclusions:

  • Provided detailed insights into the polarization transfer pathways in DNP.
  • Established the existence and dimensions of a spin-diffusion barrier around trityl radicals.
  • Demonstrated the influence of electron-electron spin diffusion on DNP spectral features.