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Related Concept Videos

Atomic Nuclei: Nuclear Relaxation Processes01:23

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In the absence of an external magnetic field, nuclear spin states are degenerate and randomly oriented. When a magnetic field is applied, the spins begin to precess and orient themselves along (lower energy) or against (higher energy) the direction of the field. At equilibrium, a slight excess population of spins exists in the lower energy state. Because the direction of the magnetic field is fixed as the z-axis,  the precessing magnetic moments are randomly oriented around the z-axis.
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Atomic Nuclei: Nuclear Spin State Overview01:03

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NMR-active nuclei have energy levels called 'spin states' that are associated with the orientations of their nuclear magnetic moments. In the absence of a magnetic field, the nuclear magnetic moments are randomly oriented, and the spin states are degenerate. When an external magnetic field is applied, the spin states have only 2 + 1 orientations available to them. A proton with = ½ has two available orientations. Similarly, for a quadrupolar nucleus with a nuclear spin value of one, the...
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Atomic Nuclei: Nuclear Spin State Population Distribution01:14

Atomic Nuclei: Nuclear Spin State Population Distribution

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Near absolute zero temperatures, in the presence of a magnetic field, the majority of nuclei prefer the lower energy spin-up state to the higher energy spin-down state. As temperatures increase, the energy from thermal collisions distributes the spins more equally between the two states. The Boltzmann distribution equation gives the ratio of the number of spins predicted in the spin −½ (N−) and spin +½ (N+) states.
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Atomic Nuclei: Nuclear Magnetic Moment00:59

Atomic Nuclei: Nuclear Magnetic Moment

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All atomic nuclei are positively charged. When they have a nonzero spin, they behave like rotating charges. As a consequence of their charge and spin, these nuclei generate a magnetic field (B). This, in turn, gives rise to a magnetic moment (μ), which is randomly oriented in the absence of an external magnetic field. When an external magnetic field (B0) is applied, the magnetic moment vectors can align with the field or against it in 2 + 1 orientations. A hydrogen nucleus, which is just a...
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Nuclear Overhauser Enhancement (NOE)01:06

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Irradiation of a spin-active nucleus causes an increase or decrease in the signal intensity of neighboring nuclei that are not necessarily chemically bonded or involved in J-coupling. This phenomenon, called the nuclear Overhauser enhancement (NOE), results from through-space interactions between the nuclear spins. The NOE effect decreases with increasing internuclear distance and is generally not observed beyond 4 angstroms. In NOE, dipole-dipole interactions between neighboring spin-active...
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Atomic Nuclei: Magnetic Resonance01:05

Atomic Nuclei: Magnetic Resonance

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The number of nuclear spins aligned in the lower energy state is slightly greater than those in the higher energy state. In the presence of an external magnetic field, as the spins precess at the Larmor frequency, the excess population results in a net magnetization oriented along the z axis. When a pulse or a short burst of radio waves at the Larmor frequency is applied along the x axis, the coupling of frequencies causes resonance and flips the nuclear spins of the excess population from the...
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Cryogenic Sample Loading into a Magic Angle Spinning Nuclear Magnetic Resonance Spectrometer that Preserves Cellular Viability
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Dynamic Nuclear Polarization Efficiency Increased by Very Fast Magic Angle Spinning.

Sachin R Chaudhari1, Dorothea Wisser1, Arthur C Pinon2

  • 1Institut de Sciences Analytiques, Centre de RMN à Très Hauts Champs, Université de Lyon (CNRS/ENS Lyon/UCB Lyon 1), 69100 Villeurbanne, France.

Journal of the American Chemical Society
|July 11, 2017
PubMed
Summary
This summary is machine-generated.

Dynamic nuclear polarization (DNP) now achieves high sensitivity (>100) at high magnetic fields (18.8 T) by increasing magic angle spinning (MAS) rates. This breakthrough enhances solid-state NMR spectroscopy for materials analysis.

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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) Spectroscopy
  • Materials Science
  • Physical Chemistry

Background:

  • Dynamic nuclear polarization (DNP) significantly enhances solid-state NMR sensitivity.
  • High DNP enhancements (>100) are typically limited to lower magnetic fields (<9.4 T).
  • DNP efficiency decreases substantially at higher magnetic fields.

Purpose of the Study:

  • To achieve high dynamic nuclear polarization (DNP) enhancements at high magnetic fields (18.8 T).
  • To investigate the relationship between DNP efficiency and magic angle spinning (MAS) rates at high fields.
  • To demonstrate the utility of high-field DNP for analyzing challenging materials.

Main Methods:

  • Solid-state Overhauser effect DNP experiments were conducted at 18.8 T.
  • Measurements utilized 1,3-bisdiphenylene-2-phenylallyl dissolved in o-terphenyl.
  • Experiments involved magic angle spinning (MAS) at rates up to 40 kHz.
  • A source-sink diffusion model was developed to explain polarization transfer.

Main Results:

  • Achieved solid-state Overhauser effect DNP enhancements exceeding 100 at 18.8 T.
  • Observed a rapid increase in DNP enhancement with increasing MAS rates.
  • Successfully applied the method to mesoporous alumina.
  • Acquired well-resolved DNP surface-enhanced 27Al cross-polarization spectra.

Conclusions:

  • High magnetic field DNP (>100 enhancement at 18.8 T) is feasible and efficient.
  • Magic angle spinning rate is a critical parameter for optimizing high-field DNP.
  • The developed source-sink diffusion model accurately explains polarization transfer mechanisms.
  • This approach significantly advances solid-state NMR for materials characterization.