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Related Concept Videos

Atomic Nuclei: Nuclear Magnetic Moment00:59

Atomic Nuclei: Nuclear Magnetic Moment

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...
Atomic Nuclei: Nuclear Spin State Overview01:03

Atomic Nuclei: Nuclear Spin State Overview

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...
Atomic Nuclei: Nuclear Spin01:08

Atomic Nuclei: Nuclear Spin

All atomic particles possess an intrinsic angular momentum, or 'spin'. Electrons, protons, and neutrons each have a spin value of ½, although protons and neutrons in nuclei may have higher half-integer spins owing to energetic factors.
Atomic nuclei have a net nuclear spin, , which can have an integer or half-integer value. In atomic nuclei, the spins of protons are paired against each other but not with neutrons, and vice versa. Consequently, an even number of protons does not contribute to...
Atomic Nuclei: Nuclear Relaxation Processes01:23

Atomic Nuclei: Nuclear Relaxation Processes

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. This...
Nuclear Overhauser Enhancement (NOE)01:06

Nuclear Overhauser Enhancement (NOE)

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...
Atomic Nuclei: Magnetic Resonance01:05

Atomic Nuclei: Magnetic Resonance

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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High-Temperature and High-Pressure In situ Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy
08:55

High-Temperature and High-Pressure In situ Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy

Published on: October 9, 2020

Solid effect in magic angle spinning dynamic nuclear polarization.

Björn Corzilius1, Albert A Smith, Robert G Griffin

  • 1Francis Bitter Magnet Laboratory and Department of Chemistry, Massachusetts Institute of Technology, 77 Massachusetts Avenue, Cambridge, Massachusetts 02139, USA.

The Journal of Chemical Physics
|August 17, 2012
PubMed
Summary
This summary is machine-generated.

Researchers achieved a significant enhancement in dynamic nuclear polarization (DNP) using the solid effect (SE) mechanism. This breakthrough overcomes the field dependence limitations of SE, enabling higher DNP enhancements at high magnetic fields.

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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy
  • Dynamic Nuclear Polarization (DNP)
  • Quantum mechanics

Background:

  • The solid effect (SE) is a long-standing mechanism for dynamic nuclear polarization (DNP).
  • SE's application in high magnetic field DNP is limited by its unfavorable ω(0)(-2) field dependence, stemming from the mixing of nuclear spin states.
  • This field dependence arises from the partial allowance of otherwise forbidden zero and double quantum SE transitions.

Purpose of the Study:

  • To improve instrumentation for enhanced DNP experiments utilizing the solid effect.
  • To investigate the factors influencing enhancement and buildup rates in SE-based DNP.
  • To explore the potential of SE for DNP at magnetic fields exceeding 5 T.

Main Methods:

  • Magic angle spinning (MAS) experiments at 5 T and 80 K using the trityl radical (OX063).
  • Optimization of microwave field strength and coupling efficiency from the gyrotron to the sample chamber.
  • Development of a theoretical model to correlate microwave power with polarization buildup rate and steady-state enhancement.
  • Measurement of buildup times and enhancements as a function of proton (1H) concentration for trityl and Gadolinium-1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetate (Gd-DOTA).

Main Results:

  • Achieved a DNP enhancement (ε) of 91 with trityl (OX063) at 5 T and 80 K, a 6-7 fold increase over previous reports.
  • Attributed the enhanced performance to increased internal microwave field strengths via improved gyrotron coupling.
  • The theoretical model successfully explained the dependence of buildup rate and enhancement on microwave power.
  • Identified the initial polarization step as rate-limiting for trityl, while spin diffusion of 1H nuclei limits Gd-DOTA.

Conclusions:

  • The improved instrumentation significantly enhances DNP performance via the solid effect, overcoming previous limitations.
  • The solid effect shows promise for DNP applications at fields above 5 T, provided the field dependence can be managed.
  • Understanding the rate-limiting steps (initial polarization vs. spin diffusion) is crucial for optimizing DNP experiments with different polarizing agents.