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Atomic Nuclei: Nuclear Relaxation Processes01:23

Atomic Nuclei: Nuclear Relaxation Processes

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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.
1.3K
Atomic Nuclei: Nuclear Spin State Overview01:03

Atomic Nuclei: Nuclear Spin State Overview

2.1K
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...
2.1K
Atomic Nuclei: Nuclear Spin State Population Distribution01:14

Atomic Nuclei: Nuclear Spin State Population Distribution

2.4K
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.
2.4K
Atomic Nuclei: Nuclear Magnetic Moment00:59

Atomic Nuclei: Nuclear Magnetic Moment

3.4K
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...
3.4K
Nuclear Overhauser Enhancement (NOE)01:06

Nuclear Overhauser Enhancement (NOE)

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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...
1.5K
Atomic Nuclei: Magnetic Resonance01:05

Atomic Nuclei: Magnetic Resonance

1.3K
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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ダイナミックな核極化効率は,非常に速いマジック・アングル・スピニングによって増加します.

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
まとめ

ダイナミックな核極化 (DNP) は,マジック・アングル・スピニング (MAS) の速度を増やすことで,高磁場 (18.8 T) で高感度 (> 100) を達成しています. この画期的な発見は 材料分析のための固体NMRスペクトロシーを 強化しています

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科学分野:

  • 固体核磁共振 (NMR) スペクトロシー
  • 材料科学
  • 物理化学

背景:

  • ダイナミックな核極化 (DNP) は,固体NMRの感受性を大幅に高めます.
  • 高度なDNP強化 (>100) は通常,低磁場 (<9.4T) に限定される.
  • DNPの効率は,より高い磁場では大幅に低下します.

研究 の 目的:

  • 高磁場 (18.8 T) で高ダイナミックな核極化 (DNP) の強化を達成する.
  • DNPの効率と高いフィールドでのマジック・アングル・スピニング (MAS) 速度の関係を調査する.
  • 難解な材料を分析するための高フィールドDNPの有用性を実証する.

主な方法:

  • 固体オーバーハウザー効果のDNP実験は18.8Tで行われた.
  • 測定には,オターフェニルに溶けた1,3-ビスディフェニレン-2-フェニラリルを使用した.
  • マジック・アングル・スピニング (MAS) を40 kHzまでの周波数で実験した.
  • ポラライゼーション移転を説明するために,ソース-シンク拡散モデルが開発されました.

主要な成果:

  • 固体オーバーハウザー効果のDNP強化が100を超えて18.8Tで達成された.
  • DNP強化の急速な増加とMASの増加が観察されました.
  • メソポラスアルミニウムに成功しました
  • 表面強化されたDNPの良好な解像度を持つ27Alの対極化スペクトルを取得した.

結論:

  • 高磁場DNP (18.8Tでの100増強) は実現可能で効率的です.
  • マジック・アングル・スピニング・レートは 高いフィールドのDNPを最適化するための重要なパラメータです.
  • 開発されたソースシンク拡散モデルは,極化移転メカニズムを正確に説明します.
  • このアプローチは,材料の特徴化のための固体NMRを大幅に進歩させる.