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Related Concept Videos

Double Resonance Techniques: Overview01:12

Double Resonance Techniques: Overview

853
Double resonance techniques in Nuclear Magnetic Resonance (NMR) spectroscopy involve the simultaneous application of two different frequencies or radiofrequency pulses to manipulate and observe two distinct nuclear spins. One important application of double resonance is spin decoupling, which selectively suppresses coupling with one type of nucleus while observing the NMR signal from another nucleus, simplifying the spectrum and enhancing resolution.
Spin decoupling is usually achieved by...
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NMR Spectroscopy: Spin–Spin Coupling01:08

NMR Spectroscopy: Spin–Spin Coupling

3.8K
The spin state of an NMR-active nucleus can have a slight effect on its immediate electronic environment. This effect propagates through the intervening bonds and affects the electronic environments of NMR-active nuclei up to three bonds away; occasionally, even farther. This phenomenon is called spin–spin coupling or J-coupling. Coupling interactions are mutual and result in small changes in the absorption frequencies of both nuclei involved. While nuclei of the same element are involved...
3.8K
Spin–Spin Coupling: Two-Bond Coupling (Geminal Coupling)01:20

Spin–Spin Coupling: Two-Bond Coupling (Geminal Coupling)

1.9K
Two NMR-active nuclei bonded to a central atom can be involved in geminal or two-bond coupling. Geminal coupling is commonly seen between diastereotopic protons in chiral molecules and unsymmetrical alkenes, among others.
The central atom need not be NMR-active because its electrons are affected by the electron polarization of the spin-active atoms. However, spin information is transmitted less effectively than in one-bond coupling, and 2J values are usually weaker than 1J values. The energy of...
1.9K
¹H NMR of Conformationally Flexible Molecules: Variable-Temperature NMR01:15

¹H NMR of Conformationally Flexible Molecules: Variable-Temperature NMR

1.8K
The axial and equatorial protons in cyclohexane can be distinguished by performing a variable-temperature NMR experiment. In this process, except for one proton, the remaining eleven protons are replaced by deuterium. The deuterium substitution avoids the possible peak splitting caused by the spin-spin coupling between the adjacent protons. The remaining proton flips between the axial and equatorial positions.
1.8K
Atomic Nuclei: Nuclear Spin State Population Distribution01:14

Atomic Nuclei: Nuclear Spin State Population Distribution

2.6K
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.
2.6K
NMR Spectrometers: Resolution and Error Correction01:14

NMR Spectrometers: Resolution and Error Correction

1.2K
When magnetic nuclei in a sample achieve resonance and undergo relaxation, the signal detected in NMR is an approximately exponential free induction decay. Fourier transform of an exponential decay yields a Lorentzian peak in the frequency domain. Lorentzian peaks in an NMR spectrum are defined by their amplitude, full width at half maximum, and position, where the peak width is governed by the spin-spin relaxation time alone. In real experiments, however, the applied magnetic field is rendered...
1.2K

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Related Experiment Video

Updated: Apr 5, 2026

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

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Closed-cycle cold helium magic-angle spinning for sensitivity-enhanced multi-dimensional solid-state NMR.

Yoh Matsuki1, Shinji Nakamura2, Shigeo Fukui3

  • 1Institute for Protein Research, Osaka University, 3-2 Yamadaoka, Suita, Osaka 565-0871, Japan.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|August 25, 2015
PubMed
Summary
This summary is machine-generated.

A new helium-cooling magic-angle spinning (MAS) NMR probe system offers significant sensitivity gains at cryogenic temperatures. This stable, low-cost system enhances molecular structure and dynamics studies, especially for multi-dimensional and DNP-enhanced NMR below 100 K.

Keywords:
Closed-loop helium circulationCryogenic magic-angle spinningSensitivity enhancementSolid-state NMR

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Area of Science:

  • Nuclear Magnetic Resonance (NMR) Spectroscopy
  • Cryogenic Engineering
  • Materials Science

Background:

  • Magic-angle spinning (MAS) NMR is crucial for molecular structure and dynamics but limited by low sensitivity.
  • Existing methods often struggle with stability and helium consumption at cryogenic temperatures.

Purpose of the Study:

  • To develop a novel, highly stable, and cost-effective helium-cooling MAS NMR probe system.
  • To enhance NMR sensitivity at cryogenic temperatures for broader applications.

Main Methods:

  • Implementation of a closed-loop gas recirculation mechanism for helium cooling.
  • Development of a MAS NMR probe system capable of stable operation at 35-120 K.
  • Recording high-resolution 1D and 2D NMR data at 40 K and 16.4 T.

Main Results:

  • Achieved stable MAS speeds (4-12 kHz) at cryogenic temperatures for over a week with minimal helium consumption.
  • Demonstrated an order of magnitude sensitivity gain compared to room temperature measurements.
  • Successfully recorded high-resolution NMR spectra of a crystalline tri-peptide sample.

Conclusions:

  • The developed helium-cooling MAS NMR system provides a low-cost, long-term stable solution for cryogenic NMR.
  • This technology significantly promotes the application of sensitivity-enhanced multi-dimensional MAS NMR and DNP-enhanced NMR below 100 K.
  • Enables more accessible and powerful NMR studies of molecular structure and dynamics at low temperatures.