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Related Concept Videos

NMR Spectroscopy: Spin–Spin Coupling01:08

NMR Spectroscopy: Spin–Spin Coupling

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 in...
¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

Spin systems where the difference in chemical shifts of the coupled nuclei is greater than ten times J are called first-order spin systems. These nuclei are weakly coupled, and their chemical shifts and coupling constant can generally be estimated from the well-separated signals in the spectrum.
As Δν decreases and the signals move closer, the doublets appear increasingly distorted. The intensities of the inner lines increase at the cost of those of the outer lines as the signals are slanted or...
Spin–Spin Coupling Constant: Overview01:08

Spin–Spin Coupling Constant: Overview

In bromoethane, the three methyl protons are coupled to the two methylene protons that are three bonds away. In accordance with the n+1 rule, the signal from the methyl protons is split into three peaks with 1:2:1 relative intensities. The methylene protons appear as a quartet, with the relative intensities of 1:3:3:1.
Qualitatively, any spin plus-half nucleus polarizes the spins of its electrons to the minus-half state. Consequently, the paired electron in the hydrogen–carbon bond must have a...
NMR Spectrometers: Resolution and Error Correction01:14

NMR Spectrometers: Resolution and Error Correction

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...
Spin–Spin Coupling: Two-Bond Coupling (Geminal Coupling)01:20

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

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

Atomic Nuclei: Nuclear Spin State Population Distribution

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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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

Biomolecular solid state NMR with magic-angle spinning at 25K.

Kent R Thurber1, Robert Tycko

  • 1Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases, National Institutes of Health, Building 5, Room 112, Bethesda, MD 20892-0520, USA.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|October 17, 2008
PubMed
Summary

A novel helium-cooled magic-angle spinning (MAS) probe enables low-temperature nuclear magnetic resonance (NMR) experiments on biomolecular solids. This technology enhances signal-to-noise ratios for advanced materials analysis.

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Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
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Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy

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Last Updated: Jun 28, 2026

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

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
14:55

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy

Published on: September 17, 2017

Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) Spectroscopy
  • Low-Temperature Physics
  • Biomolecular Solid-State Analysis

Background:

  • Magic-angle spinning (MAS) is crucial for high-resolution solid-state NMR.
  • Achieving stable low temperatures (down to 25K) is essential for studying dynamic processes in biomolecules.
  • Existing MAS probes often have limitations in cooling capacity and stability.

Purpose of the Study:

  • To design and construct a novel helium-cooled MAS probe for low-temperature NMR.
  • To evaluate the performance and stability of the probe for extended operation.
  • To demonstrate the utility of the probe for biomolecular solid-state NMR studies.

Main Methods:

  • Construction of a MAS probe utilizing liquid helium for sample cooling (to 25K) and nitrogen for bearing/drive gases.
  • Achieving rotor speeds of 6.7 kHz with high stability (+/-5 Hz) for extended periods.
  • Application of high proton decoupling fields (up to 130 kHz).

Main Results:

  • The helium-cooled MAS probe demonstrated stable operation at 25K with a 4-mm rotor spinning at 6.7 kHz.
  • Signal-to-noise ratios were observed to be proportional to 1/T, as expected for low-temperature NMR.
  • Successful acquisition of low-temperature 13C NMR data for amyloid fibrils (Abeta(14-23)) and a protein (HP35).

Conclusions:

  • The developed helium-cooled MAS probe is effective for low-temperature NMR experiments on biomolecular solids.
  • The probe facilitates enhanced signal-to-noise ratios, crucial for sensitive analyses.
  • Further investigations into temperature calibration, relaxation dynamics, and linewidths at low temperatures are warranted.