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Related Concept Videos

¹H NMR of Conformationally Flexible Molecules: Variable-Temperature NMR01:15

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

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.
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.
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...
Atomic Spectroscopy: Effects of Temperature01:27

Atomic Spectroscopy: Effects of Temperature

Atomization, converting samples into gas-phase atoms and ions, is essential for atomic spectroscopy. The flame temperature required for atomization affects the efficiency of the atomic spectroscopic methods by increasing the atomization efficiency and the relative population of the excited and ground states.
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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...
¹H NMR of Conformationally Flexible Molecules: Temporal Resolution00:52

¹H NMR of Conformationally Flexible Molecules: Temporal Resolution

At room temperature, the chair conformer of cyclohexane undergoes rapid ring flipping between two equivalent chair conformers at a rate of approximately 105 times per second. These two chair conformers are in equilibrium. The rapid ring flipping results in the interconversion of the axial proton to an equatorial proton and an equatorial to the axial proton. Such interconversions are too rapid and cannot be detected on the NMR timescale. Hence, the NMR spectrometer cannot distinguish between the...

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Related Experiment Video

Updated: Jun 15, 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

Thermometers for low temperature Magic Angle Spinning NMR.

T F Kemp1, G Balakrishnan, K J Pike

  • 1Department of Physics, University of Warwick, Coventry CV4 7AL, UK.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|March 16, 2010
PubMed
Summary

Temperature measurement in Magic Angle Spinning NMR probes can be accurately achieved using the (119)Sn resonance shift of Sm2Sn2O7, offering precision better than 0.5K. This method allows for rapid measurements and detection of temperature gradients.

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Area of Science:

  • Solid-state NMR Spectroscopy
  • Materials Science
  • Physical Chemistry

Background:

  • Accurate temperature measurement is crucial for NMR experiments.
  • Existing methods may have limitations in precision or speed.
  • Developing reliable thermometers for NMR probes is essential for research.

Purpose of the Study:

  • To evaluate the (119)Sn resonance shift of Sm2Sn2O7 as a thermometer for Magic Angle Spinning NMR probes.
  • To determine the temperature range and precision of this thermometer.
  • To investigate the temperature dependence of the (207)Pb chemical shift in Pb(NO3)2.

Main Methods:

  • Utilizing the chemical shift of the (119)Sn nucleus in Sm2Sn2O7 as a temperature-dependent property.
  • Measuring the (119)Sn resonance shift across a temperature range of 85-300K.
  • Analyzing the (207)Pb chemical shift in Pb(NO3)2 down to approximately 85K.

Main Results:

  • The (119)Sn shift of Sm2Sn2O7 provides a precise thermometer (better than 0.5K) across 85-300K, described by delta=223 - 9.54x10^4/T ppm.
  • High sensitivity (4.2ppm/K at 150K) allows detection of small temperature gradients.
  • Short spin-lattice relaxation times enable measurements in ~1s, facilitating tracking of rapid temperature changes.
  • The (207)Pb shift in Pb(NO3)2 shows near-linear behavior above ~130K (0.725+/-0.002ppm/K from 293-153K) but deviates at lower temperatures.

Conclusions:

  • The (119)Sn resonance of Sm2Sn2O7 is a highly effective thermometer for Magic Angle Spinning NMR probes.
  • This NMR thermometry method offers high precision, sensitivity, and speed.
  • The temperature dependence of (207)Pb chemical shift is non-linear below ~130K, requiring careful consideration for low-temperature applications.