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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

1.6K
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.
1.6K
Atomic Nuclei: Nuclear Spin State Population Distribution01:14

Atomic Nuclei: Nuclear Spin State Population Distribution

2.3K
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.
2.3K
Atomic Spectroscopy: Effects of Temperature01:27

Atomic Spectroscopy: Effects of Temperature

804
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.
At thermal equilibrium, the relative populations of excited and ground state atoms can be estimated using the Maxwell–Boltzmann distribution. For example, an increase in temperature...
804
Chemical Shift: Internal References and Solvent Effects01:17

Chemical Shift: Internal References and Solvent Effects

1.2K
In an NMR sample, precise measurement of the absolute absorption frequencies of nuclei is difficult. A standard internal reference compound is added, and the frequency difference between the reference signal and sample signals is measured.
The internal reference compound generally used in NMR spectroscopy is tetramethylsilane (TMS). TMS is preferred because it is chemically inert, soluble in NMR solvents, and easily removable. Also, the highly shielded methyl protons in TMS yield an intense...
1.2K
¹H NMR of Conformationally Flexible Molecules: Temporal Resolution00:52

¹H NMR of Conformationally Flexible Molecules: Temporal Resolution

1.2K
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...
1.2K
¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

1.4K
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...
1.4K

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High-Sensitivity Nuclear Magnetic Resonance at Giga-Pascal Pressures: A New Tool for Probing Electronic and Chemical Properties of Condensed Matter under Extreme Conditions
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Solid state NMR at very high temperatures.

Holger Kirchhain1, Leo van Wüllen1

  • 1Institute of Physics, Augsburg University, Universitätsstr. 1, 86159 Augsburg, Germany.

Progress in Nuclear Magnetic Resonance Spectroscopy
|November 30, 2019
PubMed
Summary

High-temperature Nuclear Magnetic Resonance (NMR) spectroscopy, crucial for materials science, now extends beyond 550 K. Recent advancements enable routine high-resolution studies at extreme temperatures, expanding research possibilities.

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Area of Science:

  • Materials Science
  • Physical Chemistry
  • Spectroscopy

Background:

  • High-resolution Nuclear Magnetic Resonance (NMR) is typically limited to 550 K.
  • Temperatures above 550 K (high-temperature regime) require specialized equipment and are less accessible.
  • Advancements are needed to broaden the accessibility of high-temperature NMR.

Purpose of the Study:

  • To review developments in high-resolution NMR spectroscopy at temperatures exceeding 550 K.
  • To discuss various heating and temperature monitoring techniques for high-temperature NMR.
  • To present applications of high-temperature NMR in materials science.

Main Methods:

  • Review of resistive, laser-assisted, and inductive heating methods for high-temperature NMR.
  • Discussion of temperature monitoring techniques, including chemical shift and T1 thermometers.
  • Presentation of case studies involving oxidic glasses and melts.

Main Results:

  • Demonstration of various methods to achieve high-resolution NMR at temperatures > 550 K.
  • Comparison of advantages and disadvantages of different heating and temperature monitoring approaches.
  • Successful application of high-temperature NMR to study oxidic glasses and melts.

Conclusions:

  • Significant progress has been made in high-temperature NMR technology.
  • Multiple heating and monitoring techniques now facilitate high-resolution studies above 550 K.
  • High-temperature NMR provides valuable insights into materials like glasses and melts.