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Related Concept Videos

Chemical Shift: Internal References and Solvent Effects01:17

Chemical Shift: Internal References and Solvent Effects

1.6K
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...
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Aqueous Solutions and Heats of Hydration02:42

Aqueous Solutions and Heats of Hydration

19.0K
Water and other polar molecules are attracted to ions. The electrostatic attraction between an ion and a molecule with a dipole is called an ion-dipole attraction. These attractions play an important role in the dissolution of ionic compounds in water.
When ionic compounds dissolve in water, the ions in the solid separate and disperse uniformly throughout the solution because water molecules surround and solvate the ions, reducing the strong electrostatic forces between them. This process...
19.0K
NMR Spectroscopy: Chemical Shift Overview01:15

NMR Spectroscopy: Chemical Shift Overview

4.1K
The position of the absorption signal of a sample is reported relative to the position of the signal of tetramethylsilane (TMS), which is added as an internal reference while recording spectra. The difference between the absorption frequencies of the sample and TMS (in Hz) is divided by the spectrometer operating frequency (in MHz) to obtain a dimensionless quantity called the chemical shift. It is reported on the δ (delta) scale and expressed in parts per million.
For instance, the proton...
4.1K
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
2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)01:19

2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)

1.6K
Heteronuclear single-quantum correlation spectroscopy (HSQC) is a 2D NMR technique that reveals one-bond correlations between hydrogen and a heteronucleus. The HSQC experiment is similar to the heteronuclear correlation experiment (HETCOR) but is more sensitive. In the HSQC spectrum, the proton chemical shift is plotted on the horizontal F2 axis, while the 13C chemical shift is plotted on the vertical F1 axis. The corresponding proton and 13C spectra are also shown. The HSQC contour plot does...
1.6K
¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

1.8K
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...
1.8K

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Preparation of Fungal and Plant Materials for Structural Elucidation Using Dynamic Nuclear Polarization Solid-State NMR
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Hydrate Shell Growth Measured Using NMR.

Agnes Haber1, Masoumeh Akhfash1, Charles K Loh1

  • 1School of Mechanical and Chemical Engineering, The University of Western Australia, 35 Stirling Highway, Crawley, Western Australia 6009, Australia.

Langmuir : the ACS Journal of Surfaces and Colloids
|June 24, 2015
PubMed
Summary
This summary is machine-generated.

Nuclear magnetic resonance (NMR) techniques monitored clathrate hydrate shell growth in water droplets. This revealed that hydrate shells initially grow porous and later become spherical and less porous over time.

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Area of Science:

  • Physical Chemistry
  • Materials Science
  • Chemical Engineering

Background:

  • Clathrate hydrates form complex shell structures around dispersed water droplets.
  • Understanding hydrate shell morphology is crucial for applications in gas storage and separation.

Purpose of the Study:

  • To monitor clathrate hydrate shell growth kinetics and morphology.
  • To investigate the evolution of shell structure using non-invasive techniques.

Main Methods:

  • Benchtop nuclear magnetic resonance (NMR) pulsed field gradient (PFG) and relaxation measurements were employed.
  • PFG NMR determined droplet size distribution (DSD) of unconverted water.
  • NMR relaxation monitored hydrate shell growth kinetics.

Main Results:

  • NMR techniques successfully monitored hydrate shell growth within opaque shells.
  • Initial hydrate growth is heat-transfer-limited, resulting in porous shells.
  • Later growth is mass-transfer-limited, leading to thicker, spherical, and less porous shells.

Conclusions:

  • The spherical shell model is valid for hydrate droplet systems after 24 hours of growth.
  • Hydrate shell morphology transitions from porous to spherical as growth progresses.
  • NMR is a powerful tool for studying dynamic processes in hydrate systems.