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Related Concept Videos

¹H NMR of Conformationally Flexible Molecules: Temporal Resolution00:52

¹H NMR of Conformationally Flexible Molecules: Temporal Resolution

992
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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¹H NMR of Labile Protons: Temporal Resolution01:10

¹H NMR of Labile Protons: Temporal Resolution

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Protons bonded to heteroatoms such as nitrogen and oxygen exhibit a range of chemical shift values. This is due to the varying degree of hydrogen bonding between the proton and the heteroatom in other molecules. The extent of hydrogen bonding affects the electron density around the proton, thereby giving different chemical shift values for the protons in the proton NMR spectrum.
The –OH proton in alcohols typically appears in the range of δ 2 to 5 ppm but can vary depending on the...
1.4K
NMR Spectroscopy: Chemical Shift Overview01:15

NMR Spectroscopy: Chemical Shift Overview

3.6K
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...
3.6K
¹H NMR of Conformationally Flexible Molecules: Variable-Temperature NMR01:15

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

1.4K
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.
1.4K
¹³C NMR: ¹H–¹³C Decoupling01:04

¹³C NMR: ¹H–¹³C Decoupling

1.7K
The probability of having two carbon-13 atoms next to each other is negligible because of the low natural abundance of carbon-13. Consequently, peak splitting due to carbon-carbon spin-spin coupling is not observed in spectra. However, protons up to three sigma bonds away split the carbon signal according to the n+1 rule, resulting in complicated spectra.
A broadband decoupling technique is used to simplify these complex, sometimes overlapping, signals. Broadband decoupling relies on a...
1.7K
Chemical Shift: Internal References and Solvent Effects01:17

Chemical Shift: Internal References and Solvent Effects

1.5K
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...
1.5K

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Dynamic NMR Relaxometry as a Straightforward Measurement of Concentration Variations in Colloidal Gels.

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Dynamic Nuclear Magnetic Resonance (NMR) relaxometry precisely tracks colloidal suspension concentration and particle size changes over time. This non-destructive method monitors gel drying, revealing shrinkage, desaturation, and molecular film formation.

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Area of Science:

  • Colloid and Surface Science
  • Materials Science
  • Analytical Chemistry

Background:

  • Colloidal suspensions are crucial in various industries, but monitoring their dynamic changes, especially during drying, remains challenging.
  • Understanding particle size and concentration evolution is key to controlling material properties and performance.

Purpose of the Study:

  • To demonstrate the utility of dynamic Nuclear Magnetic Resonance (NMR) relaxometry for real-time monitoring of colloidal suspensions.
  • To investigate the drying process of colloidal gels and characterize different saturation regimes.

Main Methods:

  • Dynamic NMR relaxometry was employed to measure the transverse relaxation time (T2) of colloidal suspensions.
  • The fast-exchange assumption was extended to partially saturated media for data analysis.
  • Temporal evolution of NMR relaxation characteristics was analyzed during gel drying.

Main Results:

  • NMR transverse relaxation time was found to be largely independent of gel structure at the particle scale.
  • Three distinct drying regimes were identified: homogeneous shrinkage, desaturation, and molecular film formation.
  • Detailed analysis provided insights into fluid distribution within the solid structure during desaturation and molecular film regimes.

Conclusions:

  • Dynamic NMR relaxometry offers a simple, non-destructive, and time-resolved method for precise monitoring of solid volume fraction and saturation.
  • This technique is effective for tracking colloidal suspension dynamics up to complete drying, irrespective of the specific solid structure.