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Related Concept Videos

NMR Spectroscopy Of Amines01:19

NMR Spectroscopy Of Amines

11.2K
In proton NMR spectroscopy, primary amines and secondary amines showcase their N–H protons as a broad signal in the chemical shift range between δ 0.5 and 5 ppm. The exact position in this range depends on several factors, including sample concentration, hydrogen bonding, and the type of solvent used. Since amine protons undergo fast proton exchange in solution, the protons are labile and therefore do not participate in any splitting with adjacent protons. Thus, the observed peak is...
11.2K
NMR Spectroscopy of Aromatic Compounds01:14

NMR Spectroscopy of Aromatic Compounds

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Aromatic compounds can be identified or analyzed using proton NMR and carbon‐13 NMR. Typically, aromatic hydrogens or hydrogens directly bonded to the aromatic rings are strongly deshielded by the aromatic ring current. Therefore, they absorb in the range of 6.5–8.0 ppm in proton NMR spectra. For instance, aromatic hydrogens directly bonded to the benzene ring absorb at 7.3 ppm. However, aromatic hydrogens of larger rings absorb farther upfield or downfield than the ideal range.
6.4K
NMR Spectroscopy of Benzene Derivatives01:34

NMR Spectroscopy of Benzene Derivatives

11.3K
Simple unsubstituted benzene has six aromatic protons, all chemically equivalent. Therefore, benzene exhibits only a singlet peak at δ 7.3 ppm in the 1H NMR spectrum. The observed shift is far downfield because the aromatic ring current strongly deshields the protons. Any substitution on the benzene ring makes the aromatic protons nonequivalent, and the protons split each other. The peak is, therefore, no longer a singlet and the splitting pattern and their associated coupling...
11.3K
NMR Spectroscopy: Chemical Shift Overview01:15

NMR Spectroscopy: Chemical Shift Overview

3.3K
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...
3.3K
NMR Spectroscopy: Spin–Spin Coupling01:08

NMR Spectroscopy: Spin–Spin Coupling

3.3K
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...
3.3K
NMR and Mass Spectroscopy of Carboxylic Acids01:30

NMR and Mass Spectroscopy of Carboxylic Acids

5.3K
In ¹H NMR spectroscopy, acidic protons (–COOH) of carboxylic acids are highly deshielded and absorb far downfield, at around 9–12 ppm. The chemical shift value depends on the concentration and solvent used.
While α protons of carboxylic acids absorb at 2–2.5 ppm, β protons absorb further upfield.
Carboxylic acids are easily identified by dissolving them in deuterium oxide, which results in a rapid exchange of the acidic protons with deuterium. This leads to the...
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3D printed microchannels for sub-nL NMR spectroscopy.

E Montinaro1, M Grisi1, M C Letizia1

  • 1Ecole Polytechnique Fédérale de Lausanne (EPFL), Laboratory for Microsystems, Lausanne, Switzerland.

Plos One
|May 10, 2018
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Summary

Researchers developed 3D printed microfluidics for sensitive nuclear magnetic resonance (NMR) experiments on tiny biological samples. This breakthrough enables detailed analysis of sub-nanoliter volumes, advancing studies on microscopic organisms and cells.

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Area of Science:

  • Biophysics
  • Analytical Chemistry
  • Microfluidics

Background:

  • Nuclear magnetic resonance (NMR) experiments on sub-nanoliter (sub-nL) volumes face sensitivity and sample handling challenges.
  • Existing methods struggle to position and maintain small samples near sensitive NMR detector volumes.

Purpose of the Study:

  • To demonstrate nuclear magnetic resonance (NMR) experiments on liquid and biological entities in volumes as low as 100 pL.
  • To overcome sensitivity and positioning limitations in sub-nL NMR analysis.

Main Methods:

  • Fabrication of high-resolution 3D printed microfluidic structures using two-photon polymerization (resolution < 1 μm³).
  • Integration of microfluidics with a single-chip integrated NMR probe to confine samples in the most sensitive region.
  • NMR experiments on tardigrade ova and Caenorhabditis elegans nematode sections in sub-nL volumes.

Main Results:

  • Achieved a sensitivity of 2.5x10^13 spins/√Hz at 7 T, detecting 6 pmol of 1H nuclei in 100 pL volumes within 3 hours.
  • Demonstrated spectral resolutions of 0.01 ppm for liquid samples and 0.1 ppm for biological entities.
  • Successfully performed NMR on intact sub-nL biological samples, including tardigrade ova and nematode sections.

Conclusions:

  • High-resolution 3D printed microfluidics enable sensitive NMR analysis of ultra-small biological volumes.
  • This approach facilitates NMR studies at the single-unit level for microscopic organisms and cells.
  • Potential for NMR analysis of mammalian eggs and other critical sub-nL biological entities.