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Related Concept Videos

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
NMR Spectroscopy: Chemical Shift Overview01:15

NMR Spectroscopy: Chemical Shift Overview

3.8K
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...
3.8K
¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

1.7K
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...
1.7K
NMR Spectrometers: Resolution and Error Correction01:14

NMR Spectrometers: Resolution and Error Correction

1.1K
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...
1.1K
NMR Spectrometers: Overview01:20

NMR Spectrometers: Overview

2.4K
NMR spectrometers consist of a strong magnet, a radiofrequency transmitter, and a detector attached to a computer console for recording spectra of samples containing NMR-active nuclei. In first-generation NMR instruments called continuous-wave spectrometers, the resonance frequencies of the nuclei are determined by frequency-sweep or field-sweep methods. The magnetic field strength is fixed and the rf signal is swept in the former, while the radiofrequency signal is fixed and the magnetic field...
2.4K
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

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Gradient-based solvent suppression methods on a benchtop spectrometer.

Boris Gouilleux1, Benoît Charrier1, Serge Akoka1

  • 1CEISAM CNRS, UMR6230, Université de Nantes, Nantes, France.

Magnetic Resonance in Chemistry : MRC
|July 30, 2016
PubMed
Summary
This summary is machine-generated.

Benchtop NMR spectroscopy offers new possibilities for monitoring chemical processes. This study shows gradient-based solvent suppression methods, like WET, improve spectral resolution for on-line analysis, overcoming limitations of traditional techniques.

Keywords:
WETbenchtop NMRon-line monitoringsolvent suppressionwater suppression

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Area of Science:

  • Analytical Chemistry
  • Spectroscopy
  • Chemical Engineering

Background:

  • Benchtop NMR spectroscopy is a promising tool for analyzing samples in challenging environments and for real-time process monitoring.
  • Low-field magnets in benchtop NMR reduce spectral resolution, causing peak overlaps, especially with non-deuterated solvents common in process monitoring.

Purpose of the Study:

  • To investigate efficient solvent suppression techniques for benchtop NMR spectroscopy compatible with flowing samples.
  • To evaluate the performance of gradient-based solvent suppression methods (WET, excitation sculpting) in a benchtop NMR setting for on-line monitoring.

Main Methods:

  • Implementation of WET and excitation sculpting solvent suppression techniques on a benchtop NMR spectrometer equipped with a gradient coil.
  • Comparison of analytical performance of these methods under static and on-flow conditions.
  • Evaluation of the WET-180-NOESY experiment for solvent suppression.

Main Results:

  • Gradient-based solvent suppression methods significantly improve spectral resolution and reduce peak overlap in benchtop NMR.
  • These methods are effective for on-line monitoring of chemical processes using non-deuterated solvents.
  • The WET-180-NOESY experiment demonstrated optimal performance for solvent suppression in both static and on-flow conditions.

Conclusions:

  • Gradient coil implementation is crucial for enhancing benchtop NMR capabilities, enabling advanced solvent suppression techniques.
  • Gradient-based methods offer superior performance over traditional approaches for on-line monitoring applications.
  • The WET-180-NOESY experiment is highly effective for solvent suppression in benchtop NMR, facilitating quantitative analysis.