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A pulse is a short burst of radio waves distributed over a range of frequencies that simultaneously excites all the nuclei in the sample. Upon passing a radio frequency pulse along the x-axis, the nuclei absorb energy corresponding to their Larmor frequencies and achieve resonance. This shifts the net magnetization vector from the z-axis toward the transverse plane. This angle of rotation of the magnetization vector, or the flip angle, is proportional to the duration and intensity of the pulse.
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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...
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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...
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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.
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When proton-coupled carbon-13 spectra are simplified by a broadband proton decoupling technique, structural information about the coupled protons is lost. Distortionless enhancement by polarization transfer (DEPT) is a technique that provides information on the number of hydrogens attached to each carbon in a molecule. While the DEPT experiment utilizes complex pulse sequences, the pulse delay and flip angle are specifically manipulated. The resulting signals have different phases depending on...
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Double resonance techniques in Nuclear Magnetic Resonance (NMR) spectroscopy involve the simultaneous application of two different frequencies or radiofrequency pulses to manipulate and observe two distinct nuclear spins. One important application of double resonance is spin decoupling, which selectively suppresses coupling with one type of nucleus while observing the NMR signal from another nucleus, simplifying the spectrum and enhancing resolution.
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Gradient-based pulse sequences for benchtop NMR spectroscopy.

Boris Gouilleux1, Jonathan Farjon2, Patrick Giraudeau2

  • 1Université Paris-Saclay, ICMMO, UMR CNRS 8182, RMN en Milieu Orienté, France.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|October 10, 2020
PubMed
Summary
This summary is machine-generated.

Benchtop NMR spectroscopy, enhanced by magnetic field gradients, now overcomes peak overlaps in complex mixtures. This advance expands the utility of accessible, low-cost NMR for diverse applications.

Keywords:
AuthenticationBenchtopMonitoringNMR spectroscopyPure-shiftSolvent suppressionUltrafast

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Area of Science:

  • Analytical Chemistry
  • Spectroscopy

Background:

  • Benchtop Nuclear Magnetic Resonance (NMR) spectroscopy offers accessible, low-cost high-resolution analysis outside traditional high-field settings.
  • Limitations include significant peak overlaps in complex mixtures and strong non-deuterated solvent signals, hindering analysis.
  • The recent integration of gradient coils (since 2015) has enabled advanced pulse sequences on these instruments.

Purpose of the Study:

  • To review methodological advances in benchtop NMR utilizing magnetic field gradient pulses.
  • To highlight applications enabled by these gradient-enhanced techniques.
  • To discuss future development and application perspectives.

Main Methods:

  • Focus on pulse sequences employing magnetic field gradient pulses for coherence selection and information encoding (chemical shift, diffusion).
  • Review of solvent suppression schemes, diffusion-encoded, and spatially-encoded experiments.
  • Analysis of methodological advancements and their subsequent applications.

Main Results:

  • Gradient pulses effectively address peak overlap issues common in complex mixtures analyzed by benchtop NMR.
  • New pulse sequences enable efficient solvent suppression, diffusion, and spatial encoding.
  • These advancements significantly enhance the performance and applicability of benchtop NMR.

Conclusions:

  • Magnetic field gradient pulses are crucial for unlocking the full potential of modern benchtop NMR.
  • Methodological and application-driven advances are expanding the use of these accessible spectroscopic tools.
  • Future developments promise even broader applications in various scientific fields.