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Related Concept Videos

NMR Spectrometers: Overview01:20

NMR Spectrometers: Overview

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...
NMR Spectrometers: Radiofrequency Pulses and Pulse Sequences01:17

NMR Spectrometers: Radiofrequency Pulses and Pulse Sequences

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.
NMR Spectroscopy: Chemical Shift Overview01:15

NMR Spectroscopy: Chemical Shift Overview

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

NMR Spectrometers: Resolution and Error Correction

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...
¹H NMR Signal Integration: Overview00:58

¹H NMR Signal Integration: Overview

The intensity of a signal, which can be represented by the area under the peak, depends on the number of protons contributing to that signal. The area under each peak is shown as a vertical line called an integral, with the integral value listed under it, as seen in the proton NMR spectrum of benzyl acetate. Each integral value is divided by the smallest integral value to obtain the ratio of the number of protons producing each signal. The ratio reveals the relative number of protons and not...
NMR Spectroscopy of Aromatic Compounds01:14

NMR Spectroscopy of Aromatic Compounds

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. Consider...

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NMR Spectroscopy as a Robust Tool for the Rapid Evaluation of the Lipid Profile of Fish Oil Supplements
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Clean absorption-mode NMR data acquisition.

Yibing Wu1, Arindam Ghosh, Thomas Szyperski

  • 1Department of Chemistry, State University of New York at Buffalo, Buffalo, New York 14260, USA.

Angewandte Chemie (International Ed. in English)
|January 14, 2009
PubMed
Summary
This summary is machine-generated.

New acquisition schemes using phase-shifted mirrored sampling (PMS) eliminate dispersive signals in multi-dimensional experiments. This enhances spectral resolution and peak identification, especially for complex systems with high chemical shift degeneracy.

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Area of Science:

  • Nuclear Magnetic Resonance (NMR) Spectroscopy
  • Analytical Chemistry

Background:

  • Multi-dimensional NMR experiments often suffer from dispersive signal components.
  • These components complicate peak identification and can shift peak maxima, reducing spectral resolution.
  • High chemical shift degeneracy in complex systems exacerbates these issues.

Purpose of the Study:

  • To develop novel acquisition schemes for multi-dimensional NMR experiments.
  • To eliminate dispersive signal components without requiring phase correction.
  • To enhance spectral resolution and improve peak identification.

Main Methods:

  • Implementation of phase-shifted mirrored sampling (PMS) during indirect evolution periods.
  • Acquisition schemes designed to inherently suppress dispersive signals.

Main Results:

  • Successful elimination of dispersive signal components without phase correction.
  • Significant enhancement in spectral resolution observed.
  • Improved accuracy in peak identification and maxima determination.
  • Demonstrated particular value for systems with high chemical shift degeneracy.

Conclusions:

  • Phase-shifted mirrored sampling (PMS) offers an effective method for improving spectral quality in multi-dimensional NMR.
  • The developed acquisition schemes provide enhanced resolution and reliable peak identification.
  • This technique is highly beneficial for analyzing complex molecular systems.