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Related Concept Videos

¹³C NMR: Distortionless Enhancement by Polarization Transfer (DEPT)01:20

¹³C NMR: Distortionless Enhancement by Polarization Transfer (DEPT)

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...
Two-Dimensional (2D) NMR: Overview01:12

Two-Dimensional (2D) NMR: Overview

The 1D NMR spectrum of large and complex molecules like natural products has complicated splitting patterns and overlapping signals, which can be easily interpreted using 2-dimensional (2D) NMR. Unlike 1D NMR, 2D NMR has two frequency axes that provide the coupling information between the nucleus A and nucleus B in a molecule. The process from which 2D spectra are obtained has four steps.
The first step is the preparation period, during which nucleus A is excited with a radiofrequency pulse.
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...
¹³C NMR: ¹H–¹³C Decoupling01:04

¹³C NMR: ¹H–¹³C Decoupling

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...
Double Resonance Techniques: Overview01:12

Double Resonance Techniques: Overview

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.
Spin decoupling is usually achieved by...
2D NMR: Overview of Heteronuclear Correlation Techniques01:18

2D NMR: Overview of Heteronuclear Correlation Techniques

Heteronuclear correlation spectroscopy is an analytical technique that investigates the coupling between different types of nuclei, often a proton and an X-nucleus, such as carbon-13 or nitrogen-15. This method is commonly used in nuclear magnetic resonance (NMR) spectroscopy to gain insights into complex chemical compounds' structural and compositional aspects. A typical heteronuclear correlation spectrum displays X-nucleus chemical shifts on one axis and a proton spectrum on the other axis.

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Concentration of Metabolites from Low-density Planktonic Communities for Environmental Metabolomics using Nuclear Magnetic Resonance Spectroscopy
11:47

Concentration of Metabolites from Low-density Planktonic Communities for Environmental Metabolomics using Nuclear Magnetic Resonance Spectroscopy

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Approach to high-resolution ex situ NMR spectroscopy.

C A Meriles1, D Sakellariou, H Heise

  • 1Materials Sciences Division, Lawrence Berkeley National Laboratory and Department of Chemistry, University of California, Berkeley, CA 94720, USA.

Science (New York, N.Y.)
|July 7, 2001
PubMed
Summary
This summary is machine-generated.

This study introduces a new method for high-resolution Nuclear Magnetic Resonance (NMR) experiments outside of a magnet. It enables clear spectra even with field imperfections, expanding NMR applications.

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Area of Science:

  • Analytical Chemistry
  • Physical Chemistry
  • Spectroscopy

Background:

  • Conventional Nuclear Magnetic Resonance (NMR) requires samples in highly homogeneous magnetic fields.
  • Inserting objects into high-field magnets can be impractical or undesirable for certain applications.
  • Existing methods lack the resolution needed for ex situ NMR analysis.

Purpose of the Study:

  • To develop a novel methodology for high-resolution Nuclear Magnetic Resonance (NMR) experiments performed ex situ.
  • To overcome the limitations of sample insertion into high-field magnets.
  • To enable NMR analysis in environments with inherent magnetic field inhomogeneities.

Main Methods:

  • Adaptation of nutation echo techniques.
  • Implementation of multiple-pulse sequences involving correlated, composite z-rotation pulses.
  • Utilizing matched inhomogeneous static and radiofrequency fields.

Main Results:

  • Achieved resolved Nuclear Magnetic Resonance (NMR) spectra in the presence of field inhomogeneities.
  • Successfully regained the observation of chemical shifts.
  • Demonstrated the capability for high-resolution ex situ NMR analysis of liquid samples.

Conclusions:

  • The presented methodology enables high-resolution NMR analysis outside of traditional homogeneous magnetic fields.
  • This technique expands the scope of NMR applications by allowing analysis of samples in situ or in challenging environments.
  • The use of nutation echoes and specific pulse sequences is key to achieving spectral resolution under inhomogeneous field conditions.