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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...
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...
Carbon-13 (¹³C) NMR: Overview01:10

Carbon-13 (¹³C) NMR: Overview

Carbon-13 is a naturally occurring NMR-active isotope of carbon with a low natural abundance of 1.1%. In contrast, carbon-12 is the most abundant isotope of carbon with zero nuclear spin. Therefore, it is NMR inactive. The gyromagnetic ratio of carbon-13 is smaller than that of protons. As a result, carbon-13 resonance is about 6000 times weaker than proton resonance. For a given magnetic field strength, the resonance frequency of carbon-13 is about one-fourth of the resonance frequency for...
High-Resolution Mass Spectrometry (HRMS)01:15

High-Resolution Mass Spectrometry (HRMS)

The resolution of a mass spectrometer depends on the efficiency of separating ions with different ion masses. The mass of an atom is approximated to the sum of the masses of protons and neutrons inside, considering the masses of protons and neutrons as equal. However, the masses of the proton (1.6726 × 10−24 g) and neutron (1.6749 × 10−24 g) are not truly equal. There is a minor error in the expression of atomic masses relative to the simplest atom of hydrogen. For example, the mass of helium...
2D NMR: Homonuclear Correlation Spectroscopy (COSY)01:06

2D NMR: Homonuclear Correlation Spectroscopy (COSY)

Homonuclear correlation spectroscopy, or COSY, is a 2-dimensional NMR technique that provides information about coupled protons. Typically, the geminal and vicinal coupling are observed. For example, consider the COSY spectrum of ethyl acetate, where its 1D proton NMR spectrum is plotted along the vertical and horizontal axes with their corresponding chemical shift scale. Three spots on the diagonal corresponding to the three peaks in the 1D proton spectrum are called diagonal peaks. The COSY...
¹H NMR of Labile Protons: Temporal Resolution01:10

¹H NMR of Labile Protons: Temporal Resolution

Protons bonded to heteroatoms such as nitrogen and oxygen exhibit a range of chemical shift values. This is due to the varying degree of hydrogen bonding between the proton and the heteroatom in other molecules. The extent of hydrogen bonding affects the electron density around the proton, thereby giving different chemical shift values for the protons in the proton NMR spectrum.
The –OH proton in alcohols typically appears in the range of δ 2 to 5 ppm but can vary depending on the specific...

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Related Experiment Video

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Real-Time Metabolic Detection in Living Cells Using Hyperpolarized 13C NMR
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High resolution 13C DOSY: the DEPTSE experiment.

Adolfo Botana1, Peter W A Howe, Valérie Caër

  • 1School of Chemistry, University of Manchester, Oxford Road, Manchester M13 9PL, UK.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|April 22, 2011
PubMed
Summary
This summary is machine-generated.

High Resolution Diffusion-ordered Spectroscopy (HR-DOSY) using carbon-13 (13C) offers superior resolution for NMR mixture analysis. A novel DEPTSE pulse sequence avoids signal loss, improving the efficiency of 13C HR-DOSY experiments.

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Area of Science:

  • Nuclear Magnetic Resonance (NMR) Spectroscopy
  • Analytical Chemistry
  • Physical Chemistry

Background:

  • High Resolution Diffusion-ordered Spectroscopy (HR-DOSY) is crucial for analyzing complex mixtures via NMR.
  • HR-DOSY separates components based on diffusion, but proton-1H signal overlap often complicates interpretation.
  • Carbon-13 (13C) NMR offers better spectral resolution, making it a promising alternative for DOSY.

Purpose of the Study:

  • To enhance the utility of 13C HR-DOSY for mixture analysis.
  • To address the signal-to-noise limitations in 13C DOSY experiments.
  • To introduce a more efficient pulse sequence for 13C diffusion encoding.

Main Methods:

  • Development and application of a novel DEPTSE pulse sequence for 13C DOSY.
  • Utilizing spin echo for diffusion encoding in 13C NMR to prevent signal loss.
  • Leveraging advancements like cryogenic probes to improve signal-to-noise ratios.

Main Results:

  • The DEPTSE pulse sequence effectively encodes diffusion with 13C, avoiding the signal loss inherent in proton-1H based methods.
  • 13C HR-DOSY, particularly with the DEPTSE sequence, provides high diffusion resolution with minimal spectral overlap.
  • Technical improvements have made 13C DOSY a more viable and sensitive technique for mixture analysis.

Conclusions:

  • The DEPTSE pulse sequence represents a significant advancement for 13C HR-DOSY, overcoming previous limitations.
  • 13C HR-DOSY is a powerful, high-resolution technique for NMR mixture analysis, especially when spectral overlap is a concern.
  • This method offers improved efficiency and data quality for diffusion-ordered spectroscopy.