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Related Concept Videos

¹³C NMR: ¹H–¹³C Decoupling01:04

¹³C NMR: ¹H–¹³C Decoupling

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

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

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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: Overview01:12

Double Resonance Techniques: Overview

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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.
Spin decoupling is usually achieved by...
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¹H NMR: Complex Splitting01:13

¹H NMR: Complex Splitting

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A proton M that is coupled to a proton X results in doublet signals for M. However, NMR-active nuclei can be simultaneously coupled to more than one nonequivalent nucleus. When M is coupled to a second proton A, such as in styrene oxide, each peak in the doublet is split into another doublet.
Splitting diagrams or splitting tree diagrams are routinely used to depict such complex couplings. While drawing splitting diagrams, the splitting with the larger coupling constant is usually applied...
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2D NMR: Overview of Homonuclear Correlation Techniques01:16

2D NMR: Overview of Homonuclear Correlation Techniques

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Homonuclear correlation spectroscopy (COSY) is a powerful technique used in Nuclear Magnetic Resonance (NMR) spectroscopy to study the correlations between nuclei of the same type within a molecule. It provides information about scalar couplings between adjacent nuclei, which helps determine connectivity and structural information. There are several COSY variants, each with its unique strengths and experimental parameters.
COSY90 is the standard two-dimensional (2D) COSY experiment that...
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Two-Dimensional (2D) NMR: Overview01:12

Two-Dimensional (2D) NMR: Overview

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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.
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Updated: Aug 11, 2025

Cryogenic Sample Loading into a Magic Angle Spinning Nuclear Magnetic Resonance Spectrometer that Preserves Cellular Viability
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Electron-decoupled MAS DNP with N@C60.

Nicholas Alaniva1,2, Edward P Saliba2,3, Patrick T Judge2

  • 1Laboratory of Physical Chemistry, ETH Zürich, Zürich 8093, Switzerland. nalaniva@ethz.ch.

Physical Chemistry Chemical Physics : PCCP
|February 3, 2023
PubMed
Summary
This summary is machine-generated.

Frequency-chirped microwaves effectively decouple electron and carbon-13 spins in N@C60:C60 powder. This technique enhances Nuclear Magnetic Resonance signal intensity, paving the way for advanced magnetic resonance applications.

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Hyperpolarized 13C Metabolic Magnetic Resonance Spectroscopy and Imaging
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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy.
  • Quantum spin control and manipulation.
  • Materials science and fullerene chemistry.

Background:

  • Nitrogen-vacancy centers in fullerenes (N@C60) offer potential as controllable electron-spin sources.
  • Overcoming spin-spin interactions is crucial for enhancing NMR signal sensitivity.
  • Magic-angle spinning (MAS) is a technique used to improve spectral resolution in solid-state NMR.

Purpose of the Study:

  • To demonstrate the effectiveness of frequency-chirped microwaves for electron decoupling in N@C60:C60 powder.
  • To improve the signal intensity of 13C NMR spectra using dynamic nuclear polarization (DNP).
  • To advance the use of N@C60 as a controllable electron-spin source in MAS NMR experiments.

Main Methods:

  • Application of frequency-chirped microwave pulses to decouple electron and 13C spins.
  • Utilizing dynamic nuclear polarization (DNP) to enhance 13C NMR signal.
  • Performing magic-angle spinning (MAS) NMR experiments on N@C60:C60 powder.

Main Results:

  • Achieved a 12% improvement in 13C NMR signal intensity with 7-second polarization.
  • Observed a 5% signal enhancement with 30-second polarization.
  • Demonstrated successful decoupling of electron and 13C spins, validating the microwave technique.

Conclusions:

  • Frequency-chirped microwaves are effective for electron decoupling in N@C60:C60 systems.
  • The demonstrated decoupling enhances DNP-enhanced 13C NMR signal intensity.
  • This work represents a significant step towards utilizing N@C60 as a controllable electron-spin source for advanced MAS NMR.