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Related Concept Videos

Nuclear Overhauser Enhancement (NOE)01:07

Nuclear Overhauser Enhancement (NOE)

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Irradiation of a spin-active nucleus causes an increase or decrease in the signal intensity of neighboring nuclei that are not necessarily chemically bonded or involved in J-coupling.  This phenomenon, called the Nuclear Overhauser Enhancement (NOE), results from through-space interactions between the nuclear spins. The NOE effect decreases with increasing internuclear distance and is generally not observed beyond 4 angstroms. In NOE, dipole-dipole interactions between neighboring...
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Insensitive Nuclei Enhanced by Polarization Transfer (INEPT)01:15

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Insensitive Nuclei Enhanced by Polarization Transfer (INEPT) is an advanced Nuclear Magnetic Resonance (NMR) technique specifically designed to detect and enhance the signals of low-abundance nuclei, such as carbon-13 and nitrogen-15, in small molecules. The fundamental principle behind INEPT is the transfer of polarization from a more abundant and highly polarizable nucleus, typically hydrogen-1, to the low-abundance nucleus of interest. This process effectively boosts the NMR signal of the...
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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.
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¹³C NMR: Distortionless Enhancement by Polarization Transfer (DEPT)01:20

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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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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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The spin state of an NMR-active nucleus can have a slight effect on its immediate electronic environment. This effect propagates through the intervening bonds and affects the electronic environments of NMR-active nuclei up to three bonds away; occasionally, even farther. This phenomenon is called spin–spin coupling or J-coupling. Coupling interactions are mutual and result in small changes in the absorption frequencies of both nuclei involved. While nuclei of the same element are involved...
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Preparation of Fungal and Plant Materials for Structural Elucidation Using Dynamic Nuclear Polarization Solid-State NMR
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Surface Enhanced Nuclear Magnetic Resonance Spectroscopy at Solid-Liquid Interfaces Using Overhauser Dynamic Nuclear

Yu Rao1, Domenico Gioffrè2, Marcel Levien1

  • 1Institut des Sciences et Ingénierie Chimiques, Ecole Polytechnique Fédérale de Lausanne (EPFL), CH-1015 Lausanne, Switzerland.

Journal of the American Chemical Society
|June 16, 2025
PubMed
Summary

This study introduces a novel method using exchange-mediated Overhauser effect dynamic nuclear polarization (OE-DNP) to significantly boost Nuclear Magnetic Resonance (NMR) signals from solid surfaces at the solid-liquid interface under ambient conditions.

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Area of Science:

  • Surface science
  • Solid-state NMR spectroscopy
  • Organometallic chemistry

Background:

  • Detecting solid surface sites at solid-liquid interfaces under ambient conditions is challenging.
  • Nuclear Magnetic Resonance (NMR) signal enhancement is crucial for surface characterization.

Purpose of the Study:

  • To develop an efficient method for enhancing NMR signals of solid surfaces at the solid-liquid interface at ambient temperature.
  • To enable the detection of species at both the surface and in solution for monitoring interfacial chemistry.

Main Methods:

  • Utilizing exchange-mediated Overhauser effect dynamic nuclear polarization (OE-DNP).
  • Applying the method to 31P NMR signals of triphenylphosphine (PPh3) ligands on Rh(I) surface sites in silica-supported materials.
  • Preparing materials via surface organometallic chemistry.

Main Results:

  • Achieved efficient DNP enhancements for 31P signals under ambient conditions.
  • Observed significant surface enhancement (εsurface = 20-30) and solution enhancement (εsolution up to 50).
  • Demonstrated simultaneous signal enhancement at the surface and in solution.

Conclusions:

  • The developed OE-DNP approach effectively enhances NMR signals at solid-liquid interfaces.
  • This method allows for the detection of species in both surface and solution phases.
  • Opens new possibilities for real-time monitoring of surface and interfacial chemistry.