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Related Concept Videos

Other Nuclides: 31P, 19F, 15N NMR01:16

Other Nuclides: 31P, 19F, 15N NMR

Many organic, inorganic, and biological molecules contain spin-half nuclei such as nitrogen-15, fluorine-19, and phosphorus-31. As a result, NMR studies of these nuclei have found extensive applications in chemical and biological research.
While fluorine-19 and phosphorous-31 have high natural abundances (100%) and positive gyromagnetic ratios, nitrogen-15 has a low natural abundance and a negative gyromagnetic ratio. However, nitrogen-15 is still preferred over nitrogen-14 (which has a high...
Nuclear Overhauser Enhancement (NOE)01:06

Nuclear Overhauser Enhancement (NOE)

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 spin-active...
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...
Nuclear Stability03:18

Nuclear Stability

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To hold positively charged protons together in the...
¹H NMR of Labile Protons: Deuterium (²H) Substitution00:48

¹H NMR of Labile Protons: Deuterium (²H) Substitution

This lesson illustrates the role of deuterium substitution in simplifying the NMR spectrum of compounds comprising labile protons. One method employed is the use of deuterium. Amongst the three isotopes of hydrogen, deuterium (2H) has a nucleus composed of one proton and one neutron. When the D2O solvent is added to a pure dry ethanol solution, its labile proton is substituted with deuterium.
π Electron Effects on Chemical Shift: Overview01:27

π Electron Effects on Chemical Shift: Overview

An applied magnetic field causes loosely bound π-electrons in organic molecules to circulate, producing a local or induced diamagnetic field over a large spatial volume. As the molecules tumble in solution, the field generated by π-electrons in spherical substituents results in a zero net field. However, the net field generated by π-electrons in non-spherical substituents is not zero. The effect of this induced field depends on the orientation of the molecule with respect to B0, resulting in...

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Dissolution Dynamic Nuclear Polarization Instrumentation for Real-time Enzymatic Reaction Rate Measurements by NMR
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14.1 T Liquid-State 19F Overhauser Dynamic Nuclear Polarization in an Analytical Organic Setting.

Sungsool Wi1, Jenica Lumata1, Thierry Dubroca1

  • 1National High Magnetic Field Laboratory, Tallahassee, Florida 32310, United States.

Journal of the American Chemical Society
|May 7, 2026
PubMed
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Liquid-state 19F Overhauser dynamic nuclear polarization (DNP) achieved 3- to 37-fold signal enhancements in organic liquids. This breakthrough enables high-field 19F DNP NMR for small-molecule analysis, potentially aiding in PFAS detection.

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Area of Science:

  • Nuclear Magnetic Resonance Spectroscopy
  • Dynamic Nuclear Polarization
  • Fluorine-19 NMR

Background:

  • Liquid-state Nuclear Magnetic Resonance (NMR) is crucial for chemical analysis.
  • Enhancing NMR signal sensitivity, particularly for 19F nuclei, remains a key challenge.
  • Dynamic Nuclear Polarization (DNP) is a technique to boost NMR signal intensity.

Purpose of the Study:

  • To investigate the application of liquid-state 19F Overhauser dynamic nuclear polarization (DNP) on organic compounds.
  • To assess the feasibility of high-field 19F DNP NMR using a specific polarizing agent and experimental setup.
  • To evaluate the potential of this technique for small-molecule analysis and environmental compound detection.

Main Methods:

  • Utilized 1,3-bis(diphenylene)-2-phenylallyl (BDPA) as the polarizing agent for 19F DNP.
  • Employed a modified liquid-state NMR probehead with a waveguide for microwave irradiation (395 GHz/14.1 T).
  • Performed quantitative determinations of BDPA relaxation times (T1e, T2e) at 94 GHz using pulsed-echo and inversion-recovery methods.

Main Results:

  • Achieved 19F DNP enhancement factors between 3- and 37-fold.
  • Obtained spectral resolutions comparable to standard liquid-state 19F NMR with small sample volumes (≈70 μL).
  • Determined BDPA coupling factors ranging from -0.0067 to -0.14 for various analyte and solvent systems.

Conclusions:

  • Liquid-state 19F DNP NMR is feasible for organic liquids, offering significant signal enhancement.
  • The technique shows promise for small-molecule NMR in analytical, pharmaceutical, and environmental chemistry.
  • Further resolution of heating issues is needed, but the approach broadens applicability for detecting persistent compounds like PFAS.