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¹H NMR of Labile Protons: Deuterium (²H) Substitution00:48

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

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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.
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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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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 of Conformationally Flexible Molecules: Variable-Temperature NMR01:15

¹H NMR of Conformationally Flexible Molecules: Variable-Temperature NMR

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The axial and equatorial protons in cyclohexane can be distinguished by performing a variable-temperature NMR experiment. In this process, except for one proton, the remaining eleven protons are replaced by deuterium. The deuterium substitution avoids the possible peak splitting caused by the spin-spin coupling between the adjacent protons. The remaining proton flips between the axial and equatorial positions.
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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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¹³C NMR: ¹H–¹³C Decoupling01:04

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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.
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Dissolution Dynamic Nuclear Polarization Instrumentation for Real-time Enzymatic Reaction Rate Measurements by NMR
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High-field NMR with dissolution triplet-DNP.

Akinori Kagawa1, Koichiro Miyanishi2, Naoki Ichijo2

  • 1Graduate School of Engineering Science, Osaka University, Toyonaka, Osaka 560-8531, Japan; Quantum Information and Quantum Biology Division, Institute for Open and Transdisciplinary Research Initiatives, Osaka University, Japan; PRESTO, Japan Science and Technology Agency (JST), Kawaguchi, Saitama 332-0012, Japan.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|November 1, 2019
PubMed
Summary

We developed Triplet-dynamic nuclear polarization (DNP) for real-time chemical reaction monitoring and metabolic imaging. This method achieves high nuclear polarization at room temperature for solution Nuclear Magnetic Resonance (NMR).

Keywords:
Dissolution-DNPHigh polarizationTriplet electron spin

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Area of Science:

  • Nuclear Magnetic Resonance (NMR) spectroscopy
  • Dynamic Nuclear Polarization (DNP)
  • Quantum sensing

Background:

  • Dynamic nuclear polarization (DNP) significantly enhances NMR signal sensitivity.
  • Current DNP techniques often require cryogenic temperatures, limiting real-time applications.
  • Photoexcited triplet electron spins offer a promising alternative for DNP at ambient temperatures.

Purpose of the Study:

  • To construct and evaluate a novel Triplet-DNP apparatus for solution NMR.
  • To demonstrate the capability of Triplet-DNP for achieving high nuclear polarization at room temperature.
  • To explore the application of Triplet-DNP in real-time monitoring of chemical processes.

Main Methods:

  • Integration of a Triplet-DNP apparatus with a dissolution setup for solution NMR.
  • Utilizing photoexcited triplet electron spins for polarization transfer.
  • Transfer of solid-state polarized samples to a superconducting magnet for dissolution and NMR analysis.

Main Results:

  • Successful construction of a Triplet-DNP apparatus compatible with high magnetic field solution NMR.
  • Achieved 13C polarization of 0.22% for [carboxy-13C]benzoic acid-d in the liquid state.
  • Demonstrated high nuclear polarization at room temperature, overcoming cryogenic limitations.

Conclusions:

  • Triplet-DNP is a viable technique for achieving high nuclear polarization at room temperature.
  • The developed Triplet-DNP method shows significant potential for real-time monitoring applications using solution NMR.
  • This advancement opens new avenues for metabolic imaging and reaction monitoring.