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Related Concept Videos

Double Resonance Techniques: Overview01:12

Double Resonance Techniques: Overview

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...
NMR Spectrometers: Radiofrequency Pulses and Pulse Sequences01:17

NMR Spectrometers: Radiofrequency Pulses and Pulse Sequences

A pulse is a short burst of radio waves distributed over a range of frequencies that simultaneously excites all the nuclei in the sample. Upon passing a radio frequency pulse along the x-axis, the nuclei absorb energy corresponding to their Larmor frequencies and achieve resonance. This shifts the net magnetization vector from the z-axis toward the transverse plane. This angle of rotation of the magnetization vector, or the flip angle, is proportional to the duration and intensity of the pulse.
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...
¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

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.
As Δν decreases and the signals move closer, the doublets appear increasingly distorted. The intensities of the inner lines increase at the cost of those of the outer lines as the signals are slanted or...
Insensitive Nuclei Enhanced by Polarization Transfer (INEPT)01:15

Insensitive Nuclei Enhanced by Polarization Transfer (INEPT)

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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Dissolution Dynamic Nuclear Polarization Instrumentation for Real-time Enzymatic Reaction Rate Measurements by NMR
10:54

Dissolution Dynamic Nuclear Polarization Instrumentation for Real-time Enzymatic Reaction Rate Measurements by NMR

Published on: February 23, 2016

A multi-sample 94 GHz dissolution dynamic-nuclear-polarization system.

Michael Batel1, Marcin Krajewski, Kilian Weiss

  • 1Physical Chemistry, ETH Zürich, Wolfgang-Pauli-Strasse 10, 8093 Zürich, Switzerland.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|December 7, 2011
PubMed
Summary
This summary is machine-generated.

A new multi-sample dissolution dynamic-nuclear-polarization (DNP) polarizer enables faster, more reliable experiments. This system achieves significant polarization enhancements in both solid and liquid states for advanced NMR applications.

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Area of Science:

  • Nuclear Magnetic Resonance (NMR) Spectroscopy
  • Dynamic Nuclear Polarization (DNP)
  • Cryogenics and Low-Temperature Physics

Background:

  • Dynamic Nuclear Polarization (DNP) enhances NMR signal sensitivity.
  • Traditional DNP systems often require time-consuming sample manipulation.
  • The need for rapid, repetitive measurements, especially in vivo, drives innovation.

Purpose of the Study:

  • To design and evaluate a multi-sample DNP polarizer for a wide-bore NMR magnet.
  • To enable simultaneous loading and automated sample changing at cryogenic temperatures.
  • To facilitate characterization of the DNP process across various sample compositions.

Main Methods:

  • A Helium-temperature NMR cryostat integrated with a revolver-style sample changer for up to six samples.
  • Operation at variable pressures (ambient down to 1 mbar) with liquid-Helium temperature sample exchange.
  • Incorporation of an oversized microwave cavity with Electron Paramagnetic Resonance (EPR) and NMR capabilities for process monitoring.

Main Results:

  • Solid-state DNP measurements achieved ~45% polarization for [1-(13)C]pyruvic acid using a trityl radical.
  • Liquid-state experiments demonstrated ~13% polarization, yielding an enhancement factor >16,000 at 9.4 T.
  • The multi-sample system allows for reduced sample loading/unloading times, increasing experimental throughput.

Conclusions:

  • The developed multi-sample DNP polarizer is effective for enhancing NMR sensitivity.
  • The system's design supports efficient, high-throughput DNP experiments.
  • Achieved polarization levels are promising for advanced applications in chemistry and biology.