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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.
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...
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...
NMR Spectrometers: Resolution and Error Correction01:14

NMR Spectrometers: Resolution and Error Correction

When magnetic nuclei in a sample achieve resonance and undergo relaxation, the signal detected in NMR is an approximately exponential free induction decay. Fourier transform of an exponential decay yields a Lorentzian peak in the frequency domain. Lorentzian peaks in an NMR spectrum are defined by their amplitude, full width at half maximum, and position, where the peak width is governed by the spin-spin relaxation time alone. In real experiments, however, the applied magnetic field is rendered...

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Experimental Methods for Spin- and Angle-Resolved Photoemission Spectroscopy Combined with Polarization-Variable Laser
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Observer-selective double electron-electron-spin resonance, a pulse sequence to improve orientation selection.

Sergey Milikisyants1, Edgar J J Groenen, Martina Huber

  • 1Department of Molecular Physics, Huygens Laboratory, Leiden University, Niels Bohrweg 2, PO Box 9504, 2300 RA Leiden, The Netherlands.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|April 9, 2008
PubMed
Summary

New observer-selective double electron-electron resonance (os-DEER) pulse sequences enable precise distance measurements in disordered systems. These advanced techniques overcome limitations of conventional methods, allowing for longer pulses and enhanced accuracy in electron spin resonance studies.

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Area of Science:

  • Electron Paramagnetic Resonance (EPR) Spectroscopy
  • Biophysics
  • Materials Science

Background:

  • Pulsed double electron-electron resonance (DEER) measures distances between spin labels in disordered systems up to 8 nm.
  • Conventional DEER requires pulse bandwidths exceeding the dipolar interaction, limiting measurable distances with longer pulses.

Purpose of the Study:

  • Introduce novel observer-selective DEER (os-DEER) and dead-time free os-DEER pulse sequences.
  • Overcome bandwidth limitations in DEER spectroscopy for enhanced distance measurements.
  • Enable the use of longer observer pulses for improved accuracy.

Main Methods:

  • Development and application of two new DEER pulse sequences: os-DEER and dead-time free os-DEER.
  • Utilized long observer pulses (140 ns) with bandwidths smaller than the dipolar interaction.
  • Experimental validation using a nitroxide biradical system.

Main Results:

  • The new os-DEER sequences effectively eliminate distortions caused by limited observer pulse bandwidths.
  • Successfully measured a dipolar interaction of 7.8 MHz using significantly longer observer pulses (140 ns vs. 32 ns).
  • Demonstrated the capability to determine distances and relative orientations in disordered systems with improved precision.

Conclusions:

  • Observer-selective DEER pulse sequences significantly enhance the capabilities of distance measurements in disordered systems.
  • These novel methods overcome previous limitations, allowing for more accurate and precise analysis of spin-labeled systems.
  • The developed techniques are valuable for various fields requiring detailed structural information at the nanoscale.