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Related Concept Videos

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...
Atomic Nuclei: Nuclear Spin State Population Distribution01:14

Atomic Nuclei: Nuclear Spin State Population Distribution

Near absolute zero temperatures, in the presence of a magnetic field, the majority of nuclei prefer the lower energy spin-up state to the higher energy spin-down state. As temperatures increase, the energy from thermal collisions distributes the spins more equally between the two states. The Boltzmann distribution equation gives the ratio of the number of spins predicted in the spin −½ (N−) and spin +½ (N+) states.
Atomic Nuclei: Nuclear Relaxation Processes01:23

Atomic Nuclei: Nuclear Relaxation Processes

In the absence of an external magnetic field, nuclear spin states are degenerate and randomly oriented. When a magnetic field is applied, the spins begin to precess and orient themselves along (lower energy) or against (higher energy) the direction of the field. At equilibrium, a slight excess population of spins exists in the lower energy state. Because the direction of the magnetic field is fixed as the z-axis,  the precessing magnetic moments are randomly oriented around the z-axis. This...
Atomic Nuclei: Magnetic Resonance01:05

Atomic Nuclei: Magnetic Resonance

The number of nuclear spins aligned in the lower energy state is slightly greater than those in the higher energy state. In the presence of an external magnetic field, as the spins precess at the Larmor frequency, the excess population results in a net magnetization oriented along the z axis. When a pulse or a short burst of radio waves at the Larmor frequency is applied along the x axis, the coupling of frequencies causes resonance and flips the nuclear spins of the excess population from the...
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...

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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

High frequency dynamic nuclear polarization.

Qing Zhe Ni1, Eugenio Daviso, Thach V Can

  • 1Francis Bitter Magnet Laboratory, ‡Department of Chemistry, and §Plasma Science and Fusion Center, Massachusetts Institute of Technology , Cambridge, Massachusetts 02139, United States.

Accounts of Chemical Research
|April 20, 2013
PubMed
Summary
This summary is machine-generated.

Dynamic Nuclear Polarization (DNP) significantly enhances the sensitivity of Magic Angle Spinning Nuclear Magnetic Resonance (MAS NMR) experiments. This breakthrough enables routine structural analysis of challenging biological and material samples.

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Preparation of Fungal and Plant Materials for Structural Elucidation Using Dynamic Nuclear Polarization Solid-State NMR
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Preparation of Fungal and Plant Materials for Structural Elucidation Using Dynamic Nuclear Polarization Solid-State NMR

Published on: February 12, 2019

Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) Spectroscopy
  • Biophysics
  • Materials Science

Background:

  • Magic Angle Spinning (MAS) NMR is crucial for molecular structure determination, but often limited by low sensitivity, especially for low-gamma nuclei (e.g., Carbon-13, Nitrogen-15) and quadrupolar nuclei (e.g., Oxygen-17, Aluminum-27).
  • Dynamic Nuclear Polarization (DNP) offers a powerful solution by transferring high polarization from electron spins to nuclei, overcoming sensitivity limitations inherent in traditional NMR.
  • Early DNP experiments were restricted to static samples and low magnetic fields, necessitating advancements for contemporary MAS NMR applications.

Purpose of the Study:

  • To review the scientific and technical advancements that have made high-frequency Dynamic Nuclear Polarization (DNP) a widely applicable technique for enhancing MAS NMR sensitivity.
  • To discuss the mechanisms, microwave sources, and polarizing agents crucial for modern DNP-MAS NMR.
  • To illustrate the utility of DNP-enhanced MAS NMR through applications in structural biology, particularly for membrane and amyloid proteins.

Main Methods:

  • Development of high-frequency gyrotron microwave sources operating in the subterahertz range (150-660 GHz).
  • Engineering of cryogenic MAS probes enabling in situ microwave irradiation.
  • Design of advanced biradical polarizing agents for efficient polarization transfer at lower concentrations.

Main Results:

  • Significant improvements in DNP efficiency, achieving enhancement factors of approximately 4 with reduced paramagnet concentrations.
  • Routine applicability of DNP-enhanced MAS NMR to diverse scientific challenges, notably in biological and material sciences.
  • Successful application to membrane and amyloid proteins, yielding unique structural insights.

Conclusions:

  • Recent technological and methodological advances have established high-frequency DNP as a routine and powerful tool for enhancing MAS NMR sensitivity.
  • DNP-MAS NMR provides unprecedented structural information for complex systems, including challenging biomolecules.
  • The continued development of DNP techniques promises broader applications in chemistry, biology, and materials science.