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Related Concept Videos

NMR Spectrometers: Overview01:20

NMR Spectrometers: Overview

NMR spectrometers consist of a strong magnet, a radiofrequency transmitter, and a detector attached to a computer console for recording spectra of samples containing NMR-active nuclei. In first-generation NMR instruments called continuous-wave spectrometers, the resonance frequencies of the nuclei are determined by frequency-sweep or field-sweep methods. The magnetic field strength is fixed and the rf signal is swept in the former, while the radiofrequency signal is fixed and the magnetic field...
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...
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.
Chemical Shift: Internal References and Solvent Effects01:17

Chemical Shift: Internal References and Solvent Effects

In an NMR sample, precise measurement of the absolute absorption frequencies of nuclei is difficult. A standard internal reference compound is added, and the frequency difference between the reference signal and sample signals is measured.
The internal reference compound generally used in NMR spectroscopy is tetramethylsilane (TMS). TMS is preferred because it is chemically inert, soluble in NMR solvents, and easily removable. Also, the highly shielded methyl protons in TMS yield an intense...
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...
2D NMR: Overview of Homonuclear Correlation Techniques01:16

2D NMR: Overview of Homonuclear Correlation Techniques

Homonuclear correlation spectroscopy (COSY) is a powerful technique used in Nuclear Magnetic Resonance (NMR) spectroscopy to study the correlations between nuclei of the same type within a molecule. It provides information about scalar couplings between adjacent nuclei, which helps determine connectivity and structural information. There are several COSY variants, each with its unique strengths and experimental parameters.
COSY90 is the standard two-dimensional (2D) COSY experiment that...

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Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
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Resonator with reduced sample heating and increased homogeneity for solid-state NMR.

Alexander Krahn1, Uwe Priller, Lyndon Emsley

  • 1Bruker Biospin GmbH, Silberstreifen, D-76287 Rheinstetten, Germany.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|January 12, 2008
PubMed
Summary

This study introduces a novel multifrequency-tunable Nuclear Magnetic Resonance (NMR) resonator designed to minimize radiofrequency (rf) electric field-induced sample heating, crucial for sensitive biological samples in ionic buffers.

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Area of Science:

  • Nuclear Magnetic Resonance (NMR) Spectroscopy
  • Physical Chemistry
  • Biophysical Chemistry

Background:

  • Radiofrequency (rf) electric fields in solenoidal NMR coils cause sample heating, particularly in lossy samples like proteins in ionic buffers.
  • This heating effect, proportional to frequency, can necessitate reduced rf pulse power, risking sample deterioration and data quality.

Purpose of the Study:

  • To develop and evaluate a multifrequency-tunable NMR resonator that mitigates rf sample heating.
  • To enhance the magneto-electric ratio by electrically shielding the sample from the NMR coil.

Main Methods:

  • Design of a novel NMR resonator with an integrated conductive sheet for sample electrical shielding.
  • Derivation of expressions for B1 efficiency based on magnetic and electric filling factors.
  • Experimental comparison of resonator performance, including rf efficiency, homogeneity, signal-to-noise ratio, and rf sample heating, at 700 MHz.

Main Results:

  • The proposed resonator design effectively shields the sample from rf electric fields, reducing heating.
  • The derived expressions allow for direct comparison of different resonator designs based on key performance metrics.
  • Experimental data validated the resonator's performance with various samples, including ethylene glycol, glycine, and a model protein.

Conclusions:

  • The multifrequency-tunable NMR resonator offers a viable solution to the problem of rf sample heating in solid-state NMR.
  • This advancement enables higher rf pulse power and improved data acquisition for sensitive samples without compromising sample integrity.