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Related Concept Videos

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...
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...
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 Spectroscopy: Chemical Shift Overview01:15

NMR Spectroscopy: Chemical Shift Overview

The position of the absorption signal of a sample is reported relative to the position of the signal of tetramethylsilane (TMS), which is added as an internal reference while recording spectra. The difference between the absorption frequencies of the sample and TMS (in Hz) is divided by the spectrometer operating frequency (in MHz) to obtain a dimensionless quantity called the chemical shift. It is reported on the δ (delta) scale and expressed in parts per million.
For instance, the proton...
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.

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High-Temperature and High-Pressure In situ Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy
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Shiftless nuclear magnetic resonance spectroscopy.

Chin H Wu1, Stanley J Opella

  • 1Department of Chemistry and Biochemistry, University of California, San Diego, 9500 Gilman Drive, La Jolla, California 92093-0307, USA.

The Journal of Chemical Physics
|February 13, 2008
PubMed
Summary

High-resolution solid-state nuclear magnetic resonance (NMR) spectroscopy without chemical shift frequencies is now feasible. This technique allows detailed characterization of molecular structures, including bond lengths and angles, using dipole-dipole couplings.

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Area of Science:

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

Background:

  • Traditional solid-state NMR spectroscopy relies on chemical shift frequencies for spectral analysis.
  • Limitations in resolution and interpretation can arise from complex spectral overlaps in solid samples.
  • Development of novel NMR techniques is crucial for advancing molecular structure determination.

Purpose of the Study:

  • To describe the acquisition and analysis of high-resolution one- and two-dimensional solid-state NMR spectra.
  • To demonstrate a shiftless NMR spectroscopy method that utilizes dipole-dipole couplings.
  • To characterize molecular structures, including bond lengths and angles, without relying on chemical shifts.

Main Methods:

  • Acquisition of one- and two-dimensional solid-state NMR spectra.
  • Implementation of shiftless NMR spectroscopy variations.
  • Correlation of dipole-dipole and dipole-dipole couplings in a model peptide ((15)N labeled N-acetyl-leucine).

Main Results:

  • Successful acquisition of high-resolution solid-state NMR spectra without chemical shift frequencies.
  • Demonstration of a two-dimensional experiment correlating dipole-dipole couplings.
  • Characterization of bond lengths and angles from a two-dimensional powder pattern of a polycrystalline sample.

Conclusions:

  • Shiftless solid-state NMR spectroscopy is a feasible and powerful technique for structural analysis.
  • This method provides high resolution, enabling the characterization of individual sites in solid samples.
  • The technique offers a novel approach to determine precise molecular geometry, including bond lengths and angles.