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Related Concept Videos

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...
NMR Spectroscopy: Spin–Spin Coupling01:08

NMR Spectroscopy: Spin–Spin Coupling

The spin state of an NMR-active nucleus can have a slight effect on its immediate electronic environment. This effect propagates through the intervening bonds and affects the electronic environments of NMR-active nuclei up to three bonds away; occasionally, even farther. This phenomenon is called spin–spin coupling or J-coupling. Coupling interactions are mutual and result in small changes in the absorption frequencies of both nuclei involved. While nuclei of the same element are involved in...
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: 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...
Interpreting ¹H NMR Signal Splitting: The (n + 1) Rule01:10

Interpreting ¹H NMR Signal Splitting: The (n + 1) Rule

In the AX proton spin system, proton A can sense the two spin states of a coupled proton X, resulting in a doublet NMR signal with two peaks of equal (1:1) intensity. When proton A is coupled to two equivalent protons (AX2 spin system), the spin states of each X can be aligned with or against the external field, creating three possible scenarios. This results in a 1:2:1  triplet signal, where the central peak corresponds to the chemical shift of A and is twice as large or intense as the others.
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...

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High-Temperature and High-Pressure In situ Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy
08:55

High-Temperature and High-Pressure In situ Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy

Published on: October 9, 2020

Progress in multiple-quantum magic-angle spinning NMR spectroscopy.

João Rocha1, Cláudia M Morais, Christian Fernandez

  • 1Department of Chemistry, CICECO, University of Aveiro, 3810-193, Aveiro, Portugal, Rocha@dq.ua.pt.

Topics in Current Chemistry
|December 14, 2011
PubMed
Summary
This summary is machine-generated.

High-resolution solid-state NMR spectroscopy using multiple-quantum magic-angle spinning (MQMAS) enables detailed studies of quadrupolar nuclei in diverse materials. Advances in MQMAS and related techniques offer powerful tools for materials science and chemistry research.

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Area of Science:

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

Background:

  • Quadrupolar nuclei (I>1/2) with half-integer spins present challenges in solid-state NMR analysis.
  • Traditional NMR methods often yield low-resolution spectra for these nuclei.
  • Materials of academic and industrial interest, including minerals, ceramics, glasses, and biological samples, contain important quadrupolar nuclei.

Purpose of the Study:

  • To review recent advancements in solid-state NMR spectroscopy for quadrupolar nuclei.
  • To highlight the impact of multiple-quantum (MQ) magic-angle spinning (MAS) NMR on materials research.
  • To discuss the evolution and current state of MQMAS NMR techniques and related methods.

Main Methods:

  • Multiple-Quantum (MQ) Magic-Angle Spinning (MAS) NMR spectroscopy.
  • Satellite Transition (ST) MAS NMR.
  • Inverse-STMAS NMR, fast amplitude modulation.
  • Techniques utilizing dipolar interactions (e.g., cross-polarization MQMAS, MQ heteronuclear correlation spectroscopy - HETCOR).
  • J-coupling based experiments (e.g., J-HMQC).

Main Results:

  • MQMAS NMR has significantly improved the study of quadrupolar nuclei in solids.
  • High-resolution solid-state NMR spectra are now achievable for key nuclei like (11)B, (17)O, (23)Na, (27)Al, (71)Ga, and (91)Nb.
  • A variety of advanced MQMAS-related techniques have been developed since 1995, expanding analytical capabilities.

Conclusions:

  • Recent developments in MQMAS NMR have revolutionized the investigation of quadrupolar nuclei in solids.
  • These advanced NMR techniques are crucial for characterizing diverse materials in both academic and industrial settings.
  • The continued evolution of MQMAS and related methods promises further insights into material structures and properties.