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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...
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...
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.
Atomic Nuclei: Types of Nuclear Relaxation01:28

Atomic Nuclei: Types of Nuclear Relaxation

Nuclear relaxation restores the equilibrium population imbalance and can occur via spin–lattice or spin–spin mechanisms, which are first-order exponential decay processes.
In spin–lattice or longitudinal relaxation, the excited spins exchange energy with the surrounding lattice as they return to the lower energy level. Among several mechanisms that contribute to spin–lattice relaxation, magnetic dipolar interactions are significant. Here, the excited nucleus transfers energy to a nearby...
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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Related Experiment Video

Updated: Jul 10, 2026

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses
08:55

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

Published on: June 7, 2018

A solid-state NMR method for solution of zeolite crystal structures.

Darren H Brouwer1, Richard J Darton, Russell E Morris

  • 1School of Chemistry, University of Southampton, Southampton, SO17 1BJ, United Kingdom.

Journal of the American Chemical Society
|July 21, 2005
PubMed
Summary
This summary is machine-generated.

Determining zeolite structures is challenging. A new method combines powder X-ray diffraction (XRD) and nuclear magnetic resonance (NMR) spectroscopy to solve complex zeolite crystal structures.

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High-Temperature and High-Pressure In situ Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy
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Last Updated: Jul 10, 2026

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses
08:55

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Cryogenic Sample Loading into a Magic Angle Spinning Nuclear Magnetic Resonance Spectrometer that Preserves Cellular Viability
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High-Temperature and High-Pressure In situ Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy

Published on: October 9, 2020

Area of Science:

  • Materials Science
  • Solid-State Chemistry
  • Crystallography

Background:

  • Zeolite structure determination typically relies on powder X-ray diffraction (XRD) due to difficulties in growing large single crystals.
  • Solving zeolite structures from powder XRD data is challenging due to the phase problem and overlapping reflections.

Purpose of the Study:

  • To develop a novel method for solving complex zeolite crystal structures.
  • To overcome limitations of traditional powder XRD methods for zeolite structure determination.

Main Methods:

  • Integration of powder X-ray diffraction (XRD) and solid-state nuclear magnetic resonance (NMR) spectroscopy.
  • Utilizing (29)Si double-quantum dipolar recoupling NMR to probe Si-Si distances within the zeolite framework.
  • Combining NMR-derived structural information with unit cell parameters and space group.

Main Results:

  • Successfully solved structural models for two purely siliceous zeolite blind test samples.
  • Demonstrated the efficacy of the combined XRD and NMR approach for structure solution.
  • Achieved successful refinement of the solved structural models against powder XRD data.

Conclusions:

  • The combined powder XRD and NMR spectroscopy method provides a robust approach for zeolite structure determination.
  • This integrated technique overcomes key challenges in solving complex zeolite structures.
  • The method facilitates accurate structural modeling essential for understanding zeolite properties and applications.