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Related Concept Videos

2D NMR: Overview of Homonuclear Correlation Techniques01:16

2D NMR: Overview of Homonuclear Correlation Techniques

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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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NMR Spectrometers: Overview01:20

NMR Spectrometers: Overview

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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...
1.2K
NMR Spectrometers: Radiofrequency Pulses and Pulse Sequences01:17

NMR Spectrometers: Radiofrequency Pulses and Pulse Sequences

879
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.
879
2D NMR: Homonuclear Correlation Spectroscopy (COSY)01:06

2D NMR: Homonuclear Correlation Spectroscopy (COSY)

1.2K
Homonuclear correlation spectroscopy, or COSY, is a 2-dimensional NMR technique that provides information about coupled protons. Typically, the geminal and vicinal coupling are observed. For example, consider the COSY spectrum of ethyl acetate, where its 1D proton NMR spectrum is plotted along the vertical and horizontal axes with their corresponding chemical shift scale. Three spots on the diagonal corresponding to the three peaks in the 1D proton spectrum are called diagonal peaks. The COSY...
1.2K
NMR Spectroscopy: Spin–Spin Coupling01:08

NMR Spectroscopy: Spin–Spin Coupling

1.5K
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...
1.5K
¹H NMR: Complex Splitting01:13

¹H NMR: Complex Splitting

1.3K
A proton M that is coupled to a proton X results in doublet signals for M. However, NMR-active nuclei can be simultaneously coupled to more than one nonequivalent nucleus. When M is coupled to a second proton A, such as in styrene oxide, each peak in the doublet is split into another doublet.
Splitting diagrams or splitting tree diagrams are routinely used to depict such complex couplings. While drawing splitting diagrams, the splitting with the larger coupling constant is usually applied...
1.3K

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SASSY NMR: Simultaneous Solid and Solution Spectroscopy.

Rajshree Ghosh Biswas1, Ronald Soong1, Amy Jenne1

  • 1Environmental NMR Centre, University of Toronto Scarborough, 1265 Military Trail, Toronto, ON M1C 1A4, Canada.

Angewandte Chemie (International Ed. in English)
|January 1, 2023
PubMed
Summary
This summary is machine-generated.

SimultAneous Solid and Solution spectroscopY (SASSY) allows researchers to study all sample phases, including solids and liquids, at once using standard NMR equipment. This novel technique enhances process monitoring and sample analysis efficiency.

Keywords:
In VivoLiquid-State NMRMultiphase Process MonitoringNMR SpectroscopySolid-State NMR

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Area of Science:

  • Analytical Chemistry
  • Spectroscopy
  • Materials Science

Background:

  • Studying multiphase samples intact is crucial for understanding chemical, biological, and environmental reactivity.
  • Sequential analysis of solids and liquids can lead to missed information in non-observed phases.
  • Standard NMR equipment typically analyzes solid or solution states separately.

Purpose of the Study:

  • Introduce SimultAneous Solid and Solution spectroscopY (SASSY) for simultaneous observation of all phases in multiphase samples.
  • Demonstrate SASSY's ability to differentiate between solid, gel, and liquid phases.
  • Highlight SASSY's efficiency compared to sequential analysis methods.

Main Methods:

  • Utilized standard, solid-state Nuclear Magnetic Resonance (NMR) equipment.
  • Developed and applied the SASSY technique for simultaneous solid-state and solution-state NMR.
  • Validated results against traditional separate 13C CP-MAS solid-state and 13C solution-state NMR experiments.

Main Results:

  • SASSY successfully observed and differentiated all phases (crystalline solids, gels, liquids) in multiphase samples simultaneously.
  • Achieved full sensitivity across all observed phases in every scan.
  • Demonstrated identical results to sequential experiments but with a fraction of the spectrometer time.

Conclusions:

  • SASSY provides a highly efficient method for analyzing multiphase samples.
  • The technique simplifies process monitoring and enables comprehensive analysis of complex systems.
  • SASSY's ease of implementation suggests broad applicability across diverse research fields.