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Related Concept Videos

2D NMR: Overview of Heteronuclear Correlation Techniques01:18

2D NMR: Overview of Heteronuclear Correlation Techniques

Heteronuclear correlation spectroscopy is an analytical technique that investigates the coupling between different types of nuclei, often a proton and an X-nucleus, such as carbon-13 or nitrogen-15. This method is commonly used in nuclear magnetic resonance (NMR) spectroscopy to gain insights into complex chemical compounds' structural and compositional aspects. A typical heteronuclear correlation spectrum displays X-nucleus chemical shifts on one axis and a proton spectrum on the other axis.
2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)01:19

2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)

Heteronuclear single-quantum correlation spectroscopy (HSQC) is a 2D NMR technique that reveals one-bond correlations between hydrogen and a heteronucleus. The HSQC experiment is similar to the heteronuclear correlation experiment (HETCOR) but is more sensitive. In the HSQC spectrum, the proton chemical shift is plotted on the horizontal F2 axis, while the 13C chemical shift is plotted on the vertical F1 axis. The corresponding proton and 13C spectra are also shown. The HSQC contour plot does...
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...
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...
2D NMR: Homonuclear Correlation Spectroscopy (COSY)01:06

2D NMR: Homonuclear Correlation Spectroscopy (COSY)

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...
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...

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High-Temperature and High-Pressure In situ Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy
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Double-quantum filtered heteronuclear correlation spectroscopy under magic angle spinning.

Yao-Hung Tseng1, Yi-Ling Tsai, Tim W T Tsai

  • 1Department of Chemistry, National Taiwan University, 1, Section 4, Roosevelt Road, Taipei, Taiwan.

Solid State Nuclear Magnetic Resonance
|February 6, 2007
PubMed
Summary

This study introduces a new method using double-quantum filtering in spectroscopy to measure the van Vleck second moment in multiple-spin systems. This technique is effective for analyzing bone and tooth structures like dentin.

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Area of Science:

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

Background:

  • The van Vleck second moment provides crucial information about spin interactions in multiple-spin systems.
  • Accurate determination of this moment is essential for understanding material properties, particularly in biological tissues.
  • Existing methods may lack the resolution or simplicity for certain applications.

Purpose of the Study:

  • To develop a straightforward experimental method for extracting the van Vleck second moment.
  • To apply this method to biological mineral systems like bone and teeth.
  • To characterize the P-31 homonuclear second moment in rat dentin.

Main Methods:

  • Incorporation of a double-quantum (DQ) filter into heteronuclear correlation spectroscopy pulse sequences.
  • Acquisition of DQ excitation profiles by measuring a series of 2D NMR spectra.
  • Testing the method on model compounds (hydroxyapatite and brushite) to assess the influence of spinning frequency and proton decoupling.

Main Results:

  • Demonstrated the feasibility of the DQ-filtered method for measuring the van Vleck second moment.
  • Successfully characterized the P-31 homonuclear second moment of the apatite component in rat dentin.
  • Validated the method's sensitivity to experimental parameters like spinning frequency and proton decoupling.

Conclusions:

  • The developed DQ-filtered NMR method offers a simple and effective approach for determining the van Vleck second moment in multiple-spin systems.
  • This technique is well-suited for the high-resolution study of bone, enamel, and dentin.
  • The findings contribute to a better understanding of the structural and dynamic properties of mineralized biological tissues.