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Related Concept Videos

¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

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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...
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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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2D NMR: Overview of Heteronuclear Correlation Techniques01:18

2D NMR: Overview of Heteronuclear Correlation Techniques

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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...
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2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)01:19

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

NMR Spectroscopy: Spin–Spin Coupling

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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...
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NMR Spectroscopy: Chemical Shift Overview01:15

NMR Spectroscopy: Chemical Shift Overview

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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...
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Multiple acquisition/multiple observation separated local field/chemical shift correlation solid-state magic angle

Bibhuti B Das1, Stanley J Opella1

  • 1Department of Chemistry and Biochemistry, University of California, San Diego, La Jolla, CA 92093, USA.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|July 16, 2014
PubMed
Summary

Multiple acquisition spectroscopy (MACSY) experiments allow multiple data sets to be recorded in a single experiment. This technique significantly reduces experimental time for complex solid-state NMR studies, enhancing efficiency.

Keywords:
CXCR1Dipolar couplingsDual acquisitionDual observationMACSYPELFProtein NMRR-INEPT

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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy.
  • Advanced spectroscopic techniques.

Background:

  • Traditional multi-dimensional NMR experiments require significant experimental time.
  • Efficient data acquisition is crucial for complex structural analysis.

Purpose of the Study:

  • To demonstrate Multiple Acquisition Spectroscopy (MACSY) experiments.
  • To integrate MACSY with separated local field spectroscopy for correlation NMR.
  • To showcase time-saving potential in solid-state NMR.

Main Methods:

  • Incorporation of separated local field spectroscopy into homonuclear and heteronuclear correlation spectroscopy.
  • Development of MACSY experiments for simultaneous acquisition of multiple free induction decays.
  • Application to solid-state NMR studies.

Main Results:

  • Demonstration of MACSY experiments in homonuclear and heteronuclear correlation spectroscopy.
  • Successful measurement of heteronuclear dipolar couplings.
  • Acquisition of four different 3D spectra within a single experiment.

Conclusions:

  • MACSY experiments offer substantial time savings for solid-state NMR.
  • Measured heteronuclear dipolar couplings aid in structure determination.
  • MACSY enhances resolution by providing an additional frequency axis.