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2D NMR: Overview of Homonuclear Correlation Techniques

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: Overview of Heteronuclear Correlation Techniques

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.

¹H NMR: Interpreting Distorted and Overlapping Signals

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...

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

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...

2D NMR: Homonuclear Correlation Spectroscopy (COSY)

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...

NMR Spectrometers: Resolution and Error Correction

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...

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Related Experiment Video

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High Resolution Phonon-assisted Quasi-resonance Fluorescence Spectroscopy

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High-resolution absorptive intermolecular multiple-quantum coherence NMR spectroscopy under inhomogeneous fields.

Meijin Lin¹, Yanqin Lin, Xi Chen

¹Department of Electronic Science, Fujian Provincial Key Laboratory of Plasma and Magnetic Resonance, State Key Laboratory of Physical Chemistry of Solid Surfaces, Xiamen University, Xiamen 361005, China.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)

|December 31, 2011

Summary

This study introduces a new NMR method for enhanced spectral resolution. The technique achieves faster acquisition and improved clarity in intermolecular multiple-quantum coherence spectra, with potential for in vivo applications.

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Area of Science:

Nuclear Magnetic Resonance (NMR) Spectroscopy
Quantum Coherence Phenomena

Background:

Intermolecular multiple-quantum coherence (iMQC) enhances NMR spectral resolution.
Existing methods can suffer from artifacts and limited speed.

Purpose of the Study:

To develop a novel pulse sequence for fast acquisition of high-resolution NMR spectra.
To achieve double the spectral resolution in intermolecular multi-quantum coherences (iMQCs) without sensitivity loss.

Main Methods:

Design of a CT-iDH pulse sequence combining intermolecular double-quantum filter (iDQF) and a modified constant-time (CT) scheme.
Utilizing intermolecular zero-quantum coherences (iZQCs) and intermolecular double-quantum coherences (iDQCs) for signal generation.
Implementation of a 2D shearing manipulation method.

Main Results:

Fast acquisition of high-resolution iZQCs and iDQCs spectra without strong coupling artifacts.
Realization of double-absorption lineshapes in 2D iMQCs spectra under inhomogeneous fields.
Theoretical and experimental validation of spectral linewidth reduction by half compared to original iMQC spectra.

Conclusions:

The CT-iDH method significantly improves NMR spectral resolution and acquisition speed.
The technique offers doubled resolution and maintained sensitivity, overcoming previous limitations.
Potential applications in in vivo spectroscopy are suggested due to the method's efficiency and resolution enhancement.