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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: 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: 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...
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...
Two-Dimensional (2D) NMR: Overview01:12

Two-Dimensional (2D) NMR: Overview

The 1D NMR spectrum of large and complex molecules like natural products has complicated splitting patterns and overlapping signals, which can be easily interpreted using 2-dimensional (2D) NMR. Unlike 1D NMR, 2D NMR has two frequency axes that provide the coupling information between the nucleus A and nucleus B in a molecule. The process from which 2D spectra are obtained has four steps.
The first step is the preparation period, during which nucleus A is excited with a radiofrequency pulse.
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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Structure and Coordination Determination of Peptide-metal Complexes Using 1D and 2D 1H NMR
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Published on: December 16, 2013

An insight into sequential order in two-dimensional correlation spectroscopy.

Qi Jia1, Nan-Nan Wang, Zhi-Wu Yu

  • 1Key Laboratory of Bioorganic Phosphorous Chemistry & Chemical Biology (Ministry of Education), Department of Chemistry, Tsinghua University, Beijing 100084, China.

Applied Spectroscopy
|March 14, 2009
PubMed
Summary
This summary is machine-generated.

Generalized two-dimensional correlation spectroscopy (2D-COS) reliably determines event order for monotonic changes without local sequences. Plotting intensity versus perturbation factor is recommended before 2D-COS analysis for accurate event sequencing.

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Area of Science:

  • Spectroscopy
  • Chemical Kinetics
  • Data Analysis

Background:

  • Generalized two-dimensional correlation spectroscopy (2D-COS) is crucial for determining the sequential order of events.
  • Questions arise regarding 2D-COS effectiveness for non-periodic changes and local sequential orders.
  • Understanding the precise meaning of the sequential order parameter in 2D-COS is necessary.

Purpose of the Study:

  • To investigate the reliability of 2D-COS for determining sequential order under various spectral change patterns.
  • To clarify the interpretation of the sequential order parameter derived from 2D-COS analysis.
  • To provide guidelines for applying 2D-COS to complex dynamic processes.

Main Methods:

  • Simulated spectral data were analyzed assuming different band intensity change behaviors (logarithmic, exponential, hyperbolic, polynomial).
  • The relationship between event half-time, half-intensity, and sequential order determined by 2D-COS was examined.
  • The impact of monotonic changes and local sequential orders on 2D-COS results was evaluated.

Main Results:

  • For monotonic changes without local sequential orders, 2D-COS correctly identifies the prior event, which typically has a shorter half-time and greater half-intensity.
  • Plotting intensity versus the perturbation factor before 2D-COS analysis is a useful preliminary step for assessing event order.
  • 2D-COS analysis is deemed unnecessary when obvious local sequential orders are present but reliable for determining sequential order otherwise.

Conclusions:

  • 2D-COS is a robust method for determining the sequential order of events, especially when changes are monotonic and lack local complexities.
  • The sequential order parameter from 2D-COS correlates with kinetic parameters like half-time and half-intensity under specific conditions.
  • Pre-analysis visualization of intensity changes against perturbation factors enhances the interpretation of 2D-COS results for dynamic processes.