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When proton-coupled carbon-13 spectra are simplified by a broadband proton decoupling technique, structural information about the coupled protons is lost. Distortionless enhancement by polarization transfer (DEPT) is a technique that provides information on the number of hydrogens attached to each carbon in a molecule. While the DEPT experiment utilizes complex pulse sequences, the pulse delay and flip angle are specifically manipulated. The resulting signals have different phases depending on...
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The probability of having two carbon-13 atoms next to each other is negligible because of the low natural abundance of carbon-13. Consequently, peak splitting due to carbon-carbon spin-spin coupling is not observed in spectra. However, protons up to three sigma bonds away split the carbon signal according to the n+1 rule, resulting in complicated spectra.
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2D NMR: Overview of Homonuclear Correlation Techniques01:16

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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.
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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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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 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...
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A Reproducible Workflow for Modelling of 1H to 13C Polarization Transfer Kinetics Using Solid-State NMR.

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Summary

This study introduces a new workflow for quantitative solid-state NMR (nuclear magnetic resonance) analysis. It enhances reproducibility and speed by automating spectral processing and kinetic modeling.

Keywords:
13CVCT‐CP‐MASkinetics modellingreproducibilitysolid‐state NMR

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Area of Science:

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

Background:

  • Quantitative analysis of solid-state NMR data, particularly from cross-polarization magic-angle spinning (CP-MAS) experiments, involves complex signal processing.
  • Current methods often rely on semi-manual peak fitting and diverse laboratory tools, hindering reproducibility and efficiency.

Purpose of the Study:

  • To develop a fully reproducible and open workflow for quantitative solid-state NMR data analysis.
  • To streamline the process from raw time-domain data (FIDs) to kinetic model parameters.

Main Methods:

  • Implementation of an adaptive bucketing approach (Extraction of Relevant Variables for Analysis - ERVA) within the NMRProcFlow application to automatically segment 13C spectra.
  • Development of an online platform for fitting intensity curves over contact time using multiple models, incorporating objective fit quality and parameter sensitivity metrics.

Main Results:

  • The proposed workflow automates spectral segmentation and kinetic modeling, significantly reducing manual intervention.
  • The integrated approach offers a fast, user-friendly, and transparent method for quantitative solid-state NMR analysis.

Conclusions:

  • This novel workflow enhances the reproducibility and throughput of quantitative solid-state NMR.
  • It provides a robust platform for extracting kinetic model parameters, opening new avenues for research.