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XANES-Based Quantification of Carbon Functional Group Concentrations.

Corentin Le Guillou1, Sylvain Bernard2, Francisco De la Pena1

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Quantifying functional groups in organic materials using X-ray absorption near edge structure (XANES) spectroscopy is now possible. This new method precisely measures carbon functional group concentrations and ratios, validated with nuclear magnetic resonance.

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Area of Science:

  • Materials Science
  • Analytical Chemistry
  • Spectroscopy

Background:

  • X-ray absorption spectroscopy (XAS) in the soft X-ray range is crucial for identifying functional groups in organic compounds and carbon materials.
  • Quantifying the concentration of these functional groups using XAS has been a significant challenge in various research fields.

Purpose of the Study:

  • To develop a precise method for quantifying carbon functional group concentrations using X-ray absorption near edge structure (XANES) spectroscopy.
  • To establish a reliable correlation between measured optical densities in XANES spectra and the actual concentrations of functional groups.
  • To validate the developed quantification method against established techniques like nuclear magnetic resonance (NMR).

Main Methods:

  • Utilized XANES spectra from reference materials (polymers and compounds with known molecular composition).
  • Developed an alternative normalization method for total carbon content and spectral deconvolution.
  • Correlated measured optical densities with functional group concentrations to establish a quantitative relationship.

Main Results:

  • Achieved precise quantification of the N/C atomic ratio with a standard deviation (σ1) of 0.02 atom %.
  • Quantified concentrations of specific functional groups: [aromatic + olefinic] (σ1 = 3.7 atom %), [ketone + phenol + nitrile] (σ1 = 2.2 atom %), [aliphatic] (σ1 = 11.2 atom %), and [carboxylic] (σ1 = 7.4 atom %).
  • Validated the quantification method by comparing results with NMR data from pyrolized lignin samples.
  • Developed and provided an easy-to-use Python program to automate XANES-based quantification.

Conclusions:

  • The developed XANES-based methodology enables accurate quantification of carbon functional group concentrations in organic materials.
  • This approach overcomes previous limitations in XAS analysis, offering precise measurements of elemental ratios and functional group abundances.
  • The availability of an automated Python tool facilitates wider adoption and application of this quantitative technique in research.