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Related Concept Videos

Attenuated Total Reflectance (ATR) Infrared Spectroscopy: Overview01:13

Attenuated Total Reflectance (ATR) Infrared Spectroscopy: Overview

Attenuated total reflectance (ATR) infrared spectroscopy is a powerful analytical technique used to study the composition of materials. It is widely employed in chemistry, materials science, forensic science, and other fields where sample characterization is required. ATR has several advantages over traditional transmission IR spectroscopy, including the requirement of little to no sample preparation and the ability to analyze a wide range of samples.
The ATR process begins by directing a beam...

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Advances in Nanoscale Infrared Spectroscopy to Explore Multiphase Polymeric Systems
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Monitoring a Polyurethane Synthesis by Fiber-Coupled Attenuated Total Reflection Fourier Transform Infrared

Marina de Gea Neves1, Miriam Unger2, Heinz W Siesler1

  • 1Department of Physical Chemistry, University of Duisburg-Essen, D-45117 Essen, Germany.

Applied Spectroscopy
|June 20, 2026
PubMed
Summary

This study used multivariate curve resolution alternating least squares (MCR-ALS) to analyze polymerization data. The method effectively tracked polymer phase changes during step-growth polymerization, offering new insights.

Keywords:
ATR FT-IRMCR-ALSPolyurethane polymerizationfiber-coupled attenuated total reflection Fourier transform infrared spectroscopyhydrogen bondingmultivariate curve resolutionreaction kinetics

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Area of Science:

  • Polymer Chemistry
  • Spectroscopy
  • Chemical Engineering

Background:

  • Step-growth polymerization is crucial for producing various polymers.
  • Monitoring polymerization kinetics and phase transitions is complex.
  • Traditional methods may struggle with overlapping spectral data.

Purpose of the Study:

  • To apply multivariate curve resolution alternating least squares (MCR-ALS) for analyzing in situ ATR FT-IR data of a specific polymerization.
  • To investigate the evolution of dissolved and precipitated polymer phases during polymerization.
  • To demonstrate the utility of MCR-ALS in interpreting complex polymerization processes.

Main Methods:

  • In situ monitoring of 1,4-butanediol and 4,4'-diphenylmethanediisocyanate (MDI) polymerization using fiber-coupled attenuated total reflection Fourier transform infrared (ATR FT-IR) spectroscopy.
  • Application of multivariate curve resolution alternating least squares (MCR-ALS) to temperature-dependent spectral data (40-70 °C).
  • Decomposition of overlapping spectral bands to extract concentration profiles of distinct chemical and physical species.

Main Results:

  • MCR-ALS successfully deconvoluted overlapping urethane-related bands.
  • Quantitative concentration profiles for dissolved and precipitated polymer phases were extracted.
  • The results align with previous kinetic studies while providing enhanced detail on transient species and phase evolution.
  • Demonstrated MCR-ALS's capability to differentiate between chemically and physically distinct polymer species.

Conclusions:

  • Multivariate analysis, specifically MCR-ALS, offers significant advantages for interpreting complex polymerization data.
  • MCR-ALS provides quantitative insights into polymerization kinetics and phase transitions.
  • This approach enhances the understanding of polymer formation processes, including phase separation.