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In Situ Monitoring of Heterogeneous Hydrosilylation Reactions Using Infrared and Raman Spectroscopy: Normalization

Xiaoyun Chen1, Yang Cheng2, Masashi Matsuba3

  • 1Analytical Science, Dow Inc., Midland, MI, USA.

Applied Spectroscopy
|June 21, 2019
PubMed
Summary

In situ Raman spectroscopy provides more accurate quantitation for heterogeneous reactions than in situ attenuated total reflection Fourier transform infrared (ATR FT-IR) spectroscopy. Phase-specific normalization is key for precise monitoring of SiH and allyl functional groups in biphasic systems.

Keywords:
FT-IRFourier transform infraredIn situRamanhydrosilylationsilicone polyether

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Area of Science:

  • Chemical Engineering
  • Spectroscopy
  • Reaction Kinetics

Background:

  • Heterogeneous reaction systems are crucial in the chemical industry.
  • In situ monitoring via vibrational spectroscopy offers real-time data without sampling.
  • Multiphase systems present unique challenges for spectroscopic analysis.

Purpose of the Study:

  • To investigate the kinetics of Pt-catalyzed hydrosilylation reactions between allyl polyether and SiH-containing silicone.
  • To compare the efficacy of in situ Raman and ATR FT-IR spectroscopy for monitoring biphasic reactions.
  • To evaluate the impact of phase-specific normalization on quantitation accuracy.

Main Methods:

  • Utilized in situ Raman and attenuated total reflection Fourier transform infrared (ATR FT-IR) spectroscopy.
  • Investigated the Pt-catalyzed hydrosilylation of allyl polyether and SiH-silicone.
  • Employed phase-specific normalization using internal standards.
  • Acquired Raman data with two immersion optics of varying focal lengths.

Main Results:

  • The reaction mixture remained biphasic throughout most of the reaction.
  • In situ Raman spectroscopy, with phase-specific normalization, yielded more accurate quantitation of SiH and allyl groups compared to ATR FT-IR.
  • Wavelength-dependent penetration depth of ATR mode is suggested as the reason for lower accuracy.
  • Advantages and limitations of different Raman immersion optics were demonstrated.

Conclusions:

  • Phase-specific normalization is essential for accurate in situ quantitation in biphasic heterogeneous reactions.
  • Raman spectroscopy is a powerful tool for monitoring complex reaction systems.
  • ATR FT-IR's penetration depth can limit its accuracy in certain multiphase environments.