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Application of PM-IRRAS to study thin films on industrial and environmental samples

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Abstract

Polarization modulation–infrared reflection absorption spectroscopy (PM-IRRAS) was employed to analyze two unique samples: (1) an industrially prepared alkoxysilane-pretreated aluminum alloy (AA6111) in the absence and presence of a ∼600-nm-thick lubricant coating and (2) a chemical warfare agent simulant, triethyl phosphate (TEP), on glass. For the pretreated aluminum samples, PM-IRRAS spectra were analyzed for three distinct regions; the SiO stretching vibration around 1120 cm−1, the NH2 bending mode at ∼1600 cm−1 and the CH stretching region around 2900 cm−1. Our results showed that increasing the curing temperature (from 55 to 100 °C) improved the overall extent of cross-linking within the siloxane network. In addition, the spectra of lubricant (top coating) and the underlying siloxane layer for the aluminum samples with lubricant were collected for the same sample. Our results show that the nature of the siloxane film remains intact and unaltered after deposition of the lubricant top-coat. For detection of TEP on glass, the band at 1268 cm−1, corresponding to the P═O vibration, was monitored. A droplet of TEP solution in dichloromethane was deposited on glass. After solvent evaporation had occurred, the intensity of the P═O vibration band was used to construct calibration curves to determine the experimental limit of detection, which was found to be ∼200 μg for TEP on glass.

Schematic of a akoxysilane network and PM-IRRAS spectrum of the alkoxysilane film at aluminum surface

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Abbreviations

PM-IRRAS:

Polarization modulation–infrared reflection absorption spectroscopy

TEP:

Triethyl phosphate

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Acknowledgements

This work was supported by a contract W7702-09R236 from DRDC and NSERC Engage grant. The authors express their gratitude to Mr. Michael Grossutti for ATR spectrum of Sephadex.

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Authors and Affiliations

  1. Department of Chemistry, University of Guelph, Guelph, ON, N1G 2W1, Canada

    Annia H. Kycia, Kallum Koczkur, J. Jay Leitch & Jacek Lipkowski

  2. Chemistry Department, Acadia University, Wolfville, NS, B4P 2R6, Canada

    Vlad Zamlynny

  3. Defence Research & Development Canada - Suffield, P.O. Box 4000, Medicine Hat, AB, T1A 8K6, Canada

    Michael W. P. Petryk

Authors
  1. Annia H. Kycia
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  2. Kallum Koczkur
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  3. J. Jay Leitch
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  4. Jacek Lipkowski
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  5. Vlad Zamlynny
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  6. Michael W. P. Petryk
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Corresponding author

Correspondence to Jacek Lipkowski.

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Published in the topical collection Characterization of Thin Films and Membranes with guest editors Daniel Mandler and Pankaj Vadgama.

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Kycia, A.H., Koczkur, K., Leitch, J.J. et al. Application of PM-IRRAS to study thin films on industrial and environmental samples. Anal Bioanal Chem 405, 1537–1546 (2013). https://doi.org/10.1007/s00216-012-6469-6

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  • DOI: https://doi.org/10.1007/s00216-012-6469-6

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