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Fourier-transform infrared (FTIR) spectroscopy for monitoring and determining the degree of crystallisation of polyhydroxyalkanoates (PHAs)

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Abstract

FTIR spectroscopy has been used to monitor and determine the degree of crystallisation in a sample of polyhydroxybutyrate-co-14%valerate (PHB–co-14%HV). Time series spectra of solution-cast films of the polymer revealed spectral changes attributed to the onset of crystallisation. Curve fitting was used to obtain an absolute measure of crystallinity. Mean centred principal-component analysis (PCA) revealed that 99.9% of the spectral variance could be attributed to factor 1. The loadings plot for factor 1 contained features attributable to crystalline and amorphous phases. These features were opposite in sign, indicating that changes in the spectra with the onset of crystallisation are simultaneous and opposite in direction, i.e. as the crystalline band increases the amorphous band decreases. Cross-peaks in asynchronous 2D correlation maps indicate there are likely to be very minor components that are changing out of phase. The presence of these minor components is supported by examination of the loadings of higher factors in the PCA model. PCA has been shown to be suitable for determining the number of dynamic spectral features and has enabled relative and objective monitoring of crystallisation kinetics.

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Acknowledgments

Acknowledgment is given to the Austrian Science Fund for support of this work, within project no. 15531, and to the Australian Research Council and Monash Graduate Scholarship and travel grant from the Australian Centre of Green Chemistry, School of Chemistry, Monash University.

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Authors and Affiliations

  1. Institute of Chemical Technologies and Analytics, Vienna University of Technology, Getreidemarkt 9/164AC, 1060, Vienna, Austria

    Mustafa Kansiz, Ana Domínguez-Vidal & Bernhard Lendl

  2. School of Chemistry and Centre for Green Chemisty, Monash University, Wellington Rd, Clayton, Melbourne, VIC, 3800, Australia

    Mustafa Kansiz & Don McNaughton

Authors
  1. Mustafa Kansiz
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  2. Ana Domínguez-Vidal
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  3. Don McNaughton
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  4. Bernhard Lendl
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Correspondence to Bernhard Lendl.

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Kansiz, M., Domínguez-Vidal, A., McNaughton, D. et al. Fourier-transform infrared (FTIR) spectroscopy for monitoring and determining the degree of crystallisation of polyhydroxyalkanoates (PHAs). Anal Bioanal Chem 388, 1207–1213 (2007). https://doi.org/10.1007/s00216-007-1337-5

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  • DOI: https://doi.org/10.1007/s00216-007-1337-5

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