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Journal of Thermal Analysis and Calorimetry

, Volume 107, Issue 2, pp 669–674 | Cite as

A Comparison of the use of FTIR spectroscopy with DSC in the characterisation of melting and crystallisation in polycaprolactone

  • S. H. Murphy
  • G. A. Leeke
  • M. J. Jenkins
Article

Abstract

The infrared spectrum of polycaprolactone has been recorded as a function of temperature in the range where melting and crystallisation of the polymer can occur. Examination of the carbonyl band of the spectra reveals a clear morphological sensitivity; heating the semi-crystalline polymer through the melting region results in a decrease in the intensity of the crystalline component of the carbonyl band. Accordingly, there was a subsequent increase in intensity of the crystalline carbonyl band on cooling. To enable comparison of these findings with a more conventional method of thermal analysis, similar experiments were conducted using a differential scanning calorimeter. The heated ATR accessory adopted for use in the FTIR spectrometer imposed significant limitations in the range of possible heating and cooling rates, but when these rates were carefully matched between FTIR and DSC, close correlation between the melting point and onset of re-crystallisation was observed. The results confirm that FTIR can be used as an alternative, if more laborious, way of investigating melting and re-crystallisation.

Keywords

Polycaprolactone (PCL) Crystallisation Melting DSC FTIR 

References

  1. 1.
    Zhu G, Xu Q, Qin R, Yan H, Liang G. Effect of [gamma]-radiation on crystallization of polycaprolactone. Radiat Phys chem. 2005;74:42–50.CrossRefGoogle Scholar
  2. 2.
    Hutmacher DW. Scaffolds in tissue engineering bone and cartilage. Biomaterials. 2000;21:2529–43.CrossRefGoogle Scholar
  3. 3.
    Acierno S, Di Maio E, Iannace S, Grizzuti N. Structure development during crystallization of polycaprolactone. Rheol Acta. 2006;45:387–92.CrossRefGoogle Scholar
  4. 4.
    Jenkins MJ, Harrison KL. The effect of crystalline morphology on the degradation of PCL in a solution of PBS and lipase. Polym Adv Technol. 2008;19:1901–6.CrossRefGoogle Scholar
  5. 5.
    Coleman MM, Zarian J. Fourier-transform infrared studies of polymer blends. II. Poly(ε-caprolactone)-poly(vinyl chloride) system. J Polym Sci. 1979;17:837–50.Google Scholar
  6. 6.
    Wang J, Cheung MK, Mi Y. Miscibility and morphology in crystalline/amorphous blends of poly(caprolactone)/poly(4-vinylphenol) as studied by DSC, FTIR, and 13C solid state NMR. Polymer. 2002;43:1357–64.CrossRefGoogle Scholar
  7. 7.
    Jiang H, Wu P, Yang Y. Variable Temperature FTIR Study of Poly(ethylene-co-vinyl alcohol)-graft-poly(ε-caprolactone). Biomacromolecules. 2003;4:1343–7.CrossRefGoogle Scholar
  8. 8.
    Yong H, Yoshio I. Novel FTIR method for determining the crystallinity of poly(ε-caprolactone). Polym Int. 2000;49:623–6.CrossRefGoogle Scholar
  9. 9.
    Xu J, Guo B-H, Yang R, et al. In situ FTIR study on melting and crystallization of polyhydroxyalkanoates. Polymer. 2002;43:6893–9.CrossRefGoogle Scholar
  10. 10.
    Kansiz M, Domínguez-Vidal A, McNaughton D, Lendl B. Fourier-transform infrared (FTIR) spectroscopy for monitoring and determining the degree of crystallisation of polyhydroxyalkanoates (PHAs). Anal Bioanal Chem. 2007;388:1207–13.CrossRefGoogle Scholar

Copyright information

© Akadémiai Kiadó, Budapest, Hungary 2011

Authors and Affiliations

  1. 1.School of Metallurgy and MaterialsUniversity of BirminghamBirminghamUK
  2. 2.School of Chemical EngineeringUniversity of BirminghamBirminghamUK

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