Journal of Thermal Analysis and Calorimetry
Volume/Issue:
Volume 107: Issue 2
A Comparison of the use of FTIR spectroscopy with DSC in the characterisation of melting and crystallisation in polycaprolactone
Authors:
S. H. Murphy School of Metallurgy and Materials, University of Birmingham, Edgbaston, Birmingham B15 2TT, UK

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G. A. Leeke School of Chemical Engineering, University of Birmingham, Edgbaston, Birmingham B15 2TT, UK

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M. J. Jenkins School of Metallurgy and Materials, University of Birmingham, Edgbaston, Birmingham B15 2TT, UK

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Pages:
669–674
Online Publication Date:
17 Jul 2011
Publication Date:
01 Feb 2012
Article Category:
Research Article
DOI:
https://doi.org/10.1007/s10973-011-1771-7
Keywords:
Polycaprolactone (PCL); Crystallisation; Melting; DSC; FTIR
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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.

  • 1. Zhu, G, Xu, Q, Qin, R, Yan, H, Liang, G. 2005 Effect of [gamma]-radiation on crystallization of polycaprolactone. Radiat Phys chem. 74:42–50. .

    • Crossref
    • Search Google Scholar
    • Export Citation

  • 2. Hutmacher, DW. Scaffolds in tissue engineering bone and cartilage. Biomaterials. 2000;21:2529–2543. .

  • 3. Acierno, S, Di Maio, E, Iannace, S, Grizzuti, N. 2006 Structure development during crystallization of polycaprolactone. Rheol Acta. 45:387–392. .

    • Crossref
    • Search Google Scholar
    • Export Citation

  • 4. Jenkins, MJ, Harrison, KL. 2008 The effect of crystalline morphology on the degradation of PCL in a solution of PBS and lipase. Polym Adv Technol. 19:1901–1906. .

    • Crossref
    • Search Google Scholar
    • Export Citation

  • 5. Coleman, MM, Zarian, J. 1979 Fourier-transform infrared studies of polymer blends. II. Poly(∊-caprolactone)-poly(vinyl chloride) system. J Polym Sci. 17:837–850.

    • Search Google Scholar
    • Export Citation

  • 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;43:1357–1364. .

    • Crossref
    • Search Google Scholar
    • Export Citation

  • 7. Jiang, H, Wu, P, Yang, Y. Variable Temperature FTIR Study of Poly(ethylene-co-vinyl alcohol)-graft-poly(∊-caprolactone). Biomacromolecules. 2003;4:1343–1347. .

    • Crossref
    • Search Google Scholar
    • Export Citation

  • 8. Yong, H, Yoshio, I. 2000 Novel FTIR method for determining the crystallinity of poly(∊-caprolactone). Polym Int. 49:623–626. .

    • Crossref
    • Search Google Scholar
    • Export Citation

  • 9. Xu, J, Guo, B-H, Yang, R, et al. In situ FTIR study on melting and crystallization of polyhydroxyalkanoates. Polymer. 2002;43:6893–6899. .

    • Crossref
    • Search Google Scholar
    • Export Citation

  • 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;388:1207–1213. .

    • Crossref
    • Search Google Scholar
    • Export Citation
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Cover Journal of Thermal Analysis and Calorimetry
Journal of Thermal Analysis and Calorimetry
Print ISSN:
1388-6150
Online ISSN:
1572-8943

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Journal of Thermal Analysis and Calorimetry
Language English
Size A4
Year of
Foundation		 1969
Volumes
per Year		 1
Issues
per Year		 24
Founder Akadémiai Kiadó
Founder's
Address		 H-1117 Budapest, Hungary 1516 Budapest, PO Box 245.
Publisher Akadémiai Kiadó
Springer Nature Switzerland AG
Publisher's
Address		 H-1117 Budapest, Hungary 1516 Budapest, PO Box 245.
CH-6330 Cham, Switzerland Gewerbestrasse 11.
Responsible
Publisher		 Chief Executive Officer, Akadémiai Kiadó
ISSN 1388-6150 (Print)
ISSN 1588-2926 (Online)

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