A new experimental technique combining highly sensitive heat flow measurements (microcalorimetry) with the simultaneous detection of chemiluminescence intensity was developed. A perfusion ampoule was connected by fibre optics to an external photo-multiplier and photon counter device. The perfusion ampoule was placed in a 201 calorimetric unit used with a 2277 TAM thermostat. The simultaneous approach offers the advantage of using the same sample and experimental conditions, which reduces the risk for experimental artefacts. Results from the combined equipment confirmed the existence of a time shift between the oxidation profiles of unstabilised polypropylene (PP) previously reported using non-simultaneous MC and CL techniques. The results demonstrate that microcalorimetry is a highly sensitive and versatile tool in studying oxidation of polymers. The success of implementing fibre optics into a perfusion ampoule implies further the possibilities of introducing other probes for the simultaneous detection of oxygen uptake, formation of oxidation products and for studying the effects of UV irradiation among others. © 2003 Elsevier Science Ltd. All rights reserved.
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