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Chromatographic Fingerprinting - a Tool for Classification and for Predicting the Degradation State of Degradable Polyethylene
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.
2005 (English)In: Polymer degradation and stability, ISSN 0141-3910, E-ISSN 1873-2321, Vol. 89, no 1, 50-63 p.Article in journal (Refereed) Published
Abstract [en]

The number of degradable polyethylene films on the market is increasing. These degradable films show different degradation behaviour depending on the pro-oxidant system incorporated in them. The degradation of the films gives rise to complex collections of degradation products. The key question in this work was to classify the types of pro-oxidant systems in degradable polyethylene films and the state of degradation of the films. The classification was performed with chromatographic fingerprints of carboxylic acids, the most abundant type of degradation product. The acids were extracted from films oxidised at 80 ° C and were thereafter methylated and analysed by GC-MS. Classification and prediction models were obtained by Multivariate Data Analysis. The diacids were grouped according to both the type of pro-oxidant system and the state of degradation. This showed that both the type of pro-oxidant system and the state of degradation are predictable from the diacid fingerprints. The monoacids were shown to be useful for classifying materials from their initial compositions of stearates but not for predicting the degradation state. The goal was also to see how changes in activation energies for hydroperoxides, noticed earlier with chemiluminescence, were reflected in the degradation mechanisms. The observed increase in chemiluminescence peak temperature of the polyoctylene-containing film was related to the initial degradation of the polyoctylene.

Place, publisher, year, edition, pages
2005. Vol. 89, no 1, 50-63 p.
Keyword [en]
classification, prediction, chromatographic fingerprinting, degradation mechanisms, pro-oxidant systems, chemiluminescence
National Category
Chemical Sciences
Identifiers
URN: urn:nbn:se:kth:diva-5137DOI: 10.1016/j.polymdegradstab.2005.01.002ISI: 000229569500008Scopus ID: 2-s2.0-17044390382OAI: oai:DiVA.org:kth-5137DiVA: diva2:7932
Note
QC 20100903Available from: 2005-05-25 Created: 2005-05-25 Last updated: 2017-12-04Bibliographically approved
In thesis
1. Chromatography and extraction techniques for new evaluation methods of polyolefins long-term performance
Open this publication in new window or tab >>Chromatography and extraction techniques for new evaluation methods of polyolefins long-term performance
2005 (English)Doctoral thesis, comprehensive summary (Other scientific)
Abstract [en]

Chromatography and extraction techniques, and also chemiluminescence have been utilized to develop new rapid and informative tools in the evaluation of long-term properties and environmental effects of polymeric materials.

Methods were developed for classification of materials and for early and rapid degradation detection. Degradable polyethylene films were classified on the basis of their incorporated prooxidant systems using chromatographic fingerprinting of carboxylic acids, the dominating type of degradation product. The fingerprints were also shown to be useful for prediction of the degradation states and evaluation of the degradation mechanisms. Classification and prediction models were obtained by Multivariate Data Analysis, where the diacids were grouped according to both their type of prooxidant system and their state of degradation. The use of total luminescence intensity (TLI) measurements was also investigated as a means of classifying films and for the early detection of degradation. Comparisons were carried out with common techniques, e.g. FTIR and DSC, after both thermal and UV oxidation. TLI gave an earlier detection of degradation and was more sensitive than carbonyl index and crystallinity measurements to relative differences in degradation between the materials. It furthermore offered complementary information regarding changes in activation energies during the course of the degradation. The results were compared with the chromatographic fingerprints.

A new way to evaluate the low temperature long-term stabilisation efficiency of antioxidants was investigated. A prooxidant was used to obtain catalytic oxidation, instead of using thermal acceleration, to evaluate the stabilisation efficiency of antioxidants at low temperatures but still during reasonably short aging times. Comparisons were made between polypropylene films stabilised with primary antioxidants (Irganox 1076, Irganox 1010 and α-tocopherol) with and without the prooxidant manganese stearate at different temperatures. The relative efficiencies of the antioxidants obtained under prooxidant acceleration test correlated better than thermal acceleration test with the results of a long-term low temperature test.

Additives in plastic packaging materials may affect the environment after migration from the packaging to e.g. their contents, especially if they consist of organic aqueous solutions or oils. The use of Solid-Phase Microextraction (SPME) for the specific task of extraction from an organic aqueous solution such as a simulated food or pharmaceutical solution consisting of 10 vol-% ethanol in water was investigated. Methods were developed and evaluated for extraction both with direct sampling and with headspace sampling. If the extraction method and temperature were selected to suit the concentration levels of the analytes, it was possible to quantify several degradation products simultaneously. Comparisons made with Solid Phase Extraction showed the advantage of SPME for this purpose.

Place, publisher, year, edition, pages
Stockholm: KTH, 2005. 86 p.
Series
Trita-FPT-Report, ISSN 1652-2443 ; 2005:20
Keyword
Chemical engineering, polymer, chromatographic fingerprinting, gas-chromatography – mass spectrometry, GC-MS, degradable polyethylene, prooxidant systems, chemiluminescence, oxidation, degradation mechanisms, accelerated ageing, antioxidants, transformation products, microwave assisted extraction, MAE, solid-phase microextraction, SPME, volatiles, solid phase extraction, SPE, Kemiteknik
National Category
Chemical Engineering
Identifiers
urn:nbn:se:kth:diva-219 (URN)91-7178-097-1 (ISBN)
Public defence
2005-06-16, K2, Teknikringen 28, Stockholm, 13:00
Opponent
Supervisors
Note
QC 20100929Available from: 2005-05-25 Created: 2005-05-25 Last updated: 2010-09-29Bibliographically approved

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