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A statistical design of experiments for optimizing the MALDI-TOF-MS sample preparation of polymers. An application in the assessment of the thermo-mechanical degradation mechanisms of poly (ethylene terephthalate)
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Polymeric Materials.ORCID iD: 0000-0002-2139-7460
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.ORCID iD: 0000-0002-5394-7850
2011 (English)In: Analytica Chimica Acta, ISSN 0003-2670, E-ISSN 1873-4324, Vol. 692, no 1-2, 85-95 p.Article in journal (Refereed) Published
Abstract [en]

The sample preparation procedure for MALDI-TOF MS of polymers is addressed in this study by the application of a statistical Design of Experiments (DoE). Industrial poly (ethylene terephthalate) (PET) was chosen as model polymer. Different experimental settings (levels) for matrixes, analyte/matrix proportions and concentrations of cationization agent were considered. The quality parameters used for the analysis were signal-to-noise ratio and resolution. A closer inspection of the statistical results provided the study not only with the best combination of factors for the MALDI sample preparation, but also with a better understanding of the influence of the different factors, individually or in combination, to the signal. The application of DoE for the improvement of the MALDI measure of PET stated that the best combination of factors and levels was the following: matrix (dithranol), proportion analyte/matrix/cationization agent (1/15/1, V/V/V), and concentration of cationization agent (2 g L-1). In a second part, multiple processing by means of successive injection cycles was used to simulate the thermo-mechanical degradation effects on the oligomeric distribution of PET under mechanical recycling. The application of MALDI-TOF-MS showed that thermo-mechanical degradation primarily affected initially predominant cyclic species. Several degradation mechanisms were proposed, remarking intramolecular transesterification and hydrolysis. The ether links of the glycol unit in PET were shown to act as potential reaction sites, driving the main reactions of degradation.

Place, publisher, year, edition, pages
2011. Vol. 692, no 1-2, 85-95 p.
Keyword [en]
Matrix-assisted laser desorption/ionization time-of-flight, Mass spectrometry, Design of Experiments, Poly (ethylene terephthalate), Recycling, Thermo-mechanical degradation
National Category
Analytical Chemistry
Identifiers
URN: urn:nbn:se:kth:diva-33988DOI: 10.1016/j.aca.2011.02.063ISI: 000290426200009Scopus ID: 2-s2.0-79954631048OAI: oai:DiVA.org:kth-33988DiVA: diva2:418432
Note
QC 20110523Available from: 2011-05-23 Created: 2011-05-23 Last updated: 2017-12-11Bibliographically approved

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Strömberg, E.Karlsson, S.

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