Assessing the MALDI-TOF MS sample preparation procedure to analyze the influence of thermo-oxidative ageing and thermo-mechanical degradation on poly (Lactide)
2011 (English)In: European Polymer Journal, ISSN 0014-3057, E-ISSN 1873-1945, Vol. 47, no 7, 1416-1428 p.Article in journal (Refereed) Published
Multiple processing by means of successive injection cycles was used to simulate the thermo-mechanical degradation effects on the oligomeric distribution of PLA under mechanical recycling. Likewise, an accelerated thermal ageing over PLA glass transition was performed in order to simulate its service life. MALDI-TOF MS was used for the analysis and the sample preparation procedure was assessed by means of a statistical Design of Experiments (DoE). The quality effects in use for the analysis were signal-to-noise ratio and Resolution. Different matrixes, analyte/matrix proportions and the use of NaTFA as cationization agent were considered. A deep inspection of the statistical results provided 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 measurement of PLA stated that the best combination of factors (levels) was the following: matrix (s-DHB), proportion analyte/matrix (1/5 V/V), and no use of cationization agent. Degradation primarily affected the initially predominant cyclic [LA(C)](n) and linear H-[LA(L)](n)-OH species, where LA stands for a PLA repeating unit. Intramolecular and intermolecular transesterifications as well as hydrolytic and homolytic reactions took place during the formation and disappearance of oligomeric species. In both degradation mechanisms induced by thermal ageing and thermo-mechanical degradation, the formation of H-[LA(L)](n)-O-CH(3) by intermolecular transesterifications was highlighted.
Place, publisher, year, edition, pages
2011. Vol. 47, no 7, 1416-1428 p.
Matrix-Assisted Laser Desorption/Ionization, Time-of-Flight Mass Spectrometry (MALDI-TOF MS), Design of Experiments (DoE), Polylactide (PLA), Thermo-mechanical degradation, Thermo-oxidative ageing
IdentifiersURN: urn:nbn:se:kth:diva-37549DOI: 10.1016/j.eurpolymj.2011.05.001ISI: 000293051800008ScopusID: 2-s2.0-79959368839OAI: oai:DiVA.org:kth-37549DiVA: diva2:434668
QC 201108162011-08-162011-08-152011-08-16Bibliographically approved