Composition of ultrathin binary polymer brushes by thermogravimetry–gas chromatography–mass spectrometry
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In the present paper, a reliable and rugged thermogravimetry–gas chromatography–mass spectrometry (TGA–GC–MS) method was developed to determine the composition of ultrathin films consisting of binary blends of functional polystyrene (PS) and polymethylmethacrylate (PMMA) grafted to a silicon wafer. A general methodology will be given to address the composition determination problem for binary or even multicomponent polymer brush systems using the PS/PMMA-based samples as a paradigmatic example. In this respect, several distinct tailor-made materials were developed to ensure reliable calibration and validation stages. The analytical method was tested on unknown samples to follow the composition evolution in PS/PMMA brushes during the grafting reaction. A preferential grafting of the PMMA was revealed in full agreement with its preferential interaction with the SiO2 polar surface.
KeywordsThermogravimetry–gas chromatography–mass spectrometry Composition determination Method validation Ultrathin film analysis Polymer brushes
Financial support by PRIN 2010–2014 “Materiali Polimerici Nanostrutturati con Strutture Molecolari e Cristalline Mirate” is acknowledged.
Compliance with ethical standards
Conflict of interest
The authors declare that they have no competing interests.
- 2.Tokareva I, Tokarev I, Minko S, Hutter E, Fendler, JH. Ultrathin molecularly imprinted polymer sensors employing enhanced transmission surface plasmon resonance spectroscopy. Chem Commun (Camb). 2006;3343–3345. doi: 10.1039/b604841b.
- 21.Shiono A, Hosaka A, Watanabe C, Teramae N, Nemoto N, Ohtani H. Thermoanalytical characterization of polymers: a comparative study between thermogravimetry and evolved gas analysis using a temperature-programmable pyrolyzer. Polym Test. 2015;42:54–61. doi: 10.1016/j.polymertesting.2014.12.011.CrossRefGoogle Scholar
- 22.Kaal ER, Kurano M, Geißler M, Schoenmakers P, Janssen HG. On-line SEC-Py-GC-MS for the automated comprehensive characterization of copolymers. LC GC Eur. 2007;20:444–52.Google Scholar
- 24.Chojnacka A, Ghaffar A, Feilden A, Treacher K, Janssen H-G, Schoenmakers P. Pyrolysis-gas chromatography-mass spectrometry for studying N-vinyl-2-pyrrolidone-co-vinyl acetate copolymers and their dissolution behaviour. Anal Chim Acta. 2011;706:305–11. doi: 10.1016/j.aca.2011.05.052.CrossRefGoogle Scholar
- 32.Conterosito E, Palin L, Antonioli D, Viterbo D, Mugnaioli E, Kolb U, et al. Structural characterisation of complex layered double hydroxides and TGA-GC-MS study on thermal response and carbonate contamination in nitrate- and organic-exchanged hydrotalcites. Chemistry. 2015;21:14975–86. doi: 10.1002/chem.201500450.CrossRefGoogle Scholar