title: Assessment of a new method for the analysis of decomposition gases of polymers by a combining thermogravimetric solid-phase extraction and thermal desorption gas chromatography mass spectrometry.
abstract: For analysis of the gaseous thermal decomposition products of polymers, the common techniques are thermogravimetry, combined with Fourier transformed infrared spectroscopy (TGA-FTIR) and mass spectrometry (TGA-MS). These methods offer a simple approach to the decomposition mechanism, especially for small decomposition molecules. Complex spectra of gaseous mixtures are very often hard to identify because of overlapping signals. In this paper a new method is described to adsorb the decomposition products during controlled conditions in TGA on solid-phase extraction (SPE) material: twisters. Subsequently the twisters were analysed with thermal desorption gas chromatography mass spectrometry (TDS-GC-MS), which allows the decomposition products to be separated and identified using an MS library. The thermoplastics polyamide 66 (PA 66) and polybutylene terephthalate (PBT) were used as example polymers. The influence of the sample mass and of the purge gas flow during the decomposition process was investigated in TGA. The advantages and limitations of the method were presented in comparison to the common analysis techniques, TGA-FTIR and TGA-MS.
authors.affiliation: BAM Federal Institute of Material Research and Testing, Unter den Eichen 87, 12205 Berlin, Germany.
authors.forename: E
authors.initials: E
authors.lastname: Duemichen
authors.affiliation: BAM Federal Institute of Material Research and Testing, Unter den Eichen 87, 12205 Berlin, Germany. Electronic address: ulrike.braun@bam.de.
authors.forename: U
authors.initials: U
authors.lastname: Braun
authors.affiliation: Beuth University of Applied Sciences, Luxemburger Straße 10, 13353 Berlin, Germany.
authors.forename: R
authors.initials: R
authors.lastname: Senz
authors.affiliation: Beuth University of Applied Sciences, Luxemburger Straße 10, 13353 Berlin, Germany.
authors.forename: G
authors.initials: G
authors.lastname: Fabian
authors.affiliation: BAM Federal Institute of Material Research and Testing, Unter den Eichen 87, 12205 Berlin, Germany.
authors.forename: H
authors.initials: H
authors.lastname: Sturm
mesh_terms: D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D011091:Polyesters / Q000737:chemistry*; D011108:Polymers / Q000737:chemistry*; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000379:methods*; D017550:Spectroscopy, Fourier Transform Infrared; D013818:Thermogravimetry
chemical_list: D011091:Polyesters; D011108:Polymers; C041733:poly(1,4-butylene terephthalate)
keywords: Degradation; Polymer; Solid-phase extraction; TDS–GC–MS; TGA–FTIR; TGA–MS