TY - JOUR A1 - Dümichen, Erik A1 - Braun, Ulrike A1 - Senz, R. A1 - Fabian, G. A1 - Sturm, Heinz T1 - 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 JF - Journal of chromatography A N2 - 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. KW - TDS-GC-MS KW - TGA-FTIR KW - TGA-MS KW - Degradation KW - Polymer KW - Solid-phase extraction PY - 2014 DO - https://doi.org/10.1016/j.chroma.2014.05.057 SN - 0021-9673 VL - 1354 SP - 117 EP - 128 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-31046 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Goedecke, Caroline A1 - Dittmann, Daniel A1 - Eisentraut, Paul A1 - Wiesner, Yosri A1 - Schartel, Bernhard A1 - Klack, Patrick A1 - Braun, Ulrike T1 - Evaluation of thermoanalytical methods equipped with evolved gas analysis for the detection of microplastic in environmental samples JF - Journal of Analytical and Applied Pyrolysis N2 - Microplastic particles are currently detected in almost all environmental compartments. The results of detection vary widely, as a multitude of very different methods are used with very different requirements for analytical validity. In this work four thermoanalytical methods are compared and their advantages and limitations are discussed. One of them is thermal extraction-desorption gas chromatography mass spectrometry (TED-GC/MS), an analysis method for microplastic detection that has become established in recent years. In addition, thermogravimetric analysis coupled with Fourier-transform infrared spectroscopy (TGA-FTIR) and mass spectrometry (TGA-MS) were applied, two methods that are less common in this field but are still used in other research areas. Finally, microscale combustion calorimeter (MCC) was applied, a method not yet used for microplastic detection. The presented results are taken from a recently published interlaboratory comparison test by Becker et al. (2020). Here a reference material consisting of suspended matter and specified added polymer masses was examined, and only the results of the recoveries were presented. In the present paper, however, the results for the individual polymers are discussed in detail and individual perspectives for all instruments are shown. It was found that TED-GC/MS is the most suitable method for samples with unknown matrix and unknown, variable kinds and contents of microplastic. TGA-FTIR is a robust method for samples with known matrix and with defined kinds of microplastic. TGA-MS may offer a solution for the detection of PVC particles in the future. MCC can be used as a very fast and simple screening method for the identification of a potential microplastic load of standard polymers in unknown samples. KW - Microplastic KW - TED-GC/MS KW - TGA-MS KW - TGA-FTIR KW - MCC KW - Thermal analysis PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-516687 DO - https://doi.org/10.1016/j.jaap.2020.104961 VL - 152 SP - 104961 PB - Elsevier B.V. AN - OPUS4-51668 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lörchner, Dominique A1 - Dittmann, Daniel A1 - Braun, Ulrike A1 - Kroh, L. W. A1 - Köppen, Robert T1 - Investigation of two triazine-based heterocyclic brominated flame retardants by coupled thermogravimetry-Fourier transform infrared spectroscopy JF - Journal of Analytical and Applied Pyrolysis N2 - In this study, the thermal decomposition of 1,3,5-tris-(2,3-dibromopropyl)-1,3,5-triazine-2,4,6-trione (TDBPTAZTO) and 2,4,6-tris-(2,4,6-tribromo-phenoxy)-1,3,5-triazine (TTBP-TAZ) were investigated for the first time by thermogravimetric analysis. Both compounds were thermal degraded between 225 and 350 °C (TDBP-TAZTO) as well as 300 and 400 °C (TTBP-TAZ). As a result, mass loss (%) of 98.5% for TTBP-TAZ and 95.4% for TDBP-TAZTO at 600 °C under N2 were observed. The major pyrolytic degradation products of TTBP-TAZ were formed in a single step and identified by FTIR analysis as 2,4,6-tribromophenol and further bromine-substituted aromatic compounds. In comparison, TDBP-TAZTO was pyrolytic degraded in two steps, whereby on the first step the release of hydrogen Bromide and 1,3,5-triallyl-1,3,5-triazine-2,4,6-trione could be detected. In the second minor step, isocyanic acid could be additionally identified. Subsequently, the obtained products of the TGA-FTIR measurements were used for a targeted search for mass fragments in mass spectrometry measurements. For TTBP-TAZ, only the degradation product 1,3,5-tribromobenzene could be detected by MS/MS analyzes. No comparable thermal degradation products, except hydrogen bromide, were observed in the MS/MS spectra of TDBP-TAZTO. Therefore, the search of further mass fragments was not possible compared to the findings of the TGA-FTIR measurements. KW - Pyrolysis KW - Thermal decomposition KW - TGA-FTIR KW - Mass spectrometry PY - 2019 DO - https://doi.org/10.1016/j.jaap.2019.104635 VL - 141 SP - 104635-1 EP - 104635-5 PB - Elsevier B.V. AN - OPUS4-48506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Perret, Birgit A1 - Schartel, Bernhard T1 - TGA-FTIR: From the investigation of pyrolysis to the elucidation of fire retardancy mechanisms JF - UserCom KW - TGA-FTIR KW - Flammschutz KW - Pyrolyse PY - 2010 VL - 32 SP - 16 EP - 19 AN - OPUS4-23905 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Perret, Birgit A1 - Schartel, Bernhard T1 - TGA-FTIR: Détermination des mécanismes ignifuges par l´étude de la pyrolyse JF - UserCom KW - TGA-FTIR KW - Flammschutz KW - Pyrolyse PY - 2010 VL - 32 SP - 16 EP - 19 AN - OPUS4-23906 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Perret, Birgit A1 - Schartel, Bernhard T1 - TGA-FTIR: Von der Untersuchung der Pyrolyse zur Aufklärung von Flammschutzmechanismen JF - UserCom KW - TGA-FTIR KW - Flammschutz KW - Pyrolyse PY - 2010 VL - 32 SP - 16 EP - 19 AN - OPUS4-23904 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -