TY - CONF A1 - Dümichen, Erik T1 - Investigation of a flame retardant high-temperature polyamide T2 - Tag der Chemie CY - Berlin, Germany DA - 2010-06-16 PY - 2010 AN - OPUS4-21522 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Seefeldt, Henrik A1 - Dümichen, Erik A1 - Braun, Ulrike T1 - Flame retardancy of glass fiber reinforced high temperature polyamide by use of aluminum diethylphosphinate: thermal and thermo-oxidative effects N2 - Glass fiber reinforced polyamide (PA) 6T/DT flame retarded with aluminum diethylphosphinate (AlPi) was tested to assess its flame retardant properties. Models for the decomposition of PA 6T/DT with and without AlPi are presented. Thermal decomposition was measured by performing TGA with Fourier transform infrared (FTIR) spectroscopy and FTIR spectroscopy in the condensed phase. Fire behavior was studied using a cone calorimeter and flammability was tested with UL 94 and the limiting oxygen index. AlPi works as an effective flame retardant for glass fiber reinforced PA 6T/DT materials, acting in the gas phase. Also observed was condensed-phase action, which occurs especially under oxidative conditions before the samples ignite. KW - Flame retardancy KW - High tmeperature polyamide 6T/DT KW - Aluminum phosphinate KW - Degradation PY - 2013 DO - https://doi.org/10.1002/pi.4497 SN - 0959-8103 SN - 1097-0126 SN - 0007-1641 VL - 62 IS - 11 SP - 1608 EP - 1616 PB - Wiley InterScience CY - Chichester, West Sussex AN - OPUS4-29386 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dümichen, Erik T1 - Investigation of the Degradation Mechanism of Transition Metal Doped Polyamides and Polyesters T2 - PDDG CY - Paris, France DA - 2013-09-01 PY - 2013 AN - OPUS4-29078 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dümichen, Erik T1 - Neue Verfahren zur Untersuchung der Polymerdegradation und Aushärtung N2 - Es werden neue analytische Verfahren für die thermische und thermo-oxidative Degradation von Polymeren dargestellt sowie für die Analyse des Netzwerkaufbaus von Epoxidharzen. CY - Hochschule Hamm-Lippstadt DA - 16.12.2014 KW - Polymeranayltik PY - 2014 AN - OPUS4-42154 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dümichen, Erik T1 - Prüfung der Beständigkeit von Kunststoffen im täglichen Gebrauch - thermische Analyseverfahren und Anwendungen an der Bundesanstalt für Materialforschung und -prüfung T2 - Campus Bizz, Hochschule Hamm-Lippstadt CY - Hamm-Lippstadt, Deutschland DA - 2014-12-16 PY - 2014 AN - OPUS4-32334 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dümichen, Erik T1 - The impact of metal oxide particles on the thermal and thermo-oxidative degradation of polyamide 66 T2 - MoDeSt 2014 CY - Portorož, Slovenia DA - 2014-08-31 PY - 2014 AN - OPUS4-31501 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dümichen, Erik T1 - Decomposition gas analysis of polymers by thermogravimetry solid-phase extraction thermal desorption gas chromatography mass spectrometry (TGA-SPE/TDS-GC-MS) T2 - GEFTA 2014 (Gesellschaft für Thermische Analyse e. V.) CY - Berlin, Germany DA - 2014-09-16 PY - 2014 AN - OPUS4-31502 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 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 - Dümichen, Erik A1 - Barthel, Anne-Kathrin A1 - Braun, Ulrike A1 - Bannick, Claus Gerhard A1 - Brand, K. A1 - Jekel, M. A1 - Senz, R. T1 - Analysis of polyethylene microplastics in environmental samples, using a thermal decomposition method N2 - Small polymer particles with a diameter of less than 5 mm called microplastics find their way into the environment from polymer debris and industrial production. Therefore a method is needed to identify and quantify microplastics in various environmental samples to generate reliable concentration values. Such concentration values, i.e. quantitative results, are necessary for an assessment of microplastic in environmental media. This was achieved by thermal extraction in thermogravimetric analysis (TGA), connected to a solid-phase adsorber. These adsorbers were subsequently analysed by thermal desorption gas chromatography mass spectrometry (TDS-GC-MS). In comparison to other chromatographic methods, like pyrolyse gas chromatography mass spectrometry (Py-GC-MS), the relatively high sample masses in TGA (about 200 times higher than used in Py-GC-MS) analysed here enable the measurement of complex matrices that are not homogenous on a small scale. Through the characteristic decomposition products known for every kind of polymer it is possible to identify and even to quantify polymer particles in various matrices. Polyethylene (PE), one of the most important representatives for microplastics, was chosen as an example for identification and quantification. KW - Microplastic KW - Identification and quantification of polymers KW - Thermogravimetric analysis KW - Evolved gas analysis KW - Gas chromatography mass spectroscopy PY - 2015 DO - https://doi.org/10.1016/j.watres.2015.09.002 SN - 0043-1354 VL - 85 SP - 451 EP - 457 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-34337 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dümichen, Erik A1 - Braun, Ulrike A1 - Kraemer, R. A1 - Deglmann, P. A1 - Senz, R. T1 - Thermal extraction combined with thermal desorption: A powerful tool to investigate the thermo-oxidative degradation of polyamide 66 materials N2 - Using thermogravimetric analysis (TGA) with a solid-phase adsorber for thermal extraction, followed by subsequently analysing the adsorber with thermo-desorption gas chromatography mass spectrometry (TDS-GC–MS) enables measurement of polymer degradation under oxidizing atmosphere, and the identification of certain complex hydrocarbon degradation products by chromatographic separation and defined mass patterns. This technique, thermal-extraction desorption gas chromatography mass spectrometry (TED-GC–MS) was used to investigate the thermo-oxidative degradation of PA 66 and PA 66 doped with 2 wt% of metal oxide particles. In TGA pure PA 66 formed more residue under an oxidizing atmosphere than an inert one. In contrast to the measurements under inert atmosphere, several condensed aromatic species containing nitrogen could be identified in thermo-oxidative measurements. These degradation products were formed through condensation reactions of primary amides originating from imide hydrolysis. The formation of such highly condensed species also causes higher char formation. Four metal oxides have shown an impact on the thermo-oxidative degradation of PA 66: Fe2O3 on η-Al2O3 < pure Fe2O3 = Fe2O3 on γ-Al2O3 < pure ZnO. For ZnO even a char-stabilizing effect could be observed. A catalytic effect of these metal oxides causes more condensed cyclopentanone and pyridine derivates. Thus, more water is formed and released, resulting in increased hydrolysis of the imides and degradation at lower temperatures. KW - PA 66 KW - Metal oxide particles KW - Thermo-oxidation KW - Thermogravimetry KW - Solid-phase extraction PY - 2015 DO - https://doi.org/10.1016/j.jaap.2015.08.006 SN - 0165-2370 SN - 1873-250X VL - 115 SP - 288 EP - 298 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-34338 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -