TY - JOUR A1 - Braun, Ulrike A1 - Lorenz, Edelgard A1 - Weimann, Christiane A1 - Sturm, Heinz A1 - Karimov, I. A1 - Ettl, J. A1 - Meier, R. A1 - Wohlgemuth, W. A. A1 - Berger, H. A1 - Wildgruber, M. T1 - Mechanic and surface properties of central-venous port catheters after removal: A comparison of polyurethane and Silicon rubber materials N2 - Central venous port devices made of two different polymeric materials, thermoplastic polyurethane (TPU)and silicone rubber (SiR), were compared due their material properties. Both naïve catheters as well as catheters after removal from patients were investigated. In lab experiments the influence of various chemo-therapeutic solutions on material properties was investigated, where as the samples after removal were compared according to the implanted time inpatient. The macroscopic,mechanical performance was assessed with dynamic, specially adapted tests for elasticity. The degradation status of the materials was determined with common tools of polymer characterisation, such as infrared spectroscopy, molecular weight measurements and various methods of thermal analysis. The surface morphology was an alysed using scanning electron microscopy. A correlation between material properties and clinical performance was proposed. The surface morphology and chemical composition of the polyurethane catheter materials can potentially result in increased susceptibility of the catheter to bloodstream infections and thrombotic complications. The higher mechanic failure,especially with increasing implantation time of the silicone catheters is related to the lower mechanical performance compared to the polyurethane material as well as loss of barium sulphate filler particles near the surface of the catheter. This results in preformed microscopic notches, which act as predetermined sites of fracture. KW - Thermoplastic polyurethane (TPU) KW - Silicone rubber (SiR) KW - Catheters KW - Central venous access port KW - Complication KW - Structure propertyrelationship KW - Mechanical testing PY - 2016 DO - https://doi.org/10.1016/j.jmbbm.2016.08.002 SN - 1751-6161 SN - 1878-0180 VL - 64 SP - 281 EP - 291 PB - Elsevier Ltd. AN - OPUS4-37178 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Naumann, Annette A1 - Seefeldt, Henrik A1 - Stephan, Ina A1 - Braun, Ulrike A1 - Noll, Matthias T1 - Material resistance of flame retarded wood-plastic composites against fire and fungal decay N2 - Flame retarded wood-plastic composites (WPCs) should allow safe application in areas of fire risk. Halogen-free flame retardants can contain high amounts of nitrogen, phosphorus or sulphur, which may serve as nutrition source for wood degrading fungi and accelerate wood decay. Therefore, the material resistance of WPCs with each of four flame retardants against both fire or fungal decay was examined in comparison to WPC without flame retardant. Expandable graphite showed the best performance against fire in cone calorimetry and radiant panel testing. Two ammonium polyphosphates and a third nitrogen-containing flame retardant were not as effective. Contrary to the possibility that flame retardants might enhance fungal decay of WPC, the opposite effect occurred in case of the wood-degrading fungi Trametes versicolor and Coniophora puteana according to determination of mass loss and decrease of bending modulus of elasticity. Only the surface mould Alternaria alternata slightly increased the degradation of WPCs with nitrogen-containing flame retardants compared to WPC without flame retardant according to mass loss data and FTIR-ATR analyses. Finally, WPC including expandable graphite as flame retardant was effective against both fire and fungal decay. KW - Wood-plastic composite (WPC) KW - Flame retardants KW - Fire behaviour KW - Fungal decay KW - Fourier transform infrared - attenuated total reflexion (FTIR-ATR) spectroscopy KW - Microscopy PY - 2012 DO - https://doi.org/10.1016/j.polymdegradstab.2012.03.031 SN - 0141-3910 SN - 1873-2321 VL - 97 IS - 7 SP - 1189 EP - 1196 PB - Applied Science Publ. CY - London AN - OPUS4-26058 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Kunststoffe in der Umwelt: Elastomere, Thermoplaste und Duroplaste – worüber sprechen wir eigentlich und was sind die analytischen Herausforderungen? N2 - Übersichtsvortrag zur Thematik Kunststoffe in der Umwelt. Es werden Aspekte zu Definitionen, Eigenschaften und Analytischen Möglichkeiten und Herrausforderungen angesprochen. T2 - Arbeitsgespräch der Ressortforschungseinrichtungen CY - Berlin, Germany DA - 26.11.2018 KW - Mikroplastik KW - Umwelt KW - Polymere Eigenschaften PY - 2018 AN - OPUS4-47183 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stark, Wolfgang A1 - Teteris, Gundars A1 - Braun, Ulrike A1 - Bohmeyer, W. A1 - Lange, K. T1 - Kontrolle der Vernetzungsreaktion bei reaktiven Harzen - DSC, Rheologie, DMA, FTIR und Online-Ultraschall im Vergleich N2 - Faserverbundbauteile werden durch Tränkung von Fasergewebe mit flüssigem Harz, in der Regel Epoxidharzen, und anschließender Härtung des Harzes gefertigt. Dabei kann man das Gewebe im Vorfeld mit reaktivem Harz tränken und als so genanntes Prepreg verarbeiten oder man injiziert das frisch mit dem Härter gemischte Harz in ein Werkzeug, in dem das Gewebe bereits liegt - z. B. beim RTM-Prozess. Ausgehend von der Aufgabenstellung, eine Prepregherstellung mit hohem Qualitätsstandard zu realisieren und Möglichkeiten der Fertigungskontrolle für den Prepreg-Verarbeiter aufzuzeigen, wurde an einem für die Prepregherstellung vorgesehenen Harzsystem eine weitgehende Charakterisierung des Aushärtungsverlaufs vorgenommen. Wegen der Schwierigkeit, schnell konstante Aushärtungstemperaturen zu erreichen, wurden bei allen Methoden mit einer Heizrate von 1 K/min von RT bis 200 °C aufgeheizt. T2 - Technomer 2011 - 22. Fachtagung über Verarbeitung und Anwendung von Polymeren CY - Chemnitz, Deutschland DA - 10.11.2011 KW - Thermoanalyse KW - Lineare Aufheizung KW - Online Prozesskontrolle KW - Epoxidharz KW - Prepreg PY - 2011 SN - 978-3-939382-10-2 IS - Kap. 1.1 SP - 1 EP - 9 AN - OPUS4-24910 LA - deu 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 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 - Braun, Ulrike A1 - Lorenz, Edelgard A1 - Maskos, Michael T1 - Investigation of the durability of poly(ether urethane) in water and air N2 - In this study some relevant aspects of the durability of an aromatic poly(ether urethanes) was investigated. Hydrolytic and oxidative treatments at increased temperatures were applied. The induced changes in the materials under investigation were characterised by complementary polymer characterisation methods, such as ATR-FTIR, DSC and mechanical testing. The thermal and hydrolytic treatment did not significantly affect the chemical composition of the materials. Changes can be observed in the microstructure of the materials. PY - 2011 DO - https://doi.org/10.5301/IJAO.2011.6408 SN - 0391-3988 VL - 34 IS - 2 SP - 129 EP - 133 PB - Wichtig Ed. CY - Milano [u.a.] AN - OPUS4-23729 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaunich, Matthias A1 - Böhning, Martin A1 - Braun, Ulrike A1 - Teteris, G. A1 - Stark, W. T1 - Investigation of the curing state of ethylene/vinyl acetate copolymer (EVA) for photovoltaic applications by gel content determination, rheology, DSC and FTIR N2 - The cure behaviour of a specific ethylene vinyl acetate material as used for encapsulation of photovoltaic modules was analysed by rheometer, differential scanning calorimetry and Fourier transform infrared spectroscopy to test for a suitable replacement for the laborious determination of gel content. The results show that all applied methods are capable of describing the effects of the cross-linking process. Some provide results very similar to those yielded by analysis of the insoluble content, but the question remains as to whether indirect methods should be preferred over the direct measurement of physical properties, e.g. as performed by the curemeter. A material stored for one year was also tested to demonstrate the effect of extended storage on cure behaviour and how this is detected by different methods. This complements the other methods, which were clearly able to detect the different cure behaviour of the aged EVA, whereas determination of the gel content could not. KW - Photovoltaic cell encapsulation KW - EVA KW - Incoming goods control KW - Insoluble content KW - Rheometer PY - 2016 DO - https://doi.org/10.1016/j.polymertesting.2016.03.013 SN - 0142-9418 VL - 52 IS - 1 SP - 133 EP - 140 PB - Elsevier Ltd. CY - Oxford, UK AN - OPUS4-35918 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Schartel, Bernhard T1 - Interaction of Red Phosphorus, Melanine Polyphosphate and Magnesium Hydroxide as Fire Retardant in HIPS T2 - 9th European Meeting on Fire Retardancy and Protection of Materials, FRPM '03 CY - Lille, France DA - 2003-09-17 PY - 2003 AN - OPUS4-4028 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Wachtendorf, Volker A1 - Geburtig, Anja A1 - Braun, Ulrike A1 - Schartel, Bernhard A1 - Trubiroha, Peter T1 - Influence of weathering on the stability of flame retardancy in polymeric materials for outdoor use T2 - 4th European weathering symposium - Natural and artificial ageing of polymers CY - Budapest, Hungary DA - 2009-09-16 KW - Flame retardancy KW - Weathering KW - Stability KW - Polymeric material KW - Outdoor PY - 2009 SN - 978-3-9810472-8-8 IS - CEEES Publication No. 11 SP - 313 EP - 326 PB - DWS Werbeagentur und Verlag GmbH CY - Karlsruhe AN - OPUS4-20060 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Braun, Ulrike A1 - Balabanovich, Aliaksandr A1 - Schartel, Bernhard A1 - Knoll, Uta A1 - Artner, J. A1 - Ciesielski, M. A1 - Döring, M. A1 - Perez, R. A1 - Sandler, J.K.W. A1 - Altstädt, V. A1 - Hoffmann, T. A1 - Pospiech, D. T1 - Influence of the oxidation state of phosphorus on the decomposition and fire behaviour of flame-retarded epoxy resin composites N2 - A systematic and comparative evaluation of the pyrolysis of halogen-free flame-retarded epoxy resins containing phosphine oxide, phosphinate, phosphonate, and phosphate (phosphorus contents around 2.6 wt.%) and the fire behaviour of their carbon fibre composites is presented. Decomposition pathways are proposed based on the thermal analysis (TG), TG coupled with evolved gas analysis (TG-FTIR), kinetics and analysis of the residue with FTIR and XPS. All organophosphorus-modified hardeners containing phenoxy groups lead to a reduced decomposition temperature and mass loss step for the main decomposition of the cured epoxy resin. With increasing oxidation state of the phosphorus the thermally stable residue increases, whereas the release of phosphorus-containing volatiles decreases. The flammability of the composites was investigated with LOI and UL 94 and the fire behaviour for forced-flaming conditions with cone calorimeter tests performed using different irradiations. The flame retardancy mechanisms are discussed. With increasing oxidation state of the phosphorus additional charring is observed, whereas the flame inhibition, which plays the more important role for the performance of the composites, decreases. The processing and the mechanical performance (delamination resistance, flexural properties and interlaminar bonding strength) of the fibre-reinforced composites containing phosphorus were maintained at a high level and, in some cases, even improved. The potential for optimising flame retardancy while maintaining mechanical properties is highlighted in this study. KW - Fire retardant KW - Composites KW - Organophosphorus-containing epoxy resin PY - 2006 DO - https://doi.org/10.1016/j.polymer.2006.10.022 SN - 0032-3861 SN - 1873-2291 VL - 47 IS - 26 SP - 8495 EP - 8508 PB - Springer CY - Berlin AN - OPUS4-14054 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Seefeldt, Henrik A1 - Braun, Ulrike A1 - Hofmann-Böllinghaus, Anja T1 - Influence of structure, wood content, moisture and additives on the burning behaviour of wood plastic composites T2 - Fire and materials 2011 - 12th International conference and exhibiton CY - San Francisco, CA, USA DA - 2011-01-31 PY - 2011 SP - 1 EP - 10 PB - Interscience Communications AN - OPUS4-24650 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Klöckner, P. A1 - Wagner, S. A1 - Ruhl, A.S. A1 - Eisentraut, Paul A1 - Albrecht, M. A1 - Reemtsma, T. T1 - Identification of tire wear particles based on elemental composition N2 - The identification of tire wear particles by use of ICP-MS is presented. T2 - SETAC CY - Rome, Italy DA - 13.05.2018 KW - Microplastics KW - Tire wear particles KW - ICP-MS PY - 2018 AN - OPUS4-45205 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paul, Andrea A1 - Wander, Lukas A1 - Becker, Roland A1 - Goedecke, Caroline A1 - Braun, Ulrike T1 - High-throughput NIR spectroscopic (NIRS) detection of microplastics in soil N2 - The increasing pollution of terrestrial and aquatic ecosystems with plastic debris leads to the accumulation of microscopic plastic particles of still unknown amount. To monitor the degree of contamination analytical methods are urgently needed, which help to quantify microplastics (MP). Currently, time-costly purified materials enriched on filters are investigated both by micro-infrared spectroscopy and/or micro-Raman. Although yielding precise results, these techniques are time consuming, and are restricted to the analysis of a small part of the sample in the order of few micrograms. To overcome these problems, here we tested a macroscopic dimensioned NIR process-spectroscopic method in combination with chemometrics. For calibration, artificial MP/soil mixtures containing defined ratios of polyethylene, polyethylene terephthalate, polypropylene, and polystyrene with diameters < 125 µm were prepared and measured by a process FT-NIR spectrometer equipped with a fiber optic reflection probe. The resulting spectra were processed by chemometric models including support vector machine regression (SVR), and partial least squares discriminant analysis (PLS-DA). Validation of models by MP mixtures, MP-free soils and real-world samples, e.g. and fermenter residue, suggest a reliable detection and a possible classification of MP at levels above 0.5 to 1.0 mass% depending on the polymer. The benefit of the combined NIRS chemometric approach lies in the rapid assessment whether soil contains MP, without any chemical pre-treatment. The method can be used with larger sample volumes and even allows for an online prediction and thus meets the demand of a high-throughput method. KW - Microplastics KW - Soil KW - Chemometrics KW - PLS-DA KW - Support vector machines KW - Near Infrared Spectroscopy PY - 2018 DO - https://doi.org/10.1007/s11356-018-2180-2 SN - 1614-7499 SN - 0944-1344 VL - 26 IS - 8 SP - 7364 EP - 7374 PB - Springer AN - OPUS4-45405 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Harmonization in microplastics Analysis N2 - The lecture summarizes the current status of hamonization edr microplastics analytics in Germany. T2 - Symposium on Occurrence and Fate of Microplastics CY - Beijing, China DA - 09.07.2019 KW - Microplastics KW - TED-GC-MS KW - Harmonisation PY - 2019 AN - OPUS4-49063 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Bannick, C. G. T1 - Harmonisierung von Untersuchungsverfahren für (Mikro-)Plastik in der Umwelt N2 - Im Rahmen der Thematik "Recycling von Kunststoffen" wird die Thematik "Mikroplastik" vorgestellt T2 - Berliner Recycling- und Rohstoffkonferenz CY - Berlin, Germany DA - 11.03.2019 KW - Mikroplastik KW - Standarisierung KW - Analytik PY - 2019 AN - OPUS4-47582 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gallo, Emanuela A1 - Braun, Ulrike A1 - Schartel, Bernhard A1 - Russo, P. A1 - Acierno, Domenico T1 - Halogen-free flame retarded poly(butylene terephthalate) (PBT) using metal oxides/PBT nanocomposites in combination with aluminium phosphinate N2 - The flame retardancy of poly(butylene terephthalate) (PBT) containing aluminium diethlyphosphinate (AlPi) and/or nanometric metal oxides such as TiO2 or Al2O3 was investigated. In particular the different active flame retardancy mechanisms were discovered. Thermal analysis, evolved gas analysis (TG-FTIR), flammability tests (LOI, UL 94), cone calorimeter measurements and chemical analyses of residues (ATR-FTIR) were used. AlPi acts mainly in the gas phase through the release of diethylphosphic acid, which provides flame inhibition. Part of AlPi remains in the solid phase reacting with the PBT to phosphinate-terephthalate salts that decompose to aluminium phosphate at higher temperatures. The metal oxides interact with the PBT decomposition and promote the formation of additional stable carbonaceous char in the condensed phase. A combination of metal oxides and AlPi gains the better classification in the UL 94 test thanks to the combination of the different mechanisms. KW - Poly(butylene terephthalate) KW - Flammability KW - Metal oxide nanocomposite KW - Metal phosphinate PY - 2009 DO - https://doi.org/10.1016/j.polymdegradstab.2009.04.014 SN - 0141-3910 SN - 1873-2321 VL - 94 IS - 8 SP - 1245 EP - 1253 PB - Applied Science Publ. CY - London AN - OPUS4-19516 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - General aspects of polymers and polymers in environment N2 - The presentation addresses first general aspects of polymers and polymers in environment (definitions, types, phases, morphology, density) and than summarise the possibilities of analysis. T2 - GWRC Workshop on "Microplastics in Water" CY - Nantes, France DA - 22.05.2016 KW - Microplastics KW - Polymers PY - 2016 AN - OPUS4-36901 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Dümichen, Erik A1 - Becker, Roland A1 - Barthel, Anne-Kathrin A1 - Bannick, Claus Gerhard T1 - General aspects of polymers and and polymers in environment N2 - The presentation addresses first general aspects of polymers and polymers in environment (definitions, types, phases, morphology, density) and than summarise the possibilities of analysis. T2 - 1. meeting of ISO/TC 61/SC 5/AHG "microplastics" CY - Berlin, Germany DA - 12.04.2016 KW - Microplastics KW - Polymers PY - 2016 AN - OPUS4-36758 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Weiß, André A1 - Mohr, F. A1 - Kleemeier, M. A1 - Hartwig, A. A1 - Braun, Ulrike T1 - Flame retarded epoxy resins by adding layered silicate in combination with the conventional protection-layer-building flame retardants melamine borate and ammonium polyphosphate N2 - The pyrolysis and flammability of phosphonium-modified layered silicate epoxy resin nanocomposites (EP/LS) were evaluated when LS was combined with two flame retardants, melamine borate (MB) and ammonium polyphosphate (APP), that also act via a surface protection layer. Thermogravimetry (TG), TG coupled with Fourier Transform Spectroscopy (TG-FTIR), oxygen index (LOI), UL 94 burning chamber (UL 94) and cone calorimeter were used. The glassy coating because of 10 wt % MB during combustion showed effects in the cone calorimeter test similar to nanodispersed LS, and somewhat better flame retardancy in flammability tests, such as LOI and UL 94. Adding APP to EP resulted in intumescent systems. The fire retardancy was particularly convincing when 15 wt % APP was used, especially for low external heat flux, and thus, also in flammability tests like LOI and UL 94. V0 classification is achieved when 15 wt % APP is used in EP. The flame retardancy efficiency of the protection layers formed does not increase linearly with the MB and APP concentrations used. The combination of LS with MB or APP shows antagonism; thus the performance of the combination of LS with MB or APP, respectively, was disappointing. No optimization of the carbonaceous-inorganic surface layer occurred for LS-MB. Combining LS with APP inhibited the intumescence, most probably through an increase in viscosity clearly above the value needed for intumescent behavior. KW - Nanocomposites KW - Fire retardance KW - Thermosets KW - Organoclay KW - Ammonium polyphosphate KW - Melamine borate PY - 2010 DO - https://doi.org/10.1002/app.32512 SN - 0021-8995 SN - 1097-4628 VL - 118 IS - 2 SP - 1134 EP - 1143 PB - Wiley InterScience CY - Hoboken, NJ AN - OPUS4-21725 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Braun, Ulrike A1 - Schartel, Bernhard T1 - Flame Retardant Mechanisms of Red Phosphorus and Magnesium Hydroxide in High Impact Polystyrene N2 - The flame retardant mechanisms of red phosphorus, magnesium hydroxide and red phosphorus combined with magnesium hydroxide were studied in high impact polystyrene by means of comprehensive decomposition studies and combustion tests. The study is intended to illuminate prerequisites and the potential of red phosphorus as a fire retardant for hydrocarbon polymers in the condensed phase and in the gas phase. Thermal and thermo-oxidative decomposition, decomposition kinetics and the product gases evolved were characterized using thermogravimetry coupled with Fourier transform infrared spectroscopy and mass spectroscopy, respectively. Fire behaviour was investigated with a cone calorimeter using different external heat fluxes, whereas the flammability was determined by limited oxygen indices. The combustion residues were analysed using XPS. Red phosphorus reduced the heat release in HIPS due to radical trapping in the gas phase. Magnesium hydroxide influenced fire behaviour by heat sink mechanisms, release of water and the formation of a magnesia layer acting as a barrier. The combination of both flame retardants in HIPS nearly resulted in a superposition. A slight synergy in barrier characteristics was due to the formation of magnesium phosphate, whereas a slight anti-synergism occurred in flammability and in the gas phase action. The latter effect is controlled by a decreased fuel rate due to the barrier layer rather than by an initiation of red phosphorus oxidation in the condensed phase. KW - Fire retardancy KW - Polystyrene KW - Pyrolysis KW - TG-FTIR KW - Red Phosphorus KW - Mg(OH)2 KW - Cone Calorimeter KW - Additives KW - Thermogravimetric analysis PY - 2004 DO - https://doi.org/10.1002/macp.200400255 SN - 1022-1352 SN - 1521-3935 VL - 205 IS - 16 SP - 2185 EP - 2196 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-4488 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Perez, R.M. A1 - Sandler, J.K.W. A1 - Altstädt, V. A1 - Hoffmann, T. A1 - Pospiech, D. A1 - Artner, J. A1 - Ciesielski, M. A1 - Döring, M. A1 - Braun, Ulrike A1 - Schartel, Bernhard ED - Schartel, Bernhard T1 - Flame retardant epoxy resin system for liquid composite moulding applications KW - Epoxy resin KW - Fire retardancy PY - 2007 SN - 978-3-8334-8873-3 SP - 69 EP - 84 PB - Books on Demand GmbH CY - Norderstedt AN - OPUS4-17627 LA - eng 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 - Braun, Ulrike A1 - Balabanovich, Aliaksandr A1 - Schartel, Bernhard T1 - Flame retardancy mechanisms of phosphorus containing epoxy resins: effects of oxidation state T2 - MODEST CY - San Sebastián, Spain DA - 2006-09-10 PY - 2006 AN - OPUS4-12939 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Braun, Ulrike A1 - Bahr, Horst A1 - Sturm, Heinz A1 - Schartel, Bernhard T1 - Flame retardancy mechanisms of metal phosphinates and metal phosphinates in combination with melamine cyanurate in glass-fiber reinforced poly(1,4-butylene terephthalate): the influence of metal cation N2 - The pyrolysis and fire behavior of glass-fiber reinforced poly(butylene terephthalate) (PBT/GF) with two different metal phosphinates as flame retardants in combination with and without melamine cyanurate (MC) were analyzed by means of thermogravimetry, thermogravimetry coupled with infrared spectroscopy, flammability, and cone calorimeter tests as well as scanning electron microscopy/energy dispersive X-ray spectroscopy and X-ray fluorescence spectroscopy. In PBT/GF, dosages of 13-20% of the halogen-free flame retardant aluminum phosphinate or aluminum phosphinate in combination with MC fulfill the requirements for electrical engineering and electronics applications (UL 94 = V-0; LOI > 42%), whereas the use of the same amount of zinc phosphinate or zinc phosphinate in combination with MC does not improve the fire behavior satisfactorily (UL 94 = HB; LOI = 27-28%). The performance under forced flaming conditions (cone calorimeter) is quite similar for both of the metal phosphinates. The use of aluminum and zinc salts results in similar flame inhibition predominantly due to the release of the phosphinate compounds in the gas phase. Both metal phosphinates and MC interact with the polymer changing the decomposition characteristics. However, part of the zinc phosphinate vaporizes as a complete molecule. Because of the different decomposition behavior of the metal salts, only the aluminum phosphinate results in a small amount of thermally stable carbonaceous char. In particular, the aluminum phosphinate-terephthalate formed is more stable than the zinc phosphinate-terephthalate. The small amount of char has a crucial effect on the thermal properties and mechanical stability of the residue and thus the flammability. KW - Flame retardance KW - Polyester KW - Phosphinates KW - Pyrolysis KW - Cone calorimeter PY - 2008 DO - https://doi.org/10.1002/pat.1147 SN - 1042-7147 SN - 1099-1581 VL - 19 IS - 6 SP - 680 EP - 692 PB - John Wiley & Sons, Ltd. CY - Chichester AN - OPUS4-17620 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Braun, Ulrike A1 - Sturm, Heinz A1 - Schartel, Bernhard T1 - Flame retardancy mechanisms of aluminium phosphinate in glass-fibre reinforced polyester T2 - Flame Retardants 2008 Conference CY - London, UK DA - 2008-02-12 PY - 2008 SN - 978-0-9556548-1-7 SP - 133 EP - 140 PB - Interscience Communications CY - London, UK AN - OPUS4-17785 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Sturm, Heinz A1 - Schartel, Bernhard T1 - Flame retardancy mechanisms of aluminium phosphinate in glass-fibre reinforced polyester T2 - Flame Retardants 2008 CY - London, England DA - 2008-02-12 PY - 2008 AN - OPUS4-16672 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schartel, Bernhard A1 - Braun, Ulrike ED - Menachem Lewin, T1 - Flame retardancy mechanisms of aluminium phosphinate in glass fiber reinforced thermoplastics T2 - 19th Annual BCC Conference - Recent Advances in Flame Retardancy of Polymeric Materials CY - Stamford, Connecticut, USA DA - 2008-06-09 KW - Aluminium phosphinate KW - PA 66 KW - PBT KW - Flame retardancy KW - Cone calorimeter PY - 2008 SN - 1-59623-435-0 IS - CHM007I SP - 36 EP - 47 PB - BCC Research CY - Wellesley, MA, USA AN - OPUS4-19167 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Braun, Ulrike A1 - Schartel, Bernhard A1 - Fichera, Mario Augusto A1 - Jäger, Christian T1 - Flame retardancy mechanisms of aluminium phosphinate in combination with melamine polyphosphate and zinc borate in glass-fibre reinforced polyamide 6,6 N2 - The fire retardancy mechanisms of aluminium diethylphosphinate in combination with melamine polyphosphate and zinc borate was analysed in glass-fibre reinforced polyamide 6,6. The influence of phosphorus compounds on the polyamide decomposition pathways was characterized using thermal analysis (TG), evolved gas analysis (TG–FTIR), and FTIR–ATR analysis of the residue. The Lewis acid–base interactions between the flame retardants, the amide unit, and the metal ions control the decomposition. The flammability (LOI, UL 94) and performance under forced-flaming conditions (cone calorimeter using different irradiations) were investigated. Fire residues were analysed with FTIR–ATR, SEM–EDX, and NMR. Aluminium phosphinate in polyamide 6,6 acts mainly by flame inhibition. Melamine polyphosphate shows some fuel dilution and a significant barrier effect. Using a combination of aluminium phosphinate and melamine polyphosphate results in some charring and a dominant barrier effect. These effects are improved in the presence of zinc borate due to the formation of boron–aluminium phosphates instead of aluminium phosphates. KW - Flame retardancy KW - Polyamide 6,6 KW - Metal phosphinate KW - Melamine polyphosphate KW - Zinc borate PY - 2007 SN - 0141-3910 SN - 1873-2321 VL - 92 IS - 8 SP - 1528 EP - 1545 PB - Applied Science Publ. CY - London AN - OPUS4-15707 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Braun, Ulrike A1 - Schartel, Bernhard T1 - Flame Retardancy Mechanisms of Aluminium Phosphinate in Combination with Melamine Cyanurate in Glass-Fibre-Reinforced Poly(1,4-butylene terephthalate) N2 - The flame retardancy mechanisms of aluminium diethylphosphinate (AlPi) and its combination with melamine cyanurate (MC) in glass-fibre-reinforced poly(butylene terephthalate) (PBT/GF) were analysed using TGA including evolved gas analysis (TGA-FTIR), cone calorimeter measurements using various irradiations, flammability tests (limited oxygen index, LOI, UL 94) and chemical analyses of residues (FTIR, SEM/EDX). AlPi decomposed mainly through the formation of diethylphosphinic acid and aluminium phosphate and influenced the decomposition of the PBT only slightly. AlPi acted mainly through flame inhibition. A halogen-free V-0 PBT/GF material was achieved with a LOI of 44%. Additional charring influenced the flammability. MC decomposed independently of the polymer and showed some fuel dilution effects. KW - Flame retardance KW - Metal phosphinate KW - Polyester KW - Pyrolysis KW - Thermogravimetric analysis PY - 2008 DO - https://doi.org/10.1002/mame.200700330 SN - 1438-7492 SN - 1439-2054 VL - 293 IS - 3 SP - 206 EP - 217 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-17122 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Pikacz, E. A1 - Seefeldt, Henrik A1 - Schartel, Bernhard A1 - Braun, Ulrike A1 - Karrasch, Andrea A1 - Jäger, Christian T1 - Flame retardancy in PC/Silicone rubber blends using BDP and additional additives T2 - 20th Annual conference on recent advances in flame retardancy of polymeric materials CY - Stamford, CT, USA DA - 2009-06-01 KW - Flame retardancy KW - PC blend KW - Aryl phosphate PY - 2009 SN - 1-59623-509-8 VL - 20 IS - Chapter IV-B SP - 236 EP - 246 CY - Wellesley, MA, USA AN - OPUS4-20703 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Braun, Ulrike A1 - Knoll, Uta A1 - Neubert, Dietmar A1 - Schartel, Bernhard ED - Schartel, Bernhard T1 - Fire Retarding Mechanisms of Red Phosphorus in Polybutylenterephthalate (PBT) in Combination with Melamine Cyanurate or Zinc Oxide KW - Fire retardancy KW - Polyester KW - Red phosphorus KW - Thermal analysis KW - Cone calorimeter PY - 2007 SN - 978-3-8334-8873-3 SP - 35 EP - 49 PB - Books on Demand GmbH CY - Norderstedt AN - OPUS4-17662 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Schartel, Bernhard T1 - Fire Retarding Mechanisms of Red Phosphorus in Polybutylenterephthalate T2 - 10th European Meeting on Fire Retardancy and Protection of Materials (10th European Conference on Fire Retardant Polymers), FRPM '05, BAM, Berlin CY - Berlin, Germany DA - 2005-09-07 PY - 2005 AN - OPUS4-6369 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schartel, Bernhard A1 - Braun, Ulrike A1 - Schwarz, U. A1 - Reinemann, S. ED - Lewin, M. T1 - Fire Retarded Polypropylene/Flax Biocomposites T2 - 14th Conference on Recent Advances in Flame Retardancy of Polymeric Materials ; 14th Annual BCC Conference on Flame Retardancy CY - Stamford, CT, USA DA - 2003-06-02 KW - Fire retardancy KW - PP/Flax Biocomposite KW - Expandable Graphite KW - Ammonium Polyphosphate KW - TG-FTIR KW - Cone Calorimeter PY - 2003 SN - 1-569-65930-3 VL - 14 SP - 219 EP - 228 PB - BCC CY - Norwalk, Conn. AN - OPUS4-2815 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gallo, Emanuela A1 - Schartel, Bernhard A1 - Braun, Ulrike A1 - Russo, P. A1 - Acierno, Domenico T1 - Fire retardant synergisms between nanometric Fe2O3 and aluminium phosphinate in poly(butylene terephthalate) N2 - The pyrolysis and the flame retardancy of poly(butylene terephthalate) (PBT) containing aluminum diethylphosphinate (AlPi) and nanometric Fe2O3 were investigated using thermal analysis, evolved gas analysis (Thermogravimetry-FTIR), flammability tests (LOI, UL 94), cone calorimeter measurements and chemical analysis of residue (FTIR). AlPi mainly acts as a flame inhibitor in the gas phase, through the release of diethylphosphinic acid. A small amount of Fe2O3 in PBT promotes the formation of a carbonaceous char in the condensed phase. The combination of 5 and 8 wt% AlPi, respectively, with 2 wt% metal oxides achieves V-0 classification in the UL 94 test thanks to complementary action mechanisms. Using PBT/metal oxide nanocomposites shows a significant increase in the flame retardancy efficiency of AlPi in PBT and thus opens the route to surprisingly sufficient additive contents as low as 7 wt%. KW - Poly(butylene terephthalate) (PBT) KW - Flammability KW - Metal oxide KW - Nanocomposite KW - Aluminum diethylphosphinate PY - 2011 DO - https://doi.org/10.1002/pat.1774 SN - 1042-7147 SN - 1099-1581 VL - 22 IS - 12 SP - 2382 EP - 2391 PB - John Wiley & Sons, Ltd. CY - Chichester AN - OPUS4-24915 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Schartel, Bernhard A1 - Bahr, Horst T1 - Fire Retardant Mechanisms of Phosphinates in Thermoplastics T2 - Fire Retardant Technologies 2009 CY - Preston (Lancashire), England DA - 2009-04-21 PY - 2009 AN - OPUS4-19842 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Braun, Ulrike A1 - Schwarz, U. A1 - Reinemann, S. T1 - Fire Retardancy of Polypropylene/Flax Blends N2 - A comprehensive characterization of the thermal and the fire behaviour is presented for polypropylene (PP) flax compounds containing ammonium polyphosphate (APP) and expandable graphite as fire retardants. Thermogravimetry coupled with an evolved gas analysis (TG-FTIR) was performed to ensure a significant thermal analysis. The fire response under forced flaming conditions was studied using a cone calorimeter. The external heat flux was varied between 30 and 70 kW m-2 so that the results could be evaluated for different fire scenarios and tests. Different flammability tests (UL 94, limiting oxygen index, glow wire test, GMI 60261) were performed and the results compared with the cone calorimeter data. The different char forming mechanisms are described and the resulting fire retardancy is classified. The successful and ecological friendly fire retardancy is a technological breakthrough for PP/flax biocomposites. KW - Biosomposites KW - Flame retardancy KW - Flax PY - 2003 DO - https://doi.org/10.1016/S0032-3861(03)00692-X SN - 0032-3861 SN - 1873-2291 VL - 44 IS - 20 SP - 6241 EP - 6250 PB - Springer CY - Berlin AN - OPUS4-2640 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Schartel, Bernhard T1 - Fire Retardancy Mechanisms of Red Phosphorus in Thermoplastics N2 - The thermal decomposition and the fire behavior of glass fiber reinforced polyamide 66 (PA-66) and high impact polystyrene (HIPS) containing red phosphorus (P4) were investigated. For glass fiber reinforced PA-66, P4 promotes char formation in the condensed phase. Barrier effects and the reduction of combustible volatiles were identified as fire retardancy mechanisms. For HIPS, P4 acts in the gas phase, mainly trapping radicals. The heat release per mass loss polymer is reduced due to an incomplete combustion. T2 - 12th International Conference Additives 2003 CY - San Francisco, CA, USA DA - 2003-04-06 PY - 2003 UR - http://www.executive-conference.com/conferences/archives/abstracts2003/add03_abs5b.html SP - 1(?) EP - 10(?) PB - ECM CY - Plymouth, Mich. AN - OPUS4-2502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Schartel, Bernhard T1 - Fire Retardancy Mechanisms of Red Phosphorus in Thermoplastics T2 - Additives 2003 - 12th Annual Conference on Additives and Modifiers CY - San Francisco, CA, USA DA - 2003-04-06 PY - 2003 AN - OPUS4-4010 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard A1 - Braun, Ulrike T1 - Fire Retardancy Mechanisms of Phosphorus in Thermoplastics KW - Fire retardancy KW - Red Phosphorus KW - Cone Calorimeter KW - TG-FTIR KW - TG-MS KW - HIPS KW - PBT KW - PA 66 PY - 2004 SN - 0743-0515 VL - 91 SP - 152 EP - 153 PB - Division of Polymeric Materials Science and Engineering, American Chemical Society CY - Washington, DC AN - OPUS4-3971 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Braun, Ulrike A1 - Bahr, Horst A1 - Schartel, Bernhard T1 - Fire retardancy effect of aluminium phosphinate and melamine polyphosphate in glass fibre reinforced polyamide 6 N2 - The fire retardancy mechanism of aluminium diethyl phosphinate (AlPi) and AlPi in combination with melamine polyphosphate (MPP) was investigated in glass-fibre reinforced polyamide 6 (PA6/GF) by analysing the pyrolysis, flammability and fire behaviour. AlPi in PA6/GF-AlPi partly vaporises as AlPi and partly decomposes to volatile diethylphosphinic acid (subsequently called phosphinic acid) and aluminium phosphate residue. In fire a predominant gas-phase action was observed, but the material did not reach a V-0 classification for the moderate additive content used. For the combination of both AlPi and MPP in PA6/GF-AlPi-MPP a synergistic effect occurred, because of the reaction of MPP with AlPi. Aluminium phosphate is formed in the residue and melamine and phosphinic acid are released in the gas phase. The aluminium phosphate acts as a barrier for fuel and heat transport, whereas the melamine release results in fuel dilution and the phosphinic acid formation in flame inhibition. The higher amount of aluminium phosphate in PA6/GF-AlPi-MPP stabilised the residue in flammability tests in comparison to PA6/GF-AlPi, so that this material achieved a V-0 classification in the UL 94 test. PY - 2010 DO - https://doi.org/10.1515/epoly.2010.10.1.443 SN - 1618-7229 IS - 041 SP - 1 EP - 14 PB - De Gruyter CY - [S.l.] AN - OPUS4-19821 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Fast identification of microplastics using thermal extraction methods N2 - The presentation presents an overview about existing methods of microplastic detection with a special focus on thermo-analytical methods. T2 - Perkin Elmer Workshop Microplastics CY - Vienna, Austria DA - 11.01.2018 KW - Microplastics KW - TED-GC-MS KW - Analysis PY - 2018 AN - OPUS4-43803 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dümichen, Erik A1 - Eisentraut, Paul A1 - Bannick, Claus Gerhard A1 - Barthel, Anne-Kathrin A1 - Senz, R. A1 - Braun, Ulrike T1 - Fast identification of microplastics in complex environmental samples by a thermal degradation method N2 - In order to determine the relevance of microplastic particles in various environmental media, comprehensive investigations are needed. However, no analytical method exists for fast identification and quantification. At present, optical spectroscopy methods like IR and RAMAN imaging are used. Due to their time consuming procedures and uncertain extrapolation, reliable monitoring is difficult. For analyzing polymers Py-GC-MS is a standard method. However, due to a limited sample amount of about 0.5 mg it is not suited for analysis of complex sample mixtures like environmental samples. Therefore, we developed a new thermoanalytical method as a first step for identifying microplastics in environmental samples. A sample amount of about 20 mg, which assures the homogeneity of the sample, is subjected to complete thermal decomposition. The specific degradation products of the respective polymer are adsorbed on a solid-Phase adsorber and subsequently analyzed by thermal Desorption gas chromatography mass spectrometry. For certain identification, the specific degradation products for the respective polymer were selected first. Afterwards real environmental samples from the aquatic (three different rivers) and the terrestrial (bio gas plant) systems were screened for microplastics. Mainly polypropylene (PP), polyethylene (PE) and polystyrene (PS) were identified for the samples from the bio gas plant and PE and PS from the rivers. However, this was only the first step and quantification measurements will follow. KW - Microplastics KW - Thermal desorption KW - Gas chromatography PY - 2017 DO - https://doi.org/10.1016/j.chemosphere.2017.02.010 SN - 0045-6535 SN - 1879-1298 IS - 174 SP - 572 EP - 584 PB - Elsevier AN - OPUS4-40235 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dümichen, Erik A1 - Eisentraut, Paul A1 - Bannick, Claus Gerhard A1 - Barthel, Anne-Kathrin A1 - Braun, Ulrike A1 - Senz, R. T1 - Fast identification of microplastics in complex environmental samples by a thermal degradation method N2 - n order to determine the relevance of microplastic particles in various environmental media, comprehensive investigations are needed. However, no analytical method exists for fast identification and quantification. At present, optical spectroscopy methods like IR and RAMAN imaging are used. Due to their time consuming procedures and uncertain extrapolation, reliable monitoring is difficult. For analyzing polymers Py-GC-MS is a standard method. However, due to a limited sample amount of about 0.5 mg it is not suited for analysis of complex sample mixtures like environmental samples. Therefore, we developed a new thermoanalytical method as a first step for identifying microplastics in environmental samples. A sample amount of about 20 mg, which assures the homogeneity of the sample, is subjected to complete thermal decomposition. The specific degradation products of the respective polymer are adsorbed on a solid-phase adsorber and subsequently analyzed by thermal desorption gas chromatography mass spectrometry. For certain identification, the specific degradation products for the respective polymer were selected first. Afterwards real environmental samples from the aquatic (three different rivers) and the terrestrial (bio gas plant) systems were screened for microplastics. Mainly polypropylene (PP), polyethylene (PE) and polystyrene (PS) were identified for the samples from the bio gas plant and PE and PS from the rivers. However, this was only the first step and quantification measurements will follow. KW - Thermal Degradation KW - Microplastic PY - 2017 DO - https://doi.org/10.1016/j.chemosphere.2017.02.010 VL - 174 SP - 572 EP - 584 PB - Elsevier Ltd. AN - OPUS4-42143 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wander, Lukas A1 - Vianello, A. A1 - Vollertsen, J. A1 - Westad, F. A1 - Braun, Ulrike A1 - Paul, Andrea T1 - Exploratory analysis of hyperspectral FTIR data obtained from environmental microplastics samples N2 - Hyperspectral imaging of environmental samples with infrared microscopes is one of the preferred methods to find and characterize microplastics. Particles can be quantified in terms of number, size and size distribution. Their shape can be studied and the substances can be identified. Interpretation of the collected spectra is a typical problem encountered during the analysis. The image datasets are large and contain spectra of countless particles of natural and synthetic origin. To supplement existing Analysis pipelines, exploratory multivariate data analysis was tested on two independent datasets. Dimensionality reduction with principal component analysis (PCA) and uniform manifold approximation and projection (UMAP) was used as a core concept. It allowed for improved visual accessibility of the data and created a chemical two-dimensional image of the sample. Spectra belonging to particles could be separated from blank spectra, reducing the amount of data significantly. Selected spectra were further studied, also applying PCA and UMAP. Groups of similar spectra were identified by cluster analysis using k-means, density based, and interactive manual clustering. Most clusters could be assigned to chemical species based on reference spectra. While the results support findings obtained with a ‘targeted analysis’ based on automated library search, exploratory analysis points the attention towards the group of unidientified spectra that remained and are otherwise easily overlooked. KW - Microplastics KW - FTIR KW - Exploratory analysis PY - 2020 DO - https://doi.org/10.1039/c9ay02483b VL - 12 IS - 6 SP - 781 EP - 791 PB - Royal Society of Chemistry AN - OPUS4-50396 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 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 - CONF A1 - Braun, Ulrike T1 - Entwicklung einer schnellen und robusten Methode für die Analytik von Mikroplastik in Wasser N2 - Vortrag im Rahmen der Preisverleihung zum Mülheimer Wasser Award 2018, Vorstellung der TED-GC-MS als Methode für Mikroplastik Analyse T2 - 3. Wasseranalytisches Seminar (MWAS 2018) CY - Mülheim a.d. Ruhr, Germany DA - 12.09.2018 KW - Mikroplastik KW - Analytik PY - 2018 AN - OPUS4-46459 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Eisentraut, Paul A1 - Kalbe, Ute A1 - Wachtendorf, Volker T1 - Elastomere und TPE – Gut für die Umwelt? – Kreislaufwirtschaft und Normung vereinen N2 - Der Vortrag fasst Projekte an der BAM mit Hinblick auf Elastomere und Umweltthemen zusammen. T2 - DIN Workshop: Elastomere und TPE – Gut für die Umwelt? – Kreislaufwirtschaft und Normung vereinen CY - Berlin, Germany DA - 08.08.2019 KW - Mikroplastik KW - Reifenabrieb KW - Sportböden PY - 2019 AN - OPUS4-49064 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Trappe, Volker A1 - Sturm, Heinz T1 - Einfluss der Feuchtigkeit auf die Schlichte von Glasfasern während der Lagerung T2 - DEWI-OCC CY - Bremen, Germany DA - 2014-05-20 PY - 2014 AN - OPUS4-30704 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Axel A1 - Becker, Roland A1 - Braun, Ulrike A1 - Dorgerloh, Ute T1 - Einfluss der Alterung auf das Sorptionsverhalten von Mikroplastik, eine Laborstudie mit BTEX und Etherverbindungen N2 - Die Präsenz von Mikroplastik in aquatischen Ökosystemen ist ein globales Problem und steht zunehmend im Fokus der Öffentlichkeit. In mehreren Studien konnten Anreicherungen hydrophober, organischer Schadstoffe an MP nachgewiesen werden. Der Einfluss des Alterungszustandes der MP-Partikel auf das Sorptionsverhalten von hydrophoben organischen Substanzen ist nicht hinreichend geklärt. Ziel der vorliegenden Arbeit war die Untersuchung des Sorptionsverhaltens von Schadstoffen mit Bedeutung für limnische Gewässer an künstlich gealterten Partikeln relevanter Polymere. Das Modell verwendete die Aromaten Benzol, Toluol, Ethylbenzol und Xylol (BTEX) sowie Etherverbindungen. Diese Substanzen sind oder waren Bestandteile in unterschiedlichen Kraftstoffen und finden sich daher in vielen aquatischen Ökosystemen weltweit. Als Sorbentien kamen teilkristallines Polypropylen (PP) und amorphes Polystyrol (PS) in Form von Industriepellets zum Einsatz. Die Pellets wurden jeweils sowohl unbehandelt als auch mittels UV-Bestrahlung künstlich gealtert verwendet und mikroskopisch sowie mittels XPS, FTIR und DSC charakterisiert. Die Alterung führte bei PS zu einer verringerten Sorptionskapazität, während bei PP keine Veränderung im Sorptionsverhalten beobachtet wurde. T2 - Wasser 2017 - Jahrestagung der Wasserchemischen Gesellschaft CY - Donaueschingen, Germany DA - 22.05.2017 KW - Mikroplastik KW - Organische Schadstoffe KW - Sorption KW - Polypropylen Polystyrol PY - 2017 SN - 978-3-947197-01-9 SP - 1 EP - 606 PB - Gesellschaft Dt. Chemiker AN - OPUS4-40447 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Perez, R.M. A1 - Sandler, J.K.W. A1 - Altstädt, V. A1 - Hoffmann, T. A1 - Pospiech, D. A1 - Ciesielski, M. A1 - Döring, M. A1 - Braun, Ulrike A1 - Knoll, Uta A1 - Schartel, Bernhard T1 - Effective halogen-free flame retardants for carbon fibre-reinforced epoxy composites N2 - DOPO-based flame retardants with tailored chemical structures are proposed for carbon fibre reinforced epoxy composites. Critical properties related to the fracture toughness are maintained, effectively allowing the use of such compounds in composites for demanding applications. KW - Fire retardancy KW - DOPO KW - Epoxy resin KW - LOI KW - UL94 PY - 2006 DO - https://doi.org/10.1007/s10853-006-0134-4 SN - 0022-2461 SN - 1573-4803 VL - 41 IS - 15 SP - 4981 EP - 4984 PB - Springer Science + Business Media B.V. CY - New York, USA AN - OPUS4-12641 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -