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 - Dittmann, Daniel A1 - Lucke, T. A1 - Ruhl, A. S. A1 - Winzenbacher, R. A1 - Jekel, M. A1 - Braun, Ulrike T1 - Untersuchungen zu biologischen, organischen und anorganischen Veränderungen granulierter Aktivkohlen während der Trinkwasseraufbereitung N2 - Untersuchungen zu biologischen, organischen und anorganischen Veränderungen granulierter Aktivkohlen während der Trinkwasseraufbereitung des Landeswasserversorgers Langenau. KW - Thermogravimetrie KW - Trinkwasser KW - Wasseraufbereitung KW - Aktivkohle PY - 2020 SN - 0083-6915 VL - 118 IS - 2 SP - 47 EP - 50 PB - Wiley-VCH Verlag GmbH & Co. KGaA AN - OPUS4-51434 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Analytical opportunities & Challenges in (ocean) microplastics N2 - An overview about the analytical opportunities and challenges in microplastic detection is given. T2 - ISO TC61/ Annual bioplastics & ocean microplastics symposium CY - Chengdu, People's Republic of China DA - 29.09.2019 KW - Harmonisation KW - Microplastics KW - TED-GC-MS PY - 2019 AN - OPUS4-50000 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Mikroplastik als analytische Herausforderung N2 - Der Wissenstand zum Thema Mikroplastik und Harmonisierung wird dargestellt. T2 - Laborleitertreffen Futtermittelmonitoring CY - Bonn, Germany DA - 21.11.2019 KW - Hamonisierung KW - Mikroplastik KW - TED-GC-MS PY - 2019 AN - OPUS4-50001 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Analytic of microplastics in environmental samples N2 - An overview about the existing possibilities for mircoplastic analysis is given. T2 - 2nd International Symposium on Microplastics CY - Seoul, Korea DA - 02.12.2019 KW - Harmonisation KW - Microplastics KW - TED-GC-MS PY - 2019 AN - OPUS4-50003 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Bannick, C.G. T1 - Analytik von Mikroplastik in komplexen Umweltproben N2 - Der Sachstand zur Analytik von Mikroplastik in Umweltproben wird dargestellt. T2 - Fachausstellung Kunststoffanalytik CY - Lüdenscheid, Germany DA - 04.12.2019 KW - TED-GC-MS KW - Mikroplastik KW - Analytik PY - 2019 AN - OPUS4-50005 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Messen ist nicht alles, aber ohne Messmethoden ist alles nichts! N2 - Es wir der Wissenstand zur Analytik von Mikroplastik dargestellt, sowie die Notwendigkeit der Hamonisierung der Verfahren. T2 - Jahrestagung der deutschen Labordienstleistungsbranche CY - Gießen, Berlin DA - 05.09.2019 KW - TED-GC-MS KW - Mikroplastik KW - Analytik PY - 2019 AN - OPUS4-49994 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Bannick, C.G. T1 - Analytik von Mikroplastik - Verfahren-Ergebnisse-Harmonisierung N2 - Die zunehmenden Nachweise von Kunststoffen in verschiedenen Umweltmedien erfahren in den letzten Jahren weltweit ein zunehmendes wissenschaftliches, gesellschaftliches und politisches Interesse. Besondere Aufmerksamkeit erfahren Kunststoffpartikel von 1-1.000 µm sogenanntes Mikroplastik. Es wurde mittlerweile in Wasser, Böden, Luft und Biota nachgewiesen. Obwohl die Wirkungen auf die natürlichen Umweltfunktionen noch unklar sind und kontrovers diskutiert werden, ist allein durch die ubiquitäre Präsenz eine systematische Erfassung von Eintragsquellen und Verbleib der Partikel über alle Umweltmedien notwendig, um Maßnahmen zur Reduktion der Einträge zu veranlassen. Für eine zuverlässige Erfassung sind medienübergreifende Verfahren zu entwickeln, welche die drei analytischen Schritte, Probennahme, Probenaufbereitung und Detektion beinhalten. Die Verfahren adressieren unterschiedliche Zielgruppen, welche verschiedene analytische Informationen fordern. Für die akademische Bewertung werden Verfahren mit hohem analytischen Aufwand favorisiert, welche möglichst detaillierte Information über Partikelsorte, -größe, -zahl und -oberflächenbeschaffenheit geben. Im Gegensatz dazu, fordern Anwender aus der Praxis schnelle und einfache Monitoring Verfahren, welche die Bestimmung eines Massengehaltes, bzw. eines Grenzwertes zulassen. Allen ist gemeinsam, dass ein hoher interdisziplinärer Anspruch besteht, der sowohl technische Voraussetzungen zur repräsentativen Probennahme und die Limitationen von Detektionsverfahren berücksichtigt, als auch die Fachkompetenz von Biologen, Umweltwissenschaften, Analytiker und Polymerwissenschaftler einschließt. Verfahren zum Mikroplastiknachweis müssen auch verschieden Proben mit sehr unterschiedlichen Gehalten an natürlicher Matrix gerecht werden. So müssen allein für Wasser Verfahren entwickelt werden, die Mikroplastik verschiedener Form (sphärische Partikel, komplexe Bruchstücke, Fasern) aus Medien mit sehr variablen Partikelanteil (u.a. Trinkwasser, Oberflächenwasser, Abwasser) repräsentativ erfassen sowie schnell und kostengünstig sind – einschließlich der notwendigen Probenaufbereitung. Die jeweiligen Detektionsverfahren müssen z.B. einzelne Partikel oder integrale Gehalte über drei Dekadenklassen für thermoplastische und insbesondere auch elastomere Partikelsorten erfassen können. T2 - GDCh Wissenschaftsforum Chemie CY - Aachen, Germany DA - 15.09.2019 KW - TED-GC-MS KW - Mikroplastik KW - Analytik PY - 2019 AN - OPUS4-49995 LA - deu 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 - CONF A1 - Braun, Ulrike T1 - Microplastics: Degradation properties of polymers in the environment N2 - The accumulation of plastics leaked into the environment achieve a high perception in the last years. It is uncontroversial that often an uncontrolled, high consumption of plastic products and a poor waste management resulted in plastic findings all over in the environment. However, less is known about the relevant pathways and fate of plastic in the environment. Especially plastic fragments smaller 5 mmm, so called microplastics, achieve a high attention, because their amount and risks arising from these fragments are still unknown. The basic mechanisms of plastic or more precise, of different polymer degradation processes are often not considered, resulting in unrealistic statements. For generation of fundamental understanding of this problem we developed in the last years a fast thermoanalytical method for identification and mass quantification of microplastics in complex samples. The presentation will also give a short introduction about polymer degradation. T2 - Environmental Geosciences Seminar CY - Vienna, Austria DA - 19.11.2018 KW - Microplastic KW - Analysis KW - Standardisation PY - 2018 AN - OPUS4-47182 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 - JOUR A1 - Unger, R. A1 - Braun, Ulrike A1 - Fankhänel, J. A1 - Daum, B. A1 - Arash, B. A1 - Rolfes, R. T1 - Molecular modelling of epoxy resin crosslinking experimentally validated by near-infrared spectroscopy N2 - Reliable simulation of polymers on an atomistic length scale requires a realistic representation of the cured material. A molecular modelling method for the curing of epoxy systems is presented, which is developed with respect to efficiency while maintaining a well equilibrated system. The main criterion for bond formation is the distance between reactive groups and no specific reaction probability is prescribed. The molecular modelling is studied for three different mixing ratios with respect to the curing evolution of reactive Groups and the final curing stage. For the first time, the evolution of reactive groups during the curing process predicted by the molecular modelling is validated with near-infrared spectroscopy data, showing a good agreement between simulation results and experimental measurements. With the proposed method, deeper insights into the curing mechanism of epoxy systems can be gained and it allows us to provide reliable input data for molecular Dynamics simulations of material properties. KW - Epoxy KW - NIR spectroscopy KW - Modelling PY - 2019 DO - https://doi.org/10.1016/j.commatsci.2019.01.054 SN - 0927-0256 VL - 161 SP - 223 EP - 235 PB - Elsevier AN - OPUS4-47431 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klöckner, P. A1 - Reemtsma, T. A1 - Eisentraut, Paul A1 - Braun, Ulrike A1 - Ruhl, A. S. A1 - Wagner, S. T1 - Tire and road wear particles in road environment e Quantification and assessment of particle dynamics by Zn determination after density separation N2 - In this study, a method for the determination of tire and road wear particle (TRWP) contents in particulate samples from road Environment was developed. Zn was identified as the most suitable elemental marker for TRWP, due to its high concentration in tire tread and the possibility of separation from other Zn sources. The mean concentration of 21 tire samples was 8.7 ± 2.0 mg Zn/g. Before quantification in samples from road environment, TRWP were separated from the particulate matrix by density separation. Method development was conducted using shredded tread particles (TP) as a surrogate for TRWP. Recovery of TP from spiked sediment was 95 ± 17% in a concentration range of 2 - 200 mg TP/g. TP determination was not affected by other Zn containing solids or spiked Zn-salts. By adjusting the density of the separation solution to 1.9 g/cm3, more than 90% of total TRWP were separated from the sample matrix. TRWP concentrations in particulate matter collected in two road runoff treatment Systems ranged from 0.38 to 150 mg TRWP/g. Differences in quantified TRWP contents of the two Systems indicate changes in particle dynamics due to ageing and aggregation processes. The developed method allows TRWP determination in road runoff and in environments that are influenced by road traffic. The validated separation procedure can also be applied for TRWP characterization in future studies. KW - Zinc analysis KW - Microplastics KW - Tire particles PY - 2019 VL - 222 SP - 714 EP - 721 PB - Elsevier AN - OPUS4-47433 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wesch, Ch. A1 - Elert, Anna Maria A1 - Wörner, M. A1 - Braun, Ulrike A1 - Klein, R. A1 - Paulus, M. T1 - Assuring quality in microplastic monitoring: About the value of clean-air devices as essentials for verified data N2 - Avoiding aerial microfibre contamination of environmental samples is essential for reliable analyses when it comes to the detection of ubiquitous microplastics. Almost all laboratories have contamination problems which are largely unavoidable without investments in clean-air devices. Therefore, our study supplies an approach to assess background microfibre contamination of samples in the laboratory under particle-free air conditions. We tested aerial contamination of samples indoor, in a mobile laboratory, within a laboratory fume hood and on a clean bench with particles filtration during the examining process of a fish. The used clean bench reduced aerial microfibre contamination in our laboratory by 96.5%. This highlights the value of suitable clean-air devices for valid microplastic pollution data. Our results indicate, that pollution levels by microfibres have been overestimated and actual pollution levels may be many times lower. Accordingly, such clean-air devices are recommended for microplastic laboratory applications in future research work to significantly lower error rate KW - Microplastics KW - FTIR KW - Quality KW - Environmental Science KW - Biological techniques PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-412402 DO - https://doi.org/10.1038/s41598-017-05838-4 SN - 2045-2322 VL - 7 SP - Article 5424, 1 EP - 8 PB - Nature AN - OPUS4-41240 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kömmling, Anja A1 - Chatzigiannakis, E. A1 - Beckmann, Jörg A1 - Wachtendorf, Volker A1 - von der Ehe, Kerstin A1 - Braun, Ulrike A1 - Jaunich, Matthias A1 - Schade, U. A1 - Wolff, Dietmar T1 - Discoloration Effects of High-Dose gamma-Irradiation and Long-Term Thermal Aging of (U) HMW-PE N2 - Two polyethylene types with ultra-high (UHMWPE) and high molecular weight (HMW-PE) used as neutron radiation shielding materials in casks for radioactive waste were irradiated with doses up to 600 kGy using a 60Co gammasource. Subsequently, thermal aging at 125∘C was applied for up to one year. Degradation effects in the materials were characterized using colorimetry, UV-Visspectroscopy, IR spectroscopy, and DSC. Both materials exhibited a yellowing upon irradiation.The discoloration of UHMW-PE disappeared again after thermal aging.Therefore, the yellowing is assumed to originate fromannealable color centers in the formof free radicals that are trapped in the crystalline regions of the polymer and recombine at elevated temperatures. For the antioxidantcontaining HMWPE, yellowing was observed after both irradiation and thermal aging. The color change was correlated mainly to decomposition products of the antioxidant in addition to trapped radicals as in UHMW-PE. Additionally, black spots appeared after thermal aging of HMW-PE. KW - Irradiation KW - UHMWPE KW - Colour center KW - Yellowness index PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-423992 DO - https://doi.org/10.1155/2017/1362491 SN - 1687-9422 VL - 2017 IS - Article ID 1362491 SP - 1 EP - 10 PB - Hindawi AN - OPUS4-42399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Dümichen, Erik A1 - Eisentraut, Paul T1 - Schneller Nachweis von Mikroplastik Partikeln in Umweltproben mit TED-GC-MS N2 - Der Vortrag stellt die neue entwickelte Analyse "TED-GC-MS" vor im Zusammenhang mit der Anwendung zur Mikroplastik Detektion. T2 - Gerstel Anwendertreffen CY - Mülheim/Ruhr, Germany DA - 05.10.2017 KW - Thermische Analyse KW - Mikroplastik KW - Analytik KW - GC-MS PY - 2017 AN - OPUS4-42415 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Principles for the development of standards for investigation procedures of plastics in environmental media and materials N2 - An overview about the current status of microplastic analysis is given with scope on hamonisation and standarisation. T2 - Annual ISO/TC 61 Meeting CY - Saitama, Japan DA - 24.09.2018 KW - Standardisation KW - Microplastic KW - Analysis PY - 2018 AN - OPUS4-46457 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 - JOUR A1 - Eisentraut, Paul A1 - Dümichen, Erik A1 - Ruhl, A. A1 - Jekel, M. A1 - Albrecht, M. A1 - Gehde, M. A1 - Braun, Ulrike T1 - Two Birds with One Stone-Fast and Simultaneous Analysis of Microplastics: Microparticles Derived from Thermoplastics and Tire Wear N2 - Analysis of microplastic particles (MP) in environmental samples needs sophisticated techniques and is time intensive due to sample preparation and detection. An alternative to the most common (micro ) spectroscopic techniques, FTIR or Raman spectroscopy, are the thermoanalytical methods, where specific decomposition products can be analyzed as marker compounds for different kind of plastics types and mass contents. Thermal extraction desorption gas chromatography mass spectrometry (TED-GC-MS) allows the fast identification and quantification of MP in environmental samples without sample preparation. Whereas up to now only the analysis of thermoplastic polymers was realized, this is the first time that even the analysis of tire wear (TW) content in environmental samples is possible. Various marker compounds for TW were identified. They include characteristic decomposition products of elastomers, antioxidants and vulcanization agents. Advantages and drawbacks of these marker substances were evaluated. Environmental samples from street run off were exemplarily investigated and presented. KW - TED-GC-MS KW - Microplastic KW - Tire wear PY - 2018 DO - https://doi.org/10.1021/acs.estlett.8b00446 VL - 5 IS - 10 SP - 608 EP - 613 PB - American Chemical Society AN - OPUS4-46460 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 - Deußing, G. A1 - Dümichen, Erik A1 - Braun, Ulrike T1 - Polymeranalytik Intelligent kombiniert N2 - Durch die intelligente Anbindung an die Stir Bar Sorptive Extraction (SBSE) lassen sich Zersetzungsprodukte der thermogravimetrischen Analyse (TGA) von Polymeren auf effiziente Weise anreichern, auftrennen und mittels GC/MS identifizieren. KW - Thermische Degradation KW - Mikroplastik PY - 2016 UR - http://www.gerstel.cn/de/GA51_Polymeranalytik.htm IS - 51 SP - 9 EP - 11 PB - Gerstel AN - OPUS4-42146 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Deußing, G. A1 - Dümichen, Erik A1 - Braun, Ulrike T1 - Der Fänger im Spülgas N2 - Durch die intelligente Anbindung an eine in der GC/MS gängige Extraktionstechnik (SBSE) lassen sich Zersetzungsprodukte der thermogravimetrischen Analyse (TGA) von Polymeren auf effiziente Weise anreichern, anschließend trennen und sicher identifizieren. KW - Polymeranalytik KW - Thermische Extraktion PY - 2015 UR - http://www.laborpraxis.vogel.de/so-erweitern-sie-die-moeglichkeiten-der-tga-a-490995/index2.html UR - https://files.vogel.de/vogelonline/vogelonline/issues/6773.pdf SN - 0344-1733 VL - 39 IS - 6 SP - 24 EP - 27 PB - Vogel Business Media AN - OPUS4-42149 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dümichen, Erik A1 - Eisentraut, Paul A1 - Braun, Ulrike T1 - Polymere und Mikroplastik in der Umwelt N2 - Es wird ein neues und voll automatisiertes Verfahren vorgestellt für die Analyse von Mikroplastik in der Umwelt. KW - Mikroplastik KW - TED PY - 2017 SN - 0016-3538 VL - 61 IS - 9 SP - 24 EP - 27 PB - Wiley AN - OPUS4-42170 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - About Standardization and Analytics of Microplastics N2 - Presentation about national and international standardization of microplastic analysis, as well as the project RUSEKU T2 - Industrievereinigung Chemiefaser e.V. CY - Frankfurt, Germany DA - 26.02.2019 KW - Standardisation KW - Microplastic KW - Analysis PY - 2019 AN - OPUS4-47577 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Mikroplastik in der Umwelt und im Trinkwasser: Einordnung der Relevanz und der Methodik N2 - Überblick zur Thematik Mikroplastik mit speziellem Fokus auf Trinkwasser T2 - 20. Jahrestagung Trinkwasserringversuche Nordrhein-Westfalen – Niedersachsen CY - Osnabrück, Germany DA - 06.03.2019 KW - Trinkwasser KW - Umwelt KW - Mikroplastik PY - 2019 AN - OPUS4-47578 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Müller, Axel A1 - Grathwohl, P. A1 - Vogler, M. A1 - Scholz, K. T1 - Plastik im Boden, Aktueller Forschungsstand N2 - Der Vortrag gibt einen Überblick über ein laufendes Vorhaben zum Thema Mikroplastik in Böden. T2 - NUA-Veranstaltung "Plastik in Natur und Umwelt" CY - Münster, Germany DA - 08.03.2019 KW - Mikroplastik KW - Böden KW - Analytik PY - 2019 AN - OPUS4-47579 LA - deu 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 - CONF A1 - Braun, Ulrike A1 - Eisentraut, Paul A1 - Dümichen, E. T1 - Analytik von Mikroplastik mittels Thermoextraktion Desorption Gas Chromatographie Massen Spektrometrie (TED-GC-MS): Nun auch die Luft? N2 - Der Vortrag gibt eine Überblick über die Messung von Mikroplastik mittels TED-GC-MS mit speziellem Fokus auf Luftgetragene Partikel T2 - Odour and Emissions of Plastic Materials CY - Kassel, Germany DA - 19.03.2019 KW - Mikroplastik KW - Standarisierung KW - Analytik PY - 2019 AN - OPUS4-47583 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Repräsentative Untersuchungsstrategien für ein integratives Systemverständnis von spezifischen Einträgen von Kunststoffen in die Umwelt (RUSEKU) N2 - Im Rahmen des Statuskonferenz der BMBF Fördermassnahme wurde über den Projektfortschritt berichtet. T2 - Statusfonferenz der BMBF Fördermassnahme "Plastik in der Umwelt" CY - Berlin, Germany DA - 09.04.2019 KW - Sedimenttaionskasten KW - Probenahme KW - Mikroplastik KW - TED-GC-MS PY - 2019 AN - OPUS4-47796 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Mikroplastik Analytik: Probennahme, Probenaufbereitung, Detektionsverfahren N2 - Das Diskussionspapier zur Mikroplastik Analytik wurde vorgestellt. Es entstand im Rahmen des Querschnitthemas 1 des BMBF Forschungsschwerpunktes Plastik in der Umwelt. T2 - Statuskonferenz der BMBF Fördermassnahme "Plastik in der Umwelt" CY - Berlin, Germany DA - 09.04.2019 KW - Harmonisierung KW - Mikroplastik KW - Probenahme KW - Detektion KW - Aufbereitung PY - 2019 AN - OPUS4-47797 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wander, Lukas A1 - Lommel, Lukas A1 - Meyer, Klas A1 - Braun, Ulrike A1 - Paul, Andrea T1 - Development of a low-cost method for quantifying microplastics in soils and compost using near-infrared spectroscopy N2 - Near-infrared (NIR) spectroscopy is a promising candidate for low-cost, nondestructive, and high-throughput mass quantification of micro¬plastics in environmental samples. Widespread application of the technique is currently hampered mainly by the low sensitivity of NIR spectroscopy compared to thermo-analytical approaches commonly used for this type of analysis. This study shows how the application of NIR spectroscopy for mass quantification of microplastics can be extended to smaller analyte levels by combining it with a simple and rapid microplastic enrichment protocol. For this purpose, the widely used flotation of microplastics in a NaCl solution, accelerated by centrifugation, was chosen which allowed to remove up to 99 % of the matrix at recovery rates of 83–104 %. The spectroscopic measurements took place directly on the stainless-steel filters used to collect the extracted particles to reduce sample handling to a minimum. Partial least squares regression (PLSR) models were used to identify and quantify the extracted microplastics in the mass range of 1–10 mg. The simple and fast extraction procedure was systematically optimized to meet the requirements for the quantification of microplastics from common PE-, PP-, and PS-based packaging materials with a particle size < 1 mm found in compost or soils with high natural organic matter content (> 10 % determined by loss on ignition). Microplastics could be detected in model samples at a mass fraction of 1 mg g-1. The detectable microplastic mass fraction is about an order of magnitude lower compared to previous studies using NIR spectroscopy without additional enrichment. To emphasize the cost-effectiveness of the method, it was implemented using some of the cheapest and most compact NIR spectrometers available. KW - NIR KW - Soil KW - compost KW - PLSR PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546405 DO - https://doi.org/10.1088/1361-6501/ac5e5f SN - 0957-0233 VL - 33 IS - 7 SP - 075801 EP - 075814 PB - IOP Publishing Ltd. CY - UK AN - OPUS4-54640 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kittner, Maria A1 - Eisentraut, Paul A1 - Dittmann, Daniel A1 - Braun, Ulrike T1 - Decomposability versus detectability: First validation of TED‐GC/MS for microplastic detection in different environmental matrices N2 - A fast method for microplastic detection is thermal extraction desorption‐gas chromatography/mass spectrometry (TED‐GC/MS), which uses polymer‐specific thermal decomposition products as marker compounds to determine polymer mass contents in environmental samples. So far, matrix impacts of different environmental matrices on TED‐GC/MS performance had not yet been assessed systematically. Therefore, three solid freshwater matrices representing different aquatic bodies with varying organic matter contents were spiked with a total of eight polymers. Additionally, for the first time, the two biodegradable polymers polybutylene adipate terephthalate (PBAT) and polylactide (PLA) were analysed using TED‐GC/MS. The methodological focus of this work was on detectability, quality of signal formation as well as realisation of quantification procedures and determination of the limit of detection (LOD) values. Overall, TED‐GC/MS allowed the unambiguous detection of the environmentally most relevant polymers analysed, even at low mass contents: 0.02 wt% for polystyrene (PS), 0.04 wt% for the tyre component styrene butadiene rubber (SBR) and 0.2 wt% for polypropylene (PP), polyethylene (PE) and PBAT. Further, all obtained LOD values were increased in all matrices compared to the neat polymer without matrix. The LOD of the standard polymers were increased similarly (PS: 0.21–0.34 μg, SBR: 0.27–0.38 μg, PP: 0.32–0.36 μg, PMMA: 0.64–1.30 μg, PET: 0.90–1.37 μg, PE: 3.80–6.99 μg) and their decompositions by radical scission processes were not significantly influenced by the matrices. In contrast, matrixspecific LOD increases of both biodegradable polymers PBAT (LOD: 1.41–7.18 μg) and PLA (0.84–20.46 μg) were observed, probably due to their hetero‐functional character and interactions with the matrices. In conclusion, the TED‐GC/MS performance is not solely determined by the type of the polymers but also by the composition of the matrix. KW - TED-GC/MS KW - Microplastic KW - Freshwater matrices KW - Gas chromatography KW - Mass spectrometry PY - 2023 DO - https://doi.org/10.1002/appl.202200089 SN - 2702-4288 VL - 2 IS - 3 SP - 1 EP - 12 PB - Wiley-VCH CY - Weinheim AN - OPUS4-57419 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Braun, Ulrike A1 - Eisentraut, Paul A1 - Altmann, Korinna A1 - Kittner, Maria A1 - Dümichen, Erik A1 - Thaxton, K. A1 - Kleine-Benne, E. A1 - Anumol, T. T1 - Accelerated Determination of Microplastics in Environmental Samples Using Thermal Extraction Desorption-Gas Chromatography/Mass Spectrometry (TED-GC/MS) N2 - There is growing interest in quantifying microplastics in environmental samples. This application note presents a thermal extraction desorption-gas chromatography/mass spectrometry (TED-GC/MS) method that is well suited to automation and increased sample throughput. The method is also able to detect all particle sizes in the sample as long as the limit of detection (LOD) is reached and allows analysis of larger samples of 15 to 25 mg or more. Samples were decomposed by thermogravimetric analysis (TGA), and the gaseous decomposition products were trapped on a solid-phase sorbent, followed by thermal desorption‑gas chromatography/mass spectrometry (TD-GC/MS) using an Agilent 5977B GC/MSD coupled to an Agilent 7890B GC. Target microplastic particle (MP) polymers were identified in environmental samples including surface water, finished compost, house dust, and drinking water. Quantification of MP polymers in environmental samples provided LODs of 0.06 to 2.2 μg, allowing the detection of MPs in trace amounts with sample weights of up to 1 g. Method repeatability was adequate for reliable quantification with RSDs of approximately 6 to 12%. KW - Environment KW - Microplastic particles KW - TED-GC/MS KW - Mass content KW - Thermoanalytical PY - 2020 VL - 2020 SP - 1 EP - 8 PB - Agilent Technologies Inc. CY - USA AN - OPUS4-51672 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Altmann, Korinna A1 - Braun, Ulrike A1 - Bannick, C.-G. A1 - Bednarz, M. A1 - Herper, D. A1 - Knefel, M. T1 - TED-GC/MS: Schnelle Bestimmung von Mikroplastik-Massegehalten in verschiedenen Proben N2 - Zur Ermittlung von Mikroplastik-Gehalten in verschiedenen Umweltmatrices ist ein schnelles Detektionsverfahren für die Routineanalytik notwendig. Ein solches Verfahren wird hier in Form der ThermoExtraktion/Desorption-GasChromatographie/ MassenSpektroskopie (TED-GC/MS) vorgestellt. Neben grundlegenden verfahrensspezifischen Erläuterungen zur Identifizierung und Quantifizierung von Mikroplastik werden auch exemplarische Beispiele aus unterschiedlichen Umweltkompartimenten und Produkten dargestellt. Neu vorgestellt wird ein neues Verfahren zur Analytik von Flaschenwasser. Dazu wurde ein Messfiltertiegel entwickelt, der besonders für Proben mit geringen Gehalten an abfiltrierbaren Stoffen geeignet ist KW - Mikroplasik KW - Mikroplastik-Analyse KW - TED-GC/MS KW - Thermoanalytische Verfahren KW - Mikroplastik-Massengehalte PY - 2020 VL - 2020 IS - 02 SP - 55 EP - 57 PB - Gesellschaft Deutscher Chemiker (GDCh) CY - Frankfurt am Main AN - OPUS4-50835 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Braun, Ulrike A1 - Bannick, C.G. A1 - Szewzyk, R. A1 - Ricking, M. A1 - Schniegler, S. A1 - Obermaier, N. A1 - Barthel, A. K. A1 - Altmann, Korinna A1 - Eisentraut, Paul T1 - Development and testing of a fractionated filtration for sampling of microplastics in water N2 - A harmonization of sampling, sample preparation and detection is pivotal in order to obtain comparable data on microplastics (MP) in the environment. This paper develops and proposes a suitable sampling concept for waterbodies that considers different plastic specific properties and influencing factors in the environment. Both artificial water including defined MP fractions and the discharge of a wastewater treatment plant were used to verify the derived sampling procedure, sample preparation and the subsequent analysis of MP using thermal extraction-desorption gas chromatography - mass spectrometry (TED-GC-MS). A major finding of this paper is that an application of various particle size classes greatly improves the practical handling of the sampling equipment. Size classes also enable the TED-GC-MS to provide any data on the MP size distribution, a substantial sampling property affecting both the necessary sampling volume and the optimal sampling depth. In the artificial water with defined MP fractions, the recovery rates ranged from 80 to 110%, depending on the different MP types and MP size classes. In the treated wastewater, we found both Polyethylene and polystyrene in different size classes and quantities. KW - Microplastics KW - Sampling KW - Sampling techniques KW - Water PY - 2019 DO - https://doi.org/10.1016/j.watres.2018.10.045 SN - 0043-1354 VL - 149 SP - 650 EP - 658 PB - Elsevier AN - OPUS4-47200 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wander, Lukas A1 - Lommel, Lukas A1 - Braun, Ulrike A1 - Meyer, Klas A1 - Paul, Andrea T1 - Development of a Low-Cost Method for Quantifying Microplastics in Soils and Compost Using Near-Infrared Spectroscopy N2 - Near-infrared (NIR) spectroscopy is a promising candidate for low-cost, nondestructive, and highthroughput mass quantification of microplastics in environmental samples. Widespread application of the technique is currently hampered mainly by the low sensitivity of NIR spectroscopy compared to thermoanalytical approaches commonly used for this type of analysis. This study shows how the application of NIR spectroscopy for mass quantification of microplastics can be extended to smaller analyte levels by combining it with a simple and rapid microplastic enrichment protocol. For this purpose, the widely used flotation of microplastics in a NaCl solution, accelerated by centrifugation, was chosen which allowed to remove up to 99 % of the matrix at recovery rates of 83–104 %. The spectroscopic measurements took place directly on the stainless-steel filters used to collect the extracted particles to reduce sample handling to a minimum. Partial least squares regression (PLSR) models were used to identify and quantify the extracted microplastics in the mass range of 1–10 mg. The simple and fast extraction procedure was systematically optimized to meet the requirements for the quantification of microplastics from common PE-, PP-, and PS-based packaging materials with a particle size < 1 mm found in compost or soils with high natural organic matter content (> 10 % determined by loss on ignition). Microplastics could be detected in model samples at a mass fraction of 1 mg g-1. The detectable microplastic mass fraction is about an order of magnitude lower compared to previous studies using NIR spectroscopy without additional enrichment. To emphasize the cost-effectiveness of the method, it was implemented using some of the cheapest and most compact NIR spectrometers available. KW - Mikroplastik KW - NIR KW - Sensor KW - Kompost KW - Multivariat PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552605 DO - https://doi.org/10.1088/1361-6501/ac5e5f VL - 33 IS - 7 SP - 1 EP - 13 PB - IOP Publishing Ltd. CY - Bristol AN - OPUS4-55260 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eitzen, L. A1 - Paul, S. A1 - Braun, Ulrike A1 - Altmann, Korinna A1 - Jekel, M. A1 - Ruhl, A. T1 - The challenge in preparing particle suspensions for aquatic microplastic research N2 - The occurrence of small particles consisting of organic polymers, so-called microplastic (MP), in aquatic Environments attracts increasing interest in both public and science. Recent sampling campaigns in surface Waters revealed substantial numbers of particles in the size range from a few micrometers to a few millimeters. In order to validate sample preparation, identification and quantification and to investigate the behavior of MP particles and potential toxic effects on organisms, defined MP model particles are needed. Many studies use spherical compounds that probably behave differently compared to irregularly shaped MP found in environmental samples. However, preparation and handling of MP particles are challenging tasks and have been systematically investigated in the present study. Polystyrene (PS) as a commonly found polymer with a density slightly above that of water was selected as polymer type for milling and fractionation studies. A cryogenic ball mill proved to be practical and effective to produce particles in the size range from 1 to 200 μm. The yield of small particles increased with increasing pre-cooling and milling durations. Depending on the concentration and the size, PS particles do not completely disperse in water and particles partly creep vertically up along glass walls. Stabilized MP suspensions without use of surfactants that might harm organisms are needed for toxicological studies. The stabilization of PS particle suspensions with ozone treatment reduced the wall effect and increased the number of dispersed PS particles but increased the dissolved organic carbon concentration and changed the size Distribution of the particles. KW - Reference material KW - Microplastic PY - 2018 DO - https://doi.org/10.1016/j.envres.2018.09.008 SN - 0013-9351 SN - 1096-0953 VL - 168 SP - 490 EP - 495 PB - Elsevier AN - OPUS4-46462 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Altmann, Korinna A1 - Eisentraut, Paul A1 - Ricking, M. A1 - Reiche, M. A1 - Barthel, A.-K. A1 - Bannick, C. G. T1 - New sampling strategies for optimised microplastic analysis in surface waters N2 - The occurrence of microplastic particles (MP) in nearly each environmental compartment but especially in water is well documented in an increasing amount of publication within the last few years. However, a comprehensive understanding of MP occurrence, sources and pathways in the environment as well as effects of MP on the environment is still unclear. Many of the studies are not compatible, because they used different sampling, sample preparation and detection techniques, resulting in a very broad variation and very different dimension of archived results. Hence a useful avoiding strategy for reduction the MP entry in the environment is not possible. Furthermore, the existing methods are often very time consuming, need user knowledge and labour force, which is often not acceptable for the routine monitoring of an action or sanction. The call for harmonised methods become loud and louder and promising efforts are done in this area. However, the scientific discussion is often focus on advantages and disadvantages of detection tools and sample preparation, less initiative is given to the sampling strategy. That is a pity, because every environmental scientist knows, a good analytical result depend on a good sampling strategy. The sampling of water seems on the first view easy because the sampling process include already an up concentration of the MP by means of sieves and filters. However, this filtering of water is often limited by filter cake on the sieves, consisting of high amount of natural particular matter. Hence often a small water volume is filtered, which will not own a representative amount of trait carriers or complex sieves cascades are used, which need a high technical equipment. Recently we presented a fast thermoanalytical method for the detection of polymers fractions in water samples. This method, thermo-extraction desorption gas chromatography mass spectrometry (TED-GC-MS) can analyse MP in water filtrates without sample preparations within 2-3 hours. Advantageous is the additional analysis of rubber particles from tires beside the MP. In order to come even faster we now start to develop new sampling strategies, which should be use for different water systems. It is intended to reduce the effort in the field and to elongate times for sampling to obtain a representatives result without random effects. In the present presentation we will show first result using a sedimentation box for sampling of MP from surface water. Advantages and disadvantages will be discussed and comparison to data from conventional fractionated filtration will be given. T2 - SETAC CY - Helsinki, Finland DA - 26.05.2019 KW - Microplastics KW - Sampling KW - Sampling techniques KW - Water PY - 2019 AN - OPUS4-48118 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Altmann, Korinna A1 - Herper, D. A1 - Knefel, M. A1 - Bednarz, M. A1 - Bannick, C. G. T1 - Detektion von Mikroplastik in Flaschenwasser mittels thermoanalytischer Verfahren N2 - Im Vortrag wird ein Messfiltertiegel als Zusatztool für die TED-GC/MS vorgestellt, welcher für die Probenaufbereitung von kleinen Partikelfrachten oder kleinen Partikelgrößen genutzt werden kann. Er ist Filtereinheit und Messtiegel in einem, wodurch Verluste bei der Überführung der Probe in das Messgefäß sowie Kontaminationen vermindert werden. Das beispiel ist hier die Filtration von Flaschenwasser mit anschließender Detektion mit der TED-GC/MS. T2 - BVL_Kick-off Meeting "Mikroplastik in Lebensmitteln" CY - Online meeting DA - 03.12.2020 KW - Mikroplastik KW - TED-GC/MS KW - Kleine Partikel KW - Geringe Partikelfrachten KW - Mikroplastik-Massengehalte PY - 2020 AN - OPUS4-51794 LA - deu 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 - 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 - 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 - CONF A1 - Braun, Ulrike A1 - Schartel, Bernhard T1 - Red phosphorus as Flame Retardant in Thermoplastics T2 - BASF AG CY - Ludwigshafen am Rhein, Germany DA - 2003-09-11 PY - 2003 AN - OPUS4-4027 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schartel, Bernhard A1 - Kunze, Ralf A1 - Neubert, Dietmar A1 - Braun, Ulrike ED - Lewin, M. T1 - Mechanistic Studies on PA-66 Fire Retarded with Red Phosphorus T2 - 13th Conference on Recent Advances in Flame Retardancy of Polymeric Materials ; 13th Annual BCC Conference on Flame Retardancy CY - Stamford, CT, USA DA - 2002-06-03 PY - 2002 SN - 1-569-65890-0 VL - 13 SP - 93 EP - 103 PB - BCC CY - Norwalk, Conn. AN - OPUS4-1562 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 - 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 - CONF A1 - Schartel, Bernhard A1 - Bartholmai, Matthias A1 - Braun, Ulrike T1 - Residue, Charring and Intumescence N2 - The exploration of condensed phase mechanisms such as charring and intumescence has been pushed forward in the last decades, since it is believed that focusing on these concepts will bring materials closer to an efficient and ecologically friendly fire retardancy. They promise to concentrate efficient fire retardancy at the key position between pyrolysis zone and gas phase. Examples of residue/char forming and intumescent materials are used to illustrate the influence of mass and heat barrier effects on the fire behavior of materials and general results are presented. A comprehensive understanding of the mechanisms and structure-property relationships in fire retardancy is presented. KW - Fire retardancy KW - Nanocomposites KW - Red Phosphorus KW - Intumescence KW - Cone Calorimeter PY - 2006 SN - 1-59623-221-8 VL - XV SP - 15 EP - 21 PB - BCC Research CY - Norwalk, Conn. AN - OPUS4-4068 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Altmann, Korinna A1 - Sommerfeld, Thomas A1 - Braun, Ulrike T1 - Quantification of microplastics in a freshwater suspended organic matter using different thermoanalytical methods – outcome of an interlaboratory comparison N2 - A sedimented freshwater suspended organic matter fortified with particles of polyethylene (PE), polypropylene (PP), polystyrene (PS), and polyethylene terephthalate (PET) was employed in an interlaboratory comparison of thermoanalytical methods for microplastics identification and quantification. Three laboratories performed pyrolysis gas chromatography-mass spectrometry (Py-GC-MS), three others provided results using thermal extraction desorption followed by gas chromatography coupled to mass spectrometry (TED-GC-MS). One participant performed thermogravimetry-infrared spectroscopy (TGA-FTIR) and two participants used thermogravimetry coupled to mass spectrometry (TGA-MS). Further participants used differential scanning microscopy (DSC), a procedure based on micro combustion calorimetry (MCC) and a procedure based on elemental analysis. Each participant employed a different combination of sample treatment, calibration and instrumental Settings for polymer identification and quantification. Though there is obviously room for improvements regarding the between-laboratory reproducibility and the harmonization of procedures it was seen that the participants Performing Py-GC-MS, TED-GC-MS, and TGA-FTIR were able to correctly identify all polymers and to report reasonable quantification results in the investigated concentration range (PE: 20.0 μg/mg, PP: 5.70 μg/mg; PS: 2.20 μg/mg, PET: 18.0 μg/mg). Although for the other methods limitations exists regarding the detection of specific polymers, they showed potential as alternative approaches for polymer quantification in solid environmental matrices. KW - Interlaboratory comparison KW - Microplastics KW - Suspended organic matter KW - Pyrolysis PY - 2020 DO - https://doi.org/10.1016/j.jaap.2020.104829 VL - 148 SP - 1 EP - 6 PB - Elsevier B.V. AN - OPUS4-50977 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 -