TY - JOUR A1 - Müller, Axel A1 - Goedecke, Caroline A1 - Eisentraut, Paul A1 - Piechotta, Christian A1 - Braun, Ulrike T1 - Microplastic analysis using chemical extraction followed by LC‑UV analysis: a straightforward approach to determine PET content in environmental samples N2 - Background: The ubiquitous occurrence of microplastic particles in marine and aquatic ecosystems was intensively investigated in the past decade. However, we know less about the presence, fate, and input paths of microplastic in terrestrial ecosystems. A possible entry path for microplastic into terrestrial ecosystems is the agricultural application of sewage sludge and solid bio-waste as fertilizers. Microplastic contained in sewage sludge also includes Polyethylene terephthalate (PET), which could originate as fiber from textile products or as a fragment from packaging products (foils, bottles, etc.). Information about microplastic content in such environmental samples is limited yet, as most of the used analytical methods are very time-consuming, regarding sample preparation and detection, require sophisticated analytical tools and eventually need high user knowledge. Results: Here, we present a simple, specific tool for the analysis of PET microplastic particles based on alkaline extraction of PET from the environmental matrix and subsequent determination of the monomers, terephthalic acid, using liquid chromatography with UV detection (LC-UV). The applicability of the method is shown for different types of PET in several soil-related, terrestrial environmental samples, e.g., soil, sediment, compost, fermentation residues, but also sewage sludge, suspended particles from urban water management systems, and indoor dust. Recoveries for model samples are between 94.5 and 107.1%. Limit of determination and limit of quantification are absolute masses of 0.031 and 0.121 mg PET, respectively. In order to verify the measured mass contents of the environmental samples, a method comparison with thermal extraction-desorption-gas chromatography–mass spectrometry (TED-GC/MS) was conducted. Both methods deliver similar results and corroborated each other. PET mass contents in environmental samples range from values below LOQ in agriculture soil up to 57,000 mg kg−1 in dust samples. Conclusions: We demonstrate the potential of an integral method based on chemical extraction for the Determination of PET mass contents in solid environmental samples. The method was successfully applied to various matrices and may serve as an analytical tool for further investigations of PET-based microplastic in terrestrial ecosystems. KW - Soil KW - Analysis KW - Microplastic KW - PET KW - LC-UV PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509060 DO - https://doi.org/10.1186/s12302-020-00358-x IS - 32 SP - 85 PB - Springer Open CY - Berlin AN - OPUS4-50906 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dittmann, Daniel A1 - Eisentraut, Paul A1 - Goedecke, Caroline A1 - Wiesner, Yosri A1 - Jekel, M A1 - Ruhl, A S A1 - Braun, Ulrike T1 - Specific adsorption sites and conditions derived by thermal decomposition of activated carbons and adsorbed carbamazepine N2 - The adsorption of organic micropollutants onto activated carbon is a favourable solution for the treatment of drinking water and wastewater. However, these adsorption processes are not sufficiently understood to allow for the appropriate prediction of removal processes. In this study, thermogravimetric analysis, alongside evolved gas analysis, is proposed for the characterisation of micropollutants adsorbed on activated carbon. Varying amounts of carbamazepine were adsorbed onto three different activated carbons, which were subsequently dried, and their thermal decomposition mechanisms examined. The discovery of 55 different pyrolysis products allowed differentiations to be made between specific adsorption sites and conditions. However, the same adsorption mechanisms were found for all samples, which were enhanced by inorganic constituents and oxygen containing surface groups. Furthermore, increasing the loadings led to the evolution of more hydrated decomposition products, whilst parts of the carbamazepine molecules were also integrated into the carbon structure. It was also found that the chemical composition, especially the degree of dehydration of the activated carbon, plays an important role in the adsorption of carbamazepine. Hence, it is thought that the adsorption sites may have a higher adsorption energy for specific adsorbates, when the activated carbon can then potentially increase its degree of graphitisation. KW - Aktivkohle KW - TED-GC/MS KW - Adsorption KW - Thermoanalytik PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506946 DO - https://doi.org/10.1038/s41598-020-63481-y VL - 10 IS - 1 SP - 6695 PB - Nature Publishing Group AN - OPUS4-50694 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klöckner, P. A1 - Seiwert, B. A1 - Eisentraut, Paul A1 - Braun, Ulrike A1 - Reemtsma, T. A1 - Wagner, S. T1 - Characterization of tire and road wear particles from road runoffindicates highly dynamic particle properties N2 - Tire and road wear particles (TRWPs) are heteroagglomerates of tire rubber and other particles deposited on the road surface and one of the main contributors to non-exhaust emissions of automobile traffic. In this study, samples from road environments were analyzed for their TRWP contents and concentra- tions of eight organic tire constituents. TRWP concentrations were determined by quantifying Zn in the density fraction < 1.9 g/cm ³and by thermal extraction desorption-gas chromatography-mass spectrometry (TED-GC/MS) and the concentrations ranged from 3.7 to 480 mg TRWP/g. Strong and statistically signif- icant correlations with TRWPs were found for 2-hydroxybenzothiazole and 2-aminobenzothiazole, indi- cating that these substances may be suitable markers of TRWPs. The mass distribution of TRWPs in road dust suggests that the main mass fraction formed on roads consists of coarse particles ( > 100 μm). Data for a sedimentation basin indicate that the fine fraction ( < 50 μm) is preferentially transported by road runoffinto receiving waters. The size distribution and density data of TRWP gathered by three different quantitation approaches also suggest that aging of TRWPs leads to changes in their particle density. An improved understanding of the dynamics of TRWP properties is essential to assess the distribution and dissipation of this contaminant of emerging concern in the environment. KW - Tire Wear KW - Density separation KW - Microplastic KW - Urban PY - 2020 DO - https://doi.org/10.1016/j.watres.2020.116262 VL - 185 SP - 116262 PB - Elsevier Ltd. AN - OPUS4-51256 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 - Eisentraut, Paul T1 - Microplastic analysis using TED-GC/MS: H/D-Exchange of decomposition products of D-marked polystyrene as an internal standard N2 - Deuterated polystyrene (D-PS) improves microplastic detection with TED-GC / MS, among other things through higher reproducibility. It is inexpensive (0.1 ct / analysis) and can be dosed quickly and reproducibly thanks to its good solubility (e.g. in toluene). However, certain matrices lead to an exchange of the deuterium with hydrogen. The poster shows the measuring principle, in which matrices H/D-exchange takes place, the results of kinetic studies and ways of preventing or circumventing the H/D-exchange. T2 - SALSA MAKE AND MEASURE 2021 CY - Online meeting DA - 16.09.2021 KW - Microplastic KW - H/D-Exchange KW - Internal Standard KW - TED-GC/MS KW - Thermoanalytic PY - 2021 AN - OPUS4-53681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisentraut, Paul T1 - Mikroplastikanalytik mittels TED-GC/MS: H/D-Austausch an Zersetzungsprodukten von D-markiertem Polystyrol als interner Standard N2 - Deuteriertes Polystyrol (D-PS) verbessert die Mikroplastikdetektion mit der TED-GC/MS, u.a. durch höhere Reproduzierbarkeit. Es ist kostengünstig (0,1 ct/Analyse) und durch die gute Löslichkeit (z.B. in Toluol) schnell und reproduzierbar zu dosieren. Bestimmte Matrices führen jedoch zu einem Austausch des Deuteriums durchWasserstoff. Das Poster zeigt das Messprinzip, bei welchen Matrices H/D-Austausch erfolgt, Ergebnisse von Kinetikuntersuchungen sowie Möglichkeiten, den Austausch zu verhindern oder zu umgehen. T2 - Tagung der Wasserchemischen Gesellschaft CY - Online Meeting DA - 10.05.2021 KW - Mikroplastik KW - Analyse KW - Interner Standard KW - H/D-Austausch PY - 2021 AN - OPUS4-52727 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kittner, Maria A1 - Kerndorff, A. A1 - Ricking, M. A1 - Bednarz, M. A1 - Obermaier, N. A1 - Lukas, M. A1 - Asenova, M. A1 - Bordós, G. A1 - Eisentraut, Paul A1 - Hohenblum, P. A1 - Hudcova, H. A1 - Humer, F. A1 - István, T. G. A1 - Kirchner, M. A1 - Marushevska, O. A1 - Nemejcová, D. A1 - Oswald, P. A1 - Paunovic, M. A1 - Sengl, M. A1 - Slobodnik, J. A1 - Spanowsky, K. A1 - Tudorache, M. A1 - Wagensonner, H. A1 - Liska, I. A1 - Braun, U. A1 - Bannick, C. G. T1 - Microplastics in the Danube River Basin: A First Comprehensive Screening with a Harmonized Analytical Approach N2 - In this study, carried out within the Joint Danube Survey 4, a comprehensive microplastic screening in the water column within a large European river basin from its source to estuary, including major tributaries, was realized. The objective was to develop principles of a systematic and practicable microplastic monitoring strategy using sedimentation boxes for collection of suspended particulate matter followed by its subsequent analysis using thermal extraction desorption-gas chromatography/mass spectrometry. In total, 18 sampling sites in the Danube River Basin were investigated. The obtained suspended particulate matter samples were subdivided into the fractions of >100 μm and <100 μm and subsequently analyzed for microplastic mass contents. The results showed that microplastics were detected in all samples, with polyethylene being the predominant polymer with maximum contents of 22.24 μg/mg, 3.23 μg/mg for polystyrene, 1.03 μg/mg for styrene-butadiene-rubber, and 0.45 μg/mg for polypropylene. Further, polymers such as different sorts of polyester, polyacrylates, polylactide, and natural rubber were not detected or below the detection limit. Additional investigations on possible interference of polyethylene signals by algae-derived fatty acids were assessed. In the context of targeted monitoring, repeated measurements provide more certainty in the interpretation of the results for the individual sites. Nevertheless, it can be stated that the chosen approach using an integrative sampling and determination of total plastic content proved to be successful. KW - Thermal extraction desorption-gas chromatography/mass spectrometry (TED-GC/MS), monitoring KW - Microplastics KW - River KW - Suspended particulate matter (SPM) KW - Sedimentation box (SB) PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551444 DO - https://doi.org/10.1021/acsestwater.1c00439 VL - 2 IS - 7 SP - 1174 EP - 1181 PB - ACS Publications AN - OPUS4-55144 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 - CONF A1 - Eisentraut, Paul T1 - Analysis of microplastics in environmental samples using TED-GC-MS N2 - The presence of plastic debris and especially small plastic particles in marine ecosystems has been recognized in the 1970`s. Since then various other environmental systems all over the world, like rivers, lakes and biota have been found to be polluted by plastics. Lately, agriculturally used land, waste-water treatment and biogas facilities come into focus as possibly relevant distribution vectors. To monitor the situation and investigate distribution pathways, the need for fast and reliable analytical procedures is high. Up to now, there is no standard procedure for sampling, concentrating and analyzing plastic particles in environmental samples. Our group recently reported the development of a new analyzing method for microscale plastic particles, thermal extraction desorption gas chromatography mass spectrometry (TED-GC-MS). This method consists of thermal extraction of the sample via thermogravimetric analysis, collection of the evolved gaseous decomposition products on a solid-phase adsorber and analysis of the loaded adsorber using Thermal-Desorption-GC-MS. This technique utilizes the characteristic decomposition products of polymers for identification and even quantification of plastics in environmental samples. In the present work we investigated samples of fermentation residues taken from a biogas plant. The results of sample preparation, concentration and analysis are presented as well as a comparison with alternative methods. T2 - MoDeSt 2016 CY - Cracow, Poland DA - 04.09.2016 KW - Microplastic PY - 2016 AN - OPUS4-37782 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisentraut, Paul T1 - Analysis of microplastics in environmental samples using TED-GC-MS N2 - The first analysis of environmental samples shows, that the use of TED-GC-MS is suitable to analyse microplastic in environmental samples. Compared to the micro-spectroscopic methods this method is faster and gives good hints to the occurrence of high loadings of MP in environmental samples. In consequence, the method allows the monitoring of the situation and the investigation of MP distribution pathways in environment, to assess the relevance of various inputs. T2 - 7th Late Summer Workshop "Microplastics in the aquatic environment" CY - Haltern am See, Germany DA - 25.09.2016 KW - Microplastic PY - 2016 AN - OPUS4-37785 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisentraut, Paul T1 - Kunststoffgehalte schnell bestimmen mit der TED-GC-MS N2 - Der Vortrag behandelt die Analyse von Kunststoffen in Umweltproben mit dem thermischen Verfahren TED-GC-MS. Das Verfahren und dessen Funktionsweise werden vorgestellt, erfolgte Optimierungen, Verfahrenskenndaten sowie Möglichkeiten der Quantifizierung behandelt. T2 - Projektübergreifendes Mikroplastikseminar BASEMAN, BONUS MICROPOLL, MiWa CY - Berlin, Germany DA - 16.10.2017 KW - Mikroplastik KW - Analyse KW - TED-GC-MS PY - 2018 AN - OPUS4-43927 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 - 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 - 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 - Eisentraut, Paul T1 - Turning up the heat: a thermoanalytical approach for the detection of microplastics N2 - The presentation deals with the analysis of plastics in environmental samples using the TED-GC-MS method. The method and its working principles are presented, method characteristics and application examples are given. Advantages and disadvantages compared to other methods are highlighted. T2 - Linnaeus Eco-Tech 2018 CY - Kalmar, Sweden DA - 19.11.2018 KW - Microplastics KW - Tire wear KW - Thermoanalysis KW - TED-GC-MS PY - 2018 AN - OPUS4-47185 LA - eng 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 - Braun, Ulrike A1 - Eisentraut, Paul A1 - Fuchs, S. A1 - Deglmann, P. T1 - Sulphurous additives for polystyrene: Influencing decomposition behavior in the condensed phase N2 - The thermal decomposition behaviour of polystyrene (PS) containing sulphur and phosphorus additives was investigated, using thermogravimetry coupled with Fourier transform infrared spectroscopy (TGA-FTIR). It was found that the additives influence the decomposition process of the polymer in the condensed phase, resulting in a decrease in styrene monomer formation and an increase in styrene oligmer derivatives. Via reference measurements with binary mixtures it was found that the presence of sulphur additives influences the radicalic decomposition process of PS. In combination with quantum chemical calculations it was concluded that this is due to the formation of radicals that abstract hydrogen from the polymer matrix at lower temperatures, disfavouring the radicalic decomposition pathway leading to styrene. KW - Degradation KW - Theory and modeling KW - Thermogravimetric analysis KW - Polystyrene PY - 2015 DO - https://doi.org/10.1002/APP.41665 SN - 0021-8995 SN - 1097-4628 VL - 132 IS - 12 SP - 41665, 1 EP - 13 PB - Wiley InterScience CY - Hoboken, NJ AN - OPUS4-32380 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisentraut, Paul T1 - Analyse von Mikroplastik Partikeln aus Umweltproben mit der TED-GC-MS N2 - Die weltweite Produktion von synthetischen Kunststoffen steigt stetig und ein Teil gelangt in die Umwelt. Die Kunststofffragmente werden durch Umwelteinflüsse zerkleinert und bilden schließlich Mikroplastik, dessen Gefährdungspotential intensiv diskutiert wird. Zur Beobachtung und Bewertung der Situation ist eine leistungsstarke und schnelle Analytik erforderlich, jedoch existieren noch keine harmonisierten Verfahren. Die ThermoExtraktionDesorption-GasChromatograpie-MassenSpektrometrie (TED-GC-MS) nutzt polymer-spezifische Zersetzungsprodukte und bietet durch ihre Schnelligkeit und Robustheit Vorteile gegenüber anderen Verfahren. T2 - Tagung der Wasserchemischen Gesellschaft 2017 CY - Donaueschingen, Germany DA - 22.05.2017 KW - Mikroplastik KW - Thermoanalytik KW - TED-GC-MS PY - 2017 AN - OPUS4-40452 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 - Eisentraut, Paul T1 - Analysis of tire wear particles in enviromental samples using TED-GC-MS N2 - The use of TED-GC-MS for the analysis of tire wear particles in environmental samples is presented. T2 - SETAC CY - Rome, Italy DA - 13.05.2018 KW - TED-GC-MS KW - Microplastics KW - Tire wear particles PY - 2018 AN - OPUS4-45204 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 - 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 -