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Veröffentlichung Analysis of polyethylene microplastics in environmental samples, using a thermal decomposition method(2015) Dümichen, Erik; Bannick, Claus Gerhard; Barthel, Anne-Kathrin; Braun, Ulrike; Brand, Kathrin; Jekel, Martin; Senz, RainerSmall polymer particles with a diameter of less than 5 mm called microplastics find their way into the environment from polymer debris and industrial production. Therefore a method is needed to identify and quantify microplastics in various environmental samples to generate reliable concentration values. Such concentration values, i.e. quantitative results, are necessary for an assessment of microplastic in environmental media. This was achieved by thermal extraction in thermogravimetric analysis (TGA), connected to a solid-phase adsorber. These adsorbers were subsequently analysed by thermal desorption gas chromatography mass spectrometry (TDS-GC-MS). In comparison to other chromatographic methods, like pyrolyse gas chromatography mass spectrometry (Py-GC-MS), the relatively high sample masses in TGA (about 200 times higher than used in Py-GC-MS) analysed here enable the measurement of complex matrices that are not homogenous on a small scale. Through the characteristic decomposition products known for every kind of polymer it is possible to identify and even to quantify polymer particles in various matrices. Polyethylene (PE), one of the most important representatives for microplastics, was chosen as an example for identification and quantification.Quelle: http://www.sciencedirect.comVeröffentlichung Fast identification of microplastics in complex environmental samples by a thermal degradation method(2017) Dümichen, Erik; Bannick, Claus Gerhard; Eisentraut, Paul; Barthel, Anne-KathrinIn 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. © 2017 Elsevier Ltd.Veröffentlichung Development and testing of a fractionated filtration for sampling of microplastics in water(2019) Bannick, Claus Gerhard; Obermaier, Nathan; Ricking, Mathias; Schniegler, Sara; Szewzyk, Regine; Barthel, Anne-KathrinA 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 body of water with defined MP fractions, the recovery rates ranged from 80-110%, depending on the different MP types and MP size classes. In the wastewater discharge, we found both polyethylene and polystyrene in different size classes and quantities. © 2018 Elsevier Ltd. All rights reserved.Veröffentlichung Kunststoffe und Mikrokunststoffe in der Umwelt(2019) Bannick, Claus Gerhard; Braun, UlrikeVeröffentlichung Identification and Quantification of Microplastic in Sewage Systems by TED-GC-MS(2019) Altmann, Korinna; Goedecke, Caroline; Bannick, Claus GerhardThe number of publications reporting the amount of microplastic (MP) all over the world increased rapidly. Methods used so far are very time consuming and not able to provide information on total contents. As harmonised sampling, sample preparation and analysis strategies are missing different studies can hardly be compared and quantitative data, including identification and mass contents of the polymers found, are missing. This leads to a lack of comprehensive understanding of MP occurrence, source and entry pathways into the environment. We developed a method, Thermal Extraction/Desorption-Gaschromatography-Massspectrometry, as a fast screening method for MP analysis. Solid residues of water samples are heated up to 600 C under a N2 atmosphere without any sample preparation. The collected decomposition gases are separated in a gas chromatography system and detected in a mass spectrometer. Mass contents of the identified polymers can be calculated. In this presentation we will show first results from the influent of the wastewater treatment plant Kaiserslautern (Germany) and its combined sewage system as possibly entry pathway. In order to determine the relevance of wastewater split streams analysis of grey water will be conducted. Samples are fractionally filtered by a sieve cascade with mesh sizes of 500, 100, 50 Ìm. Quelle: https://opus4.kobv.de/Veröffentlichung Harmonisierung von Untersuchungsverfahren für (Mikro-)Plastik in der Umwelt(2019) Braun, Ulrike; Bannick, Claus GerhardVeröffentlichung Occurrence of microplastics in the Danube River - a first screening(2021) Asenova, Mina; Bannick, Claus Gerhard; Bednarz, Marius; Kerndorff, Alexander; Obermaier, Nathan; Ricking, MathiasPlastics, and microplastics in particular, are still part of scientific and regulatory discussions. Their inputs from land ultimately end up in the oceans, where they remain for a long time. River systems represent an important path of entry into the oceans. The Danube is the second largest river in Europe and can therefore be an example for the occurrence of plastic in other large river systems. In JDS4 a comprehensive screening of microplastics was carried out over the entire course of the river. Sampling was performed by means of deploying sedimentation boxes into the river for 14 days; followed by thermo-analytical detection (TED-GC/MS) for determination of the total content of various plastic polymers in the collected suspended particulate matter samples. For the first time, a baseline of pollution by microplastics in the Danube River Basin has been established. In all samples almost, all analyzed polymers were detected and quantified, whereas there is no clear trend along the Danube with increasing or decreasing contents. The contents ranged between 0.05 - 22.24, 0.00 - 0.45, 0.00-1.03 and 0.00 3.32 for PE, PP, SBR and PS [(micro)g/mg] SPM, respectively. Quelle: A shared analysis of the Danube River : joint Danube survey 4 ; scientific report / Editors: Igor Liška [and five others]. - Vienna : International Commission for the Protection of the Danube River, 2021. - 1 Onlineresource (562 pages) : Illustrationen. - E-Book; Dateigröße / Dateiumfang: 44,09 MB. - ISBN 978-3-200-07450-7, Seite 487Veröffentlichung A simple model approach for the desorption of DDT and related compounds from contaminated sediment to plastic polymers(2021) Bannick, Claus Gerhard; Kerndorff, Alexander; Braun, Ulrike; Obermaier, Nathan; Ricking, MathiasVeröffentlichung Development of a routine screening method for the microplastic mass content in a wastewater treatment plant effluent(2022) Goedecke, Caroline; Eisentraut, Paul; Bannick, Claus Gerhard; Altmann, Korinna; Barthel, Anne-Kathrin; Obermaier, Nathan; Braun, Ulrike; Ricking, MathiasAn investigation of microplastic (MP) occurrence in a municipal wastewater treatment plant (WWTP) effluent with tertiary treatment was carried out. Representative sample volumes of 1 m3 were taken by applying a fractionated filtration method (500, 100, and 50 (micro)m mesh sizes). The detection of MP mass fractions by thermal extraction desorption-gas chromatography/mass spectrometry (TED-GC/MS) was achieved without the previously required additional sample pretreatment for the first time. Different types of quantification methods for the evaluation of TED-GC/MS data were tested, and their accuracy and feasibility have been proven for real samples. Polyethylene, polystyrene, and polypropylene were identified in effluent samples. The polymer mass content varied significantly between 5 and 50 mg m-3. A correlation between the MP load and the quantity of suspended matter in the WWTP effluents, particle size distribution, particle type, and operation day (i.e., weekday, season, and capacity) was not found. It can be concluded that a meaningful assessment of WWTPs requires a comprehensive sampling campaign with varying operation conditions. © 2022 The AuthorsVeröffentlichung Microplastics in the Danube River Basin: a first comprehensive screening with harmonized analytical approach(2022) Braun, Ulrike; Bannick, Claus Gerhard; Bednarz, Marius; Kerndorf, Alexander; Lukas, Marcus; Obermaier, Nathan; Ricking, MathiasIn 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 mikrom and <100 mikrom 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 mikrog/mg, 3.23 mikrog/mg for polystyrene, 1.03 mikrog/mg for styrene-butadiene-rubber, and 0.45 mikrog/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. © 2022 The Authors