TY - JOUR A1 - Putzu, Mara A1 - Wiesner, Yosri A1 - Weimann, Christiane A1 - Hodoroaba, Vasile-Dan A1 - Muniategui Lorenzo, Soledad A1 - Fernández-Gonzáles, Verónica A1 - Booth, Andy M. A1 - Igartua, Amaia A1 - Benismail, Nizar A1 - Coïc, Laureen A1 - Chivas-Joly, Carine A1 - Fenoglio, Ivana A1 - Rossi, Andrea Mario A1 - Giovannozzi, Andrea Mario A1 - Altmann, Korinna T1 - Optimization of tablet processing as a reference material for microplastic detection methods N2 - Reference materials (RMs) are essential and highly demanded tools for the development and validation of methods for microplastic (MP) quantification in complex matrices, to ensure comparable and harmonized approaches aligned with EU commission criteria for monitoring MPs (e.g., Drinking Water Directive and Urban Wastewater Treatment Directive). This study investigates different approaches for optimizing the production of polypropylene (PP) RMs in the form of water-soluble tablets, which were carefully evaluated for their homogeneity and stability according to ISO Guide 30, ISO 33401, and ISO 33405. PP particles (1–100 μm) were produced by cryomilling and embedded in a lactose/PEG matrix, then pressed into tablets (18 µg theoretical PP mass). The production process was optimized by varying (i) the size distribution of the matrix components and (ii) the mixer instrument. The materials obtained were characterized by thermogravimetric analysis to assess the homogeneity distribution of MPs with respect to PP mass in the individual tablets and their stability over a 4-month period. The most promising approach, with a homogenous mass of 19 μg (standard deviation of 4 μg), relative standard deviation of 19%, was further investigated for homogeneity by comparison with thermo-analytical mass determination methods, such as TED-GC/MS (thermal extraction desorption-gas chromatography/mass spectrometry) and Py-GC/MS (pyrolysis-gas chromatography-mass spectrometry), and for number-based characterization using micro-Raman spectroscopy. Material characterization was also examined using laser diffraction, scanning electron microscopy, and ATR-FTIR. Based on the results, the optimized processing protocol yields a PP RM suitable for quality control and method performance studies supporting standardization. KW - Microplastics KW - TED-GC/MS KW - Reference materials KW - Polypropylene PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653290 DO - https://doi.org/10.1007/s00216-025-06271-7 SN - 1618-2642 SP - 1 EP - 14 PB - Springer Science and Business Media LLC AN - OPUS4-65329 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wiesner, Yosri A1 - Eisentraut, Paul A1 - Altmann, Korinna T1 - One Year Observation of Microplastic Concentrations in the River Rhine N2 - In recent years, the quantification of microplastics (MP) in aquatic environments has gained increasing attention, particularly regarding their environmental distribution and potential exposure levels. Environmentally relevant exposure data are still essential for a realistic risk assessment of the harmful health potential of microplastics in freshwater systems. This study addresses a large data set of MP concentrations analyzed and processed under statistical aspects and provides mass concentrations as well as associated size fractions of the detected MP. Over a 12 month period, samples were collected at three locations and analyzed across three particle size fractions (100−500 μm, 50−100 μm, and 10−50 μm) using thermalextraction desorption-gas chromatography/mass spectrometry (TED-GC/MS). The most prevalent polymers identified were polyethylene (PE), polypropylene (PP), polystyrene (PS), styrene−butadiene rubber (SBR), and natural rubber (NR). Statistical analyses, including principal component and cluster analysis, revealed size-dependent patterns,minor seasonal variation and spatial variations. These findings are particularly significant for ecotoxicological research and regulatory development, especially regarding tire abrasion a rarely quantified but potentially harmful MP source. The study contributes aluable data for future environmental monitoring and supports EU directives on wastewater and drinking water quality KW - TED-GC/MS KW - Microplastics KW - Environment KW - Monitoring KW - Reference data PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-654669 DO - https://doi.org/10.1021/acsestwater.5c00530 SN - 2690-0637 SP - 1 EP - 10 PB - American Chemical Society (ACS) AN - OPUS4-65466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wiesner, Yosri A1 - Bednarz, Marius A1 - Braun, Ulrike A1 - Bannick, Claus Gerhard A1 - Ricking, Mathias A1 - Altmann, Korinna T1 - A promising approach to monitor microplastic masses in composts N2 - Inputs of plastic impurities into the environment via the application of fertilizers are regulated in Germany and the EU by means of ordinances. Robust and fast analytical methods are the basis of legal regulations. Currently, only macro- and large microplastic contents (>1 mm) are measured. Microplastics (1–1,000 µm), are not yet monitored. Thermal analytical methods are suitable for this purpose, which can determine the mass content and can also be operated fully automatically in routine mode. Thermal extraction desorption-gas chromatography/mass spectrometry (TED-GC/MS) allows the identification of polymers and the determination of mass contents in solid samples from natural environments. In accordance with the German or European Commission (EC) Fertiliser Ordinance, composting plants should be monitored for microplastic particles with this method in the future. In this context a compost plant was sampled. At the end of the rotting process, the compost was sieved and separated in a coarse (>1 mm) and a fine fraction (<1 mm). The fine fraction was processed using density separation comparing NaCl and NaI as possible salt alternative and screened for microplastic masses by TED-GC/MS with additional validation and quality assurance experiments. With TED-GC/MS total microplastics mass contents of 1.1–3.0 μg/mg in finished compost could be detected with polyethylene mainly. What differs much to the total mass of plastics in the coarse fraction with up to 60 μg/mg, which were visually searched, identified via ATR-FTIR and gravimetrically weighted. KW - Microplastics KW - TED-GC/MS KW - Compost KW - Monitoring KW - Soil PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586688 DO - https://doi.org/10.3389/fenvc.2023.1281558 SN - 2673-4486 VL - 4 SP - 1 EP - 12 PB - Frontiers Media CY - Lausanne AN - OPUS4-58668 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wiesner, Yosri A1 - Hoffmann, Thomas A1 - Range, David A1 - Altmann, Korinna T1 - Microplastics in sediments of the river Rhine—A workflow for preparation and analysis of sediment samples from aquatic river systems for monitoring purposes N2 - AbstractMicroplastics (MP) can be detected in all environmental systems. Marine and terrestrial aquatic systems, especially the transported suspended solids, have often been the focus of scientific investigations in the past. Sediments of aquatic river systems, on the other hand, were often ignored due to the time‐consuming sample preparation and analysis procedures. Spectroscopic measurement methods counting particle numbers are hardly suitable as detection methods, because there are plenty of natural particles next to a small number of MP particles. Integral methods, such as thermoanalytical methods are determining the particle mass independently of the inorganic components.In this study, a workflow for sample preparation via density separation and subsequent analysis by thermal extraction desorption‐gas chromatography/mass spectrometry is presented, which leads to representative and homogeneous samples and allows fast and robust MP mass content measurements suitable for routine analysis. Polymers were identified and quantified in all samples. Polyethylene and styrene‐butadiene rubber are the dominant polymers, besides polypropylene and polystyrene. Overall, total polymer masses between 1.18 and 337.0 µg/g could be determined. Highest MP concentrations in riverbed sediment are found in sites characterized by low flow velocities in harbors and reservoirs, while MP concentrations in sandy/gravelly bed sediments with higher flow velocities are small. KW - Microplastics KW - Density separation KW - TED-GC/MS KW - NaI PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597335 DO - https://doi.org/10.1002/appl.202200125 VL - 3 IS - 2 SP - 1 EP - 10 PB - Wiley VHC-Verlag AN - OPUS4-59733 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Drago, C A1 - Wiesner, Yosri A1 - Braun, U A1 - Giovannozi, A A1 - Fadda, M A1 - Putzu, Mara A1 - Lorenzo, S A1 - Moscoso-Pérez, C A1 - Benismail, N A1 - Palma, C A1 - Almeida, J A1 - Mattarozzi, M A1 - Barbaresi, M A1 - Piergiovanni, M A1 - Masino, M A1 - Bianchi, F A1 - Careri, M A1 - v Bavel, B A1 - Maltseva, A A1 - Sillanpää, M A1 - Pröfrock, D A1 - Wippermann, D A1 - Altmann, Korinna T1 - Harmonisation of sample preparation for microplastic analysis: Recovery rates of tablets containing microplastics as reference material for food and environmental matrix N2 - Microplastic are found ubiquitarians in the environment and food products. Up to now, their impact of risks on health and environment is still controversially discussed, but based on the precautionary principle alone, their presence should be monitored and emission should be reduced (see here also the status of existing EU regulations ). The crucial point is not only the reduction of microplastics pollution but also the introduction of legally binding, standardized procedures for their analysis. The limited availability of certified reference material as well as absence of standard operating procedures to identify, characterize and quantify microplastics according to number and mass have generated lack of comparability between different analytical methods and laboratories; but also, the need of time-consuming development of own protocols for each laboratory. Further on, harmonisation and standardisation of microplastics analysis requires specific reference materials that are used to validate the measurement and to ensure the comparability of results. In the first step, we developed tablets of a water-soluble matrix, containing defined numbers of microplastic particles or mass contents. These can be solved in water and can be handled as reference materials in bottled drinking water without additional sample preparation. These samples can be measured, using mass-based methods as thermo-analytical methods like thermal desorption-gas chromatography-mass spectrometry (TED-GC/MS) or pyrolysis–gas chromatography–mass spectrometry (Py-GC/MS) and using umber-based methods as vibrational spectroscopy like Infrared and Raman directly after filtration. The aim of this work was to delevop standard operating procedure to measure microplastics in more complex matrices and to harmonise and compare different detection and characterization methods. In fact, these matrices require different additional treatments to allow a reliable quantification and identification of microplastics. T2 - SETAC Europe 2025 CY - Vienna, Austria DA - 11.05.2025 KW - Microplastics KW - Nanoplastics PY - 2025 AN - OPUS4-63366 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wiesner, Yosri A1 - Altmann, Korinna A1 - Braun, U. T1 - Determination of Microplastic Mass Content by Thermal Extraction Desorption Gas Chromatography– Mass Spectrometry N2 - The scientific and practical challenge of detecting microplastics (MPs) in the environment in a targeted and rapid manner is solved by innovative coupling of thermogravimetric analysis with mass spectrometric methods. Fast identification and quantitative determination of most thermoplastic polymers and elastomers is possible by using thermal extraction Desorption gas chromatography–mass spectrometry (TED-GC–MS). KW - Microplastics KW - Mikroplastik KW - TED-GC/MS KW - Microplastics analytic KW - Mikroplastik Massegehalt PY - 2021 VL - 17 IS - 3 SP - 2 EP - 7 PB - MultiMedia (UK) LLC CY - Cranbury AN - OPUS4-52570 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Monikh, F. A. A1 - Baun, A. A1 - Hartmann, N. B. A1 - Kortet, R. A1 - Akkanen, J. A1 - Lee, J.-S. A1 - Shi, H. A1 - Lahive, E. A1 - Uurasjärvi, E. A1 - Tufenkji, N. A1 - Altmann, Korinna A1 - Wiesner, Yosri A1 - Grossart, H.-P. A1 - Peijnenburg, W. A1 - Kukkonen, J. V. K. T1 - Exposure protocol for ecotoxicity testing of microplastics and nanoplastics N2 - Despite the increasing concern about the harmful effects of micro- and nanoplastics (MNPs), there are no harmonized guidelines or protocols yet available for MNP ecotoxicity testing. Current ecotoxicity studies often use commercial spherical particles as models for MNPs, but in nature, MNPs occur in variable shapes, sizes and chemical compositions. Moreover, protocols developed for chemicals that dissolve or form stable dispersions are currently used for assessing the ecotoxicity of MNPs. Plastic particles, however, do not dissolve and also show dynamic behavior in the exposure medium, depending on, for example, MNP physicochemical properties and the medium’s conditions such as pH and ionic strength. Here we describe an exposure protocol that considers the particle-specific properties of MNPs and their dynamic behavior in exposure systems. Procedure 1 describes the top-down production of more realistic MNPs as representative of MNPs in nature and particle characterization (e.g., using thermal extraction desorption-gas chromatography/mass spectrometry). Then, we describe exposure system development for short- and long-term toxicity tests for soil (Procedure 2) and aquatic (Procedure 3) organisms. Procedures 2 and 3 explain how to modify existing ecotoxicity guidelines for chemicals to target testing MNPs in selected exposure systems. We show some examples that were used to develop the protocol to test, for example, MNP toxicity in marine rotifers, freshwater mussels, daphnids and earthworms. The present protocol takes between 24 h and 2 months, depending on the test of interest and can be applied by students, academics, environmental risk assessors and industries. KW - Microplastics KW - TED-GC/MS KW - Cryo milling PY - 2023 DO - https://doi.org/10.1038/s41596-023-00886-9 SN - 1754-2189 SP - 1 EP - 38 PB - Nature Protocols AN - OPUS4-58557 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Altmann, Korinna A1 - Abusafia, A A1 - Bannick, C-G A1 - Braun, U A1 - Crasselt, Claudia A1 - Dittmar, S A1 - Fuchs, M A1 - Gehde, M A1 - Hagendorf, C A1 - Heller, C A1 - Herper, D A1 - Heymann, S A1 - Kerndorff, A A1 - Knefel, M A1 - Jekel, M A1 - Lelonek, M A1 - Lunkenbein, T A1 - Obermaier, N A1 - Manhart, M A1 - Meurer, Maren A1 - Miclea, P-T A1 - Paul, A A1 - Richter, S A1 - Ricking, M A1 - Rohner, C A1 - Ruhl, A A1 - Sakai, Y A1 - Saravia Arzabe, C A1 - Scheid, C A1 - Schmitt, M A1 - Schnarr, M A1 - Schwertfirm, F A1 - Steinmetz, H A1 - Wander, Lukas A1 - Wiesner, Yosri A1 - Zechmeister, L T1 - RUSEKU - Repräsentative Untersuchungsstrategien für ein integratives Systemverständnis von spezifischen Einträgen von Kunststoffen in die Umwelt : Abschlussbericht N2 - Im Verbundprojekt RUSEKU wurde die Probenahme von Wasserproben entscheidend weiterentwickelt. Wichtig ist hierbei zu gewährleisten, dass genügend Merkmalsträger in jeder Probe untersucht werden. Es muss daher eine für den Probenahmeort repräsentative Beprobung hinsichtlich des Wasservolumens in Abhängigkeit der Partikelanzahl gewährleistet sein. Das Hauptaugenmerk lag im vorliegenden Projekt auf einer praxisnahen Beprobungsstrategie. Es wurden verschiedene Konzepte ausprobiert. • Grundsätzlich hat sich gezeigt, dass eine Stichprobe eine Momentaufnahme des MP-Massengehaltes zeigt. Es wird eine hohe Statistik, also eine Vielzahl an Messungen am gleichen Probenahmeort, benötigt, um eine valide Aussage über den MP-Gehalt zu machen. • Es zeigt sich, dass eine integrale Probenahme über mehrere Wochen mit dem SK routinemäßig möglich ist. Die erfassten MP-Massen sind reproduzierbar und robust. • Die DFZ ist für Stichproben geeignet. Partikel < 50 µm werden eventuell unterschätzt • Die fraktionierte Filtration kann für Stich- und Mischproben direkt im Feld genutzt werden. Fraktionen von 10 und 5 µm werden später im Labor Vakuum filtriert. Es erfolgt eine Fraktionierung der Probe mit Siebmaschenweiten von 1000, 500, 100, 50, 10 und 5 µm. • Die fraktionierte Filtration kann auch anschließend an die Beprobung mit dem SK zur Anwendung kommen. Wird die mit dem SK gewonnene Wasserprobe fraktioniert filtriert, kann neben einem MP-Gesamtgehalt auch eine Einschätzung über die Partikelgrößen gewonnen werden. • Für Wässer mit geringen Partikelzahlen wurde ein Messfiltertiegel entwickelt. Dieser hat eine Maschenweite von 6 µm. Seine Anwendung kann mögliche Verluste beim Transferieren vom Probenahmetool zum Messgefäß und mögliche Kontaminationen reduzieren. Die Optimierung der Probenahmestrategie wurde durch Modellversuche und Simulationen unterstützt. Modellversuche zum Sinkverhalten und Simulationen von MP in realen Gewässern verdeutlichten das komplexe Verhalten der Partikel. Es konnte gezeigt werden, dass Partikel ab einer bestimmten Größe (und kleiner) bei genügend starker Turbulenz sich in der Wassersäule unabhängig von ihrer Dichte verhalten und so auch MP mit kleiner Dichte (z.B. PE) in der gesamten Wassersäule zu finden sind. Es konnte mit dem TEM die Existenz von NP gezeigt werden. Ein wesentlicher Aspekt des RUSEKU Projektes war die Beprobung realer Kompartimente. Beprobt wurde neben Oberflächengewässern, das urbane Abwassersystem der Stadt Kaiserslautern, Waschmaschinenabwasser und Flaschenwasser. • In Oberflächengewässern wurde hauptsächlich PE gefunden. Je nach Probe und Gewässer konnten auch PP, PS, PET, PA, SBR und Acrylate nachgewiesen werden. • Im urbanen Abwassersystem der Stadt Kaiserslautern konnte an allen Probenahmestandorten MP nachgewiesen werden. Es wurde hauptsächlich PE, neben geringeren Mengen an PP, PS und SBR gefunden. Nach einem Regenereignis war der SBR Anteil deutlich erhöht. • Die Beprobung eines realen Wäschepostens, bestehend aus T-Shirts und Hemden mit PA/CO oder PES/CO Mischgewebe, zeigte einen PA- und PES-Austrag im Waschwasser. Der überwiegende Teil der detektierten Fasern ist aber auf Baumwolle zurückzuführen. Reine gravimetrische Messungen zur Detektion von MP führen zu einer starken Überschätzung. • In Flaschenwasser (PET-Flaschen) konnte MP detektiert werden. PET wurde nur im stillen Mineralwasser, nicht in Mineralwasser mit Kohlensäure gefunden werden. Teilweise wurde auch das MP-Material des Verschlusses im Wasser detektiert. • Für Luftproben konnte ein Aufbau zur größenselektiven Beprobung getestet werden. Neben der Probenahme hat das Projekt auch gezeigt, dass die TED-GC/MS geeignet für die MP-Detektion im Routinebetrieb ist. Die TED-GC/MS konnte weiter optimiert werden. Es wurden MP-Massen bestimmt. Im Projekt wurden erste realitätsnahe Referenzmaterialien für die MP Detektion hergestellt. Die Herstellung von realitätsnahen Polymeren in ausreichender Homogenität und Menge hat sich als große Herausforderung herausgestellt. KW - Mikroplastik KW - Probennahme KW - TED-GC/MS KW - Fraktionierte Filtration KW - Mikroplastikreferenzmaterial PY - 2022 SP - 1 EP - 201 AN - OPUS4-57800 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meier, F. A1 - Drexel, R. A1 - Wiesner, Yosri A1 - Altmann, Korinna A1 - Bartczak, D. A1 - Alasonati, E. T1 - Nano-sized Polypropylene as a Promising Candidate Reference Material: Preparation, Characterization and Stability in Complex Matrices N2 - The lack of nanoplastic (NPs) reference materials capable of mimicking real-world scenarios is currently hampering the development of validated extraction techniques from complex matrices, the development of analytical approaches for robust identification and quantification, and the ability to use environmentally relevant test materials in (eco)toxicity testing and hazard assessment. Here, we present a strategy towards the development of a potential NP reference material based on nano-sized polyproplyene particles (nanoPP) developed within the EURAMET-funded PlasticTrace project (https://plastictrace.eu/). The strategy includes the preparation, the physicochemical characterization and the stability assessment of nanoPP in suspension both in its pristine state, but also when spiked into complex matrices like mineral water and milk. NanoPP was produced reproducibly in a top-down approach by crushing in acetone with an UltraTurrax, filtering and change of solvent to MilliQ water. The prepared nanoPP material was subjected to a comprehensive physicochemical characterization including e.g., DLS, PTA and AF4-MALS for particle size distribution assessment, PTA and SEM for particle number concentration determination, SEM and AFM for shape analysis and pyrolysis GC-MS for chemical identification. Performed studies showed that the prepared nanoPP material is irregularly shaped and highly polydisperse with a particle size of around 180 nm (e.g., Dh,z-ave from DLS) and a particle size distribution from around 15 nm up to 135 nm (radius of gyration Rg from AF4-MALS). Storage stability studies using DLS, PTA and AF4-MALS revealed nanoPP in aqueous suspension to be stable for at least 22 months with respect to particle size distribution and number concentration rendering it a promising NP candidate reference material. However, conducted spiking experiments in mineral water and milk showed a time-dependent agglomeration of nanoPP that needs further investigation. T2 - MICROPLASTICdays CY - Ljubliana, Slovenia DA - 03.02.2026 KW - Nanoplastics KW - Reference materials PY - 2026 AN - OPUS4-65769 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -