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 - 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 - Jahnke, Annika A1 - Beck, Aaron J. A1 - Becker, Richard L. A1 - Bedulina, Daria A1 - Braun, Ulrike A1 - Gerdts, Gunnar A1 - Hildebrandt, Lars A1 - Joerss, Hanna A1 - Klein, Ole A1 - Korduan, Janine A1 - Laforsch, Christian A1 - Lannig, Gisela A1 - Leslie, Heather A. A1 - Lips, Stefan A1 - Menger, Frank A1 - Nabi, Deedar A1 - Oberbeckmann, Sonja A1 - Primpke, Sebastian A1 - Pröfrock, Daniel A1 - Ramsperger, Anja F.R.M. A1 - Römerscheid, Mara A1 - Schmitt-Jansen, Mechthild A1 - Scholz-Böttcher, Barbara M. A1 - Tröppner, Oliver A1 - Wendt-Potthoff, Katrin A1 - Kühnel, Dana T1 - Perspective article: Multisectoral considerations to enable a circular economy for plastics N2 - Plastics are widely used but improper disposal and release lead to increasing global pollution, threatening environmental and human health. To address this issue, we suggest intersectoral collaboration to achieve zero plastic pollution. The outcomes of the project P-LEACH demonstrated the enormous complexity and range of potential toxic effects of plastic-associated chemicals and micro-/nanoplastics released into water from UV-weathered plastics. We initiated an intersectoral dialogue amongst scientists, manufacturers, regulators and representatives of civil society about how to alleviate the negative impacts of plastic pollution. Circular economy offers a framework for selecting non-toxic chemicals, extending product (re)use, and waste reduction, which act to alleviate pollution when applied to plastics. We suggest three measures to advance a circular economy of plastics: 1.) Increase simplicity of chemicals in virgin plastics combined with transparent information on the contents; 2.) Consider recyclability already in plastic material and product design; 3.) Foster communication through intersectoral dialogue. Major cornerstones are the provision of standardized, easy-to-use tools to characterize plastics and plastic leachates chemically and (eco)toxicologically, the enhancement of citizen awareness enabling them to make informed choices, the creation of economic incentives for manufacturers, and sector-specific regulations to provide products that safeguard environmental and human health. KW - Plastics KW - Circular economy KW - Cross-sectoral dialogue KW - Recyclability KW - Plastic-associated chemicals PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638280 DO - https://doi.org/10.1016/j.jhazmat.2025.139326 SN - 0304-3894 VL - 496 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-63828 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Braun, Ulrike T1 - Wirkungsmechanismen von Rotem Phosphor als Flammschutzmittel in Thermoplasten N2 - Das Brandverhalten von Rotem Phosphor in HIPS, PBT und PA66 wurde untersucht. Es wurde gezeigt, wie die Wirksamkeit von Rotem Phosphor in HIPS and PBT durch Kombination mit anderen Flammschutzmitteln zu verbessern ist. N2 - Polymers are flammable due to their chemical nature. As a consequence they must be treated with flame-retardants before they can be used in fields with high flammability risks, such as transport, electronic devices and building construction. The use of red phosphorus as a fire retardant has been encouraged because it is an environmentally friendly alternative to halogenated compounds. The intention of this thesis was to evaluate the potential of red phosphorus as a flame retardant and to determine its fire-retardant mechanisms in different thermoplastics. The thermal decomposition and combustion behaviour of HIPS, PBT and PA66 containing red phosphorus was studied. It further investigated how the activity and efficiency of red phosphorus in HIPS and PBT was influenced by additional flame retardants such as melamine polyphosphate, melamine cyanurate and magnesium hydroxide. The decomposition process was characterized by means of different thermogravimetric methods (TG-FTIR, TG-MS), and the combustion behaviour by cone calorimeter measurements at various external heat fluxes. The flammability was investigated with LOI and the residue of combustion was analysed by means of XPS. Based on these results models for decomposition process were postulated. Red phosphorus can act both by promoting char formation in the condensed phase, and through radical trapping in the gas phase. Red phosphorus acts in the condensed phase in PA66, and in the gas phase in HIPS. In PBT both mechanisms were observed, depending on the pH value. When red phosphorus is combined with fuel-dilution additives such as melamine species in HIPS and PBT, both flame retardants act independently. The combustion behaviour of the combined material can be described by superposition of the distinct flame-retarded materials. In the presence of a barrier former, such as magnesium hydroxide in HIPS, the gas-phase mechanism of red phosphorus remains unaffected; however, a slight anti-synergism results. This is based on formation of a magnesium phosphate barrier, which influences the efficiency of phosphorus as a radical trap. The results showed that the activity of phosphorus as a flame retardant in thermoplastics depends on the water content of the polymer, the pH value and the presence of functional groups in the polymer. The efficiency of phosphorus as a flame retardant in the condensed and gas phases depends on combustion conditions. T3 - BAM Dissertationsreihe - 10 KW - Roter Phosphor KW - Flammschutzmittel KW - Thermoplasten PY - 2005 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-1486 SN - 978-3-86509-303-5 SN - 1613-4249 VL - 10 SP - 1 EP - 164 PB - Wirtschaftsverlag NW CY - Bremerhaven AN - OPUS4-148 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wander, Lukas A1 - Vianello, A. A1 - Vollertsen, J. A1 - Westad, F. A1 - Braun, Ulrike A1 - Paul, Andrea T1 - Exploratory analysis of hyperspectral FTIR data obtained from environmental microplastics samples N2 - Hyperspectral imaging of environmental samples with infrared microscopes is one of the preferred methods to find and characterize microplastics. Particles can be quantified in terms of number, size and size distribution. Their shape can be studied and the substances can be identified. Interpretation of the collected spectra is a typical problem encountered during the analysis. The image datasets are large and contain spectra of countless particles of natural and synthetic origin. To supplement existing Analysis pipelines, exploratory multivariate data analysis was tested on two independent datasets. Dimensionality reduction with principal component analysis (PCA) and uniform manifold approximation and projection (UMAP) was used as a core concept. It allowed for improved visual accessibility of the data and created a chemical two-dimensional image of the sample. Spectra belonging to particles could be separated from blank spectra, reducing the amount of data significantly. Selected spectra were further studied, also applying PCA and UMAP. Groups of similar spectra were identified by cluster analysis using k-means, density based, and interactive manual clustering. Most clusters could be assigned to chemical species based on reference spectra. While the results support findings obtained with a ‘targeted analysis’ based on automated library search, exploratory analysis points the attention towards the group of unidientified spectra that remained and are otherwise easily overlooked. KW - Microplastics KW - FTIR KW - Exploratory analysis PY - 2020 DO - https://doi.org/10.1039/c9ay02483b VL - 12 IS - 6 SP - 781 EP - 791 PB - Royal Society of Chemistry AN - OPUS4-50396 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - 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 - Paul, Andrea A1 - Breitfeld, S. A1 - Sauer, Andreas A1 - Becker, Roland A1 - Kalbe, Ute A1 - Bremser, Wolfram A1 - Braun, Ulrike T1 - A Raman spectroscopic method for the monitoring of microplastics in soil N2 - Due to the increasing presence of microplastic particles (MP) in the Environment and the unknown risks arising from them, there is an urgent need for analytical methods that allow for an efficient identification and quantification of microplastics (MP), i.e. particles < 5 mm, in environmental samples. So far, mostly timeconsuming (micro) infrared or micro-Raman spectroscopic methods are applied. Here an faster alternative Approach is presented based on a Raman processspectrometer with fiber-optical probes in combination with multivariate data analysis. T2 - 12. Kolloquium Prozessanalytik CY - Berlin, Germany DA - 28.11.2016 KW - Raman spectroscopy KW - Microplastics KW - Soil KW - Chemometrics KW - PLS-DA PY - 2016 SP - P10, 59 EP - 60 AN - OPUS4-38392 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 - 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 - 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 -