TY - CONF A1 - Mesquita Silva da Veiga, Marcia T1 - Ultrasonic-assisted leaching of Li and Co from black mass using deep eutectic solvent N2 - The recovery of critical metals from spent lithium-ion batteries is a key strategy for sustainable resource management and the circular economy. Conventional hydrometallurgical processes typically rely on strong mineral acids and elevated temperatures, which, although effective, generate hazardous waste and demand high energy inputs. As a greener alternative, deep eutectic solvents (DES) combine low toxicity, non-volatility, simple synthesis, and tunable physicochemical properties, making them promising media for selective metal recovery1-2. Here, we report for the first time the use of ultrasound (US) to assist the leaching of Li and Co from LiCoO₂ black mass employing a deep eutectic solvent based on choline chloride and formic acid (ChCl:HCOOH, 1:2 molar ratio). The DES was synthesized at 90 °C for 3 h under stirring (300 rpm) and was characterized in terms of its molecular structure and formation by 1H-NMR and FT-IR, as well as by its viscosity and density. For each experiment, ~0.100 g of LiCoO2 was treated with 5 g of DES-FA in an ultrasonic bath (35 kHz, 60 °C) for different irradiation times (30–120 min), followed by three sequential extractions. All measurements were performed by ICP OES. Lithium solubilization reached ~80% at 90 min, while cobalt extraction was stabilizing at ~79% after 120 min. The enhanced performance under US is attributed to sonochemical effects that promote cavitation and microjets, leading to the disruption of particle agglomerates, the thinning of diffusion layers, and the generation of highly reactive local environments. These processes accelerate deintercalation and mass transfer within the solid–liquid interface. Combined with the mild acidity of DES-FA, which enables simultaneous leaching of both metals while favoring faster kinetics for Li, ultrasound provided a synergistic effect that enhanced the overall process and preserved the distinct extraction profiles of Li and Co. The extraction behavior of the two metals can be explained by their different speciation in the DES-FA medium. Cobalt is likely reduced from Co(III) to Co(II) by formic acid and stabilized through the formation of chloro-complexes such as [CoCl4]2- with chloride anions from ChCl, favoring its solubilization. In contrast, lithium does not form stable complexes with chloride under these conditions. It is primarily extracted as a solvated cation, stabilized by the extensive hydrogen-bond network of the DES. This difference accounts for the faster leaching kinetics observed for Li compared to Co. Selective recovery was achieved by pHcontrolled precipitation, with cobalt oxalate at pH 4-5 and lithium carbonate at pH 10. The Eco-Scale score of 85 confirmed the greenness of the method. This pioneering approach highlights the potential of coupling DES chemistry with ultrasound. Together, they represent a sustainable and efficient route for recovering critical metals from battery waste. T2 - 17th Rio Symposium on Atomic Spectrometry (17th RSAS) CY - São Pedro City, Brazil DA - 09.11.2025 KW - Black mass KW - deep eutectic solvent KW - Lithium KW - Cobalt KW - Lithium-ion battery recycling KW - Ultrasound-assisted extraction KW - Lithium and cobalt recovery KW - Green hydrometallurgy PY - 2025 AN - OPUS4-64956 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klinge, A A1 - Mönig, J A1 - Ziegert, C A1 - Richter, Matthias A1 - Kalbe, Ute A1 - Horn, Wolfgang A1 - Röhlen, U A1 - Rauscher, S A1 - Roswag-Klinge, E T1 - upMIN 100 – upcycling of mineral construction and demolition waste to substitute natural aggregates in earthen building materials N2 - The construction sector is one of the most resource-intensive sectors in Germany and is responsible for 40 % of CO2 emissions. Around 517 million tons of mineral raw materials are required annually for the construction of buildings in Germany. At the same time, mineral construction waste was the largest material flow at 229.3 million tons (2020). The rates of construction and demolition waste (CDW) recycling have increased since 2000, especially for mineral waste. Nevertheless, the majority of recycled aggregates are used in technically largely unregulated applications (e.g. road construction). This downcycling leads to a loss of valuable resources for technically and economically valuable applications. The upMIN 100 research project is investigating the question of whether and to what extent recycled CDW is suitable as an additive an binder in earthen building materials. The focus is placed on grain sizes of < 2 mm, which are currently predominantly landfilled, as there are at present no regulations for their use in building products. The soil matrix of earthen building materials however, naturally contains of different grain sizes, whith < 2mm – 0,063 for aggregates and < 0.063 mm as a binder. Therefore, the focused grain sizes (sand, clay and silt) could have a high usage potential. In order to enable the use of CDW, the technical feasibility must be ensured, quality requirements for source materials (e.g. threshold values for pollutants in terms of health and environmental compatibility and hazardous substances) and permissible proportions of recycled aggregates must be defined. Two different building material developments (earth blocks and -plaster)were used to assess both, the technical feasibility as well the pollutant content of the recycled aggregate and its final emissions into the indoor air. For both materials two mixtures could be established, that also meet the mechanical specifications according to the DIN standard, such as the compressive strength. A method was developed to design material mixtures with a high amount of CDW that comply with the defined limit values. The mixtures reached a recycling rate of 28 % with high mechanical properties and 70 % with minimum strength requirements. KW - Mineral waste KW - Upcycling KW - Earthen building product KW - Circular construction PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652831 DO - https://doi.org/10.1088/1755-1315/1554/1/012084 SN - 1755-1307 VL - 1554 IS - 1 SP - 1 EP - 9 PB - IOP Publishing AN - OPUS4-65283 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weimann, Karin A1 - Farago, Patrick A1 - Mayer, Felix ED - Angulo, Sergio ED - Landmann, Mirko T1 - New sources for secondary gypsum N2 - In order to protect natural gypsum deposits and to compensate for the decreasing amount of Flue Gas Desulfurization (FGD) gypsum it is necessary to develop and explore new sources of gypsum. For this purpose, the potentials of different gypsum wastes are investigated in the study “GipsRec 2.0”, funded by the Federal Ministry of Education and Research (Germany). On the one hand, the project worked on a new processing technology for gypsum fiberboards (GFB). While the recycling of gypsum plasterboards has already been carried out on an industrial scale for several years, the recycling of gypsum fiberboards (GFB) has proven to be challenging. Gypsum fiberboards from demolition sites and offcuts from GFB production were used for these investigations. The tests were conducted on a technical scale. Furthermore, various synthetic gypsums are being investigated with regard to their suitability for gypsum production. The analyses are carried out on production residues. In this project, a promising process for gypsum fiberboard recycling could be developed, as well as other waste gypsums are investigated and evaluated with regard to their potential as secondary raw material. In addition, selected process routes are assessed for their environmental impact using a life cycle assessment (LCA) approach. T2 - RILEM - V International Conference Progress of Recycling in the Built Environment CY - Weimar, Germany DA - 10.10.2023 KW - Gypsum recycling KW - Gypsum fiberboards and synthetic gypsum KW - Environmental evaluation PY - 2023 VL - V SP - 1 EP - 10 PB - RILEM Publications Sarl CY - Bagneux, France AN - OPUS4-60315 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stolar, Tomislav A1 - Alić, Jasna A1 - Casali, Lucia A1 - Gugin, Nikita A1 - Baláž, Matej A1 - Michalchuk, Adam A1 - Emmerling, Franziska ED - Stolar, Tomislav T1 - Mechanochemistry: Looking back and ahead N2 - Starting with the discovery of fire and the preparation of food in prehistoric times, mechanochemistry is the oldest form of chemistry that humans have controlled. Mechanochemical practices, such as grinding with a mortar and pestle, continued into the Middle Ages until dedicated scientific studies began in the 19th century. Since then,research in mechanochemistry has shown that many chemicalreactions can be performed via mechanical force without or with small amounts of solvent. Besides being time, material, and energy efficient, mechanochemical reactions often yield products that differ from those obtained in solution. Therefore, not only is mechanochemistry greener and more sustainable than conventional solution chemistry, but it also has the added value of providing new reactivity and selectivity. This is especially important today, when chemists need to invent high-performance materials, intermediates, and products with the use of sustainable feedstocks and develop environmental remediation pathways. At the same time, time-resolved in situ monitoring and computational modeling are necessary for addressing fundamental questions about the atomistic, molecular, and electronic nature of mechanochemical reactivity. Integrating digitalization, robotics, and artificial intelligence tools promises to increase the reproducibility and scalability of mechanochemical processes. Further evolution of mechanochemistry is expected to have a transformative effect on the chemical industry. KW - Mechanochemistry PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653962 DO - https://doi.org/10.1016/j.chempr.2025.102880 SN - 2451-9294 VL - 12 IS - 2 SP - 1 EP - 27 PB - Elsevier BV AN - OPUS4-65396 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ryll, Tom William T1 - Researching automation of gypsum recycling N2 - This poster illustrates the recent work on a setup for automated in-situ analysis of gypsum recycling processes. Analysis in synchrotron X-rays, Raman- and UV-vis spectroscopy are made possible with this compact and mobile setup. First results from Raman spectroscopy on the conversion of gypsum to bassanite in hypersaline solutions are presented and future plans on optimization are formulated. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Recycling KW - Automation KW - Synchrotron-X-ray-diffraction KW - Raman-spectroscopy KW - Gypsum PY - 2025 AN - OPUS4-62706 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dudziak, Mateusz A1 - Riechers, Birte A1 - Maaß, Robert A1 - Michalchuk, Adam A1 - Schönhals, Andreas A1 - Szymoniak, Paulina T1 - Beyond conventional calorimetry: Unlocking thermal characterization with fast scanning techniques N2 - Fast scanning calorimetry (FSC) has emerged as a transformative technique in thermal analysis, enabling the investigation of rapid and kinetically driven thermal transitions that are inaccessible to conventional differential scanning calorimetry. This review highlights the capabilities enabled by FSC for studying a wide range of materials under extreme thermal conditions, including polymers, pharmaceuticals, metallic glasses, nanocomposites, and hydrogels. By employing ultrafast heating and cooling rates, FSC allows for the suppression of crystallization, resolution of weak transitions, and analysis of thermally labile or size-limited samples. The technique is particularly valuable for probing glass transitions, relaxation phenomena, and phase behavior in systems with complex morphologies or confined geometries. Case studies demonstrate the use of FSC in characterizing vitrification, physical aging, and interfacial dynamics, as well as its application in emerging fields such as additive manufacturing, supramolecular systems, and neuromorphic materials. Together, these examples underscore the role that FSC plays in advancing the understanding of structure-property relationships across diverse material classes. KW - Flash DSC KW - Calorimetry KW - Glass transition PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647405 DO - https://doi.org/10.1016/j.tca.2025.180177 VL - 754 SP - 1 EP - 14 PB - Elsevier B.V. AN - OPUS4-64740 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stawski, Tomasz A1 - Karafiludis, Stephanos A1 - Pimentel, Carlos A1 - Montes-Hernández, German A1 - Kochovski, Zdravko A1 - Bienert, Ralf A1 - Weimann, Karin A1 - Emmerling, Franziska A1 - Scoppola, Ernesto A1 - Van Driessche, Alexander E.S. T1 - Solution-driven processing of calcium sulfate: The mechanism of the reversible transformation of gypsum to bassanite in brines N2 - Here, we show that calcium sulfate dihydrate (gypsum) can be directly, rapidly and reversibly converted to calcium sulfate hemihydrate (bassanite) in high salinity solutions (brines). The optimum conditions for the efficient production of bassanite in a short time (<5 min) involve the use of brines with c(NaCl) > 4 M and maintaining a temperature, T > 80 °C. When the solution containing bassanite crystals is cooled down to around room temperature, eventually gypsum is formed. When the temperature is raised again to T > 80 °C, bassanite is rapidly re-precipitated. This contrasts with the better-known behaviour of the bassanite phase in low-salt environments. In low-salinity aqueous solutions, bassanite is considered to be metastable with respect to gypsum and anhydrite, and therefore gypsum-to-bassanite conversion does not occur in pure water. Interestingly, the high-salinity transformation of gypsum-to-bassanite has been reported by many authors and used in practice for several decades, although its very occurrence actually contradicts numerical thermodynamic predictions regarding solubility of calcium sulfate phases. By following the evolution of crystalline phases with in situ and time-resolved X-ray diffraction/scattering and Raman spectroscopy, we demonstrated that the phase stability in brines at elevated temperatures was inaccurately represented in the thermodynamic databases. Most notably for c(NaCl) > 4 M, and T > 80 °C gypsum becomes readily more soluble than bassanite, which induces the direct precipitation of the latter from gypsum. The fact that these transformations are controlled by the solution provides extensive opportunities for precise manipulation of crystal formation. Our experiments confirmed that bassanite remained the sole crystalline phase for many hours before reverting into gypsum. This property is extremely advantageous for practical processing and efficient crystal extraction in industrial scenarios. KW - Industrial and Manufacturing Engineering KW - Strategy and Management KW - General Environmental Science KW - Renewable Energy, Sustainability and the Environment KW - Building and Construction KW - Calcium sulfate KW - Gypsum KW - Bassanite KW - Scattering KW - Raman KW - In situ KW - Synchrotron KW - BESSY KW - MySpot PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594698 UR - https://www.sciencedirect.com/science/article/pii/S0959652624004591#appsec1 DO - https://doi.org/10.1016/j.jclepro.2024.141012 SN - 0959-6526 VL - 440 SP - 1 EP - 12 PB - Elsevier B.V. AN - OPUS4-59469 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Béalu, Zoé A1 - Walther, Johanna A1 - Abusafia, Attaallah A1 - Altmann, Korinna A1 - Meurer, Maren A1 - Gretzschel, Oliver A1 - Schäfer, Michael A1 - Steinmetz, Heidrun T1 - Removal of Organic Micropollutants and Microplastics via Ozonation Followed by Granular Activated Carbon Filtration N2 - Discharge from Wastewater Treatment Plants (WWTPs) can result in the emission of organic micropollutants (OMPs) and microplastics (MPs) into the aquatic environment. To prevent this harmful release, a pilot plant consisting of an ozonation followed by a granular activated carbon (GAC) filter was operated at a WWTP in Germany, and its side-effects on the concentrations of nitrogen (N) and phosphorous (P) compounds were measured. Over 80% of OMPs and transformation products were removed during the operating time (around 6000 bed volumes) no matter the ozone dose (from around 0.1 to 0.5 mgO3/mgDOC), except for Diatrizoic acid, whose breakthrough appeared at 3500 BV. Formation of the oxidation by-product, NDMA, increased with higher ozone doses, but the concentration remained below 100 ng/L. Bromate was formed at a higher ozone dose (0.4 mgO3/mgDOC) but at a low concentration—below 10 µg/L. The MP particles detected in the inflow (PE, SBR, PP, and PS) were effectively eliminated to a high degree, with a removal rate of at least 92%. Carbon parameters (COD, DOC, and SAC254) were removed further by the pilot plant, but to different extents. As expected, nitrate was formed during ozonation, while nitrite’s concentration decreased. Further, nitrite decreased and nitrate increased within the GAC filter, while ammonium was eliminated by at least 90%. Total P concentration decreased after the pilot, but the concentration of PO4-P increased. KW - Microplastics KW - TED-GC/MS KW - Granular Activated Carbon Filtration KW - Removal of Organic Micropollutants KW - Wastewater treatment plant PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-615209 DO - https://doi.org/10.3390/environments11110241 VL - 11 IS - 11 SP - 1 EP - 38 PB - MDPI AG AN - OPUS4-61520 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ciornii, Dmitri A1 - Hodoroaba, Vasile-Dan A1 - Wachtendorf, Volker A1 - Fengler, Petra A1 - Altmann, Korinna T1 - Interlaboratory Comparison Reveals State of the Art in Microplastic Detection and Quantification Methods N2 - In this study, we investigate the current accuracy of widely used microplastic (MP) detection methods through an interlaboratory comparison (ILC) involving ISO-approved techniques. The ILC was organized under the prestandardization platform of VAMAS (Versailles Project on Advanced Materials and Standards) and gathered a large number (84) of analytical laboratories across the globe. The aim of this ILC was (i) to test and to compare two thermo-analytical and three spectroscopical methods with respect to their suitability to identify and quantify microplastics in a water-soluble matrix and (ii) to test the suitability of the microplastic test materials to be used in ILCs. Two reference materials (RMs), polyethylene terephthalate (PET) and polyethylene (PE) as powders with rough size ranges between 10 and 200 μm, were used to press tablets for the ILC. The following parameters had to be assessed: polymer identity, mass fraction, particle number concentration, and particle size distribution. The reproducibility, SR, in thermo-analytical experiments ranged from 62%−117% (for PE) and 45.9%−62% (for PET). In spectroscopical experiments, the SR varied between 121% and 129% (for PE) and 64% and 70% (for PET). Tablet dissolution turned out to be a very challenging step and should be optimized. Based on the knowledge gained, development of guidance for improved tablet filtration is in progress. Further, in this study, we discuss the main sources of uncertainties that need to be considered and minimized for preparation of standardized protocols for future measurements with higher accuracy. KW - Microplastics KW - Interlaboratory comparison KW - PlasticsFatE KW - PET KW - PE KW - Reference materials KW - VAMAS KW - Thermo-analytical methods KW - Spectroscopical methods PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630462 DO - https://doi.org/10.1021/acs.analchem.4c05403 SN - 1520-6882 VL - 97 SP - 8719 EP - 8728 PB - ACS Publications AN - OPUS4-63046 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Herzel, Hannes A1 - Grevel, K.-D. A1 - Emmerling, Franziska A1 - Dachs, E. A1 - Benisek, A. A1 - Adam, Christian A1 - Majzlan, J. T1 - Thermodynamic properties of calcium alkali phosphates Ca(Na,K)PO4 N2 - Calcium alkali phosphates Ca(Na,K)PO4 are main constituents of bioceramics and thermochemically produced phosphorus fertilizers because of their bioavailability. Sparse thermodynamic data are available for the endmembers CaNaPO4 and CaKPO4. In this work, the missing data were determined for the low-temperature phase modifications of the endmembers CaNaPO4 and CaKPO4 and three intermediate Ca(Na,K)PO4 compositions. Standard enthalpy of formation ranges from - 2018.3 ± 2.2 kJ mol-1 to - 2030.5 ± 2.1 kJ mol-1 and standard entropy from 137.2 ± 1.0 J mol-1 K-1 to 148.6 ± 1.0 J mol-1 K-1 from sodium endmember b-CaNaPO4 to potassium endmember b0-CaKPO4. Thermodynamic functions are calculated up to 1400 K for endmembers and the sodium-rich intermediate phase b-Ca(Na0.93K0.07)PO4. Functions above 640 K are extrapolated because of the phase transition from low- to high-temperature phase. Impurities in the synthesized intermediate phases c-Ca(Na0.4K0.6)PO4 and c-Ca Na0.35K0.65)PO4 and one additional phase transition around 500 K impeded the determination of high-temperature thermodynamic functions. In general, data for phase transition temperatures agree with the previously reported phase diagrams. KW - Formation enthalpy KW - Heat capacity KW - Phase transformation KW - Bioceramics KW - Phosphorus fertilizer KW - Entropy PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507640 DO - https://doi.org/10.1007/s10853-020-04615-5 VL - 55 SP - 8477 EP - 8490 PB - Springer AN - OPUS4-50764 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stawski, Tomasz T1 - Processing of calcium sulfate in brines N2 - Calcium sulfate hemihydrate (CaSO4·0.5H2O), also known as bassanite or "plaster of Paris", serves as a precursor for the production of gypsum (dihydrate, CaSO4·2H2O), widely used in construction. Currently, ~200 MT of calcium sulfate are consumed annually. Bassanite is obtained from gypsum through a solid-state thermal treatment in kilns at temperature ranging from 150 °C to 200 °C. We introduce a more efficient and sustainable method (T < 100 ºC) that enables the direct, rapid, and reversible conversion of gypsum to bassanite using reusable high salinity aqueous solutions (brines with c[NaCl] > 4 M). These transformations are controlled by the properties of the solution, offering extensive opportunities for precise manipulation of crystal formation and recycling of gypsum waste. T2 - BESSY User Meeting 2024 CY - Berlin, Germany DA - 12.12.2024 KW - Gypsum PY - 2024 AN - OPUS4-62095 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Herzel, Hannes T1 - Phase reaction during thermochemical treatment of sewage sludge and biomass ashes with alkali compounds to increase nutrient plant availability N2 - Das Element Phosphor ist für Pflanzen, Tiere und Menschen essenziell. Um die Phosphorversorgung für Pflanzen in der Landwirtschaft zu gewährleisten, werden Phosphordünger eingesetzt. Die Nährstoffe werden hauptsächlich durch Wirtschaftsdünger (Gülle, Jauche, Stallmist) zurückgeführt. Zusätzlich werden in der konventionellen Landwirtschaft mineralische Phosphordünger eingesetzt, die vorwiegend aus dem fossilen Rohstoff Phosphorit gewonnen werden. Um die Abhängigkeit von fossilen Rohstoffen zu reduzieren, sollen nährstoffhaltige Rest- und Abfallstoffe zur Phosphordünger aufbereitet werden. In Abwasserkläranlagen fällt phosphorreicher Klärschlamm als Abfallstoff an. Der größte Anteil des Klärschlammes wird in Steinkohlekraftwerken, Zementwerken oder in Monoklärschlammverbrennungsanlagen verbrannt. Die Klärschlammaschen aus den Monoverbrennungsanlagen enthalten bis zu 12 Gew.-% Phosphor und sind daher für die Düngerherstellung geeignet. Ein geeignetes Verfahren zur Aufbereitung der Klärschlammaschen ist die thermochemische Behandlung im Drehrohrofen. Mit dem sogenannten AshDec®-Prozess, kann ein Phosphordünger hergestellt werden. Aktuell wird eine großtechnische Anlage in Altenstadt (Bayern) geplant, die im Jahr 2023 den Betrieb aufnehmen soll. Der zentrale Bestandteil ist die Phasenumwandlung von schlecht pflanzenverfügbaren Phosphaten in der Klärschlammasche (vorwiegend das Calciumphosphat Whitlockit und Aluminiumphosphat) zu gut pflanzenverfügbaren Calciumalkaliphosphaten im Produkt. Um dies zu erzielen, werden die Aschen mit Natrium- und/oder Kalium-Verbindungen gemischt und einer thermochemischen Behandlung bei 800-1000 °C zugeführt. Um die Pflanzenverfügbarkeit und Düngewirkung von Phosphaten abschätzen zu können, ist die chemische Extraktionsmethode mit neutraler Ammoniumcitratlösung geeignet. In der Dissertation werden die (Phosphor-)Phasenreaktionen und die Prozessbedingungen des thermochemischen Verfahrens untersucht, um das Verfahren gezielt zu modifizieren und die Wirtschaftlichkeit zu steigern. Die Zielphasen der thermochemischen Behandlung sind die Calciumalkaliphosphate CaNaPO4 und CaKPO4, und deren Mischphasen Ca(Na,K)PO4, welche in der Publikation 3.1 synthetisiert wurden. Für diese Calciumalkaliphosphate wurden die thermodynamischen Daten der Standardbildungsenthalpie, Standardentropie, Wärmekapazität und die Wärmemenge der Phasenumwandlung bestimmt (Publikation 3.1). Bei der thermochemischen Behandlung von Klärschlammaschen wurden als Additive Natrium- und Kaliumsulfat bei verschiedenen Temperaturen getestet. Der Einsatz von Kaliumadditiven ist erwünscht, um den Marktwert des Produktes durch die Produktion eines Phosphor-Kalium-Düngers zu erhöhen. Zusätzlich wird eine möglichst geringe Prozesstemperatur angestrebt, bei der die erwünschten Calciumalkaliphosphate gebildet werden. In den Publikationen 3.2 und 3.3 wird gezeigt, dass für Klärschlammaschen eine komplette Phasenumwandlung zu Calciumnatriumphosphaten ab 875 °C in Laborversuchen (Korundtiegel) mit dem Additiv Natriumsulfat erzielt werden kann. Der Einsatz von Kaliumsulfat erforderte notwendige Reaktionstemperaturen von über 1100 °C. Diese unterschiedlichen Reaktionstemperaturen hängen mit den Schmelzpunkten von Natriumsulfat (890 °C) und Kaliumsulfat (1070 °C) zusammen. Um Kaliumsulfat in den Prozess bei niedrigen Temperaturen zu integrieren, wurden Natriumsulfat und Kaliumsulfat vor der Behandlung gemischt. Dies führte zu einer Schmelzpunkterniedrigung und resultierte in Reaktionstemperaturen zwischen 900 °C bis 1000 °C für die untersuchten Mischungen von Natrium- und Kaliumsulfat (Publikation 3.3). Die Zusammensetzung der Calciumalkaliphosphate Ca(Na,K)PO4 war anders als erwartet. Bei der Phasenanalytik stellte sich heraus, dass bei geringem und mittlerem Anteil von Kaliumsulfat im Alkali-Additiv nur Calciumnatriumphosphate mit sehr geringen Kaliumgehalten gebildet wurden. Erst bei einem hohen Anteil von Kaliumsulfat in der Mischung der Alkalisulfate konnten kaliumhaltige Calciumalkaliphosphate nachgewiesen werden (u.a. (Ca0.9Mg0.1)(Na0.6K0.4)PO4). Dieser geringere Einbau von Kalium in die Calciumalkaliphosphate hängt mit den zusätzlich stattfindenden Reaktionen zwischen den Alkalien und den Silikaten zusammen. Es ist bekannt, dass die zugegebenen Alkalisulfate zuerst mit Silikaten und anschließend mit den Phosphaten reagieren. Silikate bauen bevorzugt Kalium ein, deswegen konnten erst kaliumhaltige Phosphate gebildet werden, wenn die Reaktion mit den Silikaten abgeschlossen war. Dies führte zu einem geringeren Kaliumanteil in den gebildeten Phosphaten im Vergleich zum Kaliumanteil der verwendeten Alkaliadditive. Das in Silikaten gebundene Kalium ist wahrscheinlich schlecht für die Pflanzen verfügbar. Dies könnte den Einsatz der produzierten Phosphor-Kalium-Dünger einschränken. Der bevorzugte Kaliumeinbau in Silikaten konnte auch in Kalkulationen mit den thermodynamischen Daten aus der Publikation 3.1 gezeigt werden. Mittels Phasenanalytik vor und nach der chemischen Extraktion, konnte die Zugehörigkeit zu verschiedenen Modifikationen der Calciumalkaliphosphaten sicher bestimmt werden und eine ungefähre Zusammensetzung dieser Calciumalkaliphosphate abgeschätzt werden. So konnte nachgewiesen werden, dass die Modifikation vom CaNaPO4 ungefähr 10 % Magnesium einbauen kann. Wenn mehr Magnesium eingebaut wird, bildet sich die Phase (Ca,Mg)NaPO4, die eine vergleichbare Struktur wie die bekannte Phase (Ca0.72Mg0.28)NaPO4 aufweist. Dieses magnesiumreiche Calciumnatriumphosphat entstand vermutlich, wenn entweder erhöhte Anteile an Kalium eingebaut wurden (Ca0.8Mg0.2)(Na0.85K0.15)PO4 (Publikation 3.3) oder die Phasenumwandlung vom Calciumphosphat Whitlockit zum Calciumalkaliphosphat CaNaPO4 noch nicht abgeschlossen war (Publikation 3.2). Wenn mehr Kalium eingebaut wird, dann entsteht eine Phase (u.a. (Ca0.9Mg0.1)(Na0.6K0.4)PO4) ähnlich zu den Mischphasen aus der Publikation 3.1. In den Publikationen 3.4 und 3.5 wurden keine Klärschlammaschen untersucht, sondern Biokohlen aus Modellklärschlämmen (Publikation 3.5) und Biomasseaschen (Publikation 3.4) aus der Vergasung oder Verbrennung einer Mischung aus Zuckerrohrbagasse und Hühnertrockenkot. Die thermochemischen Produkte der Biokohlen bzw. Biomasseaschen enthielten das gewünschte CaNaPO4 und hatten eine hohe Düngewirkung in Pflanzenwachstumsversuchen mit Sojapflanzen bzw. Gräsern. KW - AshDec KW - Recycling fertilizer KW - Calcium alkali phosphate PY - 2020 SP - 1 EP - 186 CY - Jena AN - OPUS4-54724 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stawski, Tomasz T1 - Solution-driven processing of calcium sulfate: the mechanism of the reversible transformation of gypsum to bassanite in brines N2 - Calcium sulfate hemihydrate (CaSO4ᐧ0.5H2O), also known as bassanite, has been used as a precursor to produce gypsum (dihydrate, CaSO4ᐧ2H2O) for various construction and decorative purposes since prehistoric times. The main route to obtain hemihydrate is a thermal treatment of gypsum at temperatures typically between 150 °C and 200 °C to remove some of the structural water. In this contribution, we introduce (Fig. 1) a more efficient and sustainable method (T < 100 °C) that enables the direct, rapid, and reversibly conversion of gypsum to bassanite using reusable high salinity aqueous solutions (brines with c[NaCl] > 4 M). The optimum conditions for the efficientproduction of bassanite in a short time (< 5 min) involve the use of brines with c(NaCl) > 4 M and maintaining a temperature, T > 80 °C. When the solution containing bassanite crystals is cooled down to around room temperature, eventually gypsum is formed. When the temperature is raised again to T > 80 °C, bassanite is rapidly re-precipitated. This contrasts with the typical behaviour of the bassanite phase in low salt environments. Traditionally, hemihydrate is obtained through a solid state thermal treatment because bassanite is considered to be metastable with respect to gypsum and anhydrite in aqueous solutions, and therefore gypsum-to-bassanite conversion should not occur in water. Its very occurrence actually contradicts numerical thermodynamic predictions regarding solubility of calcium sulfate phases. By following the evolution of crystalline phases with in situ and time-resolved X-ray diffraction/scattering and Raman spectroscopy, we demonstrated that the phase stability in brines at elevated temperatures is inaccurately represented in the thermodynamic databases. Most notably for c(NaCl) > 4 M, and T > 80 °C gypsum becomes readily more soluble than bassanite, which induces the direct precipitation of the latter from gypsum. The fact that these transformations are controlled by the solution provides extensive opportunities for precise manipulation of crystal formation. Our experiments confirmed that bassanite remained the sole crystalline structure for many hours before reverting into gypsum. This property is extremely advantageous for practical processing and efficient crystal extraction in industrial scenarios. T2 - Granada Münster Discussion Meeting GMDM 10 CY - Münster, Germany DA - 29.11.2023 KW - Gypsum KW - Bassanite KW - Calcium sulfate KW - Recycling KW - Scattering PY - 2024 AN - OPUS4-59162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geburtig, Anja T1 - Umfassende Analyse von Leachabels aus rezyklierten HDPE-Kanistern N2 - Es wurde untersucht, welche Substanzen aus rHDPE-Post-Consumer-Rezyklat herausgelöst und nachgewiesen werden können (Non-Target-Analytik). Die Substanzen wurden sowohl chemisch als auch anwendungsbezogen systematisiert. Diskutiert wurde die Nutzung der Ergebnisse zur Festlegung von Qualitätskriterien von rHDPE sowie zur Verbesserung des mechanischen Recycling-Prozesses. T2 - 20. Gefahrgut-Technik-Tage CY - Berlin, Germany DA - 13.11.2025 KW - rHDPE KW - Rezyklat KW - Leachables PY - 2025 AN - OPUS4-64852 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ryll, Tom William T1 - In-situ analysis of nucleation processes – case study: calcium sulfate N2 - In this project we investigate nucleation pathways by utilizing synchrotron-XRD and running a case-study on calcium sulfate phases. To accomplish this, we developed a modular automation setup for reactions in solution to run synthesis and control reaction conditions. So far we successfully characterized the recycling process of gypsum and are now investigating the formation of anhydrite. T2 - BESSY@HZB User Meeting CY - Berlin, Germany DA - 02.12.2025 KW - Recycling KW - Gypsum KW - Synchrotron-X-ray-diffraction KW - Raman-spectroscopy KW - Automation PY - 2025 AN - OPUS4-65344 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Herzel, Hannes T1 - Thermochemische P-Rückgewinnungsverfahren in Deutschland zur Düngerproduktion N2 - Die Firma Emter GmbH betreibt die Klärschlammverbrennungsanlage Altenstadt und hat in die bestehende Monoverbrennung einen thermochemischen Prozess integriert, um hochwirksame und schadstoffarme Düngemittel aus Klärschlamm herzustellen. Die Anlage ist aktuell die größte Phosphorrecyclinganlage in Deutschland mit der die Vorgaben der AbfKlärV bereits frühzeitig umgesetzt werden. Das Projekt R-Rhenania begleitet die Phosphorrecyclinganlage mit Untersuchungen zur Produktqualität, mit Gefäßversuchen und Feldversuchen im ökologischen Landbau, mit Ökobilanzierung und der Konfektionierung verschiedener Düngemittelprodukte. Viele Klärschlammaschen haben geringe Schwermetallgehalte und sind geeignet durch vergleiche thermochemische Prozesse behandelt zu werden. Mit den Daten aus dem Klärschlammasche-Monitoring der BAM können die Potentiale für die Verwertung der Aschen in den thermochemischen Prozessen wie AshDec oder CaNaPhos abgeschätzt werden. T2 - DWA Klärschlammnetzwerk Nord-Ost CY - Berlin, Germany DA - 21.01.2026 KW - Phosphor KW - Recycling KW - Thermochemisch KW - Großtechnik PY - 2026 AN - OPUS4-65611 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schlegel, Moritz-Caspar T1 - Die Ökodesign-Rahmenverordnung - Produkteffizienz neu gedacht N2 - Die Präsentation fasst das europäische Verständnis für den Begriff "Produkteffizienz" und die diesbezügliche Entwicklungen der vergangenen Jahre zusammen. Es wird eine Verbindung zwischen Rechtssetzung, Normung und Forschung hergestellt und entsprechende Beiträge zur der Transformation von einer linearen- zu einer zirkulären Wirtschaft (Circular Economy) erörtert. T2 - DIN-Mitgliederdialog CY - Berlin, Germany DA - 03.03.2026 KW - Circular economy KW - Product efficiency KW - Normung KW - Ecodesign KW - Policymaking PY - 2026 AN - OPUS4-65631 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Investigating the Thermal Decomposition of PFAS in a Full-Scale Commercial Hazardous Waste Incinerator N2 - Effective and safe treatment of per- and polyfluoroalkyl substances (PFAS)-laden waste in full-scale hazardous waste facilities is currently the only commercial method for large-scale PFAS destruction, but concerns remain about incomplete combustion and harmful byproducts. Therefore, the fate of fluorine during incineration was investigated in a full-scale hazardous waste incinerator to assess the viability and potential risks of this method. The project involves developing advanced analytical tools, including real-time infrared spectroscopy, and conducting trial burns under varied conditions. Conditions that influence incineration performance are identified, analyzing for products of incomplete destruction (PIDs), exploring the role of fly ash and surfaces in PFAS breakdown, and evaluating the potential formation of polyfluorinated dioxins and furans. Collectively, these tasks aim to deliver practical tools and guidance for scientists and engineers, while informing policymakers and the public on the benefits and potential risks of PFAS incineration. T2 - DoW Applied Innovation Workshop CY - Washington, DC, USA DA - 02.03.2026 KW - Per- and polyfluoroalkyl substances (PFAS) KW - Incineration PY - 2026 AN - OPUS4-65638 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Giovannozzi, A T1 - Metrological traceability of measurement data from nano- to small microplastics for a greener environment and food safety N2 - This talk descibes the EMPIR project PlasticTrace. Reference materials for microplastics will be developed. The production process and characterisation is explained by SEM, Raman, IR, Py-GC/MS and TED-GC/MS. Homogeneity control was successful. Stability check show no changes over 6 month. T2 - SETAC Europe 2024 CY - Sevilla, Spain DA - 05.05.2024 KW - Microplastics KW - Reference materials KW - Polymer 3R KW - TED-GC/MS PY - 2024 AN - OPUS4-60033 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Investigating the Thermal Decomposition of PFAS in a Full-Scale Commercial Hazardous Waste Incinerator (SERDP ER24-4073) N2 - Effective and safe treatment of per- and polyfluoroalkyl substances (PFAS)-laden waste in full-scale hazardous waste facilities is currently the only commercial method for large-scale PFAS destruction, but concerns remain about incomplete combustion and harmful byproducts. Therefore, the fate of fluorine during incineration was investigated in a full-scale hazardous waste incinerator to assess the viability and potential risks of this method. The project involves developing advanced analytical tools, including real-time infrared spectroscopy, and conducting trial burns under varied conditions. Conditions that influence incineration performance are identified, analyzing for products of incomplete destruction (PIDs), exploring the role of fly ash and surfaces in PFAS breakdown, and evaluating the potential formation of polyfluorinated dioxins and furans. Collectively, these tasks aim to deliver practical tools and guidance for scientists and engineers, while informing policymakers and the public on the benefits and potential risks of PFAS incineration. T2 - DoW Applied Innovation Workshop CY - Washington, DC, USA DA - 02.03.2026 KW - Per- and polyfluoroalkyl substances (PFAS) KW - Incineration PY - 2026 AN - OPUS4-65639 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ryll, Tom William T1 - In-situ analysis of nucleation processes – case study: calciumsulfate N2 - In this project we investigate nucleation pathways by utilizing synchrotron-XRD and running a case-study on calcium sulfate and its polymorphs. To accomplish this, we developed a modular automation setup for reactions in solution to run synthesis and control reaction conditions. So far we successfully characterized the recycling process of gypsum (CaSO4*2H2O) and are now investigating the formation of anhydrite (CaSO4*0H2O) as well as possible applications for the automation setup and analysis. T2 - SALSA Make & Measure 2025 CY - Berlin, Germany DA - 10.09.2025 KW - Recycling KW - Gypsum KW - Synchrotron-X-ray-diffraction KW - Raman-spectroscopy KW - Automation PY - 2025 AN - OPUS4-64138 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sanchez-Olivares, Guadalupe A1 - Brehme, Sven A1 - Calderas, F. A1 - Schartel, Bernhard T1 - Flame Retardant Polyolefins Using Fibers From Leather Waste: Adjusting Extrusion Variables to Balance the Property Profile N2 - The extrusion processing variables represent a key to the optimal use of additives and thus the development of flame-retardant polymer composites. Adjusting the property profile, for example, finding a balance between flame retardancy and mechanical properties is the main challenge. In this work, the effect of blending temperature and rotational speed on physico-mechanical properties and fire behavior of polyolefin composites was investigated. High-density polyethylene or polypropylene was used as polymer matrices; the polymers were compounded by the extrusion process using industrial-waste leather fibers as flame retardant adjuvant and commercial flame-retardant additives. A detailed rheological analysis highlighted different viscoelastic behavior, that is, a predominant elastic or viscous one. The effect of the extrusion processing variables was also investigated on the morphology, mechanical properties, thermal decomposition, fire behavior under forced flaming combustion and flammability. Important improvements were revealed with respect to using only high loading of flame retardants. For high-density polyethylene-based composites, impact resistance and elongation at break increased 8 and 7.5 times, respectively. The total heat evolved (87MJ/m2), effective heat of combustion (31.6MJ/kg), flame retardancy (UL 94 rating) results were comparable with the reference sample. Meanwhile for polypropylene composites, the impact resistance increased 2.2 times and the flame retardancy was improved from no rating in the UL 94 vertical test to V-0 rating. Tailored processing was highlighted as an autonomous and powerful approach to achieve balanced and demanding properties. KW - Biomaterials KW - Composites KW - Extrusion KW - Flame retardance KW - Leather waste KW - Polyolefins PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-656732 DO - https://doi.org/10.1002/vnl.70048 SN - 1548-0585 SN - 1083-5601 VL - 32 IS - 2 SP - 410 EP - 430 PB - Wiley Periodicals LLC. AN - OPUS4-65673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wöhlecke, Andreas T1 - Aktuelles aus dem BAM-Fachbeirat N2 - Die Anforderungen an Geokunststoffprodukte und deren Qualitätssicherung unterliegen einem stetigen Wandel, der sowohl durch technische Veränderungen als auch durch normative und organisatorische Entwicklungen geprägt ist. Insbesondere der Fachbeirat der BAM gemäß Deponieverordnung (DepV) spielt hier im Bereich der Deponietechnik eine wichtige Rolle. An dieser Stelle sollen aktuelle Themen aus dem Fachbeirat der BAM vorgestellt werden, die wesentliche Änderungen in der Zulassungs- und Anwendungspraxis betreffen. Der Beitrag beleuchtet unter anderem Veränderungen innerhalb der BAM, die Modernisierung der Publikationsformate sowie die fachliche Weiterentwicklung der Zulassungsrichtlinien. T2 - 22. Leipziger Deponiefachtagung CY - Leipzig, Germany DA - 10.03.2026 KW - Deponie KW - Geotextil KW - Abdichtungssystem PY - 2026 SN - 978-3-00-085899-4 VL - 22 SP - 15 EP - 22 PB - HWTK Leipzig CY - Leipzig AN - OPUS4-65664 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bijeljic, Jelena A1 - Niederleithinger, Ernst T1 - Concrete performance assessment based on gas permeability testing N2 - Designing of structures with medium to high performance requirements is a demanding and challenging engineering task. Depending on the location and type of the planned structure, various pre-testing methods should be applied. In recent decades, there has been a focus on the durability of concrete. Concrete is a porous material with a relatively thin protective cover layer, making it vulnerable to the penetration of external agents such as carbon dioxide. Gas permeability testing (kT), a relatively new non-destructive method (NDT), should therefore be considered. This paper presents results of gas permeability testing on a set of larger concrete samples made under controlled conditions with some paroperty variations order to find initial kT parameters important for quality assurance. KW - Concrete KW - Permeability KW - Durability KW - Torrent Tester PY - 2025 DO - https://doi.org/10.62683/ZRGAF41.2 SN - 3009-4674 VL - 41 IS - 1 SP - 15 EP - 23 PB - Faculty of Civil Engineering and Architecture, University of Nis AN - OPUS4-65715 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ryll, Tom William T1 - Multi-modal characterization for transformation of gypsum to anhydrite N2 - We investigate recycling of gypsum waste materials and have developed a method to synthesize phase pure anhydrite in solution, while contaminants could easily be separated from products. In-situ XRD measurements were conducted in a dedicated automation setup at BESSY II to find exact reaction conditions and were supported by in-situ Raman spectroscopy. T2 - Joint BAM-HZB Symposium on Multimodal Synchrotron Experiments for Next-Generation Materials Research CY - Berlin, Germany DA - 25.02.2026 KW - Recycling KW - Automation KW - Synchrotron XRD KW - Raman spectroscopy KW - Gypsum PY - 2026 AN - OPUS4-65607 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chandna, Sanjam A1 - Povolotsky, Tatyana L. A1 - Nie, Chuanxiong A1 - Schwartz, Sophia A1 - Wedepohl, Stefanie A1 - Quaas, Elisa A1 - Ludwig, Kai A1 - Boyakova, Yulia A1 - Bhatia, Sumati A1 - Meyer, Klas A1 - Falkenhagen, Jana A1 - Haag, Rainer A1 - Block, Stephan T1 - Lignin-Based Mucus-Mimicking Antiviral Hydrogels with Enzyme Stability and Tunable Porosity N2 - Mucus is a complex hydrogel that acts as a defensive and protective barrier in various parts of the human body. Therise in the level of viral infections has underscored the importance of advancing research into mucus-mimicking hydrogels for theefficient design of antiviral agents. Herein, we demonstrate the gram-scale synthesis of biocompatible, lignin-based virus-bindinginhibitors that reduce waste and ensure long-term availability. The lignin-based inhibitors are equipped with sulfate moieties, whichare known binding partners for many viruses, including SARS-CoV-2 and herpes viruses. In addition, cross-linking the synthesizedinhibitors yielded hydrogels that mimicked native mucus concerning surface functionality and rheology. The degree of sulfationexhibits a very strong impact on the mesh size distribution of the hydrogels, which provides a new means to fine-tune the steric andelectrostatic contributions of the virus−hydrogel interaction. This feature strongly impacts the sequestration capability of the lignin-based hydrogels, which is demonstrated by infection inhibition assays involving human herpes simplex virus 1, influenza A viruses,and the bacterium Escherichia coli (E. coli). These measurements showed a reduction in plaque-forming units (HSV-1) and colony-forming units (E. coli) by more than 4 orders of magnitude, indicating the potent inhibition by the lignin-based hydrogels KW - Lignin functionalization KW - Mucus-mimicking hydrogels PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625301 DO - https://doi.org/10.1021/acsami.4c18519 SP - 1 EP - 14 PB - American Chemical Society (ACS) CY - USA AN - OPUS4-62530 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wagner, Jan A1 - Dudziak, Mateusz A1 - Falkenhagen, Jana A1 - Rockel, Daniel A1 - Reimann, H.-A A1 - Schartel, Bernhard T1 - This is the way: An evidence based route to phytic-acid–based flame retardant poly(lactide acid) N2 - A systematic sequence of materials was investigated to develop phytic-acid (Phyt)–based flame retarded poly (lactide acid) (PLA), while factoring in molecular weight (MW), crystallinity and mechanical properties. Synergistic approaches were developed based on combinations with lignin and expandable graphite (EG), as well as by applying different Phyt salts of melamine (Mel), piperazine (Pip), and arginine (Arg). Compounds were twin screw extruded, injection molded, hot pressed and investigated with thermal analysis, size exclusion chromatography, infrared spectroscopy, tensile testing, limited oxygen index (LOI), UL 94, cone calorimeter, and scanning electron microscope. 16.7 wt.% flame retardant (FR) slightly enhances crystallization while MW remains unchanged in PLA Phyt Arg and PLA Phyt Mel. LOI was improved to 43.7 vol.% for PLA Phyt Arg, UL 94 V0 achieved for PLA Phyt Pip. Cone calorimeter results show total heat evolved reduced by 14 %, maximum average rate of heat emission 43 % lower, and peak heat release rate reduced by 50 % for PLA Phyt Mel. Phyt Mel combined with EG increased the char yield of PLA to 20 wt.% and 15.5 wt.% at 600 and 900 ◦C, respectively. Phyt is exploited to enhance char yield, stabilize the intumescent char, and lower the apparent effective heat of combustion. The combination of Phyt Mel and EG was proposed as an efficient FR for PLA via an evidence based developing route. KW - Polylactide acid KW - Intumescent flame retardant KW - Phosphorous flame retardant KW - Phytic acid KW - Expandable graphite KW - Melamine PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626395 DO - https://doi.org/10.1016/j.polymdegradstab.2025.111242 SN - 1873-2321 SN - 0141-3910 VL - 234 SP - 1 EP - 14 PB - Elsevier Ltd. AN - OPUS4-62639 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - 70 years size exclusion chromatography - An ongoing challenge N2 - The reason for our current activities is that polymers may also be subject to REACh regulations in the future. In this context, the determination of oligomer content is important. SEC is still the method of choice for determining molar mass distribution. The regulations aim for narrow limits and SEC has rather large error margins, which are well known to all experts. Different polymers need different methods. What to do when samples with a wide range of practical aspects, samples with higher distribution range, reduced solubility, including side components, gel content etc. need be analyzed? A concept for round robin tests and first impressions will be presented. T2 - Analytical Solutions 2025 CY - Ede, Netherlands DA - 04.06.2025 KW - Polymers KW - Size exclusion chromatography KW - REACH KW - Round Robin Tests PY - 2025 AN - OPUS4-63310 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Challenges of sec and the necessity of round robin tests N2 - Size exclusion chromatography (SEC) is still the method of choice for determining the molar mass and molar mass distribution of macromolecules. From the distribution curve molar mass averages and the oligomer content (percentage of peak area smaller than 1000 g/mol and 500 g/mol) of polymers can be derived. The determination of oligomer content is important, because it is often used in regulatory contexts as a measure of small, mobile and potentially more toxic parts of the polymer. Polymer regulations are of increasing political and societal importance. Regulations often strive for narrow limits. But SEC has rather large error margins of 10-20% for the molar mass determination performed in different laboratories or on different instruments. These variances are well known to all experts and users and have been investigated in several round robin tests in the past. These resulted in DIN and ISO standards which, in our opinion, no longer meet today's requirements. Gaps have been identified that require further harmonization. Different polymer types or classes require different methods. On the other hand, as far as we know, the margins of error in determining oligomer content have not yet been investigated. It is expected that the variation will be rather high. This is because it depends on many factors related to the experimental conditions (column sets used, solvent, temperatures, sample preparation) on the one hand, and the data evaluation mechanisms (choice of baseline and peak limits) on the other. In order to actually measure the error margins and to support this with actual data a round robin test has been performed from June to November 2024 with approx. 40 participating laboratories. Three different solvents were selected, namely THF, DMAc or DMF and water. The samples were selected taking into account a wide range of practical aspects far from narrowly distributed standards: e.g higher distribution range, reduced solubility, included side components, copolymers and dispersions with gel content. In this contribution we will present the detailed concept of this round robin test and impressions T2 - 2025 Polymer Separations GNT meeting, Dow CY - Online meeting DA - 25.02.2025 KW - Polymers KW - Size exclusion chromatography KW - REACH PY - 2025 AN - OPUS4-63314 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana A1 - Fink, Friedrich T1 - Biobased and biodegradable polymers - sustainability and circular economy N2 - The presentation shows recent results on the synthesis and modification of environmentally relevant polymers based on renewable resources and the associated development of robust, high quality analytical methods. The first topic presents analytical results for star-shaped polylactides with different degrees of functionalisation. It is shown how liquid chromatography and mass spectrometry methods complement each other in a proven way to obtain accurate molar masses and to quantify chemically heterogeneous species. The second part presents an approach to incorporate lignin into epoxy matrices to obtain covalently adaptable epoxy networks that can be reprocessed and reused. T2 - 11th International Symposium on the Separation and Characterization of Natural and Synthetic Macromolecules CY - Amsterdam, Netherlands DA - 21.01.2025 KW - Polylactides KW - Ligninbased thermosets KW - MALDI-TOF-MS KW - Gradient elution liquid adsorption chromatography KW - Atomic force spectroscopy KW - FT-IR PY - 2025 AN - OPUS4-62532 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Altmann, Korinna T1 - Deliverable 2: Summary report on: The development of pristine SI traceable reference materials for SMPs (0.1 μm - 10 μm) and NPs (< 0.1 μm), representative of partially degraded/naturally aged samples in complex food and environmental matrices, and for realistic polydisperse size distributions and irregular shapes N2 - PlasticTrace aims to address the urgent need for development and harmonisation of methods for the chemical identification, physical characterisation and quantification of released small micro/nanoplastics (SMPs/NPs) in drinking water, food and environmental matrices, as required by the EU’s Circular Economy Action Plan (CEAP). This report describs the characterisation of nanoPP analysed in the PlasticTrace project aiming to develop a reference material. The nanoPP was analysed mainly by light scattering methods. Homogeneity control was done by DLS. KW - Nanoplastics KW - Reference materials PY - 2024 N1 - Project Number 21GRD07: PlasticTrace (Tracing Micro and NanoPlastics in Food and Environment), funded by the European Union SP - 1 EP - 29 PB - European Association of National Metrology Institutes (EURAMET) CY - Braunschweig AN - OPUS4-62299 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Alić Stolar, Jasna T1 - Harnessing Mechanochemistry to Combat PFAS Contamination N2 - For over 70 years, the uncontrolled production, use, and disposal of per- and polyfluoroalkyl substances (PFAS) have led to widespread global contamination, necessitating the rapid development of innovative and efficient remediation technologies. State-of-the-art strategies rely on energy-intensive incineration, which releases greenhouse gases and smaller, volatile PFAS derivatives. Here, we present a fast, simple, and sustainable method for the complete degradation of PFAS leveraging mechanochemistry to break down the persistent carbon-fluorine bonds. Our findings indicate that liquid-assisted grinding conditions accelerate the degradation of perfluorooctanoic acid compared to neat grinding conditions, resulting in a significant reduction in energy consumption. Moreover, the fluoride released during the process binds to inorganic additives, allowing fluorine recovery as crystalline salts and preventing the formation of secondary toxic waste. The method has strong potential for scaling up and offers a green and viable solution for real-world application in PFAS decontamination. T2 - International Conference on Sustainable Chemistry for Net Zero (ICSC-NZ) CY - St. Andrews, Scotland DA - 10.06.2025 KW - Mechanochemistry KW - PFAS KW - Remediation PY - 2025 AN - OPUS4-63971 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Alić Stolar, Jasna T1 - Harnessing mechanochemistry to combat PFAS contamination N2 - For over 70 years, the uncontrolled production, use, and disposal of per- and polyfluoroalkyl substances (PFAS) have led to widespread global contamination, necessitating the rapid development of innovative and efficient remediation technologies. State-of-the-art strategies rely on energy-intensive incineration, which releases greenhouse gases and smaller, volatile PFAS derivatives. Here, we present a fast, simple, and sustainable method for the complete degradation of PFAS leveraging mechanochemistry to break down the persistent carbon-fluorine bonds. Our findings indicate that liquid-assisted grinding conditions accelerate the degradation of perfluorooctanoic acid compared to neat grinding conditions, resulting in a significant reduction in energy consumption. Moreover, the fluoride released during the process binds to inorganic additives, allowing fluorine recovery as crystalline salts and preventing the formation of secondary toxic waste. The method has strong potential for scaling up and offers a green and viable solution for real-world application in PFAS decontamination. T2 - International Conference on Sustainable Chemistry for Net Zero (ICSC-NZ) CY - St. Andrews, Scotland DA - 10.06.2025 KW - Mechanochemistry KW - PFAS KW - Remediation PY - 2025 AN - OPUS4-63970 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Alić Stolar, Jasna T1 - Harnessing mechanochemistry to combat PFAS contamination N2 - For over 70 years, the uncontrolled production, use, and disposal of per- and polyfluoroalkyl substances (PFAS) have led to widespread global contamination, necessitating the rapid development of innovative and efficient remediation technologies. State-of-the-art strategies rely on energy-intensive incineration, which releases greenhouse gases and smaller, volatile PFAS derivatives. Here, we present a fast, simple, and sustainable method for the complete degradation of PFAS leveraging mechanochemistry to break down the persistent carbon-fluorine bonds. Our findings indicate that liquid-assisted grinding conditions accelerate the degradation of perfluorooctanoic acid compared to neat grinding conditions, resulting in a significant reduction in energy consumption. Moreover, the fluoride released during the process binds to inorganic additives, allowing fluorine recovery as crystalline salts and preventing the formation of secondary toxic waste. The method has strong potential for scaling up and offers a green and viable solution for real-world application in PFAS decontamination. T2 - The International Symposium on Mechanochemistry (Mech’cheM 2025) CY - Montpellier, France DA - 04.06.2025 KW - Mechanochemistry KW - PFAS PY - 2025 AN - OPUS4-63956 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ryll, Tom William T1 - In-situ analysis of nucleation processes – case study: calciumsulfate N2 - In this project we investigate nucleation pathways by utilizing synchrotron-XRD and running a case-study on calcium sulfate and its polymorphs. To accomplish this, we developed a modular automation setup for reactions in solution to run synthesis and control reaction conditions. So far we successfully characterized the recycling process of gypsum (CaSO4*2H2O) and are now investigating the formation of anhydrite (CaSO4*0H2O) as well as possible applications for the automation setup and analysis. T2 - SALSA Make & Measure 2025 CY - Berlin, Germany DA - 10.09.2025 KW - Recycling KW - Gypsum KW - Synchrotron-X-ray-diffraction KW - Raman-spectroscopy KW - Automation PY - 2025 AN - OPUS4-64135 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wöhlecke, Andreas T1 - Aktuelles aus dem BAM-Fachbeirat N2 - Die Anforderungen an Geokunststoffprodukte und deren Qualitätssicherung unterliegen einem stetigen Wandel, der sowohl durch technische Veränderungen als auch durch normative und organisatorische Entwicklungen geprägt ist. Insbesondere der Fachbeirat der BAM gemäß Deponieverordnung (DepV) spielt hier im Bereich der Deponietechnik eine wichtige Rolle. An dieser Stelle sollen aktuelle Themen aus dem Fachbeirat der BAM vorgestellt werden, die wesentliche Änderungen in der Zulassungs- und Anwendungspraxis betreffen. Der Beitrag beleuchtet unter anderem Veränderungen innerhalb der BAM, die Modernisierung der Publikationsformate sowie die fachliche Weiterentwicklung der Zulassungsrichtlinien. T2 - 22. Leipziger Deponiefachtagung CY - Leipzig, Germany DA - 10.03.2026 KW - Deponie KW - Geotextil KW - Abdichtungssystem PY - 2026 AN - OPUS4-65665 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dudziak, Mateusz A1 - Bhatia, Riya A1 - Dey, R. A1 - Falkenhagen, Jana A1 - Ullrich, M. S. A1 - Thomsen, C. A1 - Schartel, Bernhard T1 - Wastewater phosphorus enriched algae as a sustainable flame retardant in polylactide N2 - Revolutionizing our polymer industry for adaption to a sustainable carbon circular economy has become one of today’s most demanding challenges. Exploiting renewable resources to replace fossil-fuel—based plastics with biopolymers such as poly(lactic acid) (PLA) is inevitable while using waste streams as a raw material resource at least is promising. When it comes to using PLA as technical polymer, its high flammability must be addressed by flame retardants compatible with the thermoplastic processing of PLA and its compostability. This study proposes microalgae enriched with phosphorus from wastewater (P-Algae) as an elegant way towards a kind of sustainable organophosphorus flame retardant. The concept is demonstrated by investigating the processing, pyrolysis, flammability, and fire behavior of PLA/P-Algae, while varying the P-Algae content and comparing P-Algae with four alternative bio-fillers (phosphorylated lignin, biochar, thermally treated sewage sludge, and metal phytate) with different P-contents as meaningful benchmarks. KW - PLA KW - Flame Retardancy KW - Phosphorylated Algae KW - Wastewater flame retardants KW - Zink phytate KW - Phosphorylated lignin KW - Thermally treated sludge PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-604150 DO - https://doi.org/10.1016/j.polymdegradstab.2024.110885 SN - 1873-2321 SN - 0141-3910 VL - 227 SP - 1 EP - 11 PB - Elsevier Ltd. AN - OPUS4-60415 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cherbib, S. A1 - Jlalia, I. A1 - Chabbah, T. A1 - Chatti, S. A1 - Marestin, C. A1 - Mercier, R. A1 - Weidner, Steffen A1 - Casabianca, H. A1 - Jaffrezic-Renault, N. A1 - Abderrazak, H. T1 - Design of New Partially Bio-Based Polyguanamines for the Reversible Adsorption of Phenolic Molecules from Olive Mill Wastes N2 - Olive mill wastewater produces a variety of potent antioxidants, including hydroxytyrosol, oleuropein, and tyrosol, that have been widely used in agriculture, pharmacy, and cosmetics. This study aims to design new poly(guanamine)s phases by polycondensation of modified triazine monomers with both petro-based and biosourced diamines, to act as stationary phases for the uptake of these phenolic molecules. Obtained polymers were characterized by NMR spectroscopy, differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). The adsorption results showed that the newly synthesized polymers can effectively uptake the less polar phenolic compounds, ferulic acid, and caffeic acid. The isosorbide-based polymer (P6) presented the highest sorption efficiency, due to the hydrophilic properties of isosorbide associated with the proton affinity of the triazine groups. All the phenolic compounds were successfully desorbed from the P6 polymer using a minimal amount of a methanol/acetonitrile mixture. P6 polymer could be used for four successive adsorption processes without loss of efficiency. KW - Olive mill wastewater KW - Triazine KW - Isosorbide KW - Adsorption KW - Phenolic compounds PY - 2024 DO - https://doi.org/10.1007/s42250-024-01081-3 SN - 2522-5758 SP - 1 EP - 11 PB - Springer Science and Business Media LLC AN - OPUS4-61348 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fink, Friedrich A1 - Stawski, Tomasz M. A1 - Emmerling, Franziska A1 - Falkenhagen, Jana T1 - A novel machine-learning approach to unlock technical lignin classification by NIR spectroscopy - bench to handheld N2 - In this research, the utilization of near-infrared (NIR) spectroscopy in conjunction with advanced machine learning methods is investigated for categorizing technical lignins obtained from different biomass sources and industrial procedures. Technical lignins, such as kraft, organosolv and lignosulfonates, have different chemical compositions, which continue to make uniform characterization and application in sustainable sectors extremely difficult. Fast, universally accessible analytics combined with data analysis is still an open question. For the first time three distinct NIR spectrometers—a high-performance benchtop system, a mid-priced compact device, and an economical handheld unit—were utilized to record NIR spectra of 31 unique lignin samples. The spectra underwent pre-processing through standard normal variate (SNV) transformation and Savitzky-Golay derivatives to amplify spectral features and decrease noise. Principal component analysis (PCA) was employed to reduce data complexity and extract crucial characteristics for classification purposes. Subsequently, four machine learning algorithms—Support Vector Machines (SVM), Gaussian Naive Bayes (GNB), Gaussian Process Classification (GPC), and Decision Tree Classification (DTC)—were implemented for the classification of the lignin samples. The DTC model exhibited the highest accuracy among them across different spectrometers. Although the benchtop spectrometer produced the most precise outcomes, the compact NeoSpectra system also displayed potential as a cost-efficient option. Nonetheless, the restricted spectral coverage of the handheld NIRONE spectrometer resulted in reduced classification accuracy. Our discoveries highlight the capability of NIR spectroscopy, combined with robust data analysis techniques, for the swift and non-destructive classification of technical lignins, facilitating their improved utilization in sustainable fields. KW - Technical lignins KW - NIR spectroscopy KW - Classification KW - Machine-learning KW - PCA PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634518 DO - https://doi.org/10.1016/j.chemolab.2025.105467 SN - 0169-7439 VL - 264 SP - 1 EP - 10 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-63451 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stolar, Tomislav A1 - Bayram, Dilara A1 - May, Anastasia A1 - Sundermann, Remie A1 - Prinz, Carsten A1 - Meyer, Klas A1 - Myxa, Anett A1 - Falkenhagen, Jana A1 - Emmerling, Franziska T1 - Selective mechanochemical conversion of post-consumer polyethylene terephthalate waste into hcp and fcu UiO-66 metal–organic frameworks N2 - Single-use plastics strongly contribute to plastic pollution, and less than 10% of plastic waste is recycled globally. Here, we present a selective mechanochemical protocol for converting post-consumer polyethylene terephthalate (PET) transparent bottles and coloured textile waste into the porous metal–organic framework (MOF) UiO-66 materials. We used time-resolved in situ (TRIS) synchrotron powder X-ray diffraction and Raman spectroscopy to monitor the depolymerization of PET during ball milling. To convert disodium terephthalate to UiO-66, we developed base and base-free synthetic routes that lead to fcu and hcp UiO-66 phases, respectively, including the first ever synthesis of hcp UiO-66 by mechanochemistry. Our results demonstrate the potential of mechanochemistry to selectively access fcu and hcp UiO-66 phases using post-consumer PET waste. KW - Mechanochemistry PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653958 DO - https://doi.org/10.1039/D4MR00126E SN - 2976-8683 SP - 1 EP - 8 PB - Royal Society of Chemistry (RSC) AN - OPUS4-65395 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Falkenhagen, Jana A1 - Beskers, Timo. F. A1 - Myxa, Anett A1 - Pursch, Matthias T1 - Round-robin test for size exclusion chromatography – Data summary N2 - Size exclusion chromatography (SEC or GPC) is one critical component of polymer analysis to meet the increasing requirements in regulatory context – namely, determination of Mn, as well as oligomers of less than 500 g mol-1 and 1000 g mol-1. The underlying test methods (OECD 118/119 and DIN EN ISO 13885 1 to 3) provide a framework for SEC measurements; however, they lack sufficient specificity to obtain accurate results. Previous SEC round robin tests were mostly performed on homopolymers and did not collect data on oligomer contents. A new round robin test was initiated and conceptualized within the Task force “Method Evaluation for Polymer REACh (MeEP)”, an initiative of “Industrieforum Analytik” within the German Chemical Society (GDCh). Samples for this study were selected to represent both easy benchmark polymers as well as real-life, industry-relevant polymer materials. Data collection focused on the regulatory requirements. Distribution of samples, gathering of individual results and evaluation were carried out by BAM. A data summary as initial result is reported here. Further evaluation and interpretation are a part of ongoing research. KW - Size exclusion chromatography KW - Polymers KW - Oligomer content KW - Round-robin test PY - 2026 DO - https://doi.org/10.26272/opus4-65587 SP - 1 EP - 84 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-65587 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stolar, Tomislav T1 - Mechanochemical conversion of polyethylene terephthalate into valuable metal-organic frameworks N2 - Single-use plastics are causing plastic pollution, and less than 10% of plastic waste is recycled globally. Here, we present a sustainable mechanochemical1 protocol for converting post-consumer polyethylene terephthalate (PET) textile and bottles into the porous metal-organic framework (MOF) UiO-66. We used time-resolved in situ synchrotron powder X-ray diffraction and Raman spectroscopy to monitor the depolymerization of PET during ball milling with sodium and potassium hydroxide and water as a liquid additive (Figure 1). For synthesizing UiO-66, we focused on the better performing sodium hydroxide and optimized two distinct synthetic routes to produce high-quality UiO-66. Our results demonstrate the potential of mechanochemistry to enable more circular MOF synthesis using post-consumer PET waste. T2 - The International Symposium on Mechanochemistry (Mech’cheM) 2025: New forces in Mechanochemistry CY - Montpellier, France DA - 04.06.2025 KW - Mechanochemistry KW - Plastic recycling KW - Circular economy PY - 2025 AN - OPUS4-63943 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Challenges of SEC and the necessity of round robin tests N2 - Size exclusion chromatography (SEC) is still the method of choice for determining the molar mass and molar mass distribution of macromolecules. It is a liquid chromatographic technique that separates molecules based on their size, respectively their hydrodynamic volume using a porous stationary phase that allows smaller molecules to pass through the pores while excluding larger molecules. The chromatogram from the size separation can be calibrated using polymers of known molar mass resulting in a relative molar mass distribution curve. From this distribution curve molar mass averages and the oligomer content (percentage of peak area smaller than 1000 g/mol and 500 g/mol) of polymers can be derived. The determination of oligomer content is important, because it is often used in regulatory contexts as a measure of small, mobile and potentially more toxic parts of the polymer. Polymer regulations are of increasing political and societal importance. Regulations often strive for narrow limits. But SEC has rather large error margins of 10-20% for the molar mass determination performed in different laboratories or on different instruments. These variances are well known to all experts and users and have been investigated in several round robin tests in the past. These resulted in DIN and ISO standards which, in our opinion, no longer meet today's requirements. Gaps have been identified that require further harmonization. Different polymer types or classes require different methods. On the other hand, as far as we know, the margins of error in determining oligomer content have not yet been investigated. It is expected that the variation will be rather high. This is because it depends on many factors related to the experimental conditions (column sets used, solvent, temperatures, sample preparation) on the one hand, and the data evaluation mechanisms (choice of baseline and peak limits) on the other. In order to actually measure the error margins and to support this with actual data a round robin test has been performed from June to November 2024 with approx. 40 participating laboratories. Three different solvents were selected, namely THF, DMAc or DMF and water. The samples were selected taking into account a wide range of practical aspects far from narrowly distributed standards: e.g higher distribution range, reduced solubility, included side components, copolymers and dispersions with gel content. In this contribution we will present the detailed concept of this round robin test and first impressions. T2 - 11th International Symposium on the Separation and Characterization of Natural and Synthetic Macromolecules CY - Amsterdam, Netherlands DA - 21.01.2025 KW - Size exclusion chromatography KW - Round robin tests PY - 2025 AN - OPUS4-62533 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Error margins in the Determination of Molar Mass and Oligomer Content of Polymers N2 - Size exclusion chromatography (SEC) is still the method of choice for determining the molar mass and molar mass distribution of macromolecules. It is a liquid chromatographic technique that separates molecules based on their size, respectively their hydrodynamic volume using a porous stationary phase that allows smaller molecules to pass through the pores while excluding larger molecules. The chromatogram from the size separation can be calibrated using polymers of known molar mass resulting in a relative molar mass distribution curve. From this distribution curve molar mass averages and the oligomer content (percentage of peak area smaller than 1000 g/mol and 500 g/mol) of polymers can be derived. The determination of oligomer content is important, because it is often used in regulatory contexts as a measure of small, mobile and potentially more toxic parts of the polymer. Polymer regulations are of increasing political and social importance. Regulations often set very narrow limits. SEC has rather large error margins of 10-20% for the molar mass determination performed in different laboratories or on different instruments. These variances are well known to all experts and users and have been investigated in several round robin tests in the past. These resulted in DIN and ISO standards which, in our opinion, no longer meet today's requirements. As far as we know, the margins of error in determining oligomer content have not yet been investigated. It is expected that the variation will be rather high. This is because it depends on many factors related to the experimental conditions (column sets used, solvent, temperatures, sample preparation) on the one hand, and the data evaluation mechanisms (choice of baseline and peak limits) on the other. In order to actually measure the error margins and to support this with actual data a round robin test has been performed from June to November 2024 with approx. 40 participating laboratories. Three different solvents were selected, namely THF, DMAc or DMF and water. The samples were selected together with all the experts, taking into account a wide range of practical aspects far from narrowly distributed standards: e.g higher distribution range, reduced solubility, included side components, copolymers and dispersions with gel content. In this contribution we will present the detailed concept of this round robin test and first results. T2 - SETAC Europe 35th Annual Meeting CY - Vienna, Austria DA - 11.05.2025 KW - Size exclusion chromatography KW - REACH KW - Polymers KW - Round Robin Tests PY - 2025 AN - OPUS4-63307 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Limitations of SEC: Strategies for Improved Regulatory Polymer Analysis N2 - Polymers, composed of repeating units called monomers, exhibit a diverse range of properties, with molecular weight distribution (MWD) being particularly important for regulatory risk assessments. Size exclusion chromatography (SEC), or gel permeation chromatography (GPC), is the primary technique for MWD characterization, as detailed in OECD guidelines 118 and 119, along with DIN and ISO standards. However, SEC faces significant shortcomings that complicate the accurate determination of MWD and oligomer content. These limitations include the insolubility of certain polymers, crosslinking, and ultra-high molecular weight characteristics, which can exceed SEC's separation capabilities. The presence of salts or modifiers can further interfere with oligomer content determination, and the availability of appropriate SEC columns and calibration standards limits comparability across laboratories. To enhance SEC's reliability and applicability within regulatory frameworks, innovative methods and strategies are essential. Proposed solutions involve new sample preparation techniques, advanced data interpretation methods, and the establishment of standardized methodologies to promote harmonization. This is especially crucial in light of the expected Polymer REACh (PREACh) legislation, which aims to regulate polymer registration and risk assessment within the European market. Given the anticipated complexity of the registration process, which requires extensive data generation, proactive strategies are needed to address SEC's challenges. Currently, there are no viable alternatives for oligomer content determination, and the unique properties of polymers often necessitate tailored analytical approaches. Without new methodologies and guidelines, the polymer registration process could become burdensome and costly, jeopardizing important products and markets in the EU. Key areas for improvement include extending existing norms to cover a broader range of solvents, addressing high error margins in oligomer content determination, establishing harmonized approaches for dealing with side components, and providing clarity on measuring partially soluble polymers. In conclusion, addressing SEC's limitations through the development of comprehensive guidelines and harmonization is critical for ensuring accurate and efficient polymer analysis, ultimately facilitating smoother registration processes. T2 - SETAC Europe 35th Annual Meeting CY - Vienna, Austria DA - 11.05.2025 KW - Size exclusion chromatography KW - Polymers KW - REACH PY - 2025 AN - OPUS4-63309 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stolar, Tomislav T1 - Upcycling waste PET bottles to porous UiO-66 by mechanochemistry N2 - Single-use plastics are causing plastic pollution, and less than 10% of plastic waste gets recycled globally. Most of it ends up in landfills or gets incinerated in a highly unsustainable manner. Here, I will present a sustainable mechanochemical protocol for the chemical upcycling of polyethylene terephthalate (PET) to porous UiO-66 metal-organic framework (MOF). In the first step, PET is ball-milled with sodium hydroxide and undergoes alkaline hydrolysis to disodium terephthalate (Na2TP). Time-resolved in situ monitoring of ball milling reaction by synchrotron powder X-ray diffraction shows the appearance of crystalline Na2TP after 20 min of milling. However, ex-situ analysis at different milling times by gel permeation chromatography reveals that the depolymerisation step needs more milling for completion. After two hours of ball milling, there are only trace amounts of leftover PET. For upcycling to UiO-66, a zirconium acetate cluster is added to Na2TP together with liquid additives and after milling for T2 - International Conference on Resource Chemistry 2024 CY - Alzenau, Germany DA - 13.03.2024 KW - Mechanochemistry KW - Plastic recycling KW - Circular economy PY - 2024 AN - OPUS4-62105 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fink, Friedrich A1 - Falkenhagen, Jana T1 - From bench to mini – Classification of technical lignins with NIR N2 - Lignin, a by-product of the pulp and paper industry, is the second most abundant biopolymer but remains underutilized due to its complex structure and variability in biomass origin. Classification based on biomass source is crucial for quality assurance and application predictability. This study employs near-infrared (NIR) spectroscopy to classify technical lignins from softwoods, hardwoods, straw, and grasses. Machine learning models (ML), including Support Vector Machines (SVM), Gaussian Process Classification (GPC), Gaussian Naive Bayes (GNB), and Decision Tree Classification (DTC), were developed using spectral preprocessing and principle component analysis (PCA). The models were compared with spectra from handheld and compact spectrometers. Results highlight the potential of NIR spectroscopy and machine learning to enable rapid, reliable lignin classification, paving the way for improved industrial utilization of this abundant resource. T2 - 11th International Symposium on the Separation and Characterization of Natural and Synthetic Macromolecules CY - Amsterdam, The Netherlands DA - 21.01.2025 KW - Lignin KW - Classification KW - Near infrared spectroscopy PY - 2025 AN - OPUS4-62531 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stolar, Tomislav T1 - Waste to value: upcycling PET bottles into MOFs using mechanochemistry N2 - Single-use plastics are causing plastic pollution, and less than 10% of plastic waste gets recycled globally. Most of it ends up in landfills or gets incinerated in a highly unsustainable manner. Here, I will present a sustainable mechanochemical protocol for the chemical upcycling of waste polyethylene terephthalate (PET) bottles to porous UiO-66 metal-organic framework (MOF). We used in situ and ex situ characterization to gain a deep understanding of the underlying mechanochemical process leading to high crystallinity and -porosity UiO-66. Our results show the potential of mechanochemistry for the sustainable production of high-quality value-added materials such as UiO-66 from waste PET bottles. T2 - 2024 Green Chemistry Gordon Research Conference CY - Barcelona, Spain DA - 31.07.2024 KW - Mechanochemistry KW - Plastic recycling KW - Circular economy PY - 2024 AN - OPUS4-62107 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stolar, Tomislav T1 - Mechanochemical Conversion Of Polyethylene Terephthalate Into Valuable Metal-organic Frameworks N2 - Single-use plastics are causing plastic pollution, and less than 10% of plastic waste is recycled globally. Here, we present a sustainable mechanochemical protocol for converting post-consumer polyethylene terephthalate (PET) textile and bottles into the porous metal-organic framework (MOF) UiO-66. We used time-resolved in situ synchrotron powder X-ray diffraction and Raman spectroscopy to monitor the depolymerization of PET during ball milling with sodium and potassium hydroxide and water as a liquid additive. For synthesizing UiO-66, we focused on the better performing sodium hydroxide and optimized two distinct synthetic routes to produce high-quality UiO-66. Our results demonstrate the potential of mechanochemistry to enable more circular MOF synthesis using post-consumer PET waste. T2 - International Conference on Sustainable Chemistry for Net Zero CY - St. Andrews, United Kingdom DA - 10.06.2025 KW - Mechanochemistry KW - Plastic recycling KW - Circular economy PY - 2025 AN - OPUS4-63944 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Denkler, Tilman A1 - Ehlert, Anna A1 - Bukanova, Boriana A1 - Janssens, Frank A1 - Chawla, Kartik A1 - Männistö, Toni A1 - Tamm, Martin A1 - Dao, Anh A1 - Koppelaar, Rembrandt A1 - Wolf, Marc-Andree A1 - Bernier, Carolynn A1 - Stöcker, Carsten A1 - Tan, Yao-Hua A1 - Chan, Susana Wong A1 - Claussen-Markefka, Heino A1 - Demchuk, Nataliia A1 - Simboeck, Johannes A1 - Kocia, Kamila A1 - Schneider, Andreas A1 - Raimondi, Agnese A1 - Scalia, Mauro A1 - Kluka, Michal A1 - Kars, Tobias T1 - Cross-Border E-commerce to Consumers, Digital Product Passports (DPP), and the Role of Authorities N2 - EU e‑commerce imports are surging, overwhelming authorities and allowing many unsafe or non‑compliant products to enter the market. Major reforms and digital tools—especially Digital Product Passports—are expected to help, but their exact role still needs clarification. KW - Digital Product Passport KW - Cross-border e-commerce KW - Machine-verifiable compliance PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-658039 DO - https://doi.org/10.5281/zenodo.19239072 SP - 1 EP - 64 CY - Delft (Netherlands) AN - OPUS4-65803 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -