TY - JOUR A1 - Singh, Amit Kumar A1 - Mishra, Biswajit A1 - Sinha, Om Prakash T1 - Reduction Kinetics of Fluxed Iron Ore Pellets Made of Coarse Iron Ore Particles N2 - The present work demonstrates a sustainable approach of using relatively coarser iron ore particles for ironmaking. The motivation is to reduce the energy consumption in the milling of the iron ore by utilizing coarser iron ore particles (+0.05 mm) and to select a suitable binder for improving pellet properties. Iron ore fines in the range of 0.05–0.25 mm was selected and classified into three size ranges. Fluxed iron ore pellets were prepared using lime as a binder for the basicity of 0, 1, and 2. Reduction of these pellets with a packed bed of coal fines was performed in the temperature range of 900–1200 °C for a duration of 30–120 min. The direct reduction kinetics of the iron ore pellets were studied by employing diffusion and chemical reaction control models to the experimental data. The results show that pellets made with coarser iron ore particles have improved reduction behavior and kinetics. The reduction reaction is found to be a mixed control. The activation energy for the reduction reaction varies from 44.3 to 74.76 kJ mol−1 as iron ore particle size decreases from 0.25 to 0.05 mm and basicity increases from 0 to 2. KW - Materials Chemistry KW - Metals and Alloys KW - Process Metallurgy KW - Iron making PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-598326 DO - https://doi.org/10.1002/srin.202300669 SN - 1611-3683 IS - 2300669 SP - 1 EP - 9 PB - Wiley VHC-Verlag AN - OPUS4-59832 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Wiesler, F. A1 - Hund-Rinke, K. A1 - George, E. A1 - Greef, J.-M. A1 - Holz, F. A1 - Hölze, L.E. A1 - Hülsbergen, K.-J. A1 - Martin, S. A1 - Severin, K. A1 - Spielvogel, S. A1 - Geiger, P. A1 - Nawotke, C. A1 - Kehlenbeck, H. A1 - Schenkel, H. A1 - Adam, Christian A1 - Bloem, E. A1 - Frank, D. A1 - Goldbach, H.E. A1 - Heene, M. A1 - Kratz, S. A1 - Kruse, A. A1 - Möller, K. A1 - Pinnekamp, J. A1 - Schoumans, O.F. A1 - Vogel, Christian A1 - Wulf, S. T1 - Recyclingphosphate in der Düngung – Nutzen und Grenzen N2 - Weltweit werden etwa 80–85 % aller abgebauten Rohphosphate für die Produktion von Düngemitteln verwendet. Bei noch steigendem Bedarf an Phosphor (P) geht man derzeit davon aus, dass die weltweiten P-Reserven noch über 200 Jahre ausreichen. Um den P-Vorrat langfristig abzusichern, sollte der in Reststoffen enthaltene Phosphor möglichst umfänglich genutzt werden. Dieser Forderung trägt das von der Bundesregierung 2012 erstmals beschlossene Deutsche Ressourceneffizienzprogramm ProgRess Rechnung. Rohphosphat wird auch seitens der Europäischen Kommission aufgrundseiner ökonomischen Bedeutung und des unsicheren Angebots als „kritischer Rohstoff“ eingestuft. Vor diesem Hintergrund hat die Bundesregierung in der Verordnung zur Neuordnung der Klärschlammverwertung vom 27. September 2017 in Deutschland eine verpflichtende technische Rückgewinnung von Phosphor für Abwasserbehandlungsanlagen ab einer Ausbaugröße von 100.000 Einwohnerwerten (12 Jahre nach Inkrafttreten der Verordnung) bzw. ab einer Ausbaugröße von über 50.000 Einwohnerwerten (15 Jahre nach Inkrafttreten der Verordnung) vorgeschrieben. Die Verordnung enthält keine Vorgaben hinsichtlich der anzuwendenden Technologie bei der Phosphorrückgewinnung. Ausgenommen von der Rückgewinnungspflicht sind Klärschlämme mit niedrigen Phosphorgehalten (weniger als 20 Gramm Phosphor je Kilogramm Klärschlamm-Trockenmasse). Auch die im Jahre 2017 verabschiedeten neuen Rechtsvorschriften für die Düngung verlangen zukünftig einen nachhaltigen und ressourceneffizienten Umgang mit Nährstoffen bei der landwirtschaftlichen Erzeugung und schränken die P-Zufuhr insbesondere auf hoch versorgten Böden ein (Düngeverordnung vom 26. Mai 2017). Dies wird zu einem mehr am Pflanzenbedarf orientierten und ggf. vermehrt überbetrieblichen Einsatz von wirtschaftseigenen Düngern führen. Um den politischen und gesetzlichen Anforderungen gerecht zu werden, müssen einerseits wirksame und kosteneffiziente technische Verfahren zum P-Recycling (weiter)entwickelt werden. Andererseits müssen die Recyclingprodukte die Anforderungen für eine direkte Verwendung in der Landwirtschaft oder als Rohstoff für die Herstellung von Düngemitteln erfüllen. In dem vorliegenden Standpunkt wird zunächst der potenzielle Beitrag von Reststoffen zur Deckung des P-Bedarfs in der deutschen Pflanzenproduktion geschätzt. Für die wichtigsten Reststoffe werden technische Verfahren zur P-Rückgewinnung bzw. Aufarbeitung skizziert. Auf Basis der Anforderungen der Landwirtschaft bzw. der Düngemittelindustrie an die P-Recyclingprodukte werden deren Herstellungsverfahren bewertet. Schließlich wird der Regelungs- und Forschungsbedarf formuliert. KW - Phosphor KW - Düngemittel KW - Diffusive Gradients in thin films (DGT) PY - 2020 SP - 1 EP - 19 PB - Bundesministerium für Ernährung und Landwirtschaft (BMEL) CY - Berlin AN - OPUS4-51011 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Taube, Mareike Carolin A1 - Adam, Christian A1 - Adamczyk, Burkart A1 - Beckmann, T. A1 - Reuter, M. A1 - Stelter, M. ED - Reiser, B. T1 - Recycling von metallurgischen Rückständen - Schmelzversuche zeigen, wie die Tantalrückgewinnung aus Zinnschlacken und weiteren Reststoffen optimiert werden kann N2 - Since the recycling of tantalum bearing post-consumer waste is practically not existent, metallurgical residues are the most important feed for the tantalum recycling. Most tin ores naturally contain significant quantities of refractory metals. During the smelting process in primary tin production these elements are enriched in the slag phase. This slag is a highly valuable raw material for tantalum production due to its considerable concentration of tantalum and its functioning as an additional slag former in further pyrometallurgical treatment. In this paper the first process stage of an existing pyrometallurgical process for tantalum recovery, mainly from low grade pyrometallurgical residues, is discussed. Smelting trials were carried out in a pilot-scale electric arc furnace to analyse the effect of feeding on the activity of carbon as a reducing agent. Therefore, blowing petroleum coke through an iron lance and the manual adding of coke into the melting bath were tested. During the pyrometallurgical treatment elements with a high affinity to carbon were reduced to their carbide form and enriched in the molten iron-based metal phase. The objective of the process was to reduce the oxidic tantalum completely and to enrich it into the metal phase. Furthermore, the transfer of unwanted elements such as titanium into the metal phase was aimed to be avoided. Spoon test specimens were taken from the liquid mineral melt to follow the evolution of the reduction process. The cooled down solidified melting bath was investigated by using the XRD and EDX method to characterise the slag system and to identify relevant mineral phases. N2 - Da das Recycling von tantalhaltigen Post-Consumer-Abfällen praktisch nicht existiert, stellen metallurgische Reststoffe eine äußerst wichtige Rohstoffquelle für das Tantalrecycling dar. Die meisten Zinnerze enthalten von Natur aus erhebliche Mengen an Refraktärmetallen. Diese Elemente werden in den Schlacken der pyrometallurgischen Primärzinngewinnung angereichert. Aufgrund ihrer vergleichsweise hohen Wertstoffkonzentration und ihrer Funktion als zusätzlicher Schlackenbildner stellen diese Schlacken einen wertvollen Rohstoff für die Verhüttung tantalhaltiger Reststoffe dar. In der vorliegenden Arbeit wird ein existierendes Verfahren zur Tantalrückgewinnung diskutiert, dem hauptsächlich pyrometallurgische Rückstände geringer Wertstoffkonzentration als Einsatzstoff dienen. Mit Hilfe des Verfahrens sollte dasoxidisch vorliegende Tantal vollständig reduziert und in der Metallphase angereichert werden. Weiterhin sollte vermieden werden, dass unerwünschte Elemente wie Titan in die Metallphase überführt werden. Ziel der Untersuchung war es, die ablaufenden Reduktionsprozesse besser zu verstehen, um so Ansätze für die Prozessoptimierung identifizieren zu können. KW - Lichtbogenofen KW - Pyrometallurgie KW - Recycling KW - Tantal KW - Zinnschlacke PY - 2020 SN - 0934-3482 VL - 33 SP - 10 EP - 17 PB - Rhombos-Verlag CY - Berlin AN - OPUS4-50656 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kalinka, Gerhard T1 - Recycling von Faserverbundwerkstoffen N2 - Der Vortrag beschreibt Aktivitäten der BAM zum Recycling von carbonfaser-verstärkten Verbundwerkstoffen. T2 - Fachdialog Recycling von Windenergieanlagen CY - Berlin, Germany DA - 23.09.2024 KW - Polymer Matrix Composite KW - Carbon Fibres KW - Recycling KW - Pyrolysis KW - Recycling by Design PY - 2024 AN - OPUS4-61536 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hamann, Christopher A1 - Spanka, M. A1 - Stolle, Dirk A1 - Auer, G. A1 - Weingart, Eric A1 - Al-Sabbagh, Dominik A1 - Ostermann, Markus A1 - Adam, Christian T1 - Recycling of blast-furnace sludge by thermochemical treatment with spent iron(II) chloride solution from steel pickling N2 - One of the typical wastes produced in blast-furnace (BF) ironmaking is BF sludge, which mostly consists of carbon and iron oxides, but also contains toxic trace metals such as Zn, Pb, Cd, As, and Hg that render the material hazardous. Due to the lack of an established recycling process, BF sludges are landfilled, which is ecologically questionable and costly. Here, we investigate selective removal of Zn, Pb, and Cd from BF sludge by chlorination–evaporation reactions using thermodynamic modelling and laboratory-scale experiments. Specifically, BF sludge was thermochemically treated at 650–1000 °C with a spent iron(II) chloride solution from steel pickling and the effects of process temperature and retention time on removal of Zn, Pb, and Cd were investigated. Zinc and Pb were quantitatively removed from BF sludge thermochemically treated at 900–1000 °C, whereas Fe and C as well as other major elements were mostly retained. The Zn, Pb, and Cd contents in the thermochemically treated BF sludge could be lowered from ∼56 g/kg, ∼4 g/kg, and ∼0.02 g/kg to ≤0.7 g/kg, ≤0.02 g/kg, and ≤0.008 g/kg, respectively, thus rendering the processed mineral residue a non-hazardous raw material that may be re-utilized in the blast furnace or on the sinter band. KW - Blast-furnace sludge KW - Selective chlorination KW - Zinc chloride PY - 2021 DO - https://doi.org/https://doi.org/10.1016/j.jhazmat.2020.123511 SN - 0304-3894 VL - 402 IS - 123511 SP - 1 EP - 12 PB - Elsevier CY - Amsterdam AN - OPUS4-51141 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piehl, Patrick T1 - Recovery of zinc from steel mill dusts in the rotary kiln by joint treatment with chloride-containing residues N2 - During iron and steel production, several by-products such as slags, dusts and sludges are generated in addition to pig iron and steel as primary products. While established recycling routes exist for slags, there are still considerable recycling problems for other residual materials, especially for filter dusts and sludges containing zinc and lead from waste gas purification. However, the high heavy metal contents make landfilling these dusts and sludges cost-intensive and ecologically problematic. In addition, the relatively high zinc and iron loads represent a valuable material potential, which can make reprocessing of the material with recovery of the zinc and iron loads as secondary raw materials ecologically as well as economically attractive. Against this background, a process is being developed in a cooperative project between Ferro Duo GmbH and the Federal Institute for Materials Research and Testing (BAM), in which the heavy metals (zinc, lead, cadmium, etc.) contained in the filter dusts and sludges are selectively converted into chlorides in a thermochemical process after the addition of a chlorine donor and evaporated at temperatures between 650 and 1100 °C. This process can be used to recover zinc and iron as secondary raw materials. Experiments to date in a batch reactor show that >99% of the zinc and lead can be removed from the treated material. However, a continuous process is necessary for an economical process, which is why this process is transferred to a rotary kiln and relevant process parameters are identified and optimized. The results of these investigations will be presented here. T2 - European Congress and Exhibition on Advanced Materials and Processes 2021 CY - Online meeting DA - 13.09.2021 KW - Elektroofenstaub KW - Gichtgasschlamm KW - Recycling KW - Ressourcenrückgewinnung KW - Zink PY - 2021 AN - OPUS4-53290 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Montag, D. A1 - Adam, Christian T1 - Rechtliche Vorgaben der Klärschlammverordnung und deren Auswirkungen auf die Phosphor-Rückgewinnung N2 - Im Abfalltechnik-Ausschuss der Bund/Länder-Arbeitsgemeinschaft Abfall (LAGA) wurde eine Vollzugshilfe zur Klärschlammverordnung erarbeitet, die nach Verabschiedung durch die Umweltministerkonferenz Mitte Mai 2020 als LAGA-Merkblatt M-39 veröffentlicht wurde. Im vorliegenden vierten Arbeitsbericht der DWA-Arbeitsgruppe KEK-1.1 werden verschiedene Aspekte der ab dem Jahr 2029 geltenden Regelungen aufgegriffen und damit einige Punkte des LAGA M-39 hinsichtlich der technischen Auswirkungen für den Kläranlagenbetreiber konkret ausgeführt. KW - Klärschlamm KW - Klärschlammverordnung KW - Phosphor-Rückgewinnung PY - 2022 SN - 1866-0029 VL - 5 IS - 69 SP - 406 EP - 413 PB - Gesellschaft zur Förderung der Abwassertechnik CY - Hennef AN - OPUS4-55009 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Singh, R. A1 - Vigelahn, L. A1 - Vogel, Christian A1 - Roesch, Philipp A1 - Simon, Franz-Georg A1 - Egloffstein, T. A1 - Birke, V. T1 - Rapid and Virtually Complete Mechanochemical Reductive Defluorination of Per- and Polyfluoro Alkyl Substances (PFAS) In Contaminated Soil Using Sodium and Amines as Co-milling Agents: A Promising First Approach for the Development of Novel Non-Combustion PFAS Remediation Processes for Soils N2 - PFAS contamination poses significant challenges due to their persistence, bioaccumulation, and potential adverse effects on ecosystems and human health. In recent years, conventional treatment methods, such as incineration, photolysis, and chemical oxidation, have been applied for PFAS treatment. However, these technologies have limitations in terms of their efficacy and cost-effectiveness for efficient PFAS degradation. Consequently, researchers have explored alternative approaches such as photocatalysis, sonochemical degradation, oxidation, electrochemical degradation, and mechanochemical degradation also known as DMCR (Dehalogenation by Mechanochemical Reaction) to address the remediation challenge posed by PFAS contaminated environments. Lab scale experiments were conducted using a planetary ball mill, procured from Retsch GmbH Germany, equipped with 50 mL steel grinding jars under controlled conditions to investigate the degradation of perfluorooctanoic sulfonic acid (PFOS) and perfluorooctanoic acid (PFOA) in contaminated model sand. The experiments were carried out in two stages: initially, with sand alone (15 g), and subsequently, with the addition of co-milling agents, that is, sodium metal (Na), Na with butylamine (BA), and Na with ethylenediamine (EDA) in different proportions. T2 - International CleanUp conference CY - Adelaide, Australia DA - 15.09.2024 KW - Mechanochemical treatment KW - Per- und Polyfluoroierte Alkylsubstanzen (PFAS) KW - Remediation PY - 2024 SP - 177 AN - OPUS4-61119 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Herzel, Hannes T1 - R-Rhenania – Modifiziertes Rhenania Phosphat aus der Klärschlammverbrennung mit thermochemischen Aufschluss N2 - Der Betreiber der Klärschlammverbrennungsanlage Altenstadt (Emter GmbH) integriert einen thermochemischen Prozessschritt in die vorhandene Monoverbrennung und erweitert die Anlage entsprechend, um einen Ausgangsstoff für die Düngemittelproduktion zu erzeugen und damit zur Phosphatrückgewinnung gemäß Klärschlammverordnung (AbfKlärV) beizutragen. Die Umrüstung der Anlage fand im ersten Halbjahr 2024 statt und seit Sommer 2024 steht eine Kapazität für die jährliche Produktion von 15.000 Tonnen schadstoffarmen R-Rhenania Phosphat mit hochwirksamen Phosphatverbindungen zur Verfügung. Diese Demonstrationsanlage wird durch ein wissenschaftliches Monitoring im vom BMFTR geförderte Projekt R-Rhenania (2020-2026) mit u.a. Ökobilanzierungen, Gefäß- und Feldversuche begleitet. Der Projektpartner sePura plant den produzierten Dünger vollständig regional in Bayern zu verwerten T2 - DPP Forum CY - Frankfurt am Main, Germany DA - 08.10.2025 KW - Phosphor KW - Recycling KW - CaNaPO4 KW - Pflanzenversuche KW - Klärschlamm KW - Additiv PY - 2025 AN - OPUS4-64711 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Adam, Christian T1 - R-Rhenania - Modifiziertes Rhenaniaphosphat aus Klärschlammasche für Bayern N2 - Vorstellung des Projektstands R-Rhenania aus der Förderinitiative RePhoR des BMBF. T2 - DPP FORUM 2022: Phosphor Recycling 2029 Etappenziel erreicht? CY - Frankfurt a.M., Germany DA - 13.10.2022 KW - Phosphorrückgewinnung KW - Klärschlammasche KW - thermochemische Behandlung PY - 2022 AN - OPUS4-55980 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Adam, Christian T1 - R-Rhenania - Modifiziertes Rhenania Phosphat aus Klärschlammasche für Bayern N2 - In Bayern wird Klärschlamm aus der kommunalen Abwasserreinigung weitgehend verbrannt. Monoverbrennungsanlagen - ausschließlich für kommunalen Klärschlamm - gibt es in Altenstadt, München, Gendorf, Straubing, Neu-Ulm und zukünftig auch in Augsburg. Die Anlage in Altenstadt verbrennt jährlich ca. 55.000 t Klärschlamm-Trockensubstanz und produziert dabei rund 15.000 t phosphatreiche Aschen. Die Asche aus Altenstadt wird zurzeit überwiegend direkt landwirtschaftlich genutzt. Aufgrund der niedrigen Schadstoffgehalte ist diese Nutzung nach den düngemittelrechtlichen Regelungen gesetzlich zulässig. Um der Intention der neuen Düngeverordnung (26. Mai 2017) nach hocheffizienten, d.h. gut pflanzenverfügbaren Düngemitteln zu entsprechen, ist eine Aufbereitung der Klärschlammasche geplant. Im Rahmen des R-Rhenania Projektes errichten der Betreiber der Klärschlammverbrennungsanlage Altenstadt in Bayern Emter GmbH - und der Düngemittelhersteller sePura GmbH gemeinsam eine AshDec®-Demonstrationsanlage, die im Jahr 2023 den Betrieb aufnehmen soll. Das angewandte AshDec®-Verfahren schließt die Phosphate in der Klärschlammasche thermisch im Drehrohrofen auf und macht diese für Pflanzen vollständig verfügbar. Gleichzeitig werden Schadstoffe wie Arsen, Blei und Cadmium entfernt. Den thermischen Aufschluss kennt man bereits vom erfolgreichen, aber nicht mehr produzierten Düngemittel „Rhenania-Phosphat“, das auf der Basis von Rohphosphaten hergestellt wurde. Die geplante Anlage wird neben den Aschen aus Altenstadt zusätzlich die Aschen aus weiteren bayerischen Verbrennungsanlagen verwerten und für eine Kapazität von 30.000 Jahrestonnen Asche ausgelegt sein. Der Projektpartner sePura plant den produzierten Dünger vollständig in Bayern zu verwerten. Dies verringert die Umweltbelastung durch lange Transportwege und fördert die Regionalität des Vorhabens. T2 - RePhoR Auftaktveranstaltung CY - Online meeting DA - 03.11.2020 KW - Klärschlammasche PY - 2020 AN - OPUS4-51608 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Adam, Christian A1 - Herzel, Hannes T1 - R-Rhenania - Modifiziertes Rhenania Phosphat aus Klärschlammasche für Bayern N2 - Im Verbundprojekt R-Rhenania wird eine industrielle Demonstrationsanlage am Standort der Monoverbrennungsanlage Altenstadt der Firma Emter errichtet und im Jahr 2024 den Betrieb aufnehmen. Die vorhandene Rostfeuerung-Monoverbrennung wird so umgebaut, dass ein neues thermochemisches Verfahren integriert werden kann, welches hochwirksame und schadstoffarme Dünger produziert (bis zu 17.000 t/a). Die thermochemischen Produkte werden in Gefäß- und Feldversuchen im ökologischen Landbau auf ihre Düngewirkung getestet. Die Umweltverträglichkeit der Demonstrationsanlage wird untersucht, wie auch die Übertragbarkeit des Verfahrens auf weitere Regionen. T2 - Statusseminar RePhoR CY - Frankfurt am Main, Germany DA - 03.05.2023 KW - Phosphor KW - Monoverbrennung KW - Recycling KW - Nährstoffe KW - Dünger PY - 2023 AN - OPUS4-59486 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Leube, Peter T1 - Quantification of ultrashort per- and polyfluoroalkyl substances (PFAS) in water samples via headspace gas chromatographymass spectrometry (GC-MS) - a method development N2 - Ultrashort PFAS (≤ 3 carbon atoms) were overlooked for a long time in analytical monitoring. Beside through the use of these substances, they contribute to the PFAS background in the environment through (environmental/ bio-) degradation and incomplete destruction3 of PFAS with longer carbon chains or other fluorinated compounds. As part of the German-Israeli Cooperation in Water Technology Research project „Detection, quantification, and treatment of per- and polyfluoroalkyl substances in groundwater“ (DEFEAT-PFAS), we are developing an as simple as possible direct headspace (HS-)GC-MS method to detect trifluoroacetic acid (TFA) and perfluoropropanioc acid (PFPrA), as well as trifluoroethanol (TFEtOH), pentafluoropropanol(PFPrOH) and hexafluoroiospropanol (HFIP) in water samples. Here we present the results of the PFAS mentioned in spiked ultrapure water solutions. T2 - German Israeli Water Technology Status Seminar CY - Koblenz, Germany DA - 18.06.2024 KW - Ground water KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Gas chromatography - mass spectrometry (GC-MS) PY - 2024 AN - OPUS4-60330 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Leube, Peter T1 - Quantification of ultrashort per- and polyfluoroalkyl substances (PFAS) in water samples via headspace gas chromatography-mass spectrometry (GC-MS) - a method development N2 - Per- and polyfluoroalkyl substances (PFAS) were classified as a group of highly concerning chemicals over the last decades. Because of the high persistence of PFAS, their previous use led to contamination of the environment and human population. Due to ongoing use and incomplete remediation or destruction methods, the PFAS background in the environment is growing continuously. The presence of ultrashort PFAS (with ≤3 carbon atoms) in the environment is often overlooked despite their contributions to PFAS levels. These compounds may directly contaminate the environment and arise from degradation of polyfluorinated compounds as well as incomplete PFAS destruction in certain industrial processes. Nonetheless, few approaches for targeted analysis of ultrashort PFASs have been developed, except for trifluoroacetic acid (TFA). Beside liquid (LC-MS/MS), supercritical fluid (SFC-MS/MS), and ion chromatography (IC-MS)-based systems, gas chromatography coupled with mass spectrometry (GC-MS) is a promising method for detection and quantification of ultrashort PFAS. The goal of this study was to develop a simple headspace GC-MS method for the quantification of ultrashort perfluorocarboxylic acids (PFCAs) and polyfluorinated alcohols (PFOHs) in water samples. In contrast to PFOHs, functionalization of PFCAs was required for quantification. This was done by esterification with methanol at 80 °C, which can be carried out directly in the headspace GC-MS system. Moreover, several parameters were optimized to achieve a low limit of quantification (LOQ) for the analytes used: i) The ratio of the aqueous solution, methanol, and available gas phase within the analysis vessel, ii) the concentration of additional acid in esterification mixtures of PFCAs, iii) shaking frequency and iv) shaking time before analysis. After optimizing the procedure, we were able to quantify ultrashort PFCAs and PFOHs. Thus, our developed headspace GC-MS method has the potential to be used as an alternative target analysis for ultrashort-chain PFCAs and PFOHs in various water samples (groundwater, wastewater). T2 - SETAC Europe 34th Annual Meeting CY - Seville, Spain DA - 05.05.2024 KW - Ultrashort PFAS KW - Headspace GC-MS KW - Perfluorocarboxylic acid (PFCA) KW - Polyfluorinated alcohol (PFOH) PY - 2024 AN - OPUS4-60042 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Quantification of Perfluorocarboxylic Acids in Water Samples via Static Headspace Gas Chromatography Coupled to Mass Spectrometry N2 - Perfluorocarboxylic acids (PFCAs) are one of the most prominent and studied subgroups of per- and polyfluoroalkyl substances (PFASs), which have attracted great interest in environmental and toxicology research due to their intensive use in combination with their persistence, mobility and potential threat to ecosystems and human health. The standard method to quantify PFCAs in water samples is liquid chromatography or, for additional quantification of ultrashort-chain PFCAs (carbon chain length of two or three carbon atoms) too, hydrophilic interaction liquid chromatography, in each case coupled with mass spectrometry. However, there are a lot of laboratories using MS coupled to headspace gas chromatography systems (HS-GC-MS), usually to quantify a wide range of volatile organic compounds. While PFCAs themselves are difficult to measure with HS-GC-MS in water samples, this challenge can be solved by derivatizing the acids to more volatile compounds, like esters. This approach could enable laboratories using HS-GC-MS to analyse and monitor PFCAs in environmental water samples. By following this idea, we successfully developed a HS-GC-MS method to quantify PFCAs in ultrapure water. Trifluoric acid (TFA), perfluoropropionic acid (PFPrA), perfluorobutanoic acid (PFBA) and perfluorooctanoic acid (PFOS) served as exemplary analytes of PFCAs, which were derivatized with methanol and concentrated sulfuric acid to form methyl esters. The method was optimized by varying different preparation and measurement parameters, leading to limits of detection and quantification in the two-digit ppt-range for all four analytes. The method was than tested on various real water samples, including tap and bottled water, groundwater, landfill leachate, treated wastewater and impinger water from a sewage sludge incineration experiment. Furthermore, snow samples from a ski slope were analysed too. TFA was the most frequently detected PFAA, with concentrations in the ppt and low ppb range. The detection and quantification of the remaining three PFCAs vary with the sample types and sampling location.Our results show that HS-GC-MS is suitable, and enables laboratories with this technique, to quantify PFCAs water samples. T2 - SETAC Europe CY - Vienna, Austria DA - 11.05.2025 KW - Per- and polyfluoroalkyl substances (PFAS) KW - Groundwater KW - GC-MS PY - 2025 AN - OPUS4-63094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Joachim T1 - Production of raw materials for the cement industry based on steel making slags from future hydrogen based steel production routes N2 - Increasing amounts of new types of EAFS from the DRP-EAF-route and still significant amounts of BOFS from the DRP-SAF-BOF-route will be produced while BFS will vanish. In two BMBF funded research projects, BAM and FEhS examine the application of slags from future steel production in the cement industry. The project “SlagCEM” investigated the recovery of iron from BOFS while producing a mineral product with good cementitious properties. The reduction of BOFS to recover metallic iron along with the generation of a clinker-like material for the cement industry increases the viscosity of the BOFS. This would require a process at unfeasibly high temperatures of >1.700 °C. Therefore, SlagCEM aimed to modify the BOFS to reduce the viscosity to suitable ranges at lower temperatures of ~1.600 °C. A demonstration trial (20 tons) was carried out and the potential for substitution of OPC was determined. DRI-EOS investigates the utilization of increasing amounts of DRI-based EAFS in the cement industry to compensate the reduced production of GBFS. This requires an adjustment of the slag’s chemical composition and a rapid quenching to create an amorphous structure with latent hydraulic characteristics. The project studies the behavior of the modified slag during the metallurgical process and during solidification, any possibly negative impact on the cementitious or environmental properties as well as the potential to recover metals such as Fe, Cr, Mo and V. The final results of the project “SlagCEM”, finished in 2024, as well as the current state and insights of the project “DRI-EOS”, started in July 2022, shall be presented in this talk. T2 - Euroslag 2024 CY - Bilbao, Spain DA - 23.10.2024 KW - Slag KW - Steel KW - Cement KW - Electric Arc Furnace (EAF) KW - Basic Oxygen Furnace (BOF) PY - 2024 AN - OPUS4-61839 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schraut, Katharina T1 - Production of an alite-rich material from reduced basic oxygen furnace slags N2 - Basic oxygen furnace slag (BOFS) is a by-product of steelmaking of which about 10.4 Mt are produced annually in the EU. BOFS is mostly used in road construction, earthwork and hydraulic engineering. However, in this use, the iron bound in BOFS is lost and the opportunity to produce higher value products from BOFS is forgone. In recent decades, many researchers have investigated the production of both Portland cement clinker and crude iron from BOFS via a thermochemical reductive treatment. The reductive treatment of liquid BOFS causes a reduction of iron oxides to metallic iron, which separates from the mineral phase due to its higher density and can be recovered. An advantage of this process is that simultaneously the chemical composition of the reduced BOFS is adapted to that of Portland cement clinker and the hydraulic reactive mineral alite (Ca3SiO5) is formed. In this study, German BOFS was reduced in a small-scale electric arc furnace and a low-iron mineral product rich in alite was produced. Despite a chemical and mineralogical composition similar to that of Portland cement clinker, the reduced BOFS produced less heat of hydration, and its reaction was delayed compared to Portland cement. However, adding gypsum accelerated the hydration rate of the reduced BOFS. Further research to improve the hydraulic properties of the reduced BOFS is essential. If successful, the production of a hydraulic material and crude iron from BOFS could have economic and ecological benefits for both the cement and steel industry. T2 - GeoBerlin 2023 CY - Berlin, Germany DA - 04.09.2023 KW - BOFS KW - Alite KW - Hydraulic reactivity PY - 2023 AN - OPUS4-58206 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schraut, Katharina T1 - Production of a hydraulic material from post-treated steelmaking slags N2 - Steelmaking slag is a by-product of steel production of which 4.5 Mt were produced in 2020 in Germany alone. It is mainly used in road construction, earthwork and hydraulic engineering. A smaller part is returned to the metallurgical circle, used as fertilizer or landfilled. With this use, iron oxides still contained in steelmaking slag are lost. In addition, the possibility of producing higher-grade products from steelmaking slag is foregone. In recent decades, many researchers have investigated the production of Portland cement clinker and crude iron from basic oxygen furnace slags (BOFS) via a reductive treatment. Carbothermal treatment of liquid BOFS causes a reduction of iron oxides to metallic iron, which separates from the mineral phase due to its higher density. Simultaneously, the chemical composition of the reduced slag is adapted to that of the Portland cement clinker. In this study, German BOFS was reduced in a small-scale electric arc furnace using petrol coke as a reducing agent. The resulting low-iron mineral product had a similar chemical composition to Portland cement clinker and was rich in the tricalcium silicate solid solution alite (Ca3SiO5). Based on its chemical and mineralogical composition, similar to that of Portland cement clinker, the reduced BOFS has the potential to react comparably. In our study, the reduced BOFS produced less heat of hydration compared to OPC and its hydraulic reaction was delayed. However, adding gypsum has been shown to accelerate the hydration rate of the reduced BOFS compared to that known from the calcium silicates of Portland cement clinker. Further research to improve the hydraulic properties of the reduced slag is essential. If successful, producing a hydraulic binder and crude iron from BOFS could have economic and ecological benefits for both the cement and steel industry. T2 - 16th International Congress on the Chemistry of Cement ICCC 2023 CY - Bangkok, Thailand DA - 18.09.2023 KW - Steelmaking slag KW - Alite hydraulic reactivity KW - Clinker substitute PY - 2023 AN - OPUS4-58522 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF ED - Schraut, Katharina ED - Adamczyk, Burkart ED - Adam, Christian ED - Stephan, D. ED - Simon, Sebastian ED - von Werder, Julia ED - Meng, Birgit T1 - Production of a hydraulic material from post treated steelmaking slags N2 - Steelmaking slag is a by-product of steel production, of which 4.5 Mt were produced in 2020 in Germany alone. It is mainly used in road construction, earthwork and hydraulic engineering. A smaller part is returned to the metallurgical cycle, used as fertiliser or landfilled. With this use, iron oxides still contained in steelmaking slag are lost. In addition, the possibility of producing higher-grade products from steelmaking slag is foregone. In recent decades, many researchers have investigated the production of Portland cement clinker and crude iron from basic oxygen furnace slags (BOFS) via a reductive treatment. Carbothermal treatment of liquid BOFS causes a reduction of iron oxides to metallic iron, which separates from the mineral phase due to its higher density. Simultaneously, the chemical composition of the reduced slag is adapted to that of Portland cement clinker. In this study, German BOFS was reduced in a small-scale electric arc furnace using petrol coke as a reducing agent. The resulting low-iron mineral product has a similar chemical composition to Portland cement clinker and was rich in the tricalcium silicate solid solution alite (Ca3SiO5). Based on its chemical and mineralogical composition, similar to that of Portland cement clinker, the reduced BOFS has the potential to react comparably. In our study, the reduced BOFS produced less hydration heat than OPC, and its hydraulic reaction was delayed. However, adding gypsum has shown to accelerate the hydration rate of the reduced BOFS compared to that known from the calcium silicates of Portland cement clinker. Further research to improve the hydraulic properties of the reduced slag is essential. If successful, producing a hydraulic binder and crude iron from BOFS has economic and ecological benefits for both the cement and steel industries. T2 - The 16th International Congress on the Chemistry of Cement 2023 (ICCC2023) CY - Bangkok, Thailand DA - 18.09.2023 KW - Steelmaking slag KW - Alite KW - Clinker substitute KW - Hydraulic reactivity PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-590522 UR - https://www.iccc-online.org/archive/ SP - 432 EP - 436 CY - Bangkok AN - OPUS4-59052 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Franz-Georg T1 - Product testing and performance N2 - Geosynthetic materials are applied in measures for coastal protection. Weathering or any damage of constructions, as shown by a field study in Kaliningrad Oblast (Russia), could lead to the littering of the beach or the sea (marine littering) and the discharge of possibly harmful additives into the marine environment. The ageing behavior of a widely used geotextile made of polypropylene was studied by artificial accelerated ageing in water-filled autoclaves at temperatures of 30 to 80° C and pressures of 10 to 50 bar. Tensile strength tests were used to evaluate the progress of ageing, concluding that temperature rather than pressure was the main factor influencing the ageing of geotextiles. Using a modified Arrhenius equation, it was possible to calculate the half-life for the loss of 50% of the strain, which corresponds to approximately 330 years. T2 - EuroGeo-7, Session Geosynthetics, Sustainability and Current Industry Challenges CY - Warschau, Poland DA - 04.09.2022 KW - Geosynthetics KW - Ageing KW - Autoclave tests PY - 2022 AN - OPUS4-55671 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -