TY - CONF A1 - Meermann, Björn A1 - Ley, Philip A1 - Metzger, Matthias A1 - Sturm, Manfred T1 - Fluoranalytik mittels hochauflösender-continuum source Graphitrohr Molekülabsorptionsspektrometrie (HR-CS-GFMAS) - Screening von Organofluor im Oberflächenwasser N2 - Vortrag zur Entwicklung von Organo-Fluor Summenparametermethoden auf Basis der HR-CS-GFMAS für die Umweltanalytik T2 - PerFluSan Treffen; 1. Workshop zur PFC-Sanierung_Schwerpunkt Analytik CY - Karlsruhe, Germany DA - 25.06.2019 KW - Hochauflösende-continuum source Graphitrohr Molekülabsorptionsspektrometrie (HR-CS-GFMAS) KW - Fluorierte Organische Verbindungen KW - Umweltanalytik KW - (Organisch gebundenes) Fluor-Summenparameter PY - 2019 AN - OPUS4-48632 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Smol, M. A1 - Adam, Christian T1 - Towards circular economy for phosphorus in Poland N2 - In the transition to the Circular Economy (CE) model, where the added value of products is kept as long as possible and waste is eliminated, the sustainable management of raw materials plays a key role. In above CE model, especial attention is paid to CRMs which are economically and strategically important for the European economy, but have a high-risk associated with their supply. One of the most important element which can not be replaced and is an essential element for human nutrition, yet limited resource is phosphorus (P). An importance of issues related to sustainable P management results from EU legislation, which indicated P as a Critical Raw Material (CRM). The sustainable management of P-resources is especially important for the Baltic region. A consequence of waterborne loads passing into the sea, mainly as wastewater with a high P content is the eutrophication of the Baltic Sea environment. Due to the largest inputs of P (37%) into the Baltic Sea originate from Poland, the development of sustainable solutions aimed at more rational P management for this country is externally important. T2 - International Phosphorus Workshop 9 CY - Zurich, Switzerland DA - 08.07.2019 KW - Phosphorus recovery KW - Circular economy PY - 2019 AN - OPUS4-48614 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Smol, M. A1 - Adam, Christian T1 - Possibility of recovering phosphorus from sewage sludge ash (SSA) in Poland N2 - Due to the vital importance of phosphorus (P) and its increasing scarcity as a natural resource, phosphorus recovery has recently gained significant scientific and technical interest. An interesting sources of phosphorus are sewage sludge (SS) and sewage sludge ash (SSA) due to the major part of the phosphate from P rich wastewater is transferred to the sludge (approx. 90%). Despite the fact that the raw materials base is large (PURE report indicates that in 2020 the amount of sewage sludge generated in Poland will reach 180% of the dry matter of sewage sludge produced in 2010), at present recycling of phosphorus is not a commonly used practice in Poland. T2 - International Phosphorus Workshop 9 CY - Zurich, Switzerland DA - 08.07.2019 KW - Sewage sludge ash KW - Phosphorus recovery PY - 2019 AN - OPUS4-48616 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schartel, Bernhard T1 - Flame Retardant Polyurethane: An Old, an Actual, and a Future Challenge N2 - This paper is based mainly on the results of two different projects performed in the group of the author recently (2016-2019). The three external partners involved in these two projects are competent in the preparation of FPUF (ICL IP America), RPUF (Department of Industrial Engineering, Padova University), and TPU (Fraunhofer-Institut für Betriebsfestigkeit und Systemzuverlässigkeit LBF, Darmstadt) as well as for the specimen preparation. Systematically varied sets of materials were prepared as the key basic for scientific discussion, varying the kind and combination of flame retardant, PUR structure, density, and blowing agent. A multimethodical approach based on thermogravimetry (TGA), TGA coupled with evolved gas analysis (TGA-FTIR) and pyrolysis GC-MS was used for investigating the pyrolysis. The flammability was addressed using oxygen index (OI) and testing in UL 94 burning chamber in vertical and horizontal set-up. The fire behaviour was addressed by using a cone calorimeter. Beyond these methods according to the state of the art, key experiments were performed. We addressed the dripping and the two-stage burning of TPU using a self-designed apparatus and specific data evaluation, the foam burning through quenching burning samples, using different special sample holders, and measuring temperature profiles within the burning foams. The investigation is made round by intensive analysis of the fire residues, such as comprehensive investigation of the morphology. Result on the pyrolysis (TGA-FTIR, Pyrolysis-GC/MS), flammability (UL 94, LOI), and fire behaviour (cone calorimeter) of TPU and flame retardant TPUs are shown. We discuss in detail the characteristic of PUR decomposition: the low tendency to char, and the specific two step decomposition and how these characteristics control the regimes in fire behaviour. We demonstrate that the different burning regimes are controlled by different pyrolysis products and effective heat of combustions. The resulting formation of pool fires as well as the formation of dripping is discussed in detail. The latter quite important to understand the flame retardancy applied with respect to achieve the UL 94 classification V0 nondripping or V0 non-flaming dripping. Rigid and flexible PUR foams and their flame retarded versions are investigated for different densities. Water and pentane-blown foams are compared as well as PUR and polyisocyanurate-polyurethane (PIR) foams. Horizontal testing in the cone calorimeter is used and the vertical foam specimen holder as well. Self-designed set-ups within the cone calorimeter enable a better inside in the pyrolysis front running through the foam samples as well as the development of the temperature gradient inside the foam during the fire test. The morphology change during burning was characterised by the means of quenching burning foams with liquid nitrogen and investigating the cross sections with scanning electron microscope. In sum, a rather comprehensive study was performed to work out the principle fire phenomena controlling the fire behaviour of PUR foams in a very systematic and significant way. Promising flame retardancy approaches are discussed. The importance of either combining the drain of fuel and flame inhibition or charring into an effective protection layer/multicellular structure is underlined. This contribution focusses the general conclusions and trends. It tries to increase the understanding of the specific and demanding challenge to develop flame retardant PUR materials. T2 - Interflam 2019, 15th International Interflam Conference CY - Egham, UK DA - 01.07.2019 KW - Polyurethane KW - Flame retardant KW - Dripping KW - Flammability KW - Pool fire KW - Pyrolysis KW - Decomposition KW - Foams PY - 2019 AN - OPUS4-48557 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lenz, J. A1 - Pospiech, D. A1 - Paven, M. A1 - Albach, R. W. A1 - Günther, Martin A1 - Schartel, Bernhard A1 - Voit, B. T1 - Improving the Flame Retardance of Polyisocyanurate Foams by Dibenzo[d,f][1,3,2]dioxaphosphepine 6-Oxide-Containing Additives N2 - A series of new flame retardants (FR) based on dibenzo[d,f][1,3,2]dioxaphosphepine 6-oxide (BPPO) incorporating acrylates and benzoquinone were developed previously. In this study, we examine the fire behavior of the new flame retardants in polyisocyanurate (PIR) foams. The foam characteristics, thermal decomposition, and fire behavior are investigated. The fire properties of the foams containing BPPO-based derivatives were found to depend on the chemical structure of the substituents. We also compare our results to state-of-the-art non-halogenated FR such as triphenylphosphate and chemically similar phosphinate, i.e. 9,10-dihydro-9-oxa-10- phosphaphenanthrene-10-oxide (DOPO), based derivatives to discuss the role of the phosphorus oxidation state. KW - Polyisocyanurate KW - Dibenzo[d,f][1,3,2]dioxaphosphepine 6-oxide KW - Phospha-Michael addition KW - Flame retardant KW - Foams PY - 2019 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-485590 SN - 2073-4360 VL - 11 IS - 8 SP - Article 1242 PB - MDPI AN - OPUS4-48559 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - von der Au, Marcus A1 - Schwinn, M. A1 - Kuhlmeier, K. A1 - Büchel, C. A1 - Meermann, Björn T1 - Development of an automated on-line purification HPLC single cell-ICP-MS approach for fast diatom analysis N2 - The most challenging part in performing a single cell ICP-MS (sc-ICP-MS) approach is the sample preparation, in particular the reduction of the ionic background. This step is, in many cases, time-consuming and required for each sample separately. Furthermore, sc-ICP-MS measurements are mostly carried out "manually", given the fact that present systems are not allowing for an automated change of samples. Thus, within this work, we developed an approach based on a HPLC system coupled on-line with sc-ICP-MS via a set of switching valves as well as an in-line filter for automated cell washing. This set-up enables the ionic background removal as well as analysis of single cells completely automated without any manual sample pretreatment. Our approach was applied for the analysis of the single celled diatom species Cyclotella meneghiniana, a marine diatom species, on the basis of Mg24 and facilitates testing in 11 min per sample, requiring only around 10,000 cells in a volume of 10 µL and approx. 10 mL of a 5% MeOH/95% deionized water (v/v) mixture. Even at extremely saline culturing media concentrations (up to 1000 mg L-1 magnesium) our on-line approach worked sufficiently allowing for distinction of ionic and particulate fractions. Furthermore, a set of diatom samples was analyzed completely automated without the need for changing samples manually. So, utilizing this approach enables analyzing a high quantity of samples in a short time and therefore in future the investigation of ecotoxicological effects is simplified for example in terms of metal accumulation by taking biovariability into account. KW - Single cell-ICP-MS KW - Diatoms KW - Ecotoxicology testing KW - Automated system PY - 2019 U6 - https://doi.org/10.1016/j.aca.2019.05.045 SN - 1873-4324 VL - 1077 SP - 87 EP - 94 PB - Elsevier AN - OPUS4-48567 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kotthoff, Lisa A1 - Lisec, Jan A1 - Schwerdtle, T. A1 - Koch, Matthias T1 - Prediction of transformation products of monensin by electrochemistry compared to microsomal assay and hydrolysis N2 - The knowledge of transformation pathways and identification of transformation products (TPs) of veterinary drugs is important for animal health, food, and environmental matters. The active agent Monensin (MON) belongs to the ionophore antibiotics and is widely used as a veterinary drug against coccidiosis in broiler farming. However, no electrochemically (EC) generated TPs of MON have been described so far. In this study, the online coupling of EC and mass spectrometry (MS) was used for the generation of oxidative TPs. EC-conditions were optimized with respect to working electrode material, solvent, modifier, and potential polarity. Subsequent LC/HRMS (liquid chromatography/high resolution mass spectrometry) and MS/MS experiments were performed to identify the structures of derived TPs by a suspected target analysis. The obtained EC-results were compared to TPs observed in metabolism tests with microsomes and hydrolysis experiments of MON. Five previously undescribed TPs of MON were identified in our EC/MS based study and one TP, which was already known from literature and found by a microsomal assay, could be confirmed. Two and three further TPs were found as products in microsomal tests and following hydrolysis, respectively. We found decarboxylation, O-demethylation and acid-catalyzed ring-opening reactions to be the major mechanisms of MON transformation. KW - Transformation products KW - Monensin KW - Veterinary drugs KW - Electrochemistry KW - Hydrolysis KW - LC/HRMS PY - 2019 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-485689 SN - 1420-3049 VL - 24 IS - 15 SP - 2732, 1 EP - 12 PB - MDPI CY - Basel AN - OPUS4-48568 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hamann, Christopher A1 - Adam, Christian A1 - Stolle, Dirk A1 - Spanka, M. A1 - Auer, G. T1 - Thermochemical treatment of waste products from iron and steel production N2 - Blast furnace (BF) sludge and electric arc furnace (EAF) dust are typical wastes that incur from iron and steel production. In addition to iron, calcium, carbon, and silicon they usually contain high concentrations of heavy metals such as zinc, lead, and cadmium that are potentially hazardous to the environment, rendering disposal in landfills ecologically problematic and costly. Consequently, pyrometallurgical, hydrometallurgical, and hybrid methods for selective elimination of non-ferrous heavy metals from BF sludge and EAF dust have been conceived, of which only the carbothermic reduction route taken in the so-called Waelz rotary kiln process has been proven to be economically successful. However, this process has several drawbacks regarding efficiency of heavy-metal removal and recovery of iron, and it does not allow processing of BF sludge. In this study, we investigated the efficiency and feasibility of selective chlorination and evaporation of non-ferrous heavy metals, particularly zinc and lead, in both BF sludge and EAF dust as an alternative, thermochemical processing route. To this end, hydrochloric acid and iron(II) chloride solution have been used as chlorinating agents, and the process of heavy-metal chlorination and evaporation has been investigated under inert operating conditions, at variable chlorine concentrations, and at temperatures between 500 and 1200 °C. High zinc and lead removal efficiencies of > 99.5 % were achieved with both chlorinating agents, but iron(II) chloride turned out to be overall more efficient for removal of zinc and lead from BF sludge and EAF dust. Interestingly, and in contrast to previous studies, the iron was completely retained in the processed solid residue, therefore rendering the processed residues virtually zinc- and lead-free raw materials that may either be used internally (e.g., feeding processed BF sludge and EAF dust back into the respective furnaces) or externally (e.g., for cement production). T2 - European Metallurgical Conference 2019 CY - Düsseldorf, Germany DA - 23.06.2019 KW - Blast furnace sludge KW - Electric arc furnace dust KW - Recycling KW - Selective chlorination KW - Zinc PY - 2019 SN - 978-3-940276-89-6 VL - 3 SP - 1267 EP - 1282 PB - GDMB CY - Clausthal-Zellerfeld AN - OPUS4-48362 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Taube, Mareike Carolin A1 - Adam, Christian A1 - Adamczyk, Burkart A1 - Beckmann, T. A1 - Reuter, M. A1 - Stelter, M. T1 - Influence of carbon feeding on a pyrometallurgical tantalum and niobium recycling process and the formation of carbides N2 - An existing pyrometallurgical process for tantalum and niobium recovery, mainly from low grade pyrometallurgical residues, was investigated. Series of melting experiments were carried out in a pilot-scale electric arc furnace to study how the amount, the grain size and the way of feeding affect the activity of carbon as a reducing agent. During the pyrometallurgical treatment refractory metals such as tantalum and niobium are reduced to their carbide form and enriched in the molten iron-based metal phase. The cooled down slag and metal phase were analysed to investigate thermodynamic and kinetic conditions of the carbide formation. FACT Sage simulations were also used to investigate the material system in state of thermodynamic equilibrium. Results show that mass transfer and kinetics may play an important role if compared to equilibrium analyses using FACT Sage. T2 - Euopean Metallurgical Conference (EMC) 2019 CY - Düsseldorf, Germany DA - 23.06.2019 KW - Pyrometallurgy KW - Tantalum KW - Carbide formation KW - Reduction process KW - Carbon feeding PY - 2019 SN - 978-3-940276-87-2 VL - 1 SP - 371 EP - 386 PB - GDMB Verlag GmbH CY - Clausthal-Zellerfeld AN - OPUS4-48363 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hamann, Christopher A1 - Adam, Christian A1 - Stolle, Dirk A1 - Spanka, M. A1 - Auer, G. T1 - Thermochemical treatment of waste products from iron and steel production N2 - This presentation summarizes the development of a novel thermochemical process for recycling of zinc and lead-bearing wastes (blast furnace sludge and electric arc furnace dust) that accumulate during iron and steel production. T2 - European Metallurgical Conference 2019 CY - Düsseldorf, Germany DA - 23.06.2019 KW - Blast furnace sludge KW - Electric arc furnace dust KW - Recycling KW - Selective chlorination KW - Zinc PY - 2019 AN - OPUS4-48364 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -