TY - JOUR A1 - Smol, M. A1 - Adam, Christian A1 - Kugler, Stefan T1 - Thermochemical Treatment of Sewage Sludge Ash (SSA)—Potential and Perspective in Poland N2 - Phosphorus (P) recovery from sewage sludge ash (SSA) is one of the most promising approaches of phosphate rock substitution in mineral fertilizers and might be a sustainable way to secure supply of this raw material in the future. In the current investigation, the process of thermochemical treatment of SSA was applied to SSA coming from selected mono-incineration plants of municipal sewage sludge in Poland (Cracow, Gdansk, Gdynia, Lodz, Kielce and Szczecin). The Polish SSA was thermochemically converted in the presence of sodium (Na) additives and a reducing agent (dried sewage sludge) to obtain secondary raw materials for the production of marketable P fertilizers. The process had a positive impact on the bioavailability of phosphorus and reduced the content of heavy metals in the obtained products. The P solubility in neutral Ammonium citrate, an indicator of its bioavailability, was significantly raised from 19.7–45.7% in the raw ashes and 76.5–100% in the thermochemically treated SSA. The content of nutrients in the recyclates was in the range of 15.7–19.2% P2O5, 10.8–14.2% CaO, 3.5–5.4% Na2O, 2.6–3.6% MgO and 0.9–1.3% K2O. The produced fertilizer raw materials meet the Polish norms for trace elements covered by the legislation: the content of lead was in the range 10.2–73.1 mg/kg, arsenic 4.8–22.7 mg/kg, Cadmium 0.9–2.8 mg/kg and mercury <0.05 mg/kg. Thus, these products could be potentially directly used for fertilizer production. This work also includes an analysis of the possibilities of using ashes for fertilizer purposes in Poland, based on the assumptions indicated in the adopted strategic and planning documents regarding waste management and fertilizer production. KW - Sewage Sludge Ashes KW - Critical raw materials KW - Phosphorus KW - Fertilizer KW - Sewage Sludge PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514468 DO - https://doi.org/10.3390/en13205461 VL - 13 IS - 20 SP - 5461 AN - OPUS4-51446 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Noack, M. A1 - Dittmar, A. A1 - Stöhr, M. A1 - Georgi, G. A1 - Adam, Christian A1 - Brenneis, Rudolf A1 - Kley, Gerd A1 - Lehmann, Annekatrin A1 - Handte, J. A1 - Meichle, K. A1 - Schwake, M. T1 - Thermische Regenerierung von Zeolithpulver Typ X aus der VOC-Luftreinigung N2 - Für die Entfernung von VOC (volatile organic compounds) aus der Luft von Fertigungsstätten werden vielfach mikroporöse Adsorbentien eingesetzt. Die gereinigte Luft wird rezyklisiert. Für die mit VOC beladenen Adsorbentien wird ein Regenerierungsweg für den mehrfachen Gebrauch gesucht. Bei der Regenerierung sollen die VOC möglichst vollständig desorbiert werden und mit einer geringen Gasmenge in einer katalytischen Verbrennung zu CO2 und H2O umgewandelt werden. Die Wirtschaftlichkeit der Luftreinigung wird wesentlich bestimmt durch die Sorptionskapazität des Adsorbens, die erforderliche Energie für die thermische Regenerierung und die Menge des Spülgases bei der Regenerierung. In dieser Arbeit wird der Einsatz von Typ X-Zeolithpulver in der Luftreinigung einer Lackiererei beschrieben und dessen Regenerierung im Labor mittels DTA/TG und Isothermenmessung der Schlüsselkomponenten untersucht. Ferner wurde die Regenerierung des beladenen Zeoliths in einem Labor-Drehrohrofen unter Variation der Betriebsparameter untersucht und anschließend mit ausgewählten Parametern in einem kleintechnischen Drehrohrofen durchgeführt. Die Verfahrensvarianten werden diskutiert. KW - Adsorption KW - Verfahrensentwicklung KW - VOC KW - Zeolithe PY - 2007 SN - 0009-286X SN - 1522-2640 VL - 79 IS - 6 SP - 883 EP - 889 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-14975 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Auer, G. A1 - Spanka, M. A1 - Hamann, Christopher A1 - Adam, Christian T1 - Thermal zinc extraction from steel mill dust N2 - Treatment and reusing of hazardous wastes have become significant issues of modern societies. Blast furnace sludge (BFS) and electric arc furnace dust (EAFD) are such typical wastes, because they usually contain high amounts of undesirable elements such as zinc (Zn) and lead (Pb). These elements can cause operational problems in reusing of BFS and EAFD. In this study, the Ferro Duo GmbH and the Federal Institute for Materials Research and Testing have investigated a novel approach for eliminating and/or recovering Zn and Pb from both wastes. Applied was a selective chlorination and volatilization of Zn and Pb as chlorides at temperatures between 500 °C and 1100 °C. Both product obtained, Zn and Pb in the form of ZnCl2 and PbCl2 and the purified solid mineral compound are attractive materials for further use. Hydrochloric acid and iron(II) chloride were used as chlorination agents. Exceptionally high Zn and Pb removal efficiencies of >99.5 % could be achieved with both chlorination agents, whereby iron(II) chloride exhibited better performance. KW - Blast furnace sludge KW - Chlorination KW - Electric arc furnace dust KW - Lead KW - Zinc KW - Thermochemical treatment PY - 2019 SN - 1613-2394 VL - 72 IS - 1 SP - 27 EP - 31 PB - GDMB Verlag GmbH CY - Clausthal-Zellerfeld AN - OPUS4-47288 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steckenmesser, D. A1 - Vogel, Christian A1 - Herzel, Hannes A1 - Félix, R. A1 - Adam, Christian A1 - Steffens, D. T1 - Thermal treatment of sewage sludge for phosphorus fertilizer production: a model experiment N2 - Phosphorus (P) resource availability and quality is declining and recycling P-fertilizers from waste materials are becoming increasingly important. One important secondary P resource is sewage sludge (SSL) where P is often bound as aluminum phosphate (Al-P), iron phosphate (Fe-P) and polyphosphate (poly-P), respectively. Thermal treatment in different ways is a promising way in P recycling to produce highly plant-available P-fertilizers. To investigate mechanisms behind transformation of hardly available P-species toward plant-available P forms we treated a model SSL containing different kinds of defined P sources by low-temperature conversion (LTC) at 500 °C and subsequent thermochemical treatment of the LTC product with Na additives (TCT) at 950 °C, respectively. Pot experiments with ryegrass were carried out to determine the plant availability of P of the different treatments. The poly-P (here pyrophosphates) based fertilizers had a very high plant availability after both thermal treatments. During LTC treatment the plant availability of the Fe-P and Al-P variants increased because of the Formation of Fe(II) phosphates and/or pyro-/polyphosphates. Especially the formation of Al-polyphosphate shows a high plant availability. The subsequent TCT further increased strongly the plant availability of the Fe-P variants because of the formation of highly plant-available CaNaPO4. Thus, a direct TCT without prior LTC probably also produce CaNaPO4 and is recommended for Fe-P based SSL. However, a molar Ca/P ratio of � 1 in the fertilizer is favorable for CaNaPO4 formation. Thus, the knowledge on the source of primary P in SSL is essential for choosing the accurate thermal treatment method to produce highly plant-available P-fertilizers from SSL. KW - Phosphorus KW - Sewage sludge KW - X-ray diffraction KW - X-ray absorption near-edge structure (XANES) spectroscopy KW - Fertilizer PY - 2021 DO - https://doi.org/10.1080/01904167.2021.1994595 SN - 0190-4167 VL - 45 IS - 8 SP - 1123 EP - 1133 PB - Taylor & Francis Online AN - OPUS4-53755 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Adam, Christian A1 - Kley, Gerd A1 - Simon, Franz-Georg T1 - Thermal treatment of municipal sewage sludge aiming at marketable P-fertilisers N2 - Municipal sewage sludge is a carrier of nutrients – most important phosphorus (P) – but also contains organic pollutants and heavy metals. A two steps thermal treatment is suggested based on 1. mono-incineration of sewage sludge under destruction of organic pollutants and 2. thermochemical treatment of the resulting ashes to remove heavy metals and increase P-bioavailability. The targeted products are marketable P-fertilisers. The thermochemical treatment was investigated in a gas tight lab-scale rotary furnace. Seven sewage sludge ashes of different origin and composition and one residue from gasification of sewage sludge were mixed with a chlorine donor (e.g. MgCl2) and thermochemically treated under systematic variation of operational parameters. The distributions of the heavy metals between solid and gas phase were determined. The heavy metals concentrations of the treated ashes met the legislative limits in most cases. The products from thermochemical treatment are suited raw materials for P-fertiliser production. Relevant process parameters such as temperature, type and concentration of Cl-donor and retention time were optimised for the thermochemical treatment step. KW - Sewage sludge KW - Mono-incineration KW - Ash treatment KW - Thermochemical treatment KW - Phosphorus-fertiliser PY - 2007 SN - 1345-9678 SN - 1347-5320 VL - 48 IS - 12 SP - 3056 EP - 3061 PB - Japan Institute of Metals CY - Sendai AN - OPUS4-16647 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Stemann, Jan A1 - Holldack, K. A1 - Sekine, R. A1 - Lipiec, E. A1 - Adam, Christian T1 - Thermal treatment of chromium (III) oxide with carbonates analyzed by far-infrared spectroscopy PY - 2015 SN - 0003-7028 SN - 1943-3530 VL - 69 IS - 10 SP - 1210 EP - 1214 PB - Society for Applied Spectroscopy CY - Frederick, Md. AN - OPUS4-34635 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Taube, Mareike Carolin A1 - Adamczyk, Burkart A1 - Adam, Christian A1 - Feldmann, Ines A1 - Ostermann, Markus A1 - Reuter, M. A1 - Stelter, M. T1 - Tantalrecycling aus pyrometallurgischen Rückständen N2 - Gegenstand dieser Arbeit ist die Untersuchung eines bestehenden pyrometallurgischen Prozesses zur Rückgewinnung von Tantal und Niob aus metallurgischen Reststoffen mit vorwiegend niedriger Wertstoffkonzentration. Zur näheren Erforschung der im vorliegenden Stoffsystem ablaufenden Reduktionsprozesse wurden in einem Elektrolichtbogenofen Schmelzversuche im Pilotmaßstab durchgeführt. Als Reduktionsmittel diente Koks, welcher mithilfe einer Argon-gespülten Eisenlanze in die flüssige mineralische Schmelze eingebracht wurde. Während der Reduktionsbehandlung werden Refraktärmetalle wie Tantal und Niob in ihre Carbide überführt und anschließend in der erschmolzenen eisenbasierten Metallphase am Boden des Reaktors angereichert. Neben Tantal und Niob gelangt auch ein Teil des im Einsatzmaterial enthaltenen Titans als unerwünschtes Begleitelement in die Metallphase. Sein Großteil verbleibt jedoch als Oxid in der Schlacke und wird dort hauptsächlich im Mineral Perowskit (CaTiO3) gebunden. Die erstarrten Schlackeproben wurden mit verschiedenen Methoden wie Röntgenfluoreszensanalyse, Röntgenbeugung und Rasterelektronenmikroskopie mit gekoppelter energiedispersiver Röntgenanalyse untersucht, um die Bildung tantalhaltiger Mineralphasen zu verschiedenen Stadien des Reduktionsprozesses zu verfolgen. Die hier gewonnenen Erkenntnisse zeigen, dass weniger die durch das Einblasen von Koks verursachte Reduktionsreaktion, sondern das Absinken der tantalreichen Eisentröpfchen in der flüssigen mineralischen Schmelze, gefolgt von ihrer Anreicherung in die Metallphase, für die Kinetik ausschlaggebend ist. N2 - An existing pyrometallurgical process for tantalum and niobium recovery, mainly from low grade pyrometallurgical residues, was investigated. Melting experiments were carried out in a pilot-scale electric arc furnace to study the material system during the reduction process caused by blowing coke into the liquid mineral melt. During the pyrometallurgical treatment refractory metals such as tantalum and niobium are converted into their carbides and enriched in the molten iron-based metal phase. Titanium is also enriched in the metal phase as an unwanted accompanying element, but most of it remains in oxidic form in the slag and is mainly bound in the mineral perovskite. Cooled down slag samples were analysed using XRF, XRD, SEM and EDX to investigate the formation of mineral phases rich in tantalum during various stages of the reduction process. The results show that the settling of the tantalum-rich iron droplets in the molten slag into the metal phase May play a greater role for the kinetics than the actual reduction reaction caused by blowing in coke. KW - Tantal KW - Recycling KW - Reduktionsprozess KW - Perowskit KW - Elektrolichtbogenofen PY - 2020 SN - 1613-2394 VL - 73 IS - 4 SP - 196 EP - 205 PB - GDMB Verlag GmbH CY - Clausthal-Zellerfeld AN - OPUS4-51064 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schraut, Katharina A1 - Adamczyk, Burkart A1 - Adam, Christian A1 - Stephan, D. A1 - Meng, Birgit A1 - Simon, Sebastian A1 - von Werder, Julia T1 - Synthesis and characterisation of alites from reduced basic oxygen furnace slags N2 - Basic oxygen furnace slags (BOFS) are by-products of the steelmaking process. Several researchers have studied the production of Portland cement clinker and metallic iron from BOFS via a reductive treatment. In this study, we applied a carbothermal reduction of BOFS in a technical-scale electric arc furnace and characterised the clinker-like products. Those clinker-like non-metallic products (NMPs) had a chemical and mineralogical composition comparable to clinker for ordinary Portland cement (OPC) and contained large elongated alite crystals as major component. The pure NMPs reacted more slowly and achieved a lower degree of hydration compared with commercial OPC. If the reactivity of the products can be further increased by employing specific adaptations, it can be used as a full clinker substitute for OPC. Nevertheless, it is also an option to use the material without further modifications as a cement component or concrete addition, which contributes to the strength development in both cases. KW - BOFS KW - Hydration products KW - Thermal analysis KW - X-ray diffraction PY - 2021 DO - https://doi.org/10.1016/j.cemconres.2021.106518 SN - 0008-8846 VL - 147 SP - 6518 PB - Elsevier Ltd. AN - OPUS4-52939 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ante, A. A1 - Trumpler, A. A1 - Niermann, S. A1 - Decker, Renate A1 - Hermann, L. A1 - Adam, Christian T1 - SUSAN - Sustainable and safe re-use of municipal sewage sludge for nutrient recovery KW - Sewage sludge KW - Phosphorus KW - Recycling KW - Thermochemical treatment KW - Heavy metal removal KW - Large scale consideration PY - 2010 SN - 0016-3651 VL - 151 IS - 13 SP - 78 EP - 84 PB - Oldenbourg-Industrieverl. CY - München AN - OPUS4-22097 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dombinov, V. A1 - Herzel, Hannes A1 - Meiller, M. A1 - Müller, F. A1 - Willbold, S. A1 - Zang, J. W. A1 - da Fonseca-Zang, W. A. A1 - Adam, Christian A1 - Klose, H. A1 - Poorter, H. A1 - Jablonowski, N. D. A1 - Schrey, S. D. T1 - Sugarcane bagasse ash as fertilizer for soybeans: Effects of added residues on ash composition, mineralogy, phosphorus extractability and plant availability N2 - Sugarcane bagasse is commonly combusted to generate energy. Unfortunately, recycling strategies rarely consider the resulting ash as a potential fertilizer. To evaluate this recycling strategy for a sustainable circular economy, we characterized bagasse ash as a fertilizer and measured the effects of co-gasification and co-combustion of bagasse with either chicken manure or sewage sludge: on the phosphorus (P) mass fraction, P-extractability, and mineral P phases. Furthermore, we investigated the ashes as fertilizer for soybeans under greenhouse conditions. All methods in combination are reliable indicators helping to assess and predict P availability from ashes to soybeans. The fertilizer efficiency of pure bagasse ash increased with the ash amount supplied to the substrate. Nevertheless, it was not as effective as fertilization with triple-superphosphate and K2SO4, which we attributed to lower P availability. Co-gasification and co-combustion increased the P mass fraction in all bagasse-based ashes, but its extractability and availability to soybeans increased only when co-processed with chicken manure, because it enabled the formation of readily available Ca-alkali phosphates. Therefore, we recommend co-combusting biomass with alkali-rich residues to increase the availability of P from the ash to plants. KW - Combustion and gasification KW - Phosphate extractability and availability KW - X-ray diffraction (XRD) PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-567632 DO - https://doi.org/10.3389/fpls.2022.1041924 SN - 1664-462X VL - 13 SP - 1 EP - 13 PB - Frontiers Media CY - Lausanne AN - OPUS4-56763 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Kohl, Anka A1 - Adam, Christian T1 - Spectroscopic investigation in the mid- and far-infrared regions of phosphorus fertilizers derived from thermochemically treated sewage sludge ash N2 - Inorganic phosphorus and nitrogen-phosphorus-potassium (NPK) fertilizers based on phosphates from thermochemically treated sewage sludge ash were analyzed using mid-infrared (mid-IR) and far-infrared (FIR) spectroscopy. The different compounds present in the fertilizers were qualitatively determined with the help of recorded reference spectra of pure substances. Differentiation between various phosphates and other compounds such as sulfates, nitrates, and oxides was possible using combined interpretation of the mid-IR and FIR spectra. The results are in agreement with previous X-ray diffraction (XRD) measurements of the same samples. The main phosphate phases detected were NH4H2PO4, MgHPO4·3H2O, Mg3(PO4)2, Ca5(PO4)5Cl, CaHPO4·2H2O, Ca(H2-PO4)2·H2O, and AlPO4. Furthermore, K2SO4, NH4NO3, Fe2O3, and SiO2 were identified in the IR spectra. However, ammonium and sulfate compounds were only identified in the mid-IR region but were not detectable in the FIR region. KW - Sewage sludge ash KW - Fertilizer KW - P-fertilizer KW - Phosphorus compounds KW - Mid-infrared spectroscopy KW - Far-infrared spectroscopy PY - 2011 DO - https://doi.org/10.1366/10-06168 SN - 0003-7028 SN - 1943-3530 VL - 65 IS - 3 SP - 265 EP - 271 PB - Society for Applied Spectroscopy CY - Frederick, Md. AN - OPUS4-23270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Herzel, Hannes A1 - Dombinov, V. A1 - Vogel, Christian A1 - Willbold, S. A1 - Levandowski, G. V. A1 - Meiller, M. A1 - Müller, F. A1 - Zang, J. W. A1 - da Fonseca-Zang, W. A. A1 - Jablonowski, N. D. A1 - Schrey, S. D. A1 - Adam, Christian T1 - Soybean Fertilized by P-Phases from Bagasse-Based Materials: P-Extraction Procedures, Diffusive Gradients in Thin Films (DGT), and X-ray Diffraction Analysis (XRD) N2 - The Brazilian sugarcane industry produced around 173 million tons (Mt) of bagasse in 2018. Bagasse is a by-product of juice extraction for ethanol and sugar production and is combusted in order to generate power, producing up to 10 Mt of ash per year. This ash contains various concentrations of plant nutrients, which allow the ash to be used as a crop fertilizer. However, the concentration and extractability of phosphorus (P), an essential plant nutrient, are low in bagasse ash. To increase the P content, we co-gasified and co-combusted bagasse with P-rich chicken manure. The resulting ash was thermochemically post-treated with alkali additives (Na2SO4 and K2SO4) to increase the availability of P to plants. We aimed to: (i) investigate the effect of thermochemical post-treatment of co-gasification residue and co-combustion ash on P availability to soybeans, (ii) explore the potential of chemical extraction methods (citric acid, neutral ammonium citrate, formic acid, and Mehlich-I) and diffusive gradients in thin films (DGT) to predict the availability of P to soybeans, and (iii) identify the responsible P-phases using X-ray diffraction . We evaluated P availability to soybeans growing in Brazilian Oxisol soil in two independent greenhouse pot experiments. The positive effect of thermochemical treatment on P availability from gasification residue was confirmed through the observation of increased P uptake and biomass in soybean plants. These findings were confirmed by chemical extraction methods and DGT. The gasification residue contained whitlockite as its main P-bearing phase. Thermochemical post-treatment converted whitlockite into highly soluble CaNaPO4. In contrast, co-combustion ash already contained highly soluble Ca(Na,K)PO4 as its main P-bearing phase, making thermochemical post-treatment unnecessary for increasing P availability. In conclusion, increased extractability and availability of P for soybeans were closely connected to the formation of calcium alkali phosphate. Our findings indicate that this combined methodology allows for the prediction of P-fertilization effects of ash. KW - Sugar cane bagasse KW - Chicken manure ash KW - Thermochemical treatment KW - Nutrient KW - Plant availability PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509735 DO - https://doi.org/10.3390/agronomy10060895 VL - 10 SP - 895 EP - 6 PB - MDPI AN - OPUS4-50973 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ghiringhelli, Luca M. A1 - Baldauf, Carsten A1 - Bereau, Tristan A1 - Brockhauser, Sandor A1 - Carbogno, Christian A1 - Chamanara, Javad A1 - Cozzini, Stefano A1 - Curtarolo, Stefano A1 - Draxl, Claudia A1 - Dwaraknath, Shyam A1 - Fekete, Ádám A1 - Kermode, James A1 - Koch, Christoph T. A1 - Kühbach, Markus A1 - Ladines, Alvin Noe A1 - Lambrix, Patrick A1 - Himmer, Maja-Olivia A1 - Levchenko, Sergey V. A1 - Oliveira, Micael A1 - Michalchuk, Adam A1 - Miller, Ronald E. A1 - Onat, Berk A1 - Pavone, Pasquale A1 - Pizzi, Giovanni A1 - Regler, Benjamin A1 - Rignanese, Gian-Marco A1 - Schaarschmidt, Jörg A1 - Scheidgen, Markus A1 - Schneidewind, Astrid A1 - Sheveleva, Tatyana A1 - Su, Chuanxun A1 - Usvyat, Denis A1 - Valsson, Omar A1 - Wöll, Christof A1 - Scheffler, Matthias T1 - Shared metadata for data-centric materials science N2 - The expansive production of data in materials science, their widespread sharing and repurposing requires educated support and stewardship. In order to ensure that this need helps rather than hinders scientific work, the implementation of the FAIR-data principles (Findable, Accessible, Interoperable, and Reusable) must not be too narrow. Besides, the wider materials-science community ought to agree on the strategies to tackle the challenges that are specific to its data, both from computations and experiments. In this paper, we present the result of the discussions held at the workshop on “Shared Metadata and Data Formats for Big-Data Driven Materials Science”. We start from an operative definition of metadata, and the features that a FAIR-compliant metadata schema should have. We will mainly focus on computational materials-science data and propose a constructive approach for the FAIRification of the (meta)data related to ground-state and excited-states calculations, potential-energy sampling, and generalized workflows. Finally, challenges with the FAIRification of experimental (meta)data and materials-science ontologies are presented together with an outlook of how to meet them. KW - Library and Information Sciences KW - Statistics, Probability and Uncertainty KW - Computer Science Applications KW - Education KW - Information Systems KW - Statistics and Probability PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-584846 DO - https://doi.org/10.1038/s41597-023-02501-8 VL - 10 IS - 1 SP - 1 EP - 18 PB - Springer Science and Business Media LLC AN - OPUS4-58484 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Herzel, Hannes A1 - Krüger, Oliver A1 - Hermann, L. A1 - Adam, Christian T1 - Sewage sludge ash - A promising secondary phosphorus source for fertilizer production N2 - Sewage sludge incineration is extensively practiced in some European countries such as the Netherlands, Switzerland, Austria and Germany. A survey of German sewage sludge ash showed that the recovery potential is high, approx. 19,000 t of phosphorus per year. However, the survey also discovered that the bioavailability of phosphorus in the sewage sludge ash is poor and that more than half of the ashes cannot be used as fertilizers due to high heavy metal content. A new thermochemical process for sewage sludge ash treatment was developed that transforms the ash into marketable fertilizer products. Sewage sludge ash was thermochemically treated with sodium and potassium additives under reducing conditions, whereby the phosphate-bearing mineral phases were transformed into plant available phosphates. High P-bioavailability was achieved with a molar Na/P ratio > 1.75 in the starting materials. Sodium sulfate, carbonate and hydroxide performed comparably as additives for this calcination process. Potassium carbonate and -hydroxide have to be added in a molar K/P ratio > 2.5 to achieve comparable P-solubility. The findings of the laboratory scale investigations were confirmed by an industrial demonstration trial for an ash treatment with sodium sulfate. Simultaneously, the volatile transition metal arsenic (61% removal) as well as volatile heavy metals such as cadmium (80%), mercury (68%), lead (39%) and zinc (9%) were removed via the off-gas treatment system. The product of the demonstration trial is characterized by high bioavailability and a toxic trace element mass fraction below the limit values of the German fertilizer ordinance, thus fulfilling the quality parameters for a P-fertilizer. KW - Sewage sludge ash KW - Phosphorus recovery KW - Thermochemical treatment KW - Reducing conditions KW - Heavy metal evaporation KW - Bioavailability KW - Sodium sulfate PY - 2016 DO - https://doi.org/10.1016/j.scitotenv.2015.08.059 SN - 0048-9697 SN - 1879-1026 IS - 542 SP - 1136 EP - 1143 PB - Elsevier CY - Amsterdam AN - OPUS4-34165 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hamann, Christopher A1 - Piehl, Patrick A1 - Weingart, Eric A1 - Stolle, Dirk A1 - Al-Sabbagh, Dominik A1 - Ostermann, Markus A1 - Auer, Gerhard A1 - Adam, Christian T1 - Selective removal of zinc and lead from electric arc furnace dust by chlorination–evaporation reactions N2 - Re-melting of scrap in an electric arc furnace (EAF) results in the accumulation of filter dust from off-gas treatment that predominantly consists of iron and zinc oxides. Filter dust is classified as hazardous waste due to its high contents of potentially toxic or ecotoxic elements such as Pb, Cr, Cd, and As. A promising processing route for this waste is selective chlorination, in which the non-ferrous metal oxides are chlorinated and selectively evaporated in form of their respective chlorides from the remaining solids via the process gas flow. Here, we investigate stepwise thermochemical treatment of EAF dust with either waste iron(II) chloride solution or hydrochloric acid at 650, 800, and 1100 ◦C. The Zn and Pb contents of the thermochemically processed EAF dust could be lowered from 29.9% and 1.63% to 0.09% and 0.004%, respectively. Stepwise heating allowed high separation between zinc chloride at the 650 ◦C step and sodium-, potassium-, and lead-containing chlorides at higher temperatures. Furthermore, the lab-scale results were transferred to the use of an experimental rotary kiln highlighting the possibilities of upscaling the presented process. Selective chlorination of EAF dust with liquid chlorine donors is, therefore, suggested as a potential recycling method for Zn-enriched steelworks dusts. KW - Electric arc furnace dust KW - Zinc KW - Selective Chlorination KW - Hazardous waste KW - Resource Recovery PY - 2024 DO - https://doi.org/10.1016/j.jhazmat.2023.133421 SN - 0304-3894 VL - 465 SP - 1 EP - 13 PB - Elsevier AN - OPUS4-59345 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kratz, S. A1 - Beerbaum, B. A1 - Elsner, H. A1 - Reuvers, J. A1 - Dockhorn, T. A1 - Rechberger, H. A1 - Werner, W. A1 - Knudsen, L. A1 - Flachowsky, G. A1 - Rodehutscord, M. A1 - Adam, Christian A1 - Steingrobe, B. A1 - Schick, J. A1 - Albert, E. A1 - Leinweber, P. A1 - Ekardt, F. A1 - Embert, G. T1 - Ressourcen schonender Einsatz von Phosphor in der Landwirtschaft - Symposium des Institutes für Pflanzenbau und Bodenkunde des JKI in Braunschweig - eine Synopse KW - Klärschlamm KW - Phosphor KW - Ressource KW - Klärschlammasche KW - P-Düngemittel KW - Demonstrationsanlage PY - 2009 SN - 1867-0911 SN - 1867-0938 SN - 1865-4371 VL - 61 IS - 2 SP - 69 EP - 71 PB - Ulmer CY - Stuttgart AN - OPUS4-18928 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Simon, Franz-Georg A1 - Adam, Christian T1 - Ressourcen aus Abfall N2 - Die Beseitigung unbehandelter Abfälle auf Deponien gehört der Vergangenheit an, nicht nur weil Verordnungen diese Praxis verbieten, sondern auch, weil wegen steigender Preise für Rohstoffe und sinkender Gehalte in Erzen auch in Abfällen nach Alternativen gesucht wird. In den Aschen aus Hausmüllverbrennungsanlagen können mit einfachen Verfahren Metalle zurückgewonnen werden. Mit dem Phosphor aus Klärschlammaschen können Düngemittel hergestellt und so natürliche Ressourcen geschont werden. In beiden Fällen ist die Anreicherung der Wertstoffe durch den Verbrennungsprozess vorteilhaft, da die Effizienz von Recyclingprozessen stark von der Konzentration im Ausgangsgut abhängig ist.-------------------------------------------------------------------------------------------------------------------------------- Disposal of untreated waste has come to end due to new legislation in this field. Furthermore as a response to increasing prices for primary raw materials and decreasing ore concentrations products from waste treatment display a source for secondary raw materials. Elemental metals can be easily separated from municipal solid waste incineration bottom ash. Fertilizers can be produced using phosphate from sewage sludge ashes thus preserving natural resources. In both cases the enrichment taking place in the incineration process facilitates the resource recovery, because the efficiency of recycling processes is dependent on the concentration of the input material. KW - Klärschlammaschen KW - NE-Metalle KW - Phosphor KW - Rostaschen KW - Bottom ash KW - Nonferrous metals KW - Phosphorus KW - Sewage sludge ash PY - 2012 DO - https://doi.org/10.1002/cite.201100189 SN - 0009-286X SN - 1522-2640 VL - 84 IS - 7 SP - 999 EP - 1004 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-26209 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 - JOUR A1 - Krüger, Oliver A1 - Adam, Christian A1 - Hobohm, J. A1 - Basu, S. A1 - Kuchta, K. A1 - van Wasen, Sebastian T1 - Recycling oriented comparison of mercury distribution in new and spent fluorescent lamps and their potential risk N2 - This study compares the mercury distribution in the vapor phase, the phosphor powder and the glass matrix of new and spent fluorescent lamps. The spent fluorescent lamps were obtained at the collection yards of a public waste management company in Hamburg, Germany. An innovative systematic sampling method is utilized to collect six spent and eight corresponding new, off-the-shelf fluorescent lamp samples. The efficiency of several acid digestion methods for the determination of the elemental composition was studied and elemental mass fractions of K, Na, Y, Ca, Ba, Eu, Al, Pb, Mg, Hg, and P were measured. The study also finds aqua regia to be the best reagent for acid digestion. However, no significant difference in mercury distribution was found in the different phases of the new and spent fluorescent lamps. KW - Mercury KW - Rare earth elements KW - Hg distribution KW - Fluorescence lamps PY - 2017 DO - https://doi.org/10.1016/j.chemosphere.2016.11.104 SN - 0045-6535 SN - 1879-1298 VL - 169 SP - 618 EP - 626 PB - Elsevier AN - OPUS4-38481 LA - eng 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 - JOUR A1 - Krüger, Oliver A1 - Adam, Christian T1 - Recovery potential of German sewage sludge ash N2 - Incineration of sewage sludge is expected to increase in the future due to growing concerns about the direct use of sludge in agriculture. Sewage sludge is the pollutant sink of wastewater treatment and thus loaded with contaminants that might pose environmental hazards. Incineration degrades organic pollutants efficiently, but since the ash is currently mostly disposed of, all valuable component like phosphorus (P) and technologically relevant metals present in the sewage sludge ash (SSA) are removed from the economic cycle entirely. We conducted a complete survey of SSA from German mono-incineration facilities and determined the theoretical recovery potential of 57 elements. German SSA contains up to 19,000 t/a P which equals approximately 13% of phosphorus applied in the German agriculture in form of phosphate rock based mineral fertilizers. Thus, SSA is an important secondary resource of P. However, its P-solubility in ammonium citrate solution, an indicator for the bioavailability, is only about 26%. Treatment of SSA is recommended to enhance P bioavailability and remove heavy metals before it is applied as fertilizer. The recovery potential for technologically relevant metals is generally low, but some of these elements might be recovered efficiently in the course of P recovery exploiting synergies. KW - Sewage sludge ash KW - Recovery potential KW - Phosphorus KW - Critical raw materials KW - Bioavailability KW - Phosphorus recovery KW - Monitoring PY - 2015 DO - https://doi.org/10.1016/j.wasman.2015.01.025 SN - 0956-053X VL - 45 SP - 400 EP - 406 PB - Pergamon Press CY - New York, NY AN - OPUS4-34157 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Adam, Christian A1 - Kley, Gerd A1 - Simon, Franz-Georg A1 - Lehmann, Annekatrin T1 - Recovery of nutrients from sewage sludge - Results of the European research-project SUSAN N2 - Municipal sewage sludge is a carrier of nutrients – most important phosphorus (P) – but also contains organic pollutants and heavy metals. A two steps thermal treatment based on 1. mono-incineration of sewage sludge under destruction of organic pollutants and 2. thermochemical treatment of the resulting ashes to remove heavy metals and increase P-bioavailability is suggested by the authors. The process aims at P-fertilisers production from sewage sludge. Seven sewage sludge ashes of different origin and composition and one residue from gasification of sewage sludge were thermochemically treated. The raw ashes were mixed with a chlorine donor (e.g. MgCl2) and thermally treated in a gas tight lab-scale rotary furnace. The distributions of the heavy metals between solid and gas phase were determined. The heavy metals concentrations of the treated ashes matched the legislative limits in most cases. The products from thermochemical treatment are suited raw materials for P-fertiliser production. Relevant process parameters such as temperature, type and concentration of Cl-donor and retention time were optimised for the thermochemical treatment step. KW - Phosphorus recovery KW - Sewage sludge ash KW - Thermochemical treatment KW - Fetiliser PY - 2008 DO - https://doi.org/10.2166/wpt.2008.001 SN - 1751-231X VL - 3 IS - 1 SP - 1 EP - 8 PB - IWA Publishing AN - OPUS4-17700 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Adamczyk, Burkart A1 - Brenneis, Rudolf A1 - Adam, Christian A1 - Mudersbach, D. T1 - Recovery of chromium from AOD-converter slags N2 - Slags from the production of high-alloyed steel contain both chemically bound chromium (mainly as Cr2O3) in the mineral fraction and elemental chromium in the metallic remainders. Thermochemical post treatment of the slag in an electric arc furnace under reducing conditions enables the nearly complete recovery of the total amount of chromium in form of a metallic alloy. The best results were achieved by resistance melting (submerged electrodes) with addition of a reducing agent into the melt. The efficiencies of the reducing agents carbon, aluminium, silicon (as ferrosilicon) and silicon carbide were investigated and compared. As aluminium is the strongest reducing agent, it is less selective and reduces much more SiO2 than Cr2O3. While SiC shows only low reactivity because of its high thermal resistance, carbon and silicon had the highest reducing potentials: More than 97% of the chemically bound chromium can be recovered by application of these reducing agents. Due to the high temperature required for the reduction of the chromium compounds, the reduction of SiO2 as an undesired side reaction cannot be avoided. However, compared with mechanical procedures that are limited to the recovery of the metallic remainders, the total chromium recovery can be significantly increased by the described reductive melting procedure. KW - Arc furnace KW - By-product KW - Chromium recovery KW - High-alloyed steel KW - Reductive melting KW - Slag treatment KW - Slag KW - Thermochemical treatment PY - 2010 DO - https://doi.org/10.1002/srin.201000193 SN - 1611-3683 SN - 0177-4832 VL - 81 IS - 12 SP - 1078 EP - 1083 PB - Verl. Stahleisen CY - Düsseldorf AN - OPUS4-22898 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 - JOUR A1 - Peplinski, Burkhard A1 - Adam, Christian A1 - Michaelis, Matthias A1 - Kley, Gerd A1 - Emmerling, Franziska A1 - Simon, Franz-Georg T1 - Reaction sequences in the thermochemical treatment of sewage sludge ashes revealed by X-ray powder diffraction - A contribution to the European project SUSAN N2 - The sequence of reactions accompanying the thermochemical treatment of an iron- and aluminium-bearing sewage sludge ash was ascertained by investigating two systematic series of samples. The ash was thermochemically treated in a lab-scale rotary furnace after mixing it with a chlorine-donor, either CaCl2 or MgCl2. Within each of these two sample series only a single process parameter, the reaction temperature, was varied, namely between 350 and 1050°C. It was found, that among the numerous crystalline phases present in the raw ash only quartz and hematite continue to exist after thermochemical treatments carried out at 1050°C, whereas all other components undergo at least one decomposition-recrystallization cycle. Some of the components re-crystallize even several times. It was proved that the restructuring of the calcium- and phosphorus-bearing mineral phases proceeds via the formation of chlorspodioside, Ca2PO4Cl. The influence of the type of chlorine-donor on the final product was elucidated in detail and - to the best of our knowledge - for the first time crystalline AlPO4 was found in a sewage sludge ash and its decomposition was investigated, too. KW - XRD KW - Phosphorus recovery KW - Sewage sludge ash KW - Urban mining KW - Fertilizers PY - 2009 DO - https://doi.org/10.1524/zksu.2009.0068 SN - 0930-486X VL - 30 EPDIC 2008 SP - 459 EP - 464 PB - Oldenbourg CY - München AN - OPUS4-20562 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Raniro, H.R. A1 - Teles, A.P. A1 - Pavinato, P.S. A1 - Adam, Christian T1 - Phosphorus solubility and dynamics in a tropical soil under sources derived from wastewater and sewage sludge N2 - Conventional phosphate fertilizers are usually highly water-soluble and rapidly solubilize when moistened by the soil solution. However, if this solubilization is not in alignment with plants demand, P can react with the soil colloidal phase, becoming less available over time. This is more pronounced in acidic, oxidic tropical soils, with high P adsorption capacity, reducing the efficiency of P fertilization. Furthermore, these fertilizers are derived from phosphate rock, a non-renewable resource, generating an environmental impact. To assess these concerns, waste-recycled P sources (struvite, hazenite and AshDec®) were studied for their potential of reducing P Fixation by the soil and improving the agronomic efficiency of the P fertilization. In our work, we compared the solubilization dynamics of struvite, hazenite, AshDec® to triple superphosphate (TSP) in a sandy clay loam Ferralsol, as well as their effect on solution pH and on soil P pools (labile, moderately-labile and non-labile) via an incubation experiment. Leaching columns containing 50 g of soil with surface application of 100 mg per column (mg col􀀀 1) of P from each selected fertilizer and one control (nil-P) were evaluated for 60 days. Daily leachate samples from the column were analyzed for P content and pH. Soil was stratified in the end and submitted to P fractionation. All results were analyzed considering p < 0.05. Our findings showed that TSP and struvite promoted an acid P release reaction (reaching pHs of 4.3 and 5.5 respectively), while AshDec® and hazenite reaction was alkaline (reaching pHs of 8.4 and 8.5 respectively). Furthermore, TSP promoted the highest P release among all sources in 60 days (52.8 mg col􀀀 1) and showed rapid release dynamic in the beginning, while struvite and hazenite showed late release dynamics and lower total leached P (29.7 and 15.5 mg col􀀀 1 P respectively). In contrast, no P-release was detected in the leachate of the AshDec® over the whole trial period. Struvite promoted the highest soil labile P concentration (7938 mg kg􀀀 1), followed by hazenite (5877 mg kg􀀀 1) and AshDec® (4468 mg kg􀀀 1), all higher than TSP (3821 mg kg􀀀 1), while AshDec® showed high moderately-labile P (9214 mg kg􀀀 1), reaffirming its delayed release potential. KW - Phosphate dynamics KW - Struvite KW - Wastewater KW - Sewage sludge ash KW - CaNaPO4 KW - P speciation PY - 2022 DO - https://doi.org/10.1016/j.jenvman.2021.113984 VL - 302 IS - Part A SP - 113984 PB - Elsevier Ltd. AN - OPUS4-53600 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krüger, Oliver A1 - Fattah, K. P. A1 - Adam, Christian T1 - Phosphorus recovery from the wastewater stream - necessity and possibilities N2 - The annual demand of phosphorus (P) for fertilizer use is more than 550,000 t in Germany. Several of the input streams like mineral fertilizer produced from phosphate rock or sewage sludge are problematic due to contamination with heavy metals and organic pollutants and/or supply risks. Phosphorus recovery from the wastewater stream might help to diminish these problems. Several procedures have been developed to recover P from either sewage sludge ash (SSA) or wastewater via precipitation or crystallization as struvite. This study determined the elemental composition and trace metal mass fractions of 252 SSA samples and 17 struvite samples from wastewater treatment plants (WWTP) to see whether there are differences related to the source of the sludge (municipal/industrial) or the stage of the WWTP where the struvite is produced. Results indicated that there is no clear trend of the elemental mass fractions related to the source of the sludge. All struvite samples show very low heavy metal contents, even though the struvite precipitated from the sludge shows slightly elevated heavy metal mass fractions compared to struvite crystallized from sludge liquor. Struvite is a clean and plant available material for fertilizer production from wastewater streams and has some advantages for the wastewater treatment plant. However, since the P recovery rate of struvite processes is low (7–11%) compared to that from SSA processes (90%), recovery from SSA is necessary for a substantial P recovery from the wastewater stream. T2 - 3rd International Conference on Water, Energy and Environment (ICWEE) CY - Sharjah, United Arab Emirates DA - 24.03.2015 KW - Struvite KW - Phosphorus recovery KW - Wastewater KW - Sewage sludge ash PY - 2016 DO - https://doi.org/10.1080/19443994.2015.1103315 SN - 1944-3994 SN - 1944-3986 VL - 57 IS - 33 SP - 15619 EP - 15627 PB - Taylor & Francis CY - Philadelphia, USA AN - OPUS4-36260 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krüger, Oliver A1 - Adam, Christian T1 - Phosphorus in recycling fertilizers - analytical challenges N2 - The importance of secondary raw materials for phosphorus (P) fertilizer production is expected to increase in the future due to resource depletion, supply risks, and heavy metal contamination of fossil phosphate resources. Municipal wastewater is a promising source for P recovery. In Germany for instance, it contains almost 50% of the total amount of P that is currently applied as mineral fertilizer. Several procedures have been developed to recover and re-use P resulting in a growing number of recycling fertilizers that are currently not regulated in terms of fertilizer efficiency. We tested various materials and matrices for their total P content, solubility of P in neutral ammonium citrate (Pnac) and water, and performed robustness tests to check if existing analytical methods are suitable for those new materials. Digestion with inverse aqua regia was best suited to determine the total P content. Pnac sample preparation and analyses were feasible for all matrices. However, we found significant time and temperature dependencies, especially for materials containing organic matter. Furthermore, several materials didn’t reach equilibrium during the extractions. Thus, strict compliance of the test conditions is strongly recommended to achieve comparable results. KW - Recycling fertilizer PY - 2017 DO - https://doi.org/10.1016/j.envres.2017.02.034 SN - 0013-9351 SN - 1096-0953 VL - 155 SP - 353 EP - 358 PB - Elsevier CY - Rotterdam AN - OPUS4-39430 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sichler, Theresa Constanze A1 - Adam, Christian A1 - Becker, Roland A1 - Sauer, Andreas A1 - Ostermann, Markus A1 - Barjenbruch, M. T1 - Phosphorus determination in sewage sludge: comparison of different aqua regia digestion methods and ICP-OES, ICP-MS and photometric determination N2 - Phosphorus recycling from sewage sludge will be obligatory in Germany from 2029. Phosphorus content determination in sewage sludge is crucial to assess the prescribed recycling rates. Currently, German law regards sample preparation using aqua regia digestion in a microwave or under reflux conditions as well as instrumental phosphorus determination by ICP-OES, ICP-MS, or photometric determination with ammonium molybdate as equivalent. However, it is questionable whether these methods are indeed equivalent regarding phosphorus quantification in sludges near the limit of 20 g/kg for mandatory recycling. To answer this question, 15 sewage sludges of 11 different wastewater treatment plants were investigated with all permitted method (digestion and measurement) combinations. Moreover, one sewage sludge was also examined in an interlaboratory comparison (ILC) with 28 participants. This study shows that the above-mentioned methods differ in some cases significantly but across all method combinations and sludges, phosphorus recovery was between 80 and 121% after normalization to the grand mean (average of 15 sludges between 85 and 111%). The ILC and the examination of 15 sludges produced largely similar results. There is a tendency to higher phosphorus recovery after microwave digestion compared to reflux digestion and ICP-OES measurements determine higher phosphorus contents than ICP-MS and photometric phosphorus determination. As a result, the authors recommend ICP-OES determination of phosphorus in sewage sludge after microwave digestion. KW - Sewage sludge KW - ICP-OES KW - Phosphous recovery KW - ICP-MS KW - Photometric P determination KW - Interlaboratory comparison PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-558869 DO - https://doi.org/10.1186/s12302-022-00677-1 VL - 34 IS - 99 SP - 1 EP - 14 PB - Springer AN - OPUS4-55886 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Sekine, R. A1 - Steckenmesser, D. A1 - Lombi, E. A1 - Steffens, D. A1 - Adam, Christian T1 - Phosphorus availability of sewage sludge-based fertilizers determined by the diffusive gradients in thin films (DGT) technique N2 - The plant-availability of phosphorus (P) in fertilizers and soil can strongly influence the yield of agricultural crops. However, there are no methods to efficiently and satisfactorily analyze the plant-availability of P in sewage sludge-based P fertilizers except by undertaking time-consuming and complex pot or field experiments. We employed the diffusive gradients in thin films (DGT) technique to quantify the plant P availability of various types of P fertilizers with a novel focus on sewage sludge-based P fertilizers. Mixtures of fertilizer and soil were incubated for 3 weeks at 60% water holding capacity. DGT devices were deployed at the beginning of the incubation and again after 1, 2, and 3 weeks. Two weeks of incubation were sufficient for the formation of plant-available P in the fertilizer/soil mixtures. In a pot experiment, the DGT technique predicted maize (Zea mays L.) biomass yield and P uptake significantly more accurately than standard chemical extraction tests for P fertilizers (e.g., water, citric acid, and neutral ammonium citrate). Therefore, the DGT technique can be recommended as a reliable and robust method to screen the performance of different types of sewage sludge-based P fertilizers for maize cultivation minimizing the need for time-consuming and costly pot or field experiments. KW - Soil testing KW - Chemical extraction tests KW - Phosphate recovery KW - Plant growth experiments KW - Recycling PY - 2017 DO - https://doi.org/10.1002/jpln.201600531 VL - 180 IS - 5 SP - 594 EP - 601 PB - Wiley VCH Verlag AN - OPUS4-42413 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Adam, Christian A1 - Peplinski, Burkhard A1 - Kley, Gerd A1 - Kratz, S. A1 - Schick, J. A1 - Schnug, E. T1 - Phosphorrückgewinnung aus Klärschlammaschen - Ergebnisse aus dem EU-Projekt SUSAN N2 - Phosphor ist ein für alle Lebewesen essenzielles Element und kann in seinen Funktionen z. B. als Bestandteil der DNS und RNS sowie als Schlüsselelement beim Energiestoffwechsel (ADP/ATP) nicht ersetzt werden. Klärschlammaschen sind aufgrund ihrer hohen Gehalte an Phosphor (15–25 % P2O5) geeignete Sekundärrohstoffe für die Herstellung von P-Düngemitteln. Aufgrund der schlechten Pflanzenverfügbarkeit des Phosphors und der Gehalte an umweltrelevanten Schwermetallen sollten diese allerdings nicht direkt in der Landwirtschaft eingesetzt werden. Im Mittelpunkt des EU-Projekts SUSAN steht die Entwicklung und Optimierung einer thermochemischen Behandlung von Klärschlammaschen, mit der die Düngewirkung der Aschen auf das Niveau konventioneller Mineraldünger (Thomaskali und Superphosphat SSP) angehoben wird und die Schwermetallkonzentrationen unter die Grenzwerte nach Düngemittelverordnungen europäischer Länder abgesenkt werden. Die sehr positiven Ergebnisse, die bisher im SUSAN-Projekt erzielt wurden, und die darauf basierenden ökonomischen Betrachtungen legen eine großtechnische Umsetzung des Verfahrens nahe. KW - Klärschlamm KW - Phosphor KW - Ressource KW - Klärschlammasche KW - P-Düngemittel KW - Mineralische Phasen PY - 2008 DO - https://doi.org/10.1007/s00506-008-0152-3 SN - 0945-358X SN - 1613-7566 VL - 60 IS - 3-4 SP - 55 EP - 64 PB - Springer CY - Wien AN - OPUS4-17449 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Adam, Christian T1 - Phosphor: Von der Rückgewinnung zum Recycling N2 - Eine entscheidende Problematik nach Inkrafttreten der neuen Klärschlammverordnung ist, wie Phosphor nicht nur rückgewonnen, sondern in den Markt eingeschleust und letztlich auch in den Kreislauf zurückgeführt werden kann. Die Wege hierzu sind noch weitgehend ungeklärt. Die DWA-Arbeitsgruppe KEK- 1.1 hat aus diesem Grund einen Workshop durchgeführt, um rechtliche Anforderungen an Rezyklate, Aspekte der Rezyklatqualität und -beschaffenheit sowie den aktuellen Markt für Rezyklate zu diskutieren. Auf Basis dieses Workshops wurde ein Arbeitsbericht erstellt, der sich schwerpunktmäßig mit dem Einsatz von Rezyklaten zu Düngezwecken beschäftigt. Hierzu liegen bereits Erkenntnisse vor, und es sind bereits Praxisbeispiele in der Umsetzung. KW - Phosphor KW - Klärschlamm PY - 2018 DO - https://doi.org/10.3242/kae2018.08.005 SN - 1866-0029 VL - 65 IS - 8 SP - 710 EP - 717 PB - Gesellschaft zur Förderung der Abwassertechnik (GFA) CY - Hennef AN - OPUS4-45661 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Severin, M. A1 - Breuer, J. A1 - Rex, M. A1 - Stemann, Jan A1 - Adam, Christian A1 - Van den Weghe, H. A1 - Kücke, M. T1 - Phosphate fertilizer value of heat treated sewage sludge ash N2 - This study focuses on the question whether heat treated sewage sludge ashes are more favourable as fertilizers than untreated sewage sludge ashes (USSA) and whether their fertilization effects are comparable with commercial triple superphosphate (TSP). In a pot experiment, maize was fertilized either with one of three heat treated and Na-, Ca- and Si-compounds amended sewage sludge ashes (two glown phosphates, steel mill slag + sewage sludge ash) or USSA or TSP as control. Fertilization with USSA did not increase the biomass yield and the P uptake of maize in comparison to the P0 treatment (7.25 resp. 8.35 g dry matter/pot). Fertilization with heat treated sewage sludge ashes and TSP resulted in significantly higher yields and plant P uptakes which are on average eight times higher than treatment with USSA and P0 control. Biomass yields and P uptake of maize after fertilization with heat treated sewage sludge ashes are not significantly different from those after TSP fertilization. The main P compound in USSA is Ca3(PO4)2. By heat treatment and amendment with different sodium, calcium, sulphur and silicon containing additives or steel mill converter slag, Ca3(PO4)2 is converted to Ca- and Na-silico-phosphates, which have a higher water solubility than Ca3(PO4)2. This increased solubility is responsible for the high plant availability of this phosphates. KW - P recycling KW - Sustainability KW - P solubility PY - 2014 UR - http://www.agriculturejournals.cz/publicFiles/138177.pdf SN - 1214-1178 SN - 1805-9368 VL - 60 IS - 12 SP - 555 EP - 561 PB - Inst. CY - Prague AN - OPUS4-32147 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Adam, Christian T1 - Phosphatdüngemittel aus Klärschlammaschen N2 - Das Element Phosphor ist für alle Lebewesen essenziell und wird beispielsweise von Pflanzen in Form von Phosphaten aufgenommen. In der landwirtschaftlichen Produktion werden dem Boden die Phosphate durch Wachstum und Ernte der Pflanzen entzogen und müssen ihm in Form von Phosphatdüngemitteln wieder zugeführt werden, um die Nahrungsmittelproduktion zu sichern. Rohphosphat stellt die Grundlage unserer derzeitigen Phosphatdüngemittel dar, ist aber gleichzeitig ein endlicher Rohstoff. Des Weiteren sind insbesondere sedimentäre Rohphosphate oftmals mit erheblichen Konzentrationen toxischer Schadstoffe wie Cadmium, Uran und Thorium belastet. Eine Kreislaufführung des Phosphats sollte erfolgen, um natürliche Rohstoffvorkommen zu schonen und den Eintrag von Schadstoffen auf unsere Böden zu unterbinden. KW - Phosphat KW - Recyclingdüngemittel PY - 2020 SN - 1610-6563 IS - 3 SP - 14 EP - 15 PB - MuP Verlag GmbH CY - München AN - OPUS4-50792 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Rivard, C. A1 - Wilken, V. A1 - Muskolus, A. A1 - Adam, Christian T1 - Performance of secondary P-fertilizers in pot experiments analyzed by phosphorus X-ray absorption near-edge structure (XANES) spectroscopy N2 - A pot experiment was carried out with maize to determine the phosphorus (P) plant-availability of different secondary P-fertilizers derived from wastewater. We analyzed the respective soils by P K-edge X-ray absorption near-edge structure (XANES) spectroscopy to determine the P chemical forms that were present and determine the transformation processes. Macro- and micro-XANES spectroscopy were used to determine the chemical state of the overall soil P and identify P compounds in P-rich spots. Mainly organic P and/or P adsorbed on organic matter or other substrates were detected in unfertilized and fertilized soils. In addition, there were indications for the formation of ammonium phosphates in some fertilized soils. However, this effect was not seen in the maize yield of all P-fertilizers. The observed reactions between phosphate from secondary P-fertilizers and cofertilized nitrogen compounds should be further investigated. Formation of highly plant-available compounds such as ammonium phosphates could make secondary P-fertilizers more competitive to commercial phosphate rock-based fertilizers with positive effects on resources conservation. KW - Phosphorus KW - Pot experiments KW - Secondary P-fertilizer KW - Sewage sludge ash KW - Soil KW - X-ray absorption near-edge structure (XANES) spectroscopy PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-433782 DO - https://doi.org/10.1007/s13280-017-0973-z SN - 0044-7447 VL - 47 IS - 1 SP - 62 EP - 72 PB - Springer AN - OPUS4-43378 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hobohm, J. A1 - Kuchta, K. A1 - Krüger, Oliver A1 - van Wasen, Sebastian A1 - Adam, Christian T1 - Optimized elemental analysis of fluorescence lamp shredder waste N2 - Fluorescence lamps contain considerable amounts of rare earth elements (REE). Several recycling procedures for REE recovery from spent lamps have been established. However, despite their economic importance, the respective recycling is scarce so far, with an REE recovery rate of less than 1%. A reliable analysis of REE and other relevant metals like Yttrium is crucial for a thorough and complete recovery process. This applies both to the solid matter and aqueous phase, since most of the recycling processes include wet-chemical steps. We tested seven different reagent mixtures for microwave-assisted digestion of fluorescent lamp shredder, including hydrofluoric acid, perchloric acid, and hydrogen peroxide. We determined the concentrations of 25 of the most relevant rare earth and other trace elements (Al, P, Ti, V, Cr, Fe, Ni, Cu, Ga, Ge, As, Y, Ag, Cd, Sn, Sb, La, Ce, Eu, Gd, Tb, W, Au, Hg, and Pb) in the respective dilutions. Two independent digestions, one a mixture of perchlorid/nitric/hydrofluoric acid and the other aqua regia, showed the highest concentrations of 23 of these elements, excluding only Sn and Tb. The REE concentrations in the tested lamp shredder sample (stated in g/kg) were 10.2 (Y), 12.1 (La), 7.77 (Ce), 6.91 (Eu), 1.90 (Gd), and 4.11 (Tb). KW - Yttrium KW - Rare earth elements KW - Elemental analysis KW - Microwave-assisted digestion PY - 2016 DO - https://doi.org/10.1016/j.talanta.2015.09.068 SN - 0039-9140 VL - 147 SP - 615 EP - 620 PB - Elsevier CY - Amsterdam AN - OPUS4-34992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peplinski, Burkhard A1 - Adam, Christian A1 - Adamczyk, Burkart A1 - Müller, Ralf A1 - Michaelis, Matthias A1 - Krahl, T. A1 - Emmerling, Franziska T1 - Nanocrystalline and stacking-disordered beta-cristobalite AlPO4: the now deciphered main constituent of a municipal sewage sludge ash from a full-scale incineration facility N2 - For the first time evidence is provided that a nanocrystalline and stacking-disordered, chemically stabilized β-cristobalite form of AlPO4 occurs in a sewage sludge ash (SSA). This proof is based on a combined X-ray powder diffraction and X-ray fluorescence investigation of an SSA produced at a large-scale fluidized bed incineration facility serving a catching area with a population of 2 million. The structural and chemical characterization was carried out on 'as received' SSA samples as well as on solid residues remaining after leaching this SSA in sodium hydroxide solution. Thus, it was ascertained that the observed nanocrystalline and stacking-disordered cristobalite-like component belongs to the aluminum phosphate component of this SSA, rather than to its silicon dioxide component. In addition, a direct proof is presented that the chemically stabilized β-cristobalite form of AlPO4 does crystallize from X-ray amorphous precursors under conditions that mimic the huge heating rate and short retention time (just seconds at T ≈ 850°C), typical for fluidized bed incinerators. KW - Aluminum phosphate KW - Chemical stabilization of high-temperature forms KW - Cristobalite form KW - Stacking disorder KW - Incinerator ash KW - Sewage sludge ash PY - 2015 DO - https://doi.org/10.1017/S0885715614001213 SN - 0885-7156 VL - 30 IS - Supplement S 1 SP - S31 EP - S35 PB - JCPDS CY - Swarthmore, Pa. AN - OPUS4-33435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peplinski, Burkhard A1 - Adamczyk, Burkart A1 - Formanek, P. A1 - Meyer, Christian A1 - Krüger, O. A1 - Scharf, Holger A1 - Reinsch, Stefan A1 - Ostermann, Markus A1 - Nofz, Marianne A1 - Jäger, Christian A1 - Adam, Christian A1 - Emmerling, Franziska T1 - Nanocrystalline and stacking-disordered beta-cristobalite AlPO4 chemically stabilized at room temperature: synthesis, physical characterization, and X-ray powder diffraction data N2 - This paper reports the first successful synthesis and the structural characterization of nanocrystalline and stacking-disordered β-cristobalite AlPO4 that is chemically stabilized down to room temperature and free of crystalline impurity phases. Several batches of the title compound were synthesized and thoroughly characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy, selected area electron diffraction, energy dispersive X-ray spectroscopy mapping in SEM, solid-state 31P nuclear magnetic resonance (31P-NMR) spectroscopy including the TRAPDOR method, differential thermal analysis (DTA), gas-sorption methods, optical Emission spectroscopy, X-ray fluorescence spectroscopy, and ion chromatography. Parameters that are critical for the synthesis were identified and optimized. The synthesis procedure yields reproducible results and is well documented. A high-quality XRD pattern of the title compound is presented, which was collected with monochromatic copper radiation at room temperature in a wide 2θ range of 5°–100°. KW - Stabilization of high-temperature phase at RT KW - Nanochrystalline AlPO4 KW - Beta-christobalite structure type KW - High-cristobalite form KW - Aluminium phosphate PY - 2017 DO - https://doi.org/10.1017/S0885715617000537 SN - 1945-7413 SN - 0885-7156 VL - 32 IS - S1 SP - S193 EP - S200 PB - JCPDS-ICDD CY - Cambridge AN - OPUS4-42235 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Adam, Christian A1 - Brenneis, Rudolf A1 - Adamczyk, Burkart T1 - Möglichkeiten der thermochemischen Behandlung von Reststoffen KW - Thermochemische Stofftrennung KW - Wertstoffrückgewinnung PY - 2010 DO - https://doi.org/10.1002/cite.201050012 SN - 0009-286X SN - 1522-2640 VL - 82 IS - 9 SP - 1579 EP - 1580 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-22004 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krüger, Oliver A1 - Roskosch, A. A1 - Adam, Christian T1 - Monitoring von Klärschlammaschen N2 - Die Aschen aus der separaten Verbrennung von Klärschlamm in Deutschland besitzen ein großes Potential für die Phosphorrückgewinnung KW - Klärschlammasche KW - Monoverbrennung KW - Phosphor KW - Rückgewinnung KW - Kritische Rohstoffe KW - Seltene Erden PY - 2014 SN - 1868-9531 VL - 27 IS - 3 SP - 8 EP - 12 PB - Rhombos-Verl. CY - Berlin AN - OPUS4-31258 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Rivard, C. A1 - Tanabe, I. A1 - Adam, Christian T1 - Microspectroscopy – promising techniques to characterize phosphorus in soil N2 - Phosphorus (P) is an essential element for all forms of life and is applied as fertilizer in agriculture. The P availability for plants may be highly dependent on the chemical state of P in fertilizers and soils; however, the nature of this dependence remains obscure due to the limitations of generally applied wet chemical and instrumental analytical approaches. This paper focuses on recently developed infrared, Raman, ultraviolet and X-ray microspectroscopic techniques for the characterization of P in soil. Microspectroscopic techniques have the advantage that discrete P phases can be distinguished and characterized even if their mass fractions are very low. However, only small volumes of soil can be analyzed by microspectroscopic methods hence a combination of macro- and microspectroscopic techniques is a promising concept. KW - Infrared KW - Microspectroscopy KW - Phosphorus KW - Raman KW - Soil KW - Ultraviolet KW - X-ray absorption near-edge structure (XANES) PY - 2016 DO - https://doi.org/10.1080/00103624.2016.1228942 SN - 0010-3624 SN - 1532-2416 VL - 47 IS - 18 SP - 2088 EP - 2102 AN - OPUS4-38341 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Helfenstein, J. A1 - Massey, M. A1 - Sekine, R. A1 - Kretzschmar, R. A1 - Beiping, L. A1 - Peter, T. A1 - Chadwick, O. A1 - Tamburini, F. A1 - Rivard, C. A1 - Herzel, Hannes A1 - Adam, Christian A1 - Pradas del Real, A. A1 - Castillo-Michel, H. A1 - Zuin, L. A1 - Wang, D. A1 - Félix, R. A1 - Lassalle-Kaiser, B. A1 - Frossard, E. T1 - Microspectroscopy reveals dust-derived apatite grains in acidic, highly-weathered Hawaiian soils N2 - Dust deposition is an important source of phosphorus (P) to many ecosystems. However, there is little evidence of dust-derived P-containing minerals in soils. Here we studied P forms along a well-described climatic Gradient on Hawaii, which is also a dust deposition gradient. Soil mineralogy and soil P forms from six sites along the climatic gradient were analyzed with bulk (X-ray diffraction and P K-edge X-ray absorption near edge structure) and microscale (X-ray fluorescence, P K-edge X-ray absorption near edge structure, and Raman) analysis methods. In the wettest soils, apatite grains ranging from 5 to 30 μm in size were co-located at the micro-scale with quartz, a known continental dust indicator suggesting recent atmospheric deposition. In addition to co-location with quartz, further evidence of dust-derived P included backward trajectory modeling indicating that dust particles could be brought to Hawaii from the major global dust-loading areas in central Asia and northern Africa. Although it is not certain whether the individual observed apatite grains were derived from long-distance transport of dust, or from local dust sources such as volcanic ash or windblown fertilizer, these observations offer direct evidence that P-containing minerals have reached surface layers of highly-weathered grassland soils through atmospheric deposition. KW - Phosphorus KW - soil KW - microspectroscopy KW - Raman spectroscopy KW - XANES spectroscopy KW - x-ray diffraction PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-511522 DO - https://doi.org/10.1016/j.geoderma.2020.114681 SN - 0166-0918 SN - 1872-6259 VL - 381 SP - 114681-1 EP - 114681-11 PB - Elsevier CY - Amsterdam AN - OPUS4-51152 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roskosch, A. A1 - Adam, Christian A1 - Krüger, Oliver A1 - Wiechmann, B. T1 - Klärschlamm - Potenziale alternativer Verwertungswege N2 - In Deutschland werden gegenwärtig etwa 53 % der kommunalen Klärschlämme in Mono- und Müllverbrennungsanlagen sowie Kraft- und Zementwerken thermisch und 47 % stofflich, d.h. landwirtschaftlich (30 %) oder in landschaftsbaulichen Maßnahmen u.ä. verwertet (17 %). Bezogen auf die etwa 9,4 Mrd Kubikmeter Abwasser, die pro Jahr in Deutschland anfallen, kann von einem Potenzial von 75000 t Phosphor/a (davon ca. 67500 t P/a im Klärschlamm) ausgegangen werden. Bislang werden in der Literatur ca. 37 Verfahren zur abwasserseitigen Rückgewinnung von Phosphor beschrieben, die im Labor, im Technikumsmaßstab oder in Pilotanlagen erprobt worden sind. Weltweit wurden bisher ca. 12 davon großtechnisch umgesetzt. Etwa vier verschiedene Verfahrenstechniken lassen sich derzeit in Deutschland finden. Einige Verfahren arbeiten mit Ionenaustauschern, zum überwiegenden Teil handelt es sich jedoch um Fällungs- oder Kristallisationsverfahren, bei denen Magnesium-Ammonium-Phosphat (MAP, Struvit) entweder aus den Haupt- oder Nebenströmen einer Kläranlage oder aus dem Schlamm bzw. Schlammwasser gewonnen wird. Für den Nährstoff Phosphor konnte in den Klärschlammaschen ein Gehalt von durchschnittlich 7 % ermittelt werden. Daraus ergibt sich ein Potenzial von etwa 17500 t P/a (Tendenz steigend). Je nach Verfahren kann mit einem Rückgewinnungspotenzial von etwa 60 bis 90 % Phosphor aus der Asche (ca. 55 bis 80 % Pges bezogen auf den Kläranlagenzulauf) gerechnet werden KW - Klärschlamm KW - Phoshorrückgewinnung PY - 2012 SN - 1438-5716 SN - 0043-0986 IS - Sonderheft 2012 / Modernisierungsreport 2013 SP - 23 EP - 26 CY - Berlin AN - OPUS4-26970 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gentzmann, Marie A1 - Schraut, Katharina A1 - Vogel, Christian A1 - Gäbler, H.-E. A1 - Huthwelker, T. A1 - Adam, Christian T1 - Investigation of scandium in bauxite residues of different origin N2 - This paper focuses on the scandium speciation in bauxite residues of different origin. Insights into mineralchemical similarities and differences of these materials will be presented and links to their natural geological background discussed. The presented research should provide fundamental knowledge for the future development of efficient and viable technologies for Sc-recovery from bauxite residues derived from different bauxites and accumulating at different localities. In total, five bauxite residues were investigated which originated from Greece, Germany, Hungary and Russia (North Ural & North Timan) using a combination of different analytical tools. Those included: laser ablation inductively coupled plasma mass spectrometry, X-ray absorption near Edge structure (XANES) spectroscopy, μ-Raman spectroscopy as well as scanning electron microscopy and electron microprobe analyses. X-ray fluorescence and inductively coupled plasma mass spectrometry were used to determine the overall chemical composition. The investigated samples were found to exhibit a relatively homogenous distribution of Sc between the larger mineral particles and the fine-grained matrix except for Al-phases like diaspore, boehmite and gibbsite. These phases were found to be particularly low in Sc. The only sample where Sc mass fractions in Al-phases exceeded 50 mg/kg was the Russian sample from North Ural. Fe-phases such as goethite, hematite and chamosite (for Russian samples) were more enriched in Sc than the Al-phases. In fact, in Greek samples goethite showed a higher capacity to incorporate or adsorb Sc than hematite. Accessory minerals like zircon, rutile/anatase and ilmenite were found to incorporate higher mass fractions of Sc (>150 mg/kg), however, those minerals are only present in small amounts and do not represent major host phases for Sc. In Russian samples from North Ural an additional Ca–Mg rich phase was found to contain significant mass fractions of Sc (>500 mg/kg). μ-XANES spectroscopy was able to show that Sc in bauxite residue occurs adsorbed onto mineral surfaces as well as incorporated into the crystal lattice of certain Fe-phases. According to our observations the bauxite type, i.e. karstic or lateritic, the atmospheric conditions during bauxitization, i.e. oxidizing or reducing, and consequently the dominant Sc-bearing species in the primary Bauxite influence the occurrence of Sc in bauxite residues. In karstic bauxites, underlying carbonate rocks can work as a pH-barrier and stabilize Sc. This prevents the Sc from being mobilized and removed during bauxitization. Hence, karstic bauxites are more prone to show a Sc enrichment than lateritic bauxites. Reducing conditions during bauxitization support the incorporation of Sc into clay minerals such as chamosite, which can dissolve and reprecipitate during Bayer processing causing Sc to be redistributed and primarily adsorb onto mineral surfaces in the bauxite residue. Oxidizing conditions support the incorporation of Sc into the crystal lattice of Fe-oxides and hydroxides, which are not affected in the Bayer process. The genetic history of the bauxite is therefore the major influential factor for the Sc occurrence in bauxite residues. KW - Sc recovery KW - Scandium KW - Bauxite Residue KW - Red Mud KW - XANES PY - 2021 DO - https://doi.org/10.1016/j.apgeochem.2021.104898 SN - 0883-2927 VL - 126 SP - 104898 PB - Elsevier Ltd. AN - OPUS4-52123 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Smol, M. A1 - Adam, Christian A1 - Kugler, Stefan T1 - Inventory of Polish municipal sewage sludge ash (SSA) – Mass flows, chemical composition, and phosphorus recovery potential N2 - This paper presents an inventory of sewage sludge ashes (SSA) generated in the mono-incineration plants for municipal sewage sludge in Poland. This research focused on the detailed study of mass flows, chemical composition, and phosphorus recovery potential. There are currently 11 sludge mono-incineration plants operated with a total capacity of 160,300 Mg dry weight (d.w.) of sludge annually. Recently, a significant increase in the amount of SSA generated in these plants has been observed, reaching 26,756 Mg in 2018. Chemical composition of SSA showed significant amounts of the main nutrients: calcium (~14%), phosphorus (~13%), magnesium (~3%), and potassium (~1%). Additional main elements were iron (~14.5%), silicon (~13%), and aluminium (~6%). The main trace elements in the SSA were zinc (~3750 mg/kg) and copper (~899 mg/kg). Pollutants, according to fertilizer regulations of different countries, present in Polish SSA were chromium(~703 mg/kg), nickel (~260 mg/kg), lead (~94 mg/kg), and Cadmium (~9 mg/kg). The radionuclides, uranium, and thorium often present in higher amounts in commercial phosphate rock-based fertilizers, were only detected in SSA t low levels of 4–9 mg/kg and 2–3 mg/kg, respectively. Theoretical phosphorus recovery potential from the SSA (from plants in Cracow, Lodz, Gdansk, Gdynia, Szczecin, and Kielce) was estimated at 1613.8 Mg, of which 33.9% is bioavailable. Currently, in Poland, the recommended approach is the production of fertilizers as a result of the extraction of phosphorus from the SSA with its use in the production of secondary mineral fertilizers. Further research in this area is required considering Polish conditions and legislation. KW - Municipal sewage sludge KW - Sewage sludge ash (SSA) KW - Phosphorus KW - Recovery potential PY - 2020 DO - https://doi.org/10.1016/j.wasman.2020.07.042 VL - 116 SP - 31 EP - 39 PB - Elsevier Ltd AN - OPUS4-51093 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maresca, A. A1 - Krüger, O. A1 - Herzel, Hannes A1 - Adam, Christian A1 - Kalbe, Ute A1 - Astrup, T. F. T1 - Influence of wood ash pre-treatment on leaching behaviour, liming and fertilising potential N2 - In Denmark, increasing amounts of woody biomass are being used for the production of renewable energy, resulting in more wood ashes being generated. While these materials have been mainly landfilled, wood ashes may also be utilised for fertilizing and liming purposes on top of soils. Pre-treatments involving hardening or granulation may be carried out prior to soil application. In this study, two Danish wood ash samples were hardened and/or granulated. Lab-hardening induced rapid changes in the shape of the acid neutralisation capacity curve of the ashes. Up-flow column tests, assuming local equilibrium conditions, were employed to investigate the leaching from pre-treated ashes. Granules and loose ashes demonstrated similar leaching behaviours, indicating that similar geochemical processes were governing their leaching. In comparison with untreated fresh ashes, the hardened ashes demonstrated reduced leaching of Ca, Ba, Pb and Zn with concentration levels generally below or close to the analytical limits of quantification; to the contrary, the leaching of As, P, Sb, Si, V and Mg was enhanced in the hardened ashes. The release of alkalinity was reduced by hardening. In general, all granules were barely breakable by finger-pinching and they could withstand one month of continuous leaching, preserving their overall shape. The solubility of phosphorous in neutral ammonium citrate indicated that about 30–51% of the total P content in the ash samples was released, suggesting that the ashes could be potentially valuable as P-fertiliser if applied onto soil. KW - Wood ash KW - Phoshpor availability KW - Leaching KW - Forest soils PY - 2019 DO - https://doi.org/10.1016/j.wasman.2018.11.003 SN - 0956-053X VL - 83 SP - 113 EP - 122 PB - Elsevier AN - OPUS4-46583 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schraut, Katharina A1 - Kargl, F. A1 - Adam, Christian A1 - Ivashko, O. T1 - In situ synchrotron XRD measurements during solidification of a melt in the CaO–SiO2 system using an aerodynamic levitation system N2 - Phase formation and evolution was investigated in the CaO–SiO2 system in the range of 70–80 mol% CaO. The samples were container-less processed in an aerodynamic levitation system and crystallization was followed in situ by synchrotron x-ray diffraction at the beamline P21.1 at the German electron synchrotron (DESY). Modification changes of di- and tricalcium silicate were observed and occurred at lower temperatures than under equilibrium conditions. Despite deep sample undercooling, no metastable phase formation was observed within the measurement timescale of 1 s. For the given cooling rates ranging from 300 K s−1 to about 1 K s−1, no decomposition of tricalcium silicate was observed. No differences in phase evolution were observed between reducing and oxidizing conditions imposed by the levitation gas (Ar and Ar + O2). We demonstrate that this setup has great potential to follow crystallization in refractory oxide liquids in situ. For sub-second primary phase formation faster detection and for polymorph detection adjustments in resolution have to be implemented. KW - Aerodynamic levitation KW - Calcium silicate KW - Phase formation KW - Oxide melts KW - In situ synchrotron x-ray diffraction PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526952 DO - https://doi.org/10.1088/1361-648X/abf7e1 VL - 33 IS - 26 SP - 264003 (12pp) PB - IOP Publishing AN - OPUS4-52695 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Exner, Robert A1 - Adam, Christian T1 - Heavy metal removal from sewage sludge ash by thermochemical treatment with polyvinylchloride N2 - Sewage sludge ash (SSA) is a prospective phosphorus source for the future production of recycling P-fertilizers. Due to its high heavy metals contents and the relatively low P plant-availability, SSA must be treated before agricultural utilisation. In this paper SSA was thermochemically treated with PVC in a bench-scale rotary furnace in order to remove heavy metals via the chloride pathway. PVC has a high Cl-content of 52–53% and a high heating value that can be beneficially used for the thermochemical process. Large amounts of waste PVC are already recovered in recycling processes, but there are still some fractions that would be available for the proposed thermochemical process, for example, the low quality near-infrared(NIR)-fraction from waste separation facilities. Heavy metals were effectively removed at temperatures in the range of 800–950°C via the gas phase by utilisation of PVC as Cl-donor. The resulting P plant-availability was comparable to SSA thermochemically treated with MgCl2 as Cl-donor if MgO was used as an additive (Mg-donor). A further increase of the plant availability of phosphorus was achieved by acid post-treatment of the thermochemically treated SSA. KW - Phosphorus recovery KW - Sewage sludge ash KW - Heavy metal removal KW - Polyvinylchloride (PVC) PY - 2013 DO - https://doi.org/10.1021/es300610e SN - 0013-936X SN - 1520-5851 VL - 47 IS - 1 SP - 563 EP - 567 PB - ACS Publ. CY - Washington, DC AN - OPUS4-27556 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Adam, Christian T1 - Heavy metal removal from sewage sludge ash by thermochemical treatment with gaseous hydrochlorid acid N2 - Sewage sludge ash (SSA) is a suitable raw material for fertilizers due to its high phosphorus (P) content. However, heavy metals must be removed before agricultural application and P should be transferred into a bioavailable form. The utilization of gaseous hydrochloric acid for thermochemical heavy metal removal from SSA at approximately 1000 °C was investigated and compared to the utilization of alkaline earth metal chlorides. The heavy metal removal efficiency increased as expected with higher gas concentration, longer retention time and higher temperature. Equivalent heavy metal removal efficiency were achieved with these different Cl-donors under comparable conditions (150 g Cl/kg SSA, 1000 °C). In contrast, the bioavailability of the P-bearing compounds present in the SSA after thermal treatment with gaseous HCl was not as good as the bioavailability of the P-bearing compounds formed by the utilization of magnesium chloride. This disadvantage was overcome by mixing MgCO3 as an Mg-donor to the SSA before thermochemical treatment with the gaseous Cl-donor. A test series under systematic variation of the operational parameters showed that copper removal is more depending on the retention time than the removal of zinc. Zn-removal was declined by a decreasing ratio of the partial pressures of ZnCl2 and water. KW - Phosphorus recycling KW - Sewage sludge ash KW - Heavy metal elimination KW - Urban mining PY - 2011 DO - https://doi.org/10.1021/es2007319 SN - 0013-936X SN - 1520-5851 VL - 45 IS - 17 SP - 7445 EP - 7450 PB - ACS Publ. CY - Washington, DC AN - OPUS4-24170 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Adam, Christian A1 - Unger, M. T1 - Heavy metal removal from sewage sludge ash analyzed by thermogravimetry N2 - A high temperature (1000 °C) thermochemical process for heavy metal removal from sewage sludge ash via the chloride pathway was investigated by thermogravimetry/differential thermal analysis (TG/DTA). TG and DTA measurements gave information about secession and evaporation of water, HCl, and heavy metal chlorides at different temperatures. Additionally, gaseous water and hydrochloric acid which occurred in the process were detected by an FT-IR detector that was coupled to the TG/DTA-system. Heavy metal chlorides which were also formed in the process cannot be detected by this technique. For that reason the outlet gas of the TG/DTA-system was discharged into washing flasks filled with water for absorption. The washing flasks were replaced in temperature steps of 50 °C and the heavy metal concentrations of the solutions were determined by ICP-OES. The temperature-dependent formation/evaporation of different heavy metal chlorides was analyzed and compared for two different thermochemical processes using magnesium chloride hydrate or calcium chloride hydrate as Cl-donors. In both cases evaporation of Cd, Cu, Pb, and Zn was observed from 600 °C, whereas As, Cr, and Ni remained in the solid state. The results were discussed against the background of thermodynamic calculations. KW - Sewage sludge ash KW - Heavy metal chloride KW - Thermodynamic simulation KW - Thermogravimetry/FT-IR PY - 2011 DO - https://doi.org/10.1007/s10973-010-0966-7 SN - 1388-6150 SN - 1418-2874 SN - 0368-4466 SN - 1572-8943 VL - 103 SP - 243 EP - 248 PB - Kluwer Academic Publ. CY - Dordrecht AN - OPUS4-23157 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -