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 - 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 - GEN A1 - Hedrich, Martina A1 - Giese, Lutz A1 - Adam, Christian A1 - Haase, Oskar A1 - Segebade, Christian T1 - Recycling of Photovoltaic CdTe-Modules - Analytical Process Monitoring N2 - Along with the globally increasing energy demand the application of renewable energy sources is urgently required. According to national regulations and international treaties (e.g. Kyoto Protocol) these sources shall be sustainably available at reasonable financial effort and non-polluting during production, use and waste treatment. Using photovoltaic sources (PV), these requirements can clearly be met. All industry has to follow the best available technology and an integrative life cycle approach for their products and production. PV thin film technology strictly responds to this obligation. In order to save material resources and to minimise undesirable landfill recycling of spent PV modules is necessary. Recycling of multi-component materials containing mixed metals typically consists of three parts: liberation, separation, and recovery. In our study (RESOLVED – an EU Demonstration Project) the focus is on liberation and separation. The converting layer (CdTe) was liberated (removed) from the glass carrier by sandblasting and separated subsequently from the blast material (e.g. corundum) and other components using stepwise different separation techniques. Both the glass substrate and CdTe are subject to re-use. The overall feasibility of the recycling process is primarily governed by the efficiency of the procedure applied to the separation of CdTe from the rest (blasting material, glass residues, etc.). This was performed by water-based flotation. Several flotation procedures were studied regarding their separation yields. The distribution of CdTe in the phases involved (flotate, water, residue) was measured using energy dispersive X-ray fluorescence spectrometry (EDXRS) intended for future routine application and by instrumental large-volume photon activation analysis (IPAA) as a reference procedure. The results of both analytical methods were in satisfactory agreement. T2 - European Metallurgical Conference (EMC 2005) CY - Dresden, Germany DA - 2005-09-18 KW - Photovoltaic (PV) KW - Solar energy KW - CdTe-Modules KW - Recycling KW - Separation techniques KW - Monitoring PY - 2005 SN - 3-935797-22-2 VL - 4 SP - 1687 EP - 1696 PB - GDMB-Medienverl. CY - Clausthal-Zellerfeld AN - OPUS4-11004 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Adam, Christian A1 - Giese, Lutz A1 - Segebade, Christian A1 - Steglich, Hans-Eckhart A1 - Weimann, Karin T1 - Recycling von Photovoltaik-Dünnschichtmodulen T2 - 4. Kolloquium SORTIEREN - Innovationen und Anwendungen CY - Berlin, Deutschland DA - 2005-10-06 KW - Photovoltaik KW - Recycling KW - Dünnschichtmodul KW - Cadmiumtellurid KW - Nassmechanische Aufbereitung KW - Photonenaktivierungsanalyse PY - 2005 SP - 55 EP - 65 PB - TU Berlin CY - Berlin AN - OPUS4-11053 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steckenmesser, D. A1 - Vogel, Christian A1 - Adam, Christian A1 - Steffens, D. T1 - Effect of various types of thermochemical processing of sewage sludges on phosphorus speciation, solubility, and fertilization performance N2 - Sewage sludge has one of the highest phosphorus (P) recovery potentials of all waste materials. Therefore, P-recycling from sewage sludge could contribute to closing the P-cycle. Recently, various thermal processes for P-recovery have been developed, but there is still a demand for information on the effect of different process parameters (e.g. additives and temperature) on P-speciation and especially on the fertilization performance. In the present study, two common methods (low-temperature conversion at 400–500° C and thermochemical treatment at 950° C) were investigated and combined to produce highly bioavailable P-fertilizers from two different types of sewage sludge based on chemical phosphorus precipitation (Chem-P) and enhanced biological phosphorus removal (Bio-P). The results of P-fractionation, X-ray diffraction analysis, and pot experiments with maize showed that Bio-P sludges attain high P-plant-availability after treatment at low temperatures (400° C). In contrast, Chem-P sludges can adequately be treated at higher temperatures under reductive conditions with sodium additives to form highly bioavailable calcium-sodium-phosphate. Additionally, also highly heavy-metal contaminated sludges can be thermochemically treated at high temperatures to achieve the legal requirements for fertilizers. KW - P-recovery KW - Low-temperature-conversion KW - Thermochemical treatment KW - P-fractionation KW - P-plant-availability KW - Sewage sludge PY - 2017 DO - https://doi.org/10.1016/j.wasman.2017.02.019 SN - 0956-053X VL - 62 SP - 194 EP - 203 PB - Elsevier CY - Amsterdam AN - OPUS4-41646 LA - eng 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 - 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 - Vogel, Christian A1 - Hermann, P. A1 - Kästner, B. A1 - Adamczyk, Burkart A1 - Hoehl, A. A1 - Ulm, G. A1 - Adam, Christian T1 - Air and chlorine gas corrosion of different silicon carbides analyzed by nano-Fourier-transform infrared (nano-FTIR) spectroscopy N2 - The present study shows the potential of high-resolution imaging and nano-Fourier-transform infrared (nano-FTIR) spectroscopy for corrosion science. The protective oxidation layers of different chlorine-gas treated silicon carbides (SiCs) were characterized with these techniques. A nitrified SiC showed the highest resistant strength against chlorine corrosion at 1000 °C compared to the other SiCs. Nano-FTIR spectroscopy with a lateral resolution below 40 nm detected differences in the crystallinity of the bulk-SiC and in the transitional region to the protective layer. Furthermore, high-resolution imaging provides deep insight in the interfacial layer between bulk-SiC and the protective oxidation layer on sub-micrometer scale. KW - Nano-Fourier-transform infrared spectroscopy KW - Scattering-type scanning near-field optical microscopy (s-SNOM) KW - Synchrotron radiation KW - Corrosion KW - Silicon carbide KW - Chlorine PY - 2018 DO - https://doi.org/10.1016/j.corsci.2017.12.002 SN - 0010-938X VL - 131 SP - 324 EP - 329 PB - Elsevier AN - OPUS4-43648 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Ramsteiner, M. A1 - Sekine, R. A1 - Doolette, A. A1 - Adam, Christian T1 - Characterization of phosphorus compounds in soils by deep ultraviolet (DUV) Raman microspectroscopy N2 - Deep ultraviolet Raman microspectroscopy was successfully investigated as a new approach to analyze the chemical state of phosphorus compounds directly in soil. We demonstrate that ultraviolet excitation has the advantage to avoid the interference with the strong fluorescence, which occurs in the visible spectral range caused by organic matter in soils. Furthermore, the spatial resolution of <1 μm2 enables the detection of very small phosphorus particles. For some organic phosphorus compounds (β-glycerophosphate, aminomethylphosphonic acid), sample cooling to -100 °C is found to strongly reduce the rate of degradation induced by the illumination with the ultraviolet excitation light. However, phytic acid and adenosine monophosphate degraded even with cooling. Our results reveal the capability of deep ultraviolet Raman microspectroscopy as a high-resolution benchtop imaging technique for the analysis of local interactions between soil compounds with the potential to become an analytical key to improve the understanding of transformation mechanisms of phosphates as well as other mineral phases in soils. KW - Phosphorus speciation KW - Deep ultraviolet (DUV) Raman microspectroscopy KW - Soil PY - 2017 DO - https://doi.org/10.1002/jrs.5115 SN - 0377-0486 VL - 48 IS - 6 SP - 867 EP - 871 PB - Wiley AN - OPUS4-40508 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Adam, Christian A1 - McNaughton, D. T1 - Determination of phosphate phases in sewage sludge ash-based fertilizers by Raman microspectroscopy N2 - The chemical form of phosphate phases in sewage sludge ash (SSA)-based fertilizers was determined by Raman microspectroscopy. Raman mapping with a lateral resolution of 5 × 5 µm² easily detected different compounds present in the fertilizers with the help of recorded reference spectra of pure substances. Quartz and aluminosilicates showed Raman bands in the range of 450-520 cm-1. Phosphates with apatite structure and magnesium triphosphate were determined at around 960 and 980 cm-1, respectively. Furthermore, calcium/magnesium pyrophosphates were detected in some samples. KW - Fertilizer KW - Sewage sludge ash KW - Phosphate KW - Raman microspectroscopy PY - 2013 DO - https://doi.org/10.1366/12-06955 SN - 0003-7028 SN - 1943-3530 VL - 67 IS - 9 SP - 1101 EP - 1105 PB - Society for Applied Spectroscopy CY - Frederick, Md. AN - OPUS4-28999 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 A1 - Sekine, R. A1 - Schiller, T. A1 - Lipiec, E. A1 - McNaughton, D. T1 - Determination of phosphorus fertilizer soil reactions by Raman and synchrotron infrared microspectroscopy N2 - The reaction mechanisms of phosphate-bearing mineral phases from sewage sludge ash-based fertilizers in soil were determined by Raman and synchrotron infrared microspectroscopy. Different reaction mechanisms in wet soil were found for calcium and magnesium (pyro-) phosphates. Calcium orthophosphates were converted over time to hydroxyapatite. Conversely, different magnesium phosphates were transformed to trimagnesium phosphate. Since the magnesium phosphates are unable to form an apatite structure, the plant-available phosphorus remains in the soil, leading to better growth results observed in agricultural pot experiments. The pyrophosphates also reacted very differently. Calcium pyrophosphate is unreactive in soil. In contrast, magnesium pyrophosphate quickly formed plant-available dimagnesium phosphate. KW - Fertilizer KW - Phosphate-bearing mineral phases KW - Raman microspectroscopy KW - Sewage sludge ash KW - Soil KW - Synchrotron infrared microspectroscopy PY - 2013 DO - https://doi.org/10.1366/13-07056 SN - 0003-7028 SN - 1943-3530 VL - 67 IS - 10 SP - 1165 EP - 1170 PB - Society for Applied Spectroscopy CY - Frederick, Md. AN - OPUS4-29268 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Adam, Christian A1 - Kappen, P. A1 - Schiller, T. A1 - Lipiec, E. A1 - McNaughton, D. T1 - Chemical state of chromium in sewage sludge ash based phosphorus-fertilisers N2 - Sewage sludge ash (SSA) based P-fertilisers were produced by thermochemical treatment of SSA with Cl-donors at approximately 1000 °C. During this thermochemical process heavy metals are separated as heavy metal chlorides via the gas phase. Chromium cannot be separated under normal conditions. The risk of the development of toxic Cr(VI) during the thermochemical process was investigated. X-ray Absorption Spectroscopy measurements showed that SSA and thermochemically treated SSA with CaCl2, MgCl2 and NaCl contain Cr(III) compounds only. In contrast, treating SSA with elevated quantities of Na2CO3, to enhance the plant-availability of the phosphate phases of the fertiliser, developed approximately 10–15% Cr(VI). Furthermore, Raman microspectroscopy showed that using Mg-carbonate reduces the risk of a Cr(VI) development during thermochemical treatment. Additionally, leaching tests showed that only a Cr–water solubility >10% is an indicator for Cr(VI) in SSA based P-fertilisers. KW - Chromium KW - Fertiliser KW - Sewage sludge ash KW - Raman microspectroscopy KW - X-ray absorption spectroscopy PY - 2014 DO - https://doi.org/10.1016/j.chemosphere.2013.12.012 SN - 0045-6535 SN - 0366-7111 VL - 103 SP - 250 EP - 255 PB - Elsevier Science CY - Kidlington, Oxford AN - OPUS4-30062 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steckenmesser, D. A1 - Vogel, Christian A1 - Adam, Christian A1 - Steffens, D. T1 - Effect of various types of thermochemical processing of sewage sludges on phosphorus speciation, solubility, and fertilization performance N2 - Sewage sludge has one of the highest phosphorus (P) recovery potentials of all waste materials. Therefore, P-recycling from sewage sludge could contribute to closing the P-cycle. Recently, various thermal processes for P-recovery have been developed, but there is still a demand for information on the effect of different process parameters (e.g. additives and temperature) on P-speciation and especially on the fertilization performance. In the present study, two common methods (low-temperature conversion at 400–500 °C and thermochemical treatment at 950 °C) were investigated and combined to produce highly bioavailable P-fertilizers from two different types of sewage sludge based on chemical phosphorus precipitation (Chem-P) and enhanced biological phosphorus removal (Bio-P). The results of P-fractionation, X-ray diffraction analysis, and pot experiments with maize showed that Bio-P sludges attain high P-plant-availability after treatment at low temperatures (400 °C). In contrast, Chem-P sludges can adequately be treated at higher temperatures under reductive conditions with sodium additives to form highly bioavailable calcium-sodium-phosphate. Additionally, also highly heavy-metal contaminated sludges can be thermochemically treated at high temperatures to achieve the legal requirements for fertilizers. KW - P-recovery KW - Low-temperature-conversion KW - Thermochemical treatment KW - P-fractionation KW - P-plant-availability KW - Sewage sludge PY - 2017 DO - https://doi.org/10.1016/j.wasman.2017.02.019 SN - 0956-053X VL - 62 SP - 194 EP - 203 AN - OPUS4-39907 LA - eng 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 - Krüger, Oliver A1 - Fiedler, F. A1 - Adam, Christian A1 - Vogel, Christian A1 - Senz, R. T1 - Determination of chromium (VI) in primary and secondary fertilizer and their respective precursors N2 - Hexavalent chromium species (Cr(VI)) are often carcinogenic, of high acute toxicity, highly mobile, and thus pose a severe risk to health and environment. Fertilizers usually contain significant amounts of chromium. Therefore, a reliable analysis of chromium and the fraction of Cr(VI) are crucial for safe use of fertilizers. This problem is expected to increase in the future, since more and more recycled fertilizers emerge due to increasing fertilizer demand and respective supply risks. However, existing analytical methods have been developed for conventional fertilizers and have to be tested whether they are suitable for the new materials. Thus, we performed a wet-chemical extraction for Cr(VI) on several matrices as well as respective quality control experiments including spiking with Cr(III) and Cr(VI)compounds. We found the Cr(VI) amounts to be below 2 mg/kg except for a thermally post-treated sewage sludge ash (SSA) that showed 12.3 mg/kg. The presence of organic matter e.g. in sludge or precipitated struvite caused a reduction of spiked Cr(VI) and thus no satisfying recovery for Quality control. Cr(VI) reduction was also observed for SSA, presumably due to the presence of Fe(II) compounds. Even though the tested procedure can be hampered in some recycled fertilizer matrices, it might be adapted to be applicable also for these complex samples. KW - Chromium speciation KW - Recycling fertilizers KW - Matrix dependencies PY - 2017 DO - https://doi.org/10.1016/j.chemosphere.2017.05.011 SN - 0045-6535 VL - 182 SP - 48 EP - 53 PB - Elsevier CY - Amsterdam AN - OPUS4-40101 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Adam, Christian A1 - Vogel, Christian A1 - Rivard, C. A1 - Wilken, V. A1 - Muskolus, A. T1 - Unravelling plant-availability of recovered P-fertilizers by pot experiments and P X-ray absorption near edge structure (XANES) spectroscopy N2 - Pot experiments are often performed to analyze the plant-availability of phosphorus (P) in P-fertilizers. However, these experiments do not determine the P compounds present in the soil which are responsible for the yield increase. In order to better understand the results of pot experiments we analyzed the soils by P K-edge X-ray absorption near-edge structure (XANES) spectroscopy to determine the P species and unravel transformation processes. We carried out pot experiments with maize testing different waste water derived recycling P-fertilizers on an acidic and a neutral soil. Soils samples before sowing and after harvest were collected and prepared for analysis. A combination of macro- and µ-XANES spectroscopy was used to determine the chemical state of the overall soil P and to identify P compounds in P-rich spots localized by micro-X-ray fluorescence (µ-XRF). P K-edge macro-XANES spectroscopy detected organic P and/or P sorbed onto organic matter or other substrates in the unfertilized and fertilized soils. In addition, µ-XRF mapping in combination with P K-edge µ-XANES spectroscopy evidenced that some P phases present in recycling P-fertilizers (magnesium phosphate and calcium sodium phosphate) react with co-fertilized ammonium nitrate and form highly plant-available ammonium phosphates in the soil. In opposite, apatites were not affected by the presence of ammonium. Thus, for a boost of the plant-availability of P in recycling P-fertilizers these fertilizers should be directly co-fertilized with nitrogen (N) sources that contain a high amount of ammonium instead of nitrate. Possibly, a specific preparation of NP-fertilizers by granulation of recycling P-fertilizers with ammonium compounds and a nitrification inhibitor could enhance the plant-availability of the produced fertilizer whereby they become more competitive to commercially available NP-fertilizers based on phosphate rock. T2 - IPW8 - International Phosphorus Workshop CY - Rostock, Germany DA - 12.09.2016 KW - Phosphorus fertilizer KW - XANES spectroscopy PY - 2016 AN - OPUS4-37376 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Krüger, Oliver A1 - Herzel, Hannes A1 - Amidani, L. A1 - Adam, Christian T1 - Chemical state of mercury and selenium in sewage sludge ash based P-fertilizers N2 - Phosphorus-fertilizers from secondary resources such as sewage sludge ash (SSA) will become more important in the future as they could substitute conventional fertilizers based on the nonrenewable resource phosphate rock. Thermochemical approaches were developed which remove heavy metals from SSA prior to its fertilizer application on farmlands. We analyzed the chemical state of mercury and selenium in SSA before and after thermochemical treatment under different conditions for P-fertilizer production by X-ray absorption near edge structure (XANES) spectroscopy. In some incineration plants the mercury loaded carbon adsorber from off-gas cleaning was collected together with the SSA for waste disposal. SSAs from those plants contained mercury mainly bound to carbon/organic material. The other SSAs contained inorganic mercury compounds which are most probably stabilized in the SSA matrix and were thus not evaporated during incineration. During thermochemical treatment, carbon-bound mercury was removed quantitatively. In contrast, a certain immobile fraction of inorganic mercury compounds remained in thermochemically treated SSA, which were not clearly identified. HgSe might be one of the inorganic compounds, which is supported by results of Se K-edge XANES spectroscopy. Furthermore, the chemical state of selenium in the SSAs was very sensitive to the conditions of the thermochemical treatment. KW - X-ray absorption near edge structure (XANES) spectroscopy KW - Phosphorus recovery KW - Sewage sludge ash KW - Mercury KW - Selenium KW - Mercury selenide (HgSe) PY - 2016 UR - http://dx.doi.org/10.1016/j.jhazmat.2016.03.079 DO - https://doi.org/10.1016/j.jhazmat.2016.03.079 VL - 313 SP - 179 EP - 184 PB - Elsevier B.V. CY - Amsterdam, Netherlands AN - OPUS4-35718 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steckenmesser, D. A1 - Vogel, Christian A1 - Böhm, L. A1 - Heyde, B. A1 - Adam, Christian T1 - Fate of heavy metals and polycyclic aromatic hydrocarbons (PAH) in sewage sludge carbonisates and ashes – A risk assessment to a thermochemical phosphorus-recycling process N2 - In the near future, phosphorus (P) recycling will gain importance in terms of decreasing primary resources. Sewage sludge (SSL) is an adequate secondary P-resource for P-fertilizer production but it is also a sink for heavy metals and organic pollutants. The present study is an investigation on thermochemical P-recycling of SSL. Various temperatures and amendments were tested regarding their performance to remove heavy metals and polycyclic aromatic hydrocarbons (PAH) and simultaneous increase of the plant-availability of P. The investigations were carried out on two types of SSL originating from wastewater treatment plants with chemical P-precipitation and enhanced biological P-removal, respectively. The results show that thermochemical treatment with chlorine donors is suitable to remove the majority of heavy metals and that a combination of a gaseous chlorine donor (HCl) and sodium additives leads to both high heavy metal removal and high plant availability of P. Furthermore, plant experiments Show that almost all investigated thermochemical treatments can significantly reduce the bioavailability and plant uptake of heavy metals. Furthermore, PAHs are secondarily formed during low-temperature treatments (400–500 ° ), but can be significantly reduced by using sodium carbonate as an additive. KW - Fertilzer KW - Pollutant KW - Phosphorus PY - 2018 DO - https://doi.org/10.1016/j.wasman.2018.06.027 SN - 0956-053X VL - 78 SP - 576 EP - 587 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-45341 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Adam, Christian A1 - Vogel, Christian A1 - Wellendorf, Stephan A1 - Schick, J. A1 - Kratz, S. A1 - Schnug, E. ED - Ashley, K. ED - Mavinic, D. ED - Koch, F. T1 - Phosphorus recovery by thermochemical treatment of sewage sludge ash - Results of the European FP6-project SUSAN T2 - International conference on nutrient recovery from wastewater streams CY - Vancouver, BC, Canada DA - 2009-05-10 PY - 2009 SN - 9781843392323 SP - 417 EP - 430 PB - IWA Publishing CY - London, UK AN - OPUS4-19485 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -