TY - JOUR A1 - Simon, Franz-Georg A1 - Scholz, Philipp T1 - Sequential Extraction of Incineration Bottom Ash: Conclusions Regarding Ecotoxicity N2 - The classification of incineration bottom ash (IBA) as hazardous or non-hazardous according to ecotoxic hazard property HP14 is still under debate. In this context, only the compounds of Zn and Cu with the hazard statement code H410 are of relevance. With an approach based on the grouping of substances, it was shown that such substances are either readily water-soluble or slightly and sparingly soluble. The concentrations of readily soluble Cu and Zn compounds in IBA are far below the cut-off value of 0.1%. Slightly and sparingly soluble Zn and Cu compounds could be quantified in the first fraction of a four-step sequential extraction procedure. With the results from the complete sequence, the dimensionless synthesis toxicity index (STI) was calculated and was in the range of 494 to 1218 for the four investigated IBA samples. It was concluded that IBA can usually be classified as non-hazardous. KW - Incineration bottom ash KW - Hazard properties KW - Ecotoxicity PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-605262 DO - https://doi.org/10.3390/app14135541 SN - 2076-3417 VL - 14 IS - 13 SP - 1 EP - 12 PB - MDPI CY - Basel AN - OPUS4-60526 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schoknecht, Ute A1 - Mathies, H. T1 - The Impact of Weather Conditions on Biocides in Paints N2 - Weather conditions affect biocides on exposed outer surfaces on constructions. Contact with water causes hydrolysis and leaching of substances. Ultraviolet radiation may induce photolysis. As a result, a mixture of biocidal active substances and transformation products can be emitted into the environment. In a semi-field study, leaching of the biocidal active substances terbutryn, diuron, octylisothiazolinone, carbendazim, and selected transformation products was observed for two paints containing either a white or a red pigment. Painted test panels were exposed to natural weathering for about 1.5 years. Runoff samples were analyzed during the course of the experiment. At the end of the study, residues of biocidal active substances and transformation products were determined in sections of the test panels. Emissions of substances were mainly observed during the first few months of the experiments. Increased emissions of transformation products were observed during periods of increased global radiation and subsequent periods with relatively high amounts of driving rain. Different patterns of transformation products were observed, especially for terbutryn, both for paints containing different pigments and in experiments that were started in different periods of the year, as well as during different periods of the experiments. KW - Substance release KW - Construction products KW - Biocides KW - Transformation KW - Weathering KW - Driving rain KW - Global radiation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560651 DO - https://doi.org/10.3390/ma15207368 VL - 15 IS - 20 SP - 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-56065 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vo, P. H.N. A1 - Vogel, Christian A1 - Nguyen, H. T.M. A1 - Hamilton, B. R. A1 - Thai, P. K. A1 - Roesch, Philipp A1 - Simon, Franz-Georg A1 - Mueller, J. F. T1 - µ-X-ray fluorescence (XRF) and fluorine K-edge µ-X-ray absorption near-edge structure (XANES) spectroscopy for detection of PFAS distribution in the impacted concrete N2 - An improved understanding of the distribution of per- and polyfluoroalkyl substances (PFAS) in PFAS-impacted concrete is important for risk management and decontamination of PFAS. This study incorporates µ-X-ray fluorescence (µ-XRF) and fluorine K-edge µ-X-ray absorption near-edge structure (µ-XANES) spectroscopy to gain non-destructive insights into PFAS distribution in the impacted concrete. The μ-XRF and μ-XANES spectroscopy provided additional details on the detection of PFAS, which were not detected by the desorption electrospray ionization (DESI) imaging method conducted previously. The shorter chain PFAS were found on the top part of the concrete core (0.5 cm), and longer chain PFAS were mostly at the bottom part of the concrete core (5 cm). The inorganic fluorine fraction was also detected, and it likely hampered the detection of organic fluorine such as PFAS in the concrete. Thus, this non-destructive technique is an complementary approach to detect PFAS in contaminated concrete. KW - Beton KW - Per- and Polyfluoroalkyl substances (PFAS) KW - XANES spectroscopy PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-616711 DO - https://doi.org/10.1016/j.hazl.2024.100134 SN - 2666-9110 VL - 5 SP - 1 EP - 5 PB - Elsevier B.V. AN - OPUS4-61671 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zweigle, J. A1 - Schmidt, A. A1 - Bugsel, B. A1 - Vogel, Christian A1 - Simon, Fabian A1 - Zwiener, C. T1 - Perfluoroalkyl acid precursor or weakly fluorinated organic compound? A proof of concept for oxidative fractionation of PFAS and organofluorines N2 - Organofluorine mass balance approaches are increasingly applied to investigate the occurrence of per- and polyfluoroalkyl substances (PFAS) and other organofluorines in environmental samples more comprehensively. Usually, complex samples prevent the identification and quantification of every fluorine-containing molecule. Consequently, large unidentified fractions between fluorine sum parameters such as extractable organic fluorine (EOF) and the sum of quantified analytes are frequently reported. We propose using oxidative conversion to separate (unidentified) weakly fluorinated compounds (e.g., pesticides, pharmaceuticals) from PFAA-precursors (perfluoroalkyl chain lengths ≥ C6). We show with three organofluorine model substances (flufenamic acid, diflufenican, pantoprazole) that CF3-groups or aromatic fluorine can be quantitatively converted to inorganic fluoride and trifluoroacetic acid (TFA) by applying PhotoTOP oxidation (UV/TiO2). The principle of fluorine separation in mixtures is demonstrated by the oxidation of the three weakly fluorinated compounds together with the PFAA-precursor 6:2/6:2 fluorotelomer mercaptoalkyl phosphate diester (FTMAP). After oxidation, the products F− and TFA were separated from PFCAs ( C4) by SPE, and the fractions were analyzed individually. Closed mass balances both with and without the addition of organic matrix were achieved. Eventually, the fluorine balance was verified by total fluorine measurements with combustion ion chromatography (CIC). The proposed methods should be considered a proof of concept to potentially explain unidentified fractions of the EOF, especially if compounds with low fluorine content such as pesticides, pharmaceuticals, and their transformation products contribute largely to the EOF. Future studies are needed to show the applicability to the complexity of environmental samples. Graphical Abstract KW - Combustion Ion Chromatography KW - Per- and Polyfluoroalkyl substances (PFAS) PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613429 DO - https://doi.org/10.1007/s00216-024-05590-5 SP - 1 EP - 10 PB - Springer Science and Business Media LLC AN - OPUS4-61342 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maulas, Kryzzyl M. A1 - Paredes, Charla S. A1 - Tabelin, Carlito Baltazar A1 - Jose, Mark Anthony A1 - Opiso, Einstine M. A1 - Arima, Takahiko A1 - Park, Ilhwan A1 - Mufalo, Walubita A1 - Ito, Mayumi A1 - Igarashi, Toshifumi A1 - Phengsaart, Theerayut A1 - Villas, Edrhea A1 - Dagondon, Sheila L. A1 - Metillo, Ephrime B. A1 - Uy, Mylene M. A1 - Manua, Al James A. A1 - Villacorte-Tabelin, Mylah T1 - Isolation and Characterization of Indigenous Ureolytic Bacteria from Mindanao, Philippines: Prospects for Microbially Induced Carbonate Precipitation (MICP) N2 - Microbially induced carbonate precipitation (MICP), a widespread phenomenon in nature, is gaining attention as a low-carbon alternative to ordinary Portland cement (OPC) in geotechnical engineering and the construction industry for sustainable development. In the Philippines, however, very few works have been conducted to isolate and identify indigenous, urease-producing (ureolytic) bacteria suitable for MICP. In this study, we isolated seven, ureolytic and potentially useful bacteria for MICP from marine sediments in Iligan City. DNA barcoding using 16s rDNA identified six of them as Pseudomonas stutzeri, Pseudomonas pseudoalcaligenes, Bacillus paralicheniformis, Bacillus altitudinis, Bacillus aryabhattai, and Stutzerimonas stutzeri but the seventh was not identified since it was a bacterial consortium. Bio-cementation assay experiments showed negligible precipitation in the control (without bacteria) at pH 7, 8, and 9. However, precipitates were formed in all seven bacterial isolates, especially between pH 7 and 8 (0.7–4 g). Among the six identified bacterial species, more extensive precipitation (2.3–4 g) and higher final pH were observed in S. stutzeri, and B. aryabhattai, which indicate better urease production and decomposition, higher CO2 generation, and more favorable CaCO3 formation. Characterization of the precipitates by scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDS) and attenuated total reflectance Fourier transform spectroscopy (ATR-FTIR) confirmed the formation of three carbonate minerals: calcite, aragonite, and vaterite. Based on these results, all six identified indigenous, ureolytic bacterial species from Iligan City are suitable for MICP provided that the pH is controlled between 7 and 8. To the best of our knowledge, this is the first report of the urease-producing ability and potential for MICP of P. stutzeri, P. pseudoalcaligenes, S. stutzeri, and B. aryabhattai. KW - Calcium carbonate KW - Microbially induced carbonate precipitation (MICP) KW - Ureolytic bacteria PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600888 DO - https://doi.org/10.3390/min14040339 VL - 14 IS - 4 SP - 1 EP - 15 PB - MDPI AN - OPUS4-60088 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Capitain, C. A1 - Schüßler, M. A1 - Bugsel, B. A1 - Zweigle, J. A1 - Vogel, Christian A1 - Leube, Peter A1 - Zwiener, C. T1 - Implementation of matrix-matched semiquantification of PFAS in AFFF-contaminated soil N2 - This study presents a novel semiquantification approach for nontarget screening (NTS), combining matrix-matched calibration and ionization class-specific average calibration curves (ACCs) to address the lack of analytical reference standards for most per- and polyfluoroalkyl substances (PFAS). Ionization class-specific ACCs for carboxylic and sulfonic acids, sulfonamides, and cationic PFAS result in high accuracy, with median absolute accuracy quotients below 2.27×. The approach was applied to soil impacted by aqueous film-forming foam (AFFF) contamination. A total of 96 tentatively identified PFAS were semiquantified in addition to 28 quantified compounds based on available standards. Semiquantified concentrations exceeded those of target analytes, demonstrating the critical role of this method in capturing broader PFAS contamination. In this case, validation against extractable organofluorine (EOF) showed a 102% closed mass balance. The innovative approach not only enables comprehensive PFAS contamination assessment in complex matrices but also expands the scope of the NTS for environmental monitoring, remediation, and risk assessment of AFFF-contaminated sites. KW - Per- and polyfluoroalkyl substances (PFAS) KW - Contaminated soil KW - Non-targeted analysis KW - Combustion ion chromatography PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-629445 DO - https://doi.org/10.1021/acs.est.4c14255 SN - 1520-5851 VL - 59 IS - 14 SP - 7338 EP - 7347 PB - American Chemical Society (ACS) CY - Columbus, Ohio AN - OPUS4-62944 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Simon, Franz-Georg A1 - Vogel, Christian A1 - Kalbe, Ute T1 - Antimony and vanadium in incineration bottom ash – leaching behavior and conclusions for treatment processes N2 - Due to its large mineral fraction, incineration bottom ash (IBA) from municipal solid waste incineration is an interesting raw material that can be used for road construction or to produce secondary building materials. However, leaching chloride, sulfate, and potentially harmful heavy metals may cause problems in using IBA in civil engineering. Investigating leaching behavior is crucial for the assessment of the environmental compatibility of IBA applications. Various test procedures are available for that purpose. In the present study, a long-term leaching test of a wet-mechanically treated IBA was performed in a lysimeter for almost six years. While concentrations of chloride, sulfate and the majority of the heavy metals started to decrease rapidly with progressive liquid-to-solid ratio (L/S), antimony (Sb) and vanadium (V) behaved differently. At the beginning of the lysimeter test, the Sb and V concentrations were low, but after approximately one year of operation at an L/S ratio of around 0.8 L/kg, a steady increase was observed. It was shown that this increase is the result of low Ca concentrations due to the formation of CaCO3. With the data, the solubility products from Ca-antimonate and Ca-vanadate were calculated. The unusual leaching behavior of Sb and V should be kept in mind when considering field scenarios and evaluating the impact on the environment. KW - Bottom ash KW - Lysimeter KW - Leaching of waste materials KW - Secondary building materials PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-534317 DO - https://doi.org/10.31025/2611-4135/2021.15115 SN - 2611-4135 VL - 16 SP - 75 EP - 81 PB - CISA CY - Padua AN - OPUS4-53431 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Simon, Franz-Georg A1 - Kalbe, Ute T1 - Measurement of the Environmental Impact of Materials N2 - This Special Issue, ‘Measurement of the Environmental Impact of Materials’, is focused on the impact that materials have on the environmental compartments of soil, water and air. Leaching and emission processes, including underlying mechanisms, are a recurring topic in most published articles in the present Special Issue. Contributions have come from three continents and numerous countries (USA, Germany, France, Latvia, Poland, Russia, Japan, Korea and Thailand) indicating the global dimension of the subject. KW - Leaching KW - Recycling KW - Nano-materials PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545099 DO - https://doi.org/10.3390/ma15062208 SN - 1996-1944 VL - 15 IS - 6 SP - 1 EP - 3 PB - MDPI CY - Basel AN - OPUS4-54509 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heisterkamp, I. A1 - Gartiser, S. A1 - Schoknecht, Ute A1 - Happel, O. A1 - Kalbe, Ute A1 - Kretzschmar, M. A1 - Ilvonen, O. T1 - Investigating the ecotoxicity of construction product eluates as multicomponent mixtures N2 - The release of hazardous compounds from construction products can harm human health and the environment. To improve the sustainability of construction materials, the leaching of substances from construction products and their potential environmental impact should be assessed. Twenty-seven construction products from different product groups were examined with a combination of standardized leaching tests (dynamic surface leaching test and percolation test) and biotests (algae, daphnia, fish egg, luminescent bacteria, umu and Ames fluctuation tests). To identify the released substances, extensive qualitative and quantitative chemical analyses were performed, including gas chromatographic and liquid chromatographic screening techniques. Results: Many of the tested eluates caused signifcant ecotoxic efects. Particularly high ecotoxicities were observed for grouts (lowest ineffective dilution (LID) up to 16384) and cork granules (LID up to 24578). The results of ecotoxicity tests allow the prioritization of the eluates that should be subjected to detailed chemical analyses. Organic screening by different methods and ranking the identifed substances based on recorded hazard classification is a suitable approach to identify the relevant toxic substances. Conclusions: Determining the ecotoxicity of eluates from construction products records the summary effect of all leachable substances. This instrument is especially useful for construction products of complex and largely unknown composition. The ecotoxicological and the chemical–analytical approach complement each other in an ideal way to characterize the potential hazard of eluates from construction products and to identify the environmentally hazardous components in these eluates. Our results confirm that the proposed harmonized methods for testing eluate toxicity are an adequate and applicable procedure to move toward a more sustainable way of building and to reduce toxic effects of construction products in their use phase in the environment. KW - Construction products KW - Building materials KW - Ecotoxicity KW - Biotests KW - Leaching KW - Eluates KW - Chemical analysis KW - Analytical screening techniques KW - Mixture toxicity PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568864 DO - https://doi.org/10.1186/s12302-023-00711-w VL - 35 IS - 1 SP - 1 EP - 20 PB - Springer AN - OPUS4-56886 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roesch, Philipp A1 - Vogel, Christian A1 - Wittwer, Philipp A1 - Huthwelker, T. A1 - Borca, C. A1 - Sommerfeld, Thomas A1 - Kluge, Stephanie A1 - Piechotta, Christian A1 - Kalbe, Ute A1 - Simon, Franz-Georg T1 - Taking a Look at the Surface: µ-XRF Mapping and Fluorine K-edge µ-XANES Spectroscopy of Organofluorinated Compounds in Environmental Samples and Consumer Products N2 - For the first time, µ-X-ray fluorescence (µ-XRF) mapping combined with fluorine K-edge µ-X-ray absorption near-edge structure (µ-XANES) spectroscopy was applied to depict per- and polyfluoroalkyl substances (PFAS) contamination and inorganic fluoride in samples concentrations down to 100 µg/kg fluoride. To demonstrate the matrix tolerance of the method, several PFAS contaminated soil and sludge samples as well as selected consumer product samples (textiles, food contact paper and permanent baking sheet) were investigated. µ-XRF mapping allows for a unique element-specific visualisation at the sample surface and enables localisation of fluorine containing compounds to a depth of 1 µm. Manually selected fluorine rich spots were subsequently analysed via fluorine K-edge µ-XANES spectroscopy. To support spectral interpretation with respect to inorganic and organic chemical distribution and compound class determination, linear combination (LC) fitting was applied to all recorded µ-XANES spectra. Complementarily, solvent extracts of all samples were target-analysed via LC-MS/MS spectrometry. The detected PFAS sum values range from 20 to 1136 µg/kg dry weight (dw). All environmentally exposed samples revealed higher concentration of PFAS with a chain length >C8 (e.g. 580 µg/kg dw PFOS for Soil1), whereas the consumer product samples showed a more uniform distribution with regard to chain lengths from C4 to C8. Independent from quantified PFAS amounts via target analysis, µ-XRF mapping combined with µ-XANES spectroscopy was successfully applied to detect both point-specific concentration maxima and evenly distributed surface coatings of fluorinated organic contaminants in the corresponding samples. KW - PFAS KW - XRF KW - LC-MS/MS KW - XANES KW - Fluoride KW - Soil PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576109 DO - https://doi.org/10.1039/D3EM00107E SN - 2050-7887 SP - 1 EP - 12 PB - Royal Society of Chemistry AN - OPUS4-57610 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Simon, Franz-Georg A1 - Kalbe, Ute T1 - Case Study on Secondary Building Materials for a Greener Economy N2 - Half of global material consumption involves mineral material. The circularity is still low so that the enhanced use of secondary building material is required to close loops. Three different secondary building materials are discussed based on exemplary research results: construction and demolition waste (C&D waste), soil-like material, and incineration bottom ash (IBA). Focus was placed on the environmental compatibility of the materials examined mainly by standardized leaching tests. C&D waste was investigated after a wet treatment using a jigging machine, and soil-like material and IBA were characterized with respect to their material composition. Their environmental compatibilities in particular were studied using standard leaching tests (batch tests and column tests). It was concluded that soil-like material can mostly be utilized even when the precautionary limit values set are exceeded by a factor of less than two. For C&D waste, the fine fraction below 2 mm and the content of brick material is problematic. IBA fulfills quality level “HMVA-2” following German regulations. Improved levels of utilization might be achievable with better treatment technologies. KW - Incineration bottom ash KW - Soil-like material KW - Leaching KW - Circular economy PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576343 DO - https://doi.org/10.3390/app13106010 SN - 2076-3417 VL - 13 IS - 10 SP - 1 EP - 13 PB - MDPI CY - Basel AN - OPUS4-57634 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Roesch, Philipp A1 - Wittwer, Philipp A1 - Sommerfeld, Thomas A1 - Riedel, Maren A1 - Leube, Peter A1 - Kalbe, Ute A1 - Schoknecht, Ute A1 - Simon, Franz-Georg T1 - Per- and Polyfluoroalkyl Substances (PFAS) in Ski Waxes and Snow from Cross-Country Skiing in Germany - Comparative study of Sum Parameter and Target Analysis N2 - Per- and polyfluoroalkyl substances (PFAS) are often environmentally exposed via discharge through human consumer products, such as ski waxes. In our study we analyzed various ski waxes from the 1980s and 2020s, to determine both the sum parameter values total fluorine (TF), extractable organically bound fluorine (EOF), hydrolysable organically bound fluorine (HOF) as well as targeted PFAS analysis. This showed that modern high-performance waxes contain up to 6 % TF, but also PFAS-free labelled ski waxes contain traces of PFAS with EOF/HOF values in the low mg kg-1 range. With the ban of all fluorine-based waxes with the start of the 2023/2024 winter season this will probably change soon. Moreover, we applied our analysis methods to snow samples from a frequently used cross country ski trail (Kammloipe) in the Ore Mountain region in Germany, assessing the potential PFAS entry/discharge through ski waxes. Melted snow samples from different spots were analyzed by the adsorbable organically bound fluorine (AOF) sum parameter and PFAS target analysis and confirmed the abrasion of the ski waxes into the snow. Moreover, on a PFAS hotspot also soil samples were analyzed, which indicate that PFAS from the ski waxes adsorb after snow melting into the soil. KW - Combustion Ion Chromatography KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Consumer Products PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612760 DO - https://doi.org/10.1016/j.hazadv.2024.100484 VL - 16 SP - 1 EP - 5 PB - Elsevier B.V. AN - OPUS4-61276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schoknecht, Ute A1 - Kalbe, Ute A1 - Heisterkamp, I. A1 - Kretzschmar, M. A1 - Gartiser, S. A1 - Happel, O. A1 - Ilvonen, O. T1 - Release of substances from joint grouts based on various binder types and their ecotoxic effects N2 - Background: The leaching of substances and the ecotoxic effects of eluates were studied for joint grouts that are based on various types of binders. Eight products, two of them containing either epoxy resin, polybutadiene or polyurethane binders, or modifed cement, were investigated using harmonized leaching tests for construction products in combination with ecotoxicity tests on algae, daphnia, luminescent bacteria, fish eggs and mutagenicity in accordance with CEN/TR 17105. In addition to basic parameters, such as pH, TOC, and inorganic components, organic substances in the eluates were analysed by gas and liquid chromatography in combination with mass spectrometry. Quantitative analyses in combination with ecotoxicity data on selected substances were used to deduce which substances cause the observed ecotoxic effects. Results: Different patterns of ecotoxic effects were observed in joint grouts with different binder types. The most ecotoxic effects were observed in epoxy resin-based products, followed by polybutadiene-based products. Fewer ecotoxic effects were observed in polyurethane-based products and modifed cements. Some of these showed no ecotoxicity. Some of the substances in the eluates were identified and related to ecotoxic effects. 4-Tert-butylphenol and amines probably contributed to the ecotoxic effects of at least one of the epoxy resin-based renders, whereas cobalt is assumed to contribute to the toxic effect on algae of one of the polybutadiene-based products. However, only some of the leached substances could be identifed, and only some of the ecotoxic effects can be explained by the available information on the composition of eluates and known ecotoxic profiles of the identified substances. Conclusions: Ecotoxicity tests on eluates from leaching tests indicate whether environmentally hazardous substances can be leached from construction products. Combined ecotoxicity tests and chemical analysis of eluates from EU-wide harmonized leaching tests for construction products can provide information on substances that cause these effects. This supports the identifcation and development of environmentally friendly construction products. This study confirmed that ecotoxicity tests in accordance with CEN/TR 17105 are a tool well-suited to support the implementation of the European Commission’s zero pollution vision for 2050 and to reduce pollution to levels no longer considered harmful to health and natural ecosystems. KW - Joint grouts KW - Leaching KW - Ecotoxixity PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-562392 DO - https://doi.org/10.1186/s12302-022-00686-0 SN - 2190-4707 VL - 34 IS - 1 SP - 1 EP - 16 PB - Springer Nature CY - Berlin AN - OPUS4-56239 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roesch, Philipp A1 - Schinnen, Andrea A1 - Riedel, Maren A1 - Sommerfeld, Thomas A1 - Sawal, G. A1 - Bandow, N. A1 - Vogel, Christian A1 - Kalbe, Ute A1 - Simon, Franz-Georg T1 - Investigation of pH-dependent extraction methods for PFAS in (fluoropolymer-based) consumer products: A comparative study between targeted and sum parameter analysis N2 - Here, we report a comparative study of different sum parameter analysis methods for the extraction of per- and polyfluoroalkyl substances (PFAS) from manufactured consumer products, which can be measured by combustion ion chromatography (CIC). Therefore, a hydrolysis-based extraction method was further developed, which accounts for the addition of hydrolyzable covalently bound polyfluoroalkylated side-chain polymers (SFPs) to the extractable organic fluorine portion of the mass balance proposed as "hydrolyzable organically bound fluorine" (HOF). To test this hypothesis, the method was applied to 39 different consumer products containing fluoropolymers or monomeric PFAS taken from four different categories: outdoor textiles, paper packaging, carpeting, and permanent baking sheets. We also evaluated the method's efficiency by extracting four synthesized fluorotelomer polyacrylate reference compounds. The total fluorine (TF) and extractable organically bound fluorine (EOF) values were measured through CIC using established protocols. The TF values ranged from sub-ppb to %-levels, depending on the compound class. All samples showed results for hydrolyzed organofluorine (HOF) between 0.03 and 76.3 μg/g, while most EOF values were lower (150 mg kg−1, because of different diffusion properties for various PFAS, but also kinetic exchange limitations. KW - Combustion ion chromatography KW - Per- and polyfluoroalkyl substances (PFAS) KW - Sewage sludge KW - Fertilizer PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-583429 DO - https://doi.org/10.1039/d3va00178d SN - 2754-7000 VL - 2 IS - 10 SP - 1436 EP - 1445 PB - Royal Society of Chemistry (RSC) CY - London AN - OPUS4-58342 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kalbe, Ute A1 - Simon, Franz-Georg T1 - Potential use of incineration bottom ash in construction – Evaluation of the environmental impact N2 - Knowledge of the long-term leaching behavior of potentially harmful substances is crucial for the assessment of the environmental compatibility of reusing municipal solid-waste incineration bottom ash (MSWI BA) in construction, i.e., as a road base layer. BA fractions obtained from wet-processing aiming at the improvement of environmental quality were used to investigate the mobility of relevant substances. Eluates from laboratory-scaled leaching procedures (column percolation and lysimeters) were analyzed to learn about the long-term release of substances. Unsaturated conditions and artificial rainwater (AR) were used in the lysimeter tests to simulate field conditions. In addition, batch test eluates were generated at usual liquid-to-solid ratios (L/S) for compliance testing purposes. A variety of cations and anions was measured in the eluates. The wet treatment reduces the leaching of chloride and particularly sulfate by more than 60%. The release of typical contaminants for the treated MSWI BA such as the heavy metals Cu and Cr was well below 1% in the conducted leaching tests. An increase in the Sb concentration observed in the lysimeter experiments starting at L/S 0.75 L/kg and in the column experiment at L/S 4 L/kg is assumed to be related to decreasing concentrations of Ca and thus to the dissolution of sparingly soluble calcium antimonate. The same leaching mechanism applies with V, but the concentration levels observed are less critical regarding relevant limit values. However, on the long term the behavior of Sb could be problematic for the application of MSWI BA in construction. KW - MSWI bottom ash KW - Leaching KW - Batch tests KW - Lysimeter KW - Antimony PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508421 DO - https://doi.org/10.1007/s12649-020-01086-2 SN - 1877-2641 VL - 11 IS - 12 SP - 7055 EP - 7065 PB - Springer AN - OPUS4-50842 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heisterkamp, I. A1 - Ratte, M. A1 - Schoknecht, Ute A1 - Gartiser, S. A1 - Kalbe, Ute A1 - Ilvonen, O. T1 - Ecotoxicological evaluation of construction products: inter-laboratory test with DSLT and percolation test eluates in an aquatic biotest battery N2 - Background A European inter-laboratory test with 29 participating laboratories investigated whether a battery of four ecotoxicological tests is suitable for assessing the environmental compatibility of construction products. For this purpose, a construction product was investigated with the dynamic surface leaching test (DIN CEN/TS 16637-2) and the percolation test (DIN CEN/TS 16637-3). The eluates were produced centrally by one laboratory and were tested by the participants using the following biotests: algae test (ISO 8692), acute daphnia test (ISO 6341), luminescent bacteria test (DIN EN ISO 11348), and fish egg test (DIN EN ISO 15088). As toxicity measures, EC50 and LID values were calculated. Results Toxic effects of the eluates were detected by all four biotests. The bacteria test was by far the most sensitive, followed by the algae test and the daphnia test; the fish egg test was the least sensitive for eluates of both leaching tests. The toxicity level of the eluates was very high in the bacteria, daphnia, and algae test, with lowest ineffective dilution values of LID = 70 to LID = 13,000 and corresponding EC50 values around or even below 1 volume percent. The reproducibility (approximated by interlaboratory variability) of the biotests was good (< 53%) to very good (< 20%), regardless of the toxicity level of the eluates. The reproducibility of the algae test was up to 80%, and thus still acceptable. Conclusion It can be confirmed that the combination of leaching and ecotoxicity tests is suitable to characterize with sufficient reproducibility the environmental impact posed by the release of hazardous substances from construction products. KW - Inter-laboratory test KW - Construction products KW - Leaching tests KW - Ecotoxicity tests KW - Grouts PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529198 DO - https://doi.org/10.1186/s12302-021-00514-x VL - 33 IS - 1 SP - Article number: 75 PB - Springer AN - OPUS4-52919 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wittwer, Philipp A1 - Roesch, Philipp A1 - Vogel, Christian A1 - Simon, Fabian A1 - Gehrenkemper, Lennart A1 - Feldmann, Ines A1 - Simon, Franz-Georg T1 - Less Is More: Influence of Cross-Linking Agent Concentration on PFOS Adsorption in Chitosan N2 - As a result of the continuous use of persistent per- and polyfluoroalkyl substances (PFAS), e.g., in aviation firefighting foams, contamination with PFAS has been found in soil, groundwater, and surface water around thousands of industrial and military installations. Due to their harmful (environmental) potential, further dispersion in the environment needs to be stopped, which can be achieved by appropriate absorption materials. In this work, the influence of the cross-linking agent epichlorohydrin (ECH) concentration on the perfluorooctanesulfonic acid (PFOS) adsorption capacity of chitosan gel was investigated. It was found that higher ECH concentration during the cross-linking step decreases the PFOS adsorption capacity of the cross-linked chitosan gel from 0% to 4% ECH solution by about 15%. Using a concentration of 1%, ECH resulted still in an acid-stable material, and a maximum PFOS loading capacity of 4.04 mmol/g was obtained, one of the highest described in the literature. Furthermore, we used a rapid small-scale column test to compare the PFOS adsorption capacity of chitosan and activated carbon, each in both milled and unmilled form. Unmilled chitosan showed the highest PFOS adsorption capacity considering adsorption material dry masses (>0.9 and <0.4 mmol/g for both types of chitosan and activated carbon, respectively). Milled activated carbon proved to be the better adsorption material, considering the fixed volume of the adsorber (>99.9% PFOS adsorbed). Overall, the cross-linking agent concentration in chitosan is a crucial factor influencing its PFOS absorption potential. Our results feature cross-linked chitosan as an effective economic and ecologic alternative for PFOS adsorption in aqueous solutions. KW - Combustion Ion Chromatography KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Remediation PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618406 DO - https://doi.org/10.3390/app142311145 VL - 14 IS - 23 SP - 1 EP - 13 PB - MDPI AN - OPUS4-61840 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Urban, Klaus A1 - Ackerhans, C. A1 - Gorbushina, Anna T1 - Analysis of Carbon and Nitrogen from Atmospheric Sources by Bulk Deposition Sampling at various locations in Germany N2 - Atmospheric deposition of particulate matter is an important indicator of air pollution and a significant factor in material surface fouling. The elemental composition of this nutrient-containing dust depends largely on the exposure region and time as well as on climate. Therefore, in this paper we report an analysis of atmospheric pollutions with a self-made low-cost bulk deposition sampler directed at sampling deposition via air transport and rainfall. We used the device in diverse environments - thus comparing an urban region, an area surrounded by forest and an area mainly dominated by agriculture. The total organic carbon (TOC) and total nitrogen (TN) amounts were selected as indicator parameters and analyzed in a biweekly rhythm for three and a half and two years, respectively. The TOC value responded to particulate matter in the urban area, especially significant were the influences of the New Year's firework in urban and pollen in the rural forest area. In contrast, the TN value was more under the influence of the nitrogen emissions in the agriculture-dominated area. However, the TN value did not correlate with the NOx values in the urban area because the atmospheric nitrogen emissions in the city might originate from various emission sources. Summarizing, the TOC and TN values of the self-made low-cost bulk deposition sampler were in good agreement with environmental events of their immediate surrounding. Moreover, the selected containers and sampling procedures are universally applicable to monitor and analyze organic as well as inorganic parameters (e.g. metal ions) of atmospheric deposition. KW - Passive sampling KW - Biomonitoring KW - Air Analysis PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-609373 DO - https://doi.org/10.1016/j.envadv.2024.100583 SN - 2666-7657 VL - 17 SP - 1 EP - 9 PB - Elsevier Ltd. AN - OPUS4-60937 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duarte-Ruiz, D. A1 - Saßnick, H.-D. A1 - Ferreira De Araujo, F. A1 - Gentzmann, Marie A1 - Huthwelker, T. A1 - Cocchi, C T1 - X-ray absorption spectroscopy of scandium oxide polymorphs N2 - Scandium oxide (Sc2O3) is a rare-earth oxide with significant potential in key technological areas, but due to its limited supply a deep understanding of its characteristics in different crystalline phases is still missing. Here, we present a combined experimental and ab initio X-ray absorption spectroscopy investigation of Sc2O3 focusing on excitations from the O K-edge and the Sc L2,3-edge. While measurements are performed on a cubic sample, the most stable phase under ambient conditions, six different polymorphs are computed, including two high-pressure phases with a trigonal and monoclinic lattice in addition to the cubic phase, as well as three computationally predicted structures. Our analysis of the structural and electronic properties reveals significant similarities between the cubic polymorph and the high-pressure trigonal phase, while the monoclinic crystal exhibits distinct features. The spectra simulated for these similar phases from the solution of the Bethe–Salpeter equation show very good agreement with measurements. Additional comparison with results computed in the independent-particle approximation highlights the dominant role of electron–hole correlations in shaping the absorption features, particularly at the O K-edge, where a common pattern with the features of other sesquioxides is identified. Our findings offer new insight into the spectral fingerprints of Sc2O3 polymorphs, aiding in situ characterization and informing sustainable materials management. KW - Scandium PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-650806 DO - https://doi.org/10.1039/d5ra06446e VL - 15 IS - 56 SP - 47814 EP - 47825 AN - OPUS4-65080 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 - Walsh, Michael A1 - Schenk, Gerhard A1 - Robinson, Nicole A1 - John, Samuel A1 - Dayananda, Buddhi A1 - Krishnan, Vithya A1 - Adam, Christian A1 - Hermann, Ludwig A1 - Schmidt, Susanne T1 - The Circular Phosphorus Economy: Agronomic Performance of Recycled Fertilizers and Target Crops N2 - ABSTRACTBackgroundThe circular phosphorus (P) economy addresses economic and environmental penalties inherent to the current linear P economy. Phosphorus sources recovered from waste steams (recyclates) offer an alternative to conventional fertilizers.AimThis research aimed to assess the agronomic performance of P recyclates derived from wastewater (hazenite, struvite), treated sewage sludge ash (SSA) and compost (FOGO food organics/garden organics) with crops previously characterized for P use efficiency (PUE).MethodsPhosphorus was supplied as granules and benchmarked against conventional fertilizers or mineral solution. Grown in controlled conditions, crops received recyclates individually or as amalgamates, with or without additional water‐soluble P. We quantified P uptake, yield and phytate content, and calculated agronomic performance indicators.ResultsResults revealed that (1) crop genotypes with purportedly lower or higher PUE showed similar performance when grown with limiting P supply and/or less soluble P recyclates, (2) crop performance improved when less soluble P recyclates were combined with water‐soluble P, (3) crops produced similar yield and biomass when supplied with an organo‐mineral formulation, hazenite, or conventional fertilizer, (4) grain accumulated higher levels of the antinutrient phytate with excess soluble P.ConclusionWe conclude that suitably formulated P recyclates can supplement or replace conventional fertilizers, and that fertilizer design should consider the solubility of recyclates and a crop's ability to access less soluble P. This adds to the growing body of evidence that well‐formulated next‐generation fertilizers can efficiently nourish crops. Integrating insights from controlled experiments and field trials is a cost‐effective strategy to actualize the circular P economy. KW - Recycling fertilizer KW - Phosphate recovery KW - Sewage sludge ash KW - Struvite KW - Hazenite PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-627116 DO - https://doi.org/10.1002/jpln.202400299 SP - 1 EP - 14 PB - Wiley AN - OPUS4-62711 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Leers, K. A1 - Arnold, U. A1 - Herzel, Hannes A1 - Adam, Christian A1 - Burkhardt, J. T1 - Thermochemically Treated Sewage Sludge Ash From Pilot-Scale Production as P-Fertilizer for Spring Wheat and Maize in Different Soil Conditions N2 - Background P-fertilizers made from sewage sludge ash (SSA) may be suitable substitutes for rock phosphate (RP)-based fertilizers and contribute to sustainable use of waste. In this context, the thermochemical AshDec treatment of SSA (TC-SSA) has been continuously improved and has emerged as a possible method to produce plant-available and low-pollutant P-fertilizers. Aim Evaluation of the P-fertilizer efficacy of TC-SSA produced in pilot trials in vegetation experiments with different plants, soils, and fertilizer doses. Methods TC-SSA was tested in pot experiments for spring wheat and maize on different soils and at two doses (0.2 and 0.4 g fertilizer P pot−1) and is compared to untreated SSA (USSA), RP, Struvite, triple superphosphate (TSP), and a control without P-fertilization (Zero P). Pot experiments are complemented by an analysis of fertilizer P-solubility. Results P-solubility of SSA with different extraction methods increased due to the thermochemical treatment, whereas the water-insoluble property remained. In contrast to RP or USSA, TC-SSA enriched calcium–acetate–lactate extractable soil P to the same extent as TSP. Plant biomass and P-uptake increased with TC-SSA compared to Zero P, RP, and USSA and were in most cases equal to TSP fertilization under different soil conditions. In contrast, the effects of RP and USSA varied among soils but, mostly, did not exceed plant biomass and P-uptake of the unfertilized control. Conclusion TC-SSA has an increased fertilizer efficacy compared to USSA and is an effective P-fertilizer for spring wheat and maize in different soil conditions. KW - Phosphorus KW - Fertilizer KW - Thermochemical KW - Maize PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-648251 DO - https://doi.org/10.1002/jpln.70035 SN - 1522-2624 VL - 189 IS - 1 SP - 81 EP - 93 PB - Wiley-VCH AN - OPUS4-64825 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jovičević-Klug, Matic A1 - Souza Filho, Isnaldi R. A1 - Springer, Hauke A1 - Adam, Christian A1 - Raabe, Dierk T1 - Green steel from red mud through climate-neutral hydrogen plasma reduction N2 - AbstractRed mud is the waste of bauxite refinement into alumina, the feedstock for aluminium production1. With about 180 million tonnes produced per year1, red mud has amassed to one of the largest environmentally hazardous waste products, with the staggering amount of 4 billion tonnes accumulated on a global scale1. Here we present how this red mud can be turned into valuable and sustainable feedstock for ironmaking using fossil-free hydrogen-plasma-based reduction, thus mitigating a part of the steel-related carbon dioxide emissions by making it available for the production of several hundred million tonnes of green steel. The process proceeds through rapid liquid-state reduction, chemical partitioning, as well as density-driven and viscosity-driven separation between metal and oxides. We show the underlying chemical reactions, pH-neutralization processes and phase transformations during this surprisingly simple and fast reduction method. The approach establishes a sustainable toxic-waste treatment from aluminium production through using red mud as feedstock to mitigate greenhouse gas emissions from steelmaking. KW - Multidisciplinary PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594424 DO - https://doi.org/10.1038/s41586-023-06901-z SN - 0028-0836 VL - 625 IS - 7996 SP - 703 EP - 709 PB - Springer Science and Business Media LLC AN - OPUS4-59442 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholz, Philipp A1 - Falkenhagen, Jana A1 - Wachtendorf, Volker A1 - Brüll, Robert A1 - Simon, Franz-Georg T1 - Investigation on the Durability of a Polypropylene Geotextile under Artificial Aging Scenarios N2 - Geosynthetics are widely used in various civil engineering applications, such as geotextiles in coastal protection, and display a sustainable alternative to natural mineral materials. However, the full benefits of using geosynthetics can only be gained with a long service lifetime of the products. With the use of added stabilizers to the polymers, service lifetimes can be achieved in the range of 100 years. Therefore, accelerated aging methods are needed for the assessment of the long-term performance of geotextiles. In the present study, the behavior of geosynthetic materials made of polypropylene was investigated under artificial aging conditions involving elevated temperatures ranging from 30 to 80 °C, increased oxygen pressures ranging from 10 to 50 bar in water-filled autoclaves, and UV irradiation under atmospheric conditions. ATR-IR spectroscopy was employed to detect the increase in the carbonyl index over various aging durations, indicating the oxidative degradation of the geotextile. The most pronounced increase was observed in the case of aging through UV irradiation, followed by thermal aging. Elevated pressure, on the other hand, had a lower impact on oxidation. High-temperature size exclusion chromatography was utilized to follow the reduction in molar mass under different degradation conditions, and the results were consistent with those obtained from ATR-IR spectroscopy. In polyolefins such as polypropylene, Hindered Amine Stabilizers (HAS) are used to suppress oxidation caused by UV radiation. The quantitative analysis of HAS was carried out using a UV/Vis method and HPLC. The degradation of UV stabilizers during the aging of geotextiles is responsible for the oxidation and the reduction in the molar mass of polypropylene. From the results, it can be concluded that applications of PP geotextile without soil or sand cover might cause the risk of the formation of microplastic particles. Material selection, design, and maintenance of the construction must follow best practices, including the system’s removal or replacement at end-of-life. Otherwise, a sustainable use of geotextiles in civil engineering is not possible. KW - Geotextiles KW - Microplastic KW - Size exclusion chromatography KW - Accelerated aging PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-599739 DO - https://doi.org/10.3390/su16093559 SN - 2071-1050 VL - 16 IS - 9 SP - 1 EP - 15 PB - MDPI AG CY - Basel AN - OPUS4-59973 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meiers, Emelie A1 - Scholl, Juliane A1 - Droas, Morten A1 - Vogel, Christian A1 - Leube, Peter A1 - Sommerfeld, Thomas A1 - Bagheri, A. A1 - Adam, Christian A1 - Seubert, A. A1 - Koch, Matthias T1 - Development and evaluation of analytical strategies for the monitoring of per- and polyfluoroalkyl substances from lithium-ion battery recycling materials N2 - Per- and polyfluoroalkyl substances (PFAS) are well-known as “forever chemicals” and persistent pollutants released by different anthropogenic sources. The potential release of PFAS from accumulating electronic waste and lithium-ion battery (LIB) recycling activities has gained increasing attention in the past years. This creates a need for analytical methods tailored for the determination of PFAS out of environmental matrices related to the named activities or directly out of the concerned materials. In this work, analytical strategies for the monitoring of PFAS in LIB recycling materials were explored for a group of legacy perfluoro sulfonic- and carbonic acids (PFSA and PFCA) and of fluorinated sulfonylimides suspected to be LIB electrolyte ingredients. These analytical strategies comprehend PFAS target approaches with a herein optimized liquid chromatography tandem mass spectrometry (LC–MS/MS) method equipped with a HILIC (hydrophilic interaction liquid chromatography) column in combination with the TOP (total oxidizable precursor) assay and an adapted sample preparation method for high-matrix LIB recycling materials. The validated target method was applied to a set of LIB recycling materials: end-of-life batteries, black masses from hydrometallurgical recycling, and gas absorption solutions from thermal treatment of black masses as part of the recycling procedure. Investigation results show that the LIB industry can be connected to the release of both “LIB”-PFAS, such as the target sulfonylimides, and “already-legacy” PFAS, like the PFSA and PFCA. Especially, the presence of trifluoroacetic acid (TFA) as an emerging pollutant in every investigated LIB material type underlines the threat of PFAS emissions from LIB waste and recycling activities. KW - Per- and polyfluoroalkyl substances (PFAS) KW - Battery PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647015 DO - https://doi.org/10.1007/s00216-025-06165-8 SN - 1618-2642 VL - 417 SP - 6567 EP - 6583 PB - Springer Science and Business Media LLC AN - OPUS4-64701 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Helfenstein, J. A1 - Massey, M. A1 - Kretzschmar, R. A1 - Schade, U. A1 - Verel, R. A1 - Chadwick, O. A1 - Frossard, E. T1 - Spectroscopic analysis shows crandallite can be a major component of soil phosphorus N2 - Phosphorus (P) bioavailability is crucial for the productivity of natural and agricultural ecosystems, and soil P speciation plays a major role therein. Better understanding of P forms present in soil is thus essential to predict bioavailability. However, P speciation studies are only as powerful as the reference spectra used to interpret them, and most studies rely on a limited set of reference spectra. Most studies on soil P forms differentiate between Ca-bound P (e.g. apatite), organic P, Fe-bound P, and Al-bound P. In our analysis of a Ca, Al, and P rich soil from the Kohala region of Hawaii, we identified the mineral crandallite, CaAl3(PO4)2(OH)5·H2O, a mineral previously not considered to play a significant role in soils. Crandallite was first identified with powder X-ray diffraction. Subsequently reference spectra were collected, and the presence of crandallite was confirmed using micro-focused P K-edge X-ray absorption near edge structure (XANES) spectroscopy, micro-infrared spectroscopy, and solid-state 31P nuclear magnetic resonance (NMR) spectroscopy. Crandallite XANES spectra were distinct from other common XANES spectra due to the presence of features in the post-edge region of the spectrum. Linear combination fitting of bulk P K-edge XANES spectra allowed the determination of the proportion of crandallite to the total P content, indicating that crandallite comprises up to half, possibly even more of the soil P in the samples. Crandallite is therefore an important and potentially overlooked component of soil P, which pedogenically forms in soils with high P, Al, and Ca contents, where it could play an important role in P bioavailability. KW - Phosphorus KW - XANES spectrosocpy KW - Infrared spectroscopy KW - NMR spectrocopy PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-654968 DO - https://doi.org/10.1016/j.geoderma.2026.117712 SN - 0016-7061 VL - 467 SP - 1 EP - 10 PB - Elsevier B.V. AN - OPUS4-65496 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 - 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 - Herzel, Hannes A1 - Stemann, J. A1 - Simon, Sebastian A1 - Adam, Christian T1 - Comparison of thermochemical treatment of sewage sludge ash with sodium sulphate in laboratory-scale and pilot-scale experiments N2 - There is an ongoing debate on European scale concerning the criticality of phosphorus. In Switzerland and Germany, phosphorus recovery from phosphorus-rich waste streams will become obligatory. Sewage sludge ash is rich in phosphorus and may become an important secondary feedstock. Thermochemical treatment of sewage sludge ash with sodium sulphate under reducing conditions was shown to remove heavy metals from the solid product and produce the fully plant available crystalline phase CaNaPO4. Pilot-scale experiments in a rotary kiln were carried out at temperatures between 750 and 1000 °C and were compared to laboratory-scale experiments with crucibles. Process upscaling was successfully demonstrated but a series of differences were noticed: In comparison to laboratory-scale, solubility of phosphorus in samples from pilot-scale experiments was lower at all chosen treatment temperatures because of shorter retention time and incomplete decomposition of sodium sulphate. X-ray diffraction analysis revealed remaining phase fractions of whitlockite (Ca3-x(Mg,Fe)x(PO4)2) and sodium sulphate from the starting materials in products and thus indicated incomplete reaction. In contrast to the results of laboratory-scale experiments, the crystalline phase CaNaPO4 was clearly absent in the products from the rotary kiln but instead a Mg-bearing phase (Ca,Mg)NaPO4 was formed. Laboratory-scale experiments confirmed (Ca,Mg)NaPO4 is an intermediate phase between whitlockite and CaNaPO4. However, both crystalline phases are characterized by high plant availability. It was shown that heavy metal removal increased at higher temperatures whereas solubility and thus plant availability of phosphorus already reached its maxima at temperatures of 950 °C in pilot-scale and 875 °C in laboratory-scale experiments. KW - Crystalline phase identification KW - Heavy metal removal KW - Phosphorus availability KW - Process upscaling KW - Recovery KW - Rhenanite PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-524084 DO - https://doi.org/10.1007/s13762-021-03252-y VL - 19 IS - 3 SP - 1997 EP - 2006 PB - Springer AN - OPUS4-52408 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weimann, Karin A1 - Adam, Christian A1 - Buchert, M. A1 - Sutter, J. T1 - Environmental Evaluation of Gypsum Plasterboard Recycling N2 - Gypsum is widely used in the construction sector and its worldwide consumption has been increasing for several decades. Depending on the life-time of the used gypsum products, an increase of gypsum in construction and demolition waste follows. Especially against the background of a circular economy, the recycling of waste gypsum is of growing importance. However, the use of recycled gypsum makes only sense if it is environmentally friendly. Therefore, an evaluation of the environmental impacts of an industrial-scale processing for the recycling of post-consumer gypsum waste was conducted. The evaluation was performed with an established life cycle assessment software. Original data provided by industry and complementary data from a database for life cycle assessments were used for the calculations. Two scenarios for recycled gypsum with different transportation distances were calculated. These results are compared with results of the environmental evaluation of gypsum derived from coal-fired power plants (FGD gypsum) and natural gypsum. The results show that utilization of recycled gypsum can be environmentally advantageous compared to the use of natural gypsum or FGD gypsum, especially in the impact categories land transformation and resource consumption (abiotic depletion potential). For most environmental impact categories the specific transportation distances have a strong influence. KW - Gypsum plasterboards KW - Gypsum waste KW - Recycled gypsum KW - Environmental evaluation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522321 DO - https://doi.org/10.3390/min11020101 SN - 2075-163X VL - 11 IS - 2 SP - 101 PB - MDPI CY - Basel, Schweiz AN - OPUS4-52232 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Hoffmann, Marie A1 - Krüger, O. A1 - Murzin, V. A1 - Caliebe, W. A1 - Adam, Christian T1 - Chromium (VI) in phosphorus fertilizers determined with the diffusive gradients in thin-films (DGT) technique N2 - Phosphorus (P) fertilizers from secondary resources became increasingly important in the last years. However, these novel P-fertilizers can also contain toxic pollutants such as chromium in its hexavalent state (Cr(VI)). This hazardous form of chromium is therefore regulated with low limit values for agricultural products even though the correct determination of Cr(VI) in these fertilizers may be hampered by redox processes, leading to false results. Thus, we applied the novel diffusive gradients in thin-films (DGT) technique for Cr(VI) in fertilizers and compared the results with the standard wet chemical extraction method (German norm DIN EN 15192) and Cr K-edge X-ray Absorption near-edge structure (XANES) spectroscopy. We determined an overall good correlation between the wet chemical extraction and the DGT method. DGT was very sensitive and for most tested materials selective for the analysis of Cr(VI) in P-fertilizers. However, hardly soluble Cr(VI) compounds cannot be detected with the DGT method since only mobile Cr(VI) is analyzed. Furthermore, Cr K-edge XANES spectroscopy showed that the DGT binding layer also adsorbs small amounts of mobile Cr(III) so that Cr(VI) values are overestimated. Since certain types of the P fertilizers contain mobile Cr(III) or partly immobile Cr(VI), it is necessary to optimize the DGT binding layers to avoid aforementioned over- or underestimation. Furthermore, our investigations showed that the Cr K-edge XANES spectroscopy technique is unsuitable to determine small amounts of Cr(VI) in fertilizers (below approx. 1% of Cr(VI) in relation to total Cr). KW - Phosphorus fertilizer KW - Sewage sludge ash KW - Diffusive Gradients in thin films (DGT) KW - Chemical extraction KW - XANES spectroscopy PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509578 DO - https://doi.org/10.1007/s11356-020-08761-w SN - 0944-1344 VL - 27 SP - 24320 EP - 24328 PB - Springer AN - OPUS4-50957 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Herzel, Hannes A1 - Aydin, Zeynep A1 - Adam, Christian T1 - Crystalline phase analysis and phosphorus availability after thermochemical treatment of sewage sludge ash with sodium and potassium sulfates for fertilizer production N2 - Phosphorus rich sewage sludge ash is a promising source to produce phosphorus recycling fertilizer. However, the low plant availability of phosphorus in these ashes makes a treatment necessary. A thermochemical treatment (800–1000 °C) with alkali additives transforms poorly plant available phosphorus phases to highly plant available calcium alkali Phosphates (Ca,Mg)(Na,K)PO4. In this study, we investigate the use of K2SO4 as additive to produce a phosphorus potassium fertilizer in laboratory-scale experiments (crucible). Pure K2SO4 is not suitable as high reaction temperatures are required due to the high melting point of K2SO4. To overcome this barrier, we carried out series of experiments with mixtures of K2SO4 and Na2SO4 resulting in a lower economically feasible reaction temperature (900–1000 °C). In this way, the produced phosphorus potassium fertilizers (8.4 wt.% K, 7.6 wt.% P) was highly plant available for phosphorus indicated by complete extractable phosphorus in neutral ammonium citrate solution. The added potassium is, in contrast to sodium, preferably incorporated into silicates instead of phosphorus phases. Thus, the highly extractable phase (Ca,Mg)(Na,K)PO4 in the thermochemical products contain less potassium than expected. This preferred incorporation is confirmed by a pilot-scale trial (rotary kiln) and thermodynamic calculation. KW - Phosphorus recovery KW - Recycling fertilizer KW - Calcium alkali phosphate KW - Silicate PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-536276 DO - https://doi.org/10.1007/s10163-021-01288-3 SN - 1611-8227 IS - 23 SP - 2242 EP - 2254 PB - Springer AN - OPUS4-53627 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Raniro, H.R. A1 - Soares, T.de M. A1 - Adam, Christian A1 - Pavinato, P.S. T1 - Waste-derived fertilizers can increase phosphorus uptake by sugarcane and availability in a tropical soil N2 - The use of highly water-soluble phosphorus (P) fertilizers can lead to P fixation in the soil, reducing fertilization efficiency. Waste-derived, low water-solubility sources can potentially increase sugarcane’s P uptake compared to triple superphosphate by reducing adsorption to the soil. Aims:We aimed to test struvite, hazenite, and AshDec® for their agronomic potential as recycled fertilizers for sugarcane production in a typical tropical soil.We hypothesize that these sources can reduce P fixation in the soil, increasing its availability and sugarcane’s absorption. Methods: In a greenhouse pot experiment, two consecutive sugarcane cycles, 90 days each, were conducted in a Ferralsol. The recovered sources struvite, hazenite, AshDec®, and the conventional triple superphosphate were mixed in the soil in three P doses (30, 60, and 90 mg kg–1), aside a control (nil-P). At both harvests, sugarcane number of sprouts, plant height, stem diameter, dry mass yield, shoot phosphorus, and soil P fractionation were investigated. Results: At 90 days, struvite and hazenite performed better for dry mass yield (70.7 and 68.3 g pot–1, respectively) than AshDec® and triple superphosphate (59.8 and 57.4 g pot–1, respectively) and for shoot P, with 98.1, 91.6, 75.6, and 66.3 mg pot–1, respectively. At 180 days, struvite outperformed all treatments for dry mass yield (95.3 g pot–1) and AshDec® (75.5 mg pot–1) for shoot P. Struvite was 38% and hazenite 21% more efficient than triple superphosphate in P uptake, while AshDec® was 6% less efficient. Soil had higher labile P under struvite, hazenite, and AshDec® than triple superphosphate by the end of the first cycle, while only the later increased nonlabile P by the end of the experiment (180 days). Conclusions:Waste-derived P sources were more efficient in supplying P for sugarcane and delivering labile P in 180 days than triple superphosphate. KW - AshDec KW - Hazenite KW - P-efficiency KW - Recycled sources KW - Struvite PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-544216 DO - https://doi.org/10.1002/jpln.202100410 SN - 1436-8730 SP - 1 EP - 12 PB - Wiley-VCH GmbH AN - OPUS4-54421 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 - Sichler, Theresa Constanze A1 - Adam, Christian A1 - Barjenbruch, M. A1 - Montag, D. A1 - Mauch, Tatjana A1 - Sommerfeld, Thomas A1 - Ehm, J.H. T1 - Variation of the element composition of municipal sewage sludges in the context of new regulations on phosphorus recovery in Germany N2 - Phosphorus (P) recovery is obligatory for all sewage sludges with more than 20 g P/kg dry matter (DM) from 2029 in Germany. Nine wastewater treatment plants (WWTPs) were chosen to investigate variations of phosphorus contents and other parameters in sewage sludge over the year. Monthly sewage sludge samples from each WWTP were analyzed for phosphorus and other matrix elements (C, N, H, Ca, Fe, Al, etc.), for several trace elements (As, Cr, Mo, Ni, Pb, Sn) and loss of ignition. Among the nine WWTPs, there are four which have phosphorus contents both above and below the recovery limit of 20 g/kg DM along the year. Considering the average phosphorus content over the year, only one of them is below the limit. Compared to other matrix elements and parameters, phosphorus fuctuations are low with an average of 7% over all nine WWTPs. In total, only hydrogen and carbon are more constant in the sludge. In several WWTPs with chemical phosphorus elimination, phosphorus fuctuations showed similar courses like iron and/or aluminum. WWTPs with chamber flter presses rather showed dilution efects of calcium dosage. As result of this study, monthly phosphorus measurement is highly recommended to determine whether a WWTP is below the 20 g/kg DM limit. KW - Sewage sludge KW - Phosphorus recovery KW - Wastewater KW - Phosphorus elimination PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-557499 DO - https://doi.org/10.1186/s12302-022-00658-4 SN - 2190-4707 VL - 34 IS - 1 SP - 1 EP - 12 PB - Springer Nature CY - Berlin AN - OPUS4-55749 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 - 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 - Machado Ferreira de Araujo, F. A1 - Duarte-Ruiz, D. A1 - Saßnick, H.-D. A1 - Gentzmann, Marie C. A1 - Huthwelker, T. A1 - Cocchi, C. T1 - Electronic Structure and Core Spectroscopy of Scandium Fluoride Polymorphs N2 - Microscopic knowledge of the structural, energetic, and electronic properties of scandium fluoride is still incomplete despite the relevance of this material as an intermediate for the manufacturing of Al−Sc alloys. In a work based on first-principles calculations and X-ray spectroscopy, we assess the stability and electronic structure of six computationally predicted ScF3 polymorphs, two of which correspond to experimentally resolved single-crystal phases. In the theoretical analysis based on density functional theory (DFT), we identify similarities among the polymorphs based on their formation energies, chargedensity distribution, and electronic properties (band gaps and density of states). We find striking analogies between the results obtained for the ow- and high-temperature phases of the material, indirectly confirming that the transition occurring between them mainly consists of a rigid rotation of the lattice. With this knowledge, we examine the X-ray absorption spectra from the Sc and F K-edge contrasting firstprinciples results obtained from the solution of the Bethe−Salpeter equation on top of all-electron DFT with high-energy-resolution fluorescence detection measurements. Analysis of the computational results sheds light on the electronic origin of the absorption maxima and provides information on the prominent excitonic effects that characterize all spectra. A comparison with measurements confirms that the sample is mainly composed of the high- and low-temperature polymorphs of ScF3. However, some fine details in the experimental results suggest that the probed powder sample may contain defects and/or residual traces of metastable polymorphs. KW - Scandium KW - X-ray spectroscopy PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570727 DO - https://doi.org/10.1021/acs.inorgchem.2c04357 SN - 0020-1669 VL - 62 IS - 10 SP - 4238 EP - 4247 PB - ACS Publications CY - Washington DC AN - OPUS4-57072 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klinge, A A1 - Mönig, J A1 - Ziegert, C A1 - Richter, Matthias A1 - Kalbe, Ute A1 - Horn, Wolfgang A1 - Röhlen, U A1 - Rauscher, S A1 - Roswag-Klinge, E T1 - upMIN 100 – upcycling of mineral construction and demolition waste to substitute natural aggregates in earthen building materials N2 - The construction sector is one of the most resource-intensive sectors in Germany and is responsible for 40 % of CO2 emissions. Around 517 million tons of mineral raw materials are required annually for the construction of buildings in Germany. At the same time, mineral construction waste was the largest material flow at 229.3 million tons (2020). The rates of construction and demolition waste (CDW) recycling have increased since 2000, especially for mineral waste. Nevertheless, the majority of recycled aggregates are used in technically largely unregulated applications (e.g. road construction). This downcycling leads to a loss of valuable resources for technically and economically valuable applications. The upMIN 100 research project is investigating the question of whether and to what extent recycled CDW is suitable as an additive an binder in earthen building materials. The focus is placed on grain sizes of < 2 mm, which are currently predominantly landfilled, as there are at present no regulations for their use in building products. The soil matrix of earthen building materials however, naturally contains of different grain sizes, whith < 2mm – 0,063 for aggregates and < 0.063 mm as a binder. Therefore, the focused grain sizes (sand, clay and silt) could have a high usage potential. In order to enable the use of CDW, the technical feasibility must be ensured, quality requirements for source materials (e.g. threshold values for pollutants in terms of health and environmental compatibility and hazardous substances) and permissible proportions of recycled aggregates must be defined. Two different building material developments (earth blocks and -plaster)were used to assess both, the technical feasibility as well the pollutant content of the recycled aggregate and its final emissions into the indoor air. For both materials two mixtures could be established, that also meet the mechanical specifications according to the DIN standard, such as the compressive strength. A method was developed to design material mixtures with a high amount of CDW that comply with the defined limit values. The mixtures reached a recycling rate of 28 % with high mechanical properties and 70 % with minimum strength requirements. KW - Mineral waste KW - Upcycling KW - Earthen building product KW - Circular construction PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652831 DO - https://doi.org/10.1088/1755-1315/1554/1/012084 SN - 1755-1307 VL - 1554 IS - 1 SP - 1 EP - 9 PB - IOP Publishing AN - OPUS4-65283 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stawski, Tomasz A1 - Karafiludis, Stephanos A1 - Pimentel, Carlos A1 - Montes-Hernández, German A1 - Kochovski, Zdravko A1 - Bienert, Ralf A1 - Weimann, Karin A1 - Emmerling, Franziska A1 - Scoppola, Ernesto A1 - Van Driessche, Alexander E.S. T1 - Solution-driven processing of calcium sulfate: The mechanism of the reversible transformation of gypsum to bassanite in brines N2 - Here, we show that calcium sulfate dihydrate (gypsum) can be directly, rapidly and reversibly converted to calcium sulfate hemihydrate (bassanite) in high salinity solutions (brines). The optimum conditions for the efficient production of bassanite in a short time (<5 min) involve the use of brines with c(NaCl) > 4 M and maintaining a temperature, T > 80 °C. When the solution containing bassanite crystals is cooled down to around room temperature, eventually gypsum is formed. When the temperature is raised again to T > 80 °C, bassanite is rapidly re-precipitated. This contrasts with the better-known behaviour of the bassanite phase in low-salt environments. In low-salinity aqueous solutions, bassanite is considered to be metastable with respect to gypsum and anhydrite, and therefore gypsum-to-bassanite conversion does not occur in pure water. Interestingly, the high-salinity transformation of gypsum-to-bassanite has been reported by many authors and used in practice for several decades, although its very occurrence actually contradicts numerical thermodynamic predictions regarding solubility of calcium sulfate phases. By following the evolution of crystalline phases with in situ and time-resolved X-ray diffraction/scattering and Raman spectroscopy, we demonstrated that the phase stability in brines at elevated temperatures was inaccurately represented in the thermodynamic databases. Most notably for c(NaCl) > 4 M, and T > 80 °C gypsum becomes readily more soluble than bassanite, which induces the direct precipitation of the latter from gypsum. The fact that these transformations are controlled by the solution provides extensive opportunities for precise manipulation of crystal formation. Our experiments confirmed that bassanite remained the sole crystalline phase for many hours before reverting into gypsum. This property is extremely advantageous for practical processing and efficient crystal extraction in industrial scenarios. KW - Industrial and Manufacturing Engineering KW - Strategy and Management KW - General Environmental Science KW - Renewable Energy, Sustainability and the Environment KW - Building and Construction KW - Calcium sulfate KW - Gypsum KW - Bassanite KW - Scattering KW - Raman KW - In situ KW - Synchrotron KW - BESSY KW - MySpot PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594698 UR - https://www.sciencedirect.com/science/article/pii/S0959652624004591#appsec1 DO - https://doi.org/10.1016/j.jclepro.2024.141012 SN - 0959-6526 VL - 440 SP - 1 EP - 12 PB - Elsevier B.V. AN - OPUS4-59469 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kittner, Maria A1 - Coesfeld, Bianca A1 - Schlau, Sven A1 - Werischak, Thomas A1 - Altmann, Korinna A1 - Kalbe, Ute T1 - Simultaneous sampling for microplastics and environmental contaminants from artificial turf: development of a new integrated microplastics eluate lysimeter N2 - To get a better understanding of potentially harmful contaminant emissions from soils or materials into the environment, politics demand practical and holistic sampling concepts for environmental samples such as leachates containing polycyclic aromatic hydrocarbons (PAH) or heavy metals, and hazardous particulate matter like microplastics (MP). Of particular concern are MP emissions from artificial turf sports pitches. So far, there has been only very limited data on MP mass emissions from artificial turf potentially posing a risk to the groundwater and no sampling device that allowed simultaneous sampling for dissolved and particulate contaminants. In this study, a novel integrative microplastics eluate lysimeter was developed to determine contaminant emissions from three artificial turf systems at different ageing states (fabric-new, artificially aged, real-time aged). For the accelerated ageing, all environmental simulation parameters were based on Central German conditions and simulated outdoor stress during the turf service lifespan of 15 years. MP masses from eluates were analysed using thermal extraction desorption-gas chromatography/mass spectrometry, PAH concentrations using gas chromatography/mass spectrometry and heavy metals using inductively coupled plasma-optical emission spectroscopy. Results showed that no PAH or heavy metal concentrations from the seepage water were above German legal limits for alternative granular construction materials considering soil and groundwater protection. Furthermore, it was found that only minimal MP emissions were released from new turf systems into the seepage water (< 1 mg/m2). Ageing of the artificial turf increased MP formation, especially from rubber infill and grass fibres, which are then carried into the seepage water. The highest total MP emissions over a simulated turf lifespan of 15 years were detected in two real-time aged turf systems ranging from 136.4–252.5 mg/m2. Considerably less total MP emissions were detected in accelerated aged artificial turf systems, one of which contained a synthetic rubber infill (5.4–8.0 mg/m2) and one without rubber infill (0.2–5.3 mg/m2). In summary, it was demonstrated that the newly developed MEL generated reliable and reproducible data and has thus proven itself as an integrated, straightforward and automated sampling device for simultaneous monitoring of particulate and dissolved pollutant emissions from simple soil matrices. KW - Lysimeter KW - Microplastics KW - Artificial turf KW - Thermal extraction desorption-gas chromatography/mass spectrometry KW - TED-GC/MS KW - Polycyclic aromatic hydrocarbons KW - PAH KW - Heavy metals KW - Soil samples PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-645301 DO - https://doi.org/10.1186/s12302-025-01235-1 SN - 2190-4715 VL - 37 IS - 1 SP - 1 EP - 15 PB - Springer Open AN - OPUS4-64530 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Herzel, Hannes A1 - Grevel, K.-D. A1 - Emmerling, Franziska A1 - Dachs, E. A1 - Benisek, A. A1 - Adam, Christian A1 - Majzlan, J. T1 - Thermodynamic properties of calcium alkali phosphates Ca(Na,K)PO4 N2 - Calcium alkali phosphates Ca(Na,K)PO4 are main constituents of bioceramics and thermochemically produced phosphorus fertilizers because of their bioavailability. Sparse thermodynamic data are available for the endmembers CaNaPO4 and CaKPO4. In this work, the missing data were determined for the low-temperature phase modifications of the endmembers CaNaPO4 and CaKPO4 and three intermediate Ca(Na,K)PO4 compositions. Standard enthalpy of formation ranges from - 2018.3 ± 2.2 kJ mol-1 to - 2030.5 ± 2.1 kJ mol-1 and standard entropy from 137.2 ± 1.0 J mol-1 K-1 to 148.6 ± 1.0 J mol-1 K-1 from sodium endmember b-CaNaPO4 to potassium endmember b0-CaKPO4. Thermodynamic functions are calculated up to 1400 K for endmembers and the sodium-rich intermediate phase b-Ca(Na0.93K0.07)PO4. Functions above 640 K are extrapolated because of the phase transition from low- to high-temperature phase. Impurities in the synthesized intermediate phases c-Ca(Na0.4K0.6)PO4 and c-Ca Na0.35K0.65)PO4 and one additional phase transition around 500 K impeded the determination of high-temperature thermodynamic functions. In general, data for phase transition temperatures agree with the previously reported phase diagrams. KW - Formation enthalpy KW - Heat capacity KW - Phase transformation KW - Bioceramics KW - Phosphorus fertilizer KW - Entropy PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507640 DO - https://doi.org/10.1007/s10853-020-04615-5 VL - 55 SP - 8477 EP - 8490 PB - Springer AN - OPUS4-50764 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bandow, N. A1 - Aitken, M. D. A1 - Geburtig, Anja A1 - Kalbe, Ute A1 - Piechotta, Christian A1 - Schoknecht, Ute A1 - Simon, Franz-Georg A1 - Stephan, Ina T1 - Using Environmental Simulations to Test the Release of Hazardous Substances from Polymer-Based Products: Are Realism and Pragmatism Mutually Exclusive Objectives? N2 - The potential release of hazardous substances from polymer-based products is currently in the focus of environmental policy. Environmental simulations are applied to expose such products to selected aging conditions and to investigate release processes. Commonly applied aging exposure types such as solar and UV radiation in combination with water contact, corrosive gases, and soil contact as well as expected general effects on polymers and additional ingredients of polymer-based products are described. The release of substances is based on mass-transfer processes to the material surfaces. Experimental approaches to investigate transport processes that are caused by water contact are presented. For tailoring the tests, relevant aging exposure types and release quantification methods must be combined appropriately. Several studies on the release of hazardous substances such as metals, polyaromatic hydrocarbons, flame retardants, antioxidants, and carbon nanotubes from polymers are summarized exemplarily. Differences between natural and artificial exposure tests are discussed and demonstrated for the release of flame retardants from several polymers and for biocides from paints. Requirements and limitations to apply results from short-term artificial environmental exposure tests to predict long-term environmental behavior of polymers are presented. KW - Environmental simulations KW - Polymer-based products KW - Artificial weathering KW - Degradation KW - Leaching KW - Soil contact PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509310 DO - https://doi.org/10.3390/ma13122709 SN - 1996-1944 VL - 13 IS - 12 SP - Paper 2709, 22 PB - MDPI CY - Basel, Switzerland AN - OPUS4-50931 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -