TY - JOUR A1 - Roesch, Philipp A1 - Vogel, Christian A1 - Huthwelker, T. A1 - Wittwer, Philipp A1 - Simon, Franz-Georg T1 - Investigation of per‑ and polyfluoroalkyl substances (PFAS) in soils and sewage sludges by fluorine K‑edge XANES spectroscopy and combustion ion chromatography N2 - For the first time, fluorine K-edge X-ray absorption near-edge structure (XANES) spectroscopy was applied to detect per- and polyfluoroalkyl substances (PFAS) in various soil and sewage sludge samples. The method can be used to determine the speciation of inorganic and organic fluorides, without pre-treatment of solid samples. Therefore, XANES spectra of several inorganic fluorides as well as selected fluorinated organic compounds were recorded. While inorganic fluorides partially exhibit a variety of sharp spectral features in the XANES spectrum, almost all inspected organofluorine compounds show two distinct broad features at 688.5 and 692.0 eV. Moreover, the peak intensity ratio 688.5 eV/692.0 eV in the PFAS XANES spectrum can be inversely correlated to the chain length of the perfluoro sulfonic acid group. The detection of targeted PFAS by bulk-XANES spectroscopy in combination with linear combination fitting in soils and sewage sludges was not applicable due to the low organic fluorine to total fluorine ratio of the samples (0.01–1.84%). Nonetheless, direct analysis of pure PFAS revealed that analysis of organofluorine species might be achieved in higher concentrated samples. Furthermore, quantitative measurements by combustion ion chromatography (CIC) evaluated as sum parameters extractable organically bound fluorine (EOF) and total fluorine (TF) emphasize that besides soils, sewage sludges are a significant source of organic fluorine in agriculture (154–7209 μg/kg). KW - Sewage sludge KW - Combustion ion chromatography KW - Oil KW - X-ray absorption near-edge structure (XANES) spectroscopy KW - Per- and polyfluoroalkyl substances (PFAS) PY - 2021 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-538953 VL - 29 IS - 18 SP - 26889 EP - 26899 PB - Springer AN - OPUS4-53895 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gehrenkemper, Lennart A1 - Simon, Fabian A1 - Roesch, Philipp A1 - Fischer, E. A1 - von der Au, Marcus A1 - Pfeifer, Jens A1 - Cossmer, Antje A1 - Wittwer, Philipp A1 - Vogel, Christian A1 - Simon, Franz-Georg A1 - Meermann, Björn T1 - Determination of organically bound fluorine sum parameters in river water samples - Comparison of combustion ion chromatography (CIC) and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) N2 - In this study, we compare combustion ion chromatography (CIC) and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) with respect to their applicability for determining organically Bound fluorine sum parameters. Extractable (EOF) and adsorbable (AOF) organically bound fluorine as well as total fluorine (TF) were measured in samples fromriver Spree in Berlin, Germany, to reveal the advantages and disadvantages of the two techniques used as well as the two established fluorine sum Parameters AOF and EOF. TF concentrations determined via HR-CS-GFMAS and CIC were comparable between 148 and 270 μg/L. On average, AOF concentrations were higher than EOF concentrations, with AOF making up 0.14–0.81% of TF (determined using CIC) and EOF 0.04–0.28% of TF (determined using HR-CSGFMAS). The results obtained by the two independent methods were in good agreement. It turned out that HR-CS-GFMAS is a more sensitive and precise method for fluorine analysis compared to CIC. EOF and AOF are comparable tools in Risk evaluation for the emerging pollutants per- and polyfluorinated alkyl substances; however, EOF is much faster to conduct. KW - High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) KW - Combustion ion chromatography (CIC) KW - Per- and polyfluorinated alkyl substances (PFASs) KW - Adsorbable organically bound fluorine (AOF) KW - Extractable organically bound fluorine (EOF) KW - Surface waters PY - 2020 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-515351 SN - 1618-2650 VL - 413 IS - 28 SP - 103 EP - 115 PB - Springer CY - Berlin AN - OPUS4-51535 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 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-576109 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 - Vogel, Christian A1 - Roesch, Philipp A1 - Wittwer, Philipp A1 - Piechotta, Christian A1 - Lisec, Jan A1 - Sommerfeld, Thomas A1 - Kluge, Stephanie A1 - Herzel, Hannes A1 - Huthwelker, T. A1 - Borca, C. A1 - Simon, Franz-Georg T1 - Levels of per- and polyfluoroalkyl substances (PFAS) in various wastewater-derived fertilizers – analytical investigations from different perspectives N2 - Solid wastewater-based fertilizers were screened for per- and polyfluoroalkyl substances (PFAS) by the extractable organic fluorine (EOF) sum parameter method. The EOF values for ten sewage sludges from Germany and Switzerland range from 154 to 7209 mg kg−1. For thermal treated sewage sludge and struvite the EOF were lower with values up to 121 mg kg−1. Moreover, the application of PFAS targeted and suspect screening analysis of selected sewage sludge samples showed that only a small part of the EOF sum parameter values can be explained by the usually screened legacy PFAS. The hitherto unknown part of EOF sum parameter contains also fluorinated pesticides, pharmaceutical and aromatic compounds. Because these partly fluorinated compounds can degrade to (ultra-)short PFAS in wastewater treatment plants they should be considered as significant sources of organic fluorine in the environment. The combined results of sum parameter analysis and suspect screening reveal the need to update current regulations, such as the German fertilizer ordinance, to focus not solely on a few selected PFAS such as perfluorooctane sulfonic acid (PFOS) and perfluorooctanoic acid (PFOA) but consider an additional sum parameter approach as a more holistic alternative. Moreover, diffusion gradient in thin-films (DGT) passive samplers were utilized as an alternative simplified extraction method for PFAS in solid wastewater-based fertilizers and subsequently quantified via combustion ion chromatography. However, the DGT method was less sensitive and only comparable to the EOF values of the fertilizers in samples with >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 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-583429 VL - 2 IS - 10 SP - 1436 EP - 1445 PB - Royal Society of Chemistry (RSC) AN - OPUS4-58342 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Metz, Christian A1 - Franz, Philipp A1 - Fischer, C. A1 - Wachtendorf, Volker A1 - Maierhofer, Christiane T1 - Active thermography for quality assurance of 3D-printed polymer structures N2 - Additively manufactured test specimens made of polyamide 12 (PA 12) by Laser Sintering (LS) as well as of acrylnitril-butadien-styrol (ABS) by Fused Layer Modeling (FLM), were tested with active thermography. For this, two different excitation methods (flash and impulse excitation) were used and compared, regarding the suitability for the detection of constructed and imprinted defects. To increase the quality of the thermograms, data processing methods like thermal signal reconstruction (TSR) and Fourier-Transformation were applied. Furthermore, the long-term stability of the probes towards environmental stress, like UV-radiation, heat, water contact and frost is being investigated in the presented project with artificial weathering tests. T2 - 14th Quantitative InfraRed Thermography Conference CY - Berlin, Germany DA - 25.06.2018 KW - Additive manufacturing KW - Active thermography KW - Artificial weathering PY - 2018 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-453919 SP - Tu.3.A.2, 1 EP - 9 AN - OPUS4-45391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roesch, Philipp A1 - Vogel, Christian A1 - Simon, Franz-Georg T1 - Reductive Defluorination and Mechanochemical Decomposition of Per- and Polyfluoroalkyl Substances (PFASs): From Present Knowledge to Future Remediation Concepts N2 - Over the past two decades, per- and polyfluoroalkyl substances (PFASs) have emerged as worldwide environmental contaminants, calling out for sophisticated treatment, decomposition and remediation strategies. In order to mineralize PFAS pollutants, the incineration of contaminated material is a state-of-the-art process, but more cost-effective and sustainable technologies are inevitable for the future. Within this review, various methods for the reductive defluorination of PFASs were inspected. In addition to this, the role of mechanochemistry is highlighted with regard to its major potential in reductive defluorination reactions and degradation of pollutants. In order to get a comprehensive understanding of the involved reactions, their mechanistic pathways are pointed out. Comparisons between existing PFAS decomposition reactions and reductive approaches are discussed in detail, regarding their applicability in possible remediation processes. This article provides a solid overview of the most recent research methods and offers guidelines for future research directions. KW - PFAS KW - Reductive defluorination KW - Reductive decomposition KW - Mechanochemistry KW - Remediation PY - 2020 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-513811 VL - 17 IS - 19 SP - 1 EP - 22 PB - MDPI AG CY - Basel AN - OPUS4-51381 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholz, Philipp A1 - Putna-Nimane, I. A1 - Barda, I. A1 - Liepina-Leimane, I. A1 - Strode, E. A1 - Kileso, A. A1 - Esiukova, E. A1 - Chubarenko, B. A1 - Purina, I. A1 - Simon, Franz-Georg T1 - Environmental impact of geosynthetics in coastal protection N2 - Geosynthetic materials are applied in measures for coastal protection. Weathering or any damage of constructions, as shown by a field study in Kaliningrad Oblast (Russia), could lead to the littering of the beach or the sea (marine littering) and the discharge of possibly harmful additives into the marine environment. The ageing behavior of a widely used geotextile made of polypropylene was studied by artificial accelerated ageing in water-filled autoclaves at temperatures of 30 to 80 °C and pressures of 10 to 50 bar. Tensile strength tests were used to evaluate the progress of ageing, concluding that temperature rather than pressure was the main factor influencing the ageing of geotextiles. Using a modified Arrhenius equation, it was possible to calculate the half-life for the loss of 50% of the strain, which corresponds to approximately 330 years. Dynamic surface leaching and ecotoxicological tests were performed to determine the possible release of contaminants. No harmful effects on the test organisms were observed. KW - Geosynthetics KW - Geotextiles KW - Dynamic surface leaching test KW - Artificial ageing KW - Marine littering PY - 2021 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-520576 SN - 1996-1944 VL - 14 IS - 3 (Special issue: Measurement of the environmental impact of materials) SP - 634-1 EP - 634-13 PB - MDPI CY - Basel AN - OPUS4-52057 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Metz, Christian A1 - Franz, Philipp A1 - Fischer, C. A1 - Wachtendorf, Volker A1 - Maierhofer, Christiane T1 - Active thermography for quality assurance of 3D-printed polymer structures N2 - Additively manufactured test specimens made of polyamide 12 (PA 12) by Laser Sintering as well as of acrylonitrile butadiene styrene (ABS) by Fused Layer Modelling, were characterised with active thermography directly after manufacturing and after artificial weathering. For this, two different excitation methods (flash and pulse heating) were used and compared, regarding their suitability for the detection of constructed and imprinted defects inside the test specimens. To increase the quality of the thermograms, data processing methods like thermal signal reconstruction (TSR) and Fourier Transformation after TSR were applied. To further investigate the long-term stability of the additively manufactured test specimens towards environmental stress, like UV radiation, heat, humidity, water contact and frost with active thermography, an artificial weathering test over 2000 hours (~3 months) was applied to the specimens. The monitoring of the changes in the optical properties of the weathered plastics was supplemented by spectral reflectance and UV/VIS spectroscopy. KW - Additive manufacturing KW - Polymers KW - Artificial weathering KW - Active thermography KW - UV/VIS spectroscopy PY - 2019 U6 - https://doi.org/10.1080/17686733.2019.1686896 SN - 1768-6733 (Print) 2116-7176 (Online) VL - 18 IS - 1 SP - 50 EP - 72 PB - Taylor & Francis AN - OPUS4-49817 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chubarenko, B. A1 - Domnin, D. A1 - Simon, Franz-Georg A1 - Scholz, Philipp A1 - Leitsin, V. A1 - Tovpinets, A. A1 - Karmanov, K. A1 - Esiukova, E. T1 - Change over Time in theMechanical Properties of Geosynthetics Used in Coastal Protection in the South-Eastern Baltic N2 - The most massive design on the Baltic shore used geosynthetic materials, the landslide protection construction in Svetlogorsk (1300 m long, 90,000 m2 area, South-Eastern Baltic, Kaliningrad Oblast, Russian Federation) comprises the geotextile and the erosion control geomat coating the open-air cliff slopes. Due to changes in elastic properties during long-term use in the open air, as well as due to its huge size, this structure can become a non-negligible source of microplastic pollution in the Baltic Sea. Weather conditions affected the functioning of the structure, so it was assessed that geosynthetic materials used in this outdoor (open-air) operation in coastal protection structures degraded over time. Samples taken at points with different ambient conditions (groundwater outlet; arid places; exposure to the direct sun; grass cover; under landslide) were tested on crystallinity and strain at break. Tests showed a 39–85% loss of elasticity of the polymer filaments after 3 years of use under natural conditions. Specimens exposed to sunlight are less elastic and more prone to fail, but not as much as samples taken from shaded areas in the grass and under the landslide, which were the most brittle. KW - Geosynthetics KW - Microplastic KW - Degradation PY - 2023 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-567978 UR - https://www.mdpi.com/2077-1312/11/1/113 SN - 2077-1312 VL - 11 IS - 1 SP - 1 EP - 14 PB - MDPI CY - Basel AN - OPUS4-56797 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 (