4 Material und Umwelt
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- 4.3 Schadstofftransfer und Umwelttechnologien (81) (entfernen)
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Der Fachbeirat kommt bereits seit 13 Jahren in seiner jetzigen Form zusammen, um Zulassungsrichtlinien, weitere Dokumente und fachliche Fragestellungen zu beraten. Die Zeit bringt auch personelle Veränderungen mit sich, darüber wollen wir berichten. Derzeit wird die Zulassungsrichtlinie für Schutzschichten im Fachbeirat und in seiner Arbeitsgruppe Geotextilien und Kunststoff Dränelemente (AG Geotextilien) überarbeitet. Zudem wurde die Zulassungsrichtlinie für Kunststoffdichtungsbahnen auf den aktuellen Stand der Regelsetzung und Normung gebracht. Bestimmte Medien, die hier bei einigen Prüfungen verwendet werden, dürfen nicht mehr in der EU in Verkehr gebracht werden. Hier werden die Hintergründe und Zusammenhänge in Kürze aufgezeigt. Zuletzt wird die Diskussion in Bezug auf den Einsatz von Rezyklaten in den zugelassenen Produkten aufgeführt.
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 colocation 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.
Analytical Challenges for PFAS in Environmental Samples - Methods, Approaches and Applicability
(2022)
Per- and polyfluoroalkyl substances (PFAS) are anionic, cationic and zwitterionic synthetic products, in which the hydrogen atoms on the carbon skeleton of at least one carbon atom have been completely replaced by fluorine atoms and which include up to 1.7 M compounds, depending on the definition. As a result of continuous and prolific use, mainly in aviation firefighting foams, thousands of industrial and military installations have been found to contain contaminated soil, groundwater and surface water. Furthermore, because of the continuous contamination through PFAS containing commercial products, effluents and sewage sludge from WWTPs have been shown to be an important source of PFAS discharge into the aquatic environment. In the last few years, legacy PFAS (≥C4) have been found in various environments, including soil, water and wastewater, and their environmental pathways have been partly described.
Several long-chain PFAS species, and their respective salts are considered as persistent organic pollutants by the United Nations Stockholm Convention. These pollutants have been linked to altered immune and thyroid function, liver disease, lipid and insulin dysregulation, kidney disease, adverse reproductive and developmental outcomes, and cancer. A significant shift in the chemical industry towards production of short (C4-C7) and ultrashort (C1-C3) alternatives was observed in response to recently intensified regulations and restrictions on the use of long-chain (≥C8) PFAS. PFAS analysis in environmental samples is currently mainly done by liquid chromatography tandem mass spectrometry (LC-MS/MS). This efficient method is conducted in a targeted fashion analyzing a small subset of PFAS. The US EPA method for analysis of PFAS using LC-MS/MS for example currently lists 40 PFAS (≥C4). However, to get a better overview of the amount of “total PFAS,” sum parameter methods like total oxidizable precursor (TOP) assay and methods based on combustion ion chromatography (CIC) are in development. CIC results in data regarding the sum of absorbable organic fluorine (AOF) or extractable organic fluorine (EOF), which can also quantify other organically bound fluorine compounds such as fluorinated pesticides and pharmaceutical. Moreover, non-target and suspect screening mass spectrometry can be used to identify novel emerging PFAS and partly unknown fluorinated compounds in environmental samples. Furthermore, to analyze ultrashort PFAS (C1-C3), supercritical fluid chromatography (SFC), hydrophilic interaction chromatography (HILIC) and gas chromatography-mass spectrometry (GC-MS) are available, but further research is needed to develop reliable and accurate methods to quantify several ultrashort PFAS in environmental samples.
Additionally, for research purpose several spectroscopical methods like X-ray photoelectron spectroscopy (XPS), fluorine K-edge X-ray absorption near-edge structure (XANES)spectroscopy, particular induced gamma-ray emission (PIGE) spectroscopy and 19F nuclear magnetic resonance (NMR) spectroscopy are available.
Per- and polyfluoroalkyl substances (PFAS) are anionic, cationic and zwitterionic synthetic products, in which the hydrogen atoms on the carbon skeleton of at least one carbon atom have been completely replaced by fluorine atoms (see Figure 1) and which include more than 4730 compounds, depending on the definition. As a result of continuous and prolific use, mainly in aviation firefighting foams, thousands of industrial and military installations have been found to contain contaminated soil, groundwater and surface water. Furthermore, because of the continuous contamination through PFAS containing commercial products, effluents and sewage sludge from WWTPs have been shown to be an important source of PFAS discharge into the aquatic environment. In the last few years, legacy PFAS (≥C4) have been found in various environments, including soil, water and wastewater, and their environmental pathways have been partly described. To get a better
overview of the amount of “total PFAS,” sum parameter methods like total oxidizable precursor (TOP) assay and methods based on combustion ion chromatography (CIC) are in development. CIC results in data regarding the sum of absorbable organic fluorine (AOF) or extractable
organic fluorine (EOF), which can also quantify other organically bound fluorine compounds such as fluorinated pesticides and pharmaceutical. Additionally, for research purpose several spectroscopical methods like X-ray photoelectron spectroscopy (XPS), fluorine K-edge X-ray absorption near-edge structure (XANES) spectroscopy, particular induced gamma-ray emission (PIGE) spectroscopy and 19F nuclear magnetic resonance (NMR) spectroscopy are available. Therefore, an overview is given on various analytical techniques for PFAS in environmental samples and their application possibilities discussed for different kind of PFAS compounds
Per- und polyfluorierte Alkylsubstanzen (PFAS) im Klärschlamm - Analytische Methoden und Grenzwerte
(2022)
Per- und Polyfluoralkylsubstanzen (PFAS) sind eine Gruppe von mehr als 4700 anionischen und kationischen anthrophonen Stoffen, die aufgrund ihrer inerten chemischen Stabilität und ihrer Widerstandsfähigkeit gegen den Abbau durch Hitze oder Säuren in einer Vielzahl von Produkten verwendet werden. Infolge der ständigen Verwendung, vor allem in Feuerlöschschäumen für die Luftfahrt, wurden in Tausenden von Industrie- und Militäranlagen kontaminierte Böden und Grundwasservorkommen gefunden. Aufgrund der ständigen Verwendung von fluorierten Konsumgütern haben sich jedoch auch Abwässer und Klärschlamm aus Kläranlagen als Quelle für die Kontamination der aquatischen Umwelt mit PFAS erwiesen. Infolge der strengeren Vorschriften und Beschränkungen, die in den letzten Jahren für die Verwendung langkettiger (≥C8) PFAS erlassen wurden, findet in der chemischen Industrie eine deutliche Verlagerung hin zur Herstellung kurz- (C4-C7) und ultrakurzkettiger (C1-C3) Alternativen statt. Mit der Novellierung der Klärschlammverordnung im Jahr 2017 hat der deutsche Gesetzgeber die Ausbringung von Klärschlamm auf landwirtschaftlichen Flächen verboten, und bis 2029/2032 wird die Ausbringung von Klärschlamm in der Landwirtschaft vollständig verboten sein. Während die Belastung der Umwelt mit organischen Schadstoffen wie PFAS, Pestiziden und Arzneimitteln nicht mehr erwünscht ist, muss Phosphor (P) aus Klärschlamm weiterhin zur Herstellung hochwertiger P-Dünger für eine Kreislaufwirtschaft genutzt werden. Derzeit können pflanzenverfügbare P-Düngemittel aus Klärschlamm/Abwasser mit verschiedenen Behandlungsmethoden hergestellt werden, darunter Fällung, Auslaugung und thermische Behandlung. Der Verbleib von PFAS bei der Auslaugung, Ausfällung und Behandlung von Klärschlamm und Abwasser ist jedoch noch weitgehend unbekannt.
Per- and polyfluoroalkyl substances (PFAS) are a large group of anionic, cationic, or zwitterionic organofluorine surfactants used in the formulations of thousands of products and consumer goods, including aqueous film-forming foams (AFFF) used to suppress aviation fires in training scenarios, non-stick cookware, fast-food wrappers, water-repellent fabrics, medical equipment. Because PFAS have been extensively used in a variety of AFFF products they can be found in soils from industrial and military installations. Current decontamination strategies of PFAS-burdened soils mainly consist of adsorption methods using adsorbents for fixation of PFAS in the ground. A second option is the utilization of a “pump and treat” process, cycling polluted soils through a washing plant leading to the concentration of the pollutants in the fine fraction. Only a subsequent, high-energy consuming pyrolysis process guarantees the total destruction of all fluorinated organic contaminants. Both approaches are cost-intensive and not intended for the direct decomposition of all PFAS contaminants. Hence, there is a great demand for innovative developments and chemical treatment technologies, dealing with new strategies of tackling the PFAS problem. Previously, mechanochemical treatment of polychlorinated organic compounds in soils showed an efficient dechlorination. Thus, we investigated mechanochemical treatment of PFAS contaminated soils with various additives in a ball mill and analyzed the PFAS defluorination with gas chromatography mass spectrometry (GCMS) and liquid chromatography tandem mass spectrometry (LC-MS/MS), respectively, as well es the fluoride mineralization by ion chromatography (IC) and fluorine K-edge X-ray absorption near-edge structure (XANES) spectroscopy.
Per- and polyfluoroalkyl substances (PFAS) have emerged over the course of the last twenty years as a global pollution issue. Altogether, there are currently more than 4700 known but only partly characterized fluorinated compounds identified by the Organization for Economic Cooperation and Development (OECD), as shown by a recently published classification proposal.
The ongoing production of new, yet unrestricted PFAS alternatives has become a major challenge for environmental routine analytics, since the state-of-the-art method LC-MS/MS relies on structural information and availability of isotope standards of the targeted compound. First reported by Miyake et al., fluorine sum parameters like adsorbable organic fluorine (AOF), extractable organic fluorine (EOF) and total fluorine (TF) can be applied to survey and detect the presence of large amounts of unidentified organofluorine compounds in environmental matrices. Today fluorine sum parameters have been established as a useful supplement to classic target-analytical approaches of PFAS and were implemented for the first time as a sum value “PFAS-total” in the recently revised Drinking Water Directive (2020/2184) by the European Commission.
In contrast, X-ray absorption near-edge structure (XANES) spectroscopy has been widely applied to identify low concentration of element-specific contamination without pre-treatment in environmental samples in the past. The XANES approach enables a penetration depth of approx. 1 µm (at fluorine K-edge energy; depending on the matrix) which is significantly deeper than for X-ray photoelectron spectroscopy (XPS; penetration depth approx. 10 nm). Furthermore, the method is fast, non-destructive and only simple preparation of the samples is required.
In our work, we combined both F-XANES spectroscopy and combustion ion chromatography (CIC) in order to present a new analytical perspective on the investigation of PFAS in environmental media and material samples.
Im Rahmen des Projekts wurde 1.) eine vollständige Bewertung des Stands der Technik in der EU bei der Behandlung von Rostasche vorgenommen und 2.) eine Optimierung der Nutzung der Feinfraktion in Labor- und Feldmaßstab untersucht.
Das Konsortium bestand aus zwei Universitäten aus Deutschland und Italien, der BAM als Forschungseinrichtung des Bundes und zwei Industriepartnern aus Deutschland und Schweden mit unterschiedlichen und spezifischen Fachkompetenzen.
Im Vortrag werden die Ergebnisse des weitgehend abgeschlossenen Projekts BASH-TREAT vorgestellt.
Per- and polyfluoroalkyl substances (PFAS) are a group of anionic, cationic and zwitterionic synthetic products, in which the hydrogen atoms on the carbon skeleton of at least one carbon atom have been completely replaced by fluorine atoms and which include more than 4730 compounds, depending on the definition. As a result of continuous and prolific use, mainly in aviation firefighting foams, thousands of industrial and military installations have been found to contain contaminated soil, groundwater and surface water. As a result of the perpetual use of PFAS containing products, effluents and sewage sludge from wastewater treatment plants (WWTPs) have been observed to be an important pathway for PFAS into the environment. In Germany, phosphorus and other nutrients from sewage sludge and wastewater should be recycled in WWTPs of cities with a large population. However, it is not clear if PFAS contamination from wastewater and sewage sludge end up in novel wastewater-based fertilizers. Normally, PFAS are analyzed using PFAS protocols typically with liquid chromatography tandem mass spectrometry (LC-MS/MS) quantification. To get a better overview of the amount of “total PFAS,” we applied sum parameter methods based on combustion ion chromatography (CIC) to screen the PFAS contaminations in various sewage sludge and wastewater-based fertilizers. Furthermore, current decontamination strategies of PFAS-burdened soils mainly consist of adsorption methods using adsorbents for fixation of PFAS in the ground. A second option is the utilization of a “pump and treat” process, cycling polluted soils through a washing plant leading to the concentration of the pollutants in the fine fraction. Only a subsequent, high-energy consuming pyrolysis process guarantees the total destruction of all fluorinated organic contaminants. Both approaches are cost-intensive and not intended for the direct decomposition of all PFAS contaminants. Hence, there is a great demand for innovative developments and chemical treatment technologies, dealing with new strategies of tackling the PFAS problem.
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.
A wide range of analytical methods are used to estimate the plant-availability of soil phosphorus (P). Previous investigations showed that analytical methods based on the Diffusive Gradients in Thin films (DGT) technique provide a very good correlations to the amount of bioavailable nutrients and pollutants in environmental samples (Davison 2016, Vogel et al. 2017). However, the DGT results do not identify which P compound of the soil has the high bioavailability. But there are various spectroscopic techniques (infrared, Raman, P K-edge and L-edge XANES and P NMR spectroscopy) available to characterize P species in soils. Therefore, spectroscopic investigation of DGT binding layers after deployment allow us to determine the specific compounds. Nutrients such as phosphorus and nitrogen are often, together with other elements, present as molecules in the environment. These ions are detectable and distinguishable by infrared, P K- and L-edge X-ray absorption near-edge structure (XANES) and NMR spectroscopy, respectively. Additionally, microspectroscopic techniques make it also possible to analyze P compounds on the DGT binding layer with a lateral resolution down to 1 μm2. Therefore, species of elements and compounds of e.g. a spatial soil segment (e.g. rhizosphere) can be mapped and analyzed, providing valuable insight to understand the dynamics of nutrients in the environment.
Die Untersuchung altlastverdächtiger Flächen umfasst viele einzelne Schritte von der Probenahme über die Probenvorbehandlung bis hin zur eigentlichen Analyse, die zur Ergebnisunsicherheit beitragen. Beim Vergleich der Ergebnisse mit Bewertungsmaßstäben, um Entscheidungen zur Bewertung von Altlasten zu treffen, sind diese Faktoren zu berücksichtigen. Die Rolle von verschiedenen Unsicherheitskomponenten wird mit Blick auf Elutionsverfahren diskutiert.
The aim of this study was to investigate the passive sampler method Diffusive Gradients in Thin-films (DGT) for ammonium and nitrate in amended soils. Therefore, we used soils from a pot experiment with maize where nitrogen (N) was supplied as ammonium sulfate nitrate (ASN), without and with a nitrification inhibitor (NI). The additional use of a NI can delay the nitrification in the soil and making the ammonium available for a longer period in the soil solution after its application. Homogenized soil samples were collected directly from each pot after one week of incubation before sowing and after harvesting the maize. Nitrate and ammonium in these soil samples were extracted using DGT devices equipped with a Putolite A520E (for nitrate) and Microlite PrCH (for ammonium) binding layer. Ammonium DGT which determined the mobile and labile ammonium forms based on diffusion and the resupplies from the solid soil phase, only showed a significantly higher amount of extractable ammonium with NI compared to that without NI for some samples. However, significantly lower values were found for nitrate of treatments with NI compared to without NI after harvest. Thus, the lower nitrate amounts for treatments with NI compared to the treatments without NI after harvest indicated the delay of the nitrification process by the NI. Furthermore, we compared also the ammonium and nitrate
DGT results to chemical extraction with KCl solutions. The results demonstrated that the trends of DGT results and chemical extraction were complimentary through all the treatments.
Phosphorus (P) fertilizers from secondary resources became increasingly important in the last years. However, these novel P-fertilizers can also contain toxic pollutants. Chromium in its hexavalent state (Cr(VI)) is regulated with low limit values for agricultural products due to its high toxicity, but the determination of Cr(VI) in these novel fertilizer matrices can be hampered by redox processes that lead to false results. Thus, we applied the passive sampler technique Diffusive Gradients in Thin-films (DGT) for the determination of 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 in most cases 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) compounds which leads to overestimated Cr(VI) values. The results of certain types of P-fertilizers containing mobile Cr(III) or partly immobile Cr(VI), showed that optimization of the DGT method is required to avoid over- or underestimation of Cr(VI).
Das Jahr 2020 war vor allen Dingen von der Pandemie geprägt, die alle Bereiche des Lebens und Arbeitens beeinflusst hat und immer noch beeinflusst. Dies hat sich auch auf verschiedene Maßnahmen im Zusammenhang mit zugelassenen Produkten ausgewirkt. In diesem Zusammenhang sollen die Punkte kurz aufgeführt werden. Des Weiteren soll aufgezeigt werden, wie bei der Bearbeitung der Richtlinien, der Zulassungstätigkeit und Beurteilung der Produkte an der BAM und im Fachbeirat vorgegangen wird. Darüber hinaus soll noch einmal kurz auf die Entlassung aus der Nachsorgephase eingegangen werden. Am Ende sollen verschiedene aktuelle Fragestellungen des Fachbeirat aufgezeigt werden.
Several thousand PFAS are in circulation and the current challenge lies in detection of these compounds. Wheter environmental contamination occurs via industrial emission or direct PFAS exposure, as through the use of AFFF fire fighting foams. Wheter PFAS need to be detected in consumer products or agricultral soil, or wheter human and wildlife exposure to PFSA needs to be evaluated, suitable analytical methods are required to identifiy the target class within a hugh variety of matrices. At the same time it is critical to detect trace amounts of compounds within various matrices, we want to make sure that we consider very volatile and mobile species, simultaneously want to assure that we do not overlook less and insoluble compounds. We require methods that allow both single and multi target analysis and want to have an ideal overview with the help of sum parameters.
Here, we describe a fast and simple extraction method for the determination of per- and polyfluorinated alkyl substances (PFASs) utilizing extractable organic fluorine (EOF) sum parameter analysis and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) in soil samples. After extraction and separation of inorganic and organic fluorinated compounds, organically bound fluorinated compounds were indirectly determined via the molecular absorption of gallium mono-fluoride at 211.248 nm. The implementation of the decisions of the “Stockholm Convention on persistent organic pollutants” as well as the “Protocol on Persistent Organic Pollutants of the Convention on Long-Range Transboundary Air Pollution” of the UNECE include the reduction respectively the elimination of PFASs in the environment. Currently, regulations aim to target single compounds (mostly C8-PFAS). But the PFAS group includes over 4700 substances, which are potentially persistent and toxic, thus target analytical approaches are not suitable for a holistic approach investigating the PFAS pollutant situation. Furthermore, forbidden PFASs are substituted by short-chain PFASs, thus the number of unknow substances is steadily increasing. For this reason, sum parameter approaches are more suitable to investigate and assess the pollution situation as well as derive exposure limits. Our developed analytical method was successfully applied to determine PFASs in soil samples from a polluted site. In view of steadily increasing numbers of PFAS substances, our method will make an important contribution in assessing the pollution situation as well as support policy makers in deriving exposure limits for PFAS in the future.