Tire wear (TW) constitutes a significant source of microplastic in terrestrial ecosystems. It is known that particles emitted by roads can have an effect up to 100 m into adjacent areas. Here, we apply for the first-time thermal extraction desorption gas chromatography-mass spectrometry (TED-GC/MS) to determine TW in soil samples by detection of thermal decomposition products of styrene-butadiene rubber (SBR), without additional enrichment. Additionally, zinc contents were determined as an elemental marker for TW. Mixed soil samples were taken along three transects along a German motorway in 0.3, 2.0, and 5.0 m distance from the road. Sampling depths were 0-2, 2-5, 5-10, and 10-20 cm. Four fine fractions, 1 000-500, 500-100, 100-50, and <50 mikrom, were analyzed. TW contents based on SBR ranged from 155 to 15 898 mg kg-1. TW contents based on zinc were between 413 and 44 812 mg kg-1. Comparison of individual values of SBR and zinc reveals SBR as a more specific marker. Results confirm that most TW ends up in the topsoil within a 2 m distance. The sampling strategy resulted in representative data for a larger area. Standard deviations of quadruple TED-GC/MS determination of SBR were <10% for all grain size fractions. TED-GC/MS is a suitable analytical tool for determining TW in soil samples without the use of toxic chemicals, enrichment, or special sample preparation. © 2022 The Authors
Analysis of microplastic particles in environmental samples needs sophisticated techniques and is time intensive due to sample preparation and detection. Alternatives to the most common (micro-) spectroscopic techniques, Fourier transform infrared and Raman spectroscopy, are thermoanalytical methods, in which specific decomposition products can be analyzed as marker compounds for different kinds of plastic types and mass contents. Thermal extraction desorption gas chromatography-mass spectrometry allows the fast identification and quantification of MP in environmental samples without sample preparation. Whereas to date only the analysis of thermoplastic polymers has been realized, this is the first time that even the analysis of tire wear (TW) content in environmental samples has been possible. Various marker compounds for TW were identified. They include characteristic decomposition products of elastomers, antioxidants, and vulcanization agents. Advantages and drawbacks of these marker substances were evaluated. Environmental samples from street runoff were exemplarily investigated, and the results are presented. © 2018 American Chemical Society.
Drug therapy for diabetes mellitus has increased significantly in recent years. 1,1-Dimethylbiguanide hydrochloride (metformin) is the most common drug used for the treatment of diabetes. Metformin is not metabolized in the human body and enters the water cycle via sewage. A new gas chromatography-mass spectrometry (GC-MS) method has been developed which enables the quantification of metformin in surface water samples even at low concentrations in the ng L-1 range. A solid phase extraction (SPE) method for the preconcentration of metformin and the internal standard 1-butylbiguanide (buformin) was established, and the method parameters such as the composition and volume of the eluent were optimized. Derivatization of metformin and buformin was obtained by using n-methyl-bis (trifluoroacetamide) (MBTFA). The reaction conditions of the derivatization, such as the reaction temperature and volume of the derivatization agent, were evaluated. The limit of detection (LOD) and limit of quantification (LOQ) were determined to be 3.9 ng L-1 and 12 ng L-1 in surface water samples. Linearity was shown over a concentration range of 10-50 ng L-1. The good performance of the method was demonstrated by comparison with a liquid chromatography tandem mass spectrometry (LC-MS/MS) method. The results indicate that the GC-MS method is a reliable and sensitive alternative for the quantification of metformin in surface water. Quelle: http://pubs.rsc.org
Microplastics (MP) are ubiquitous throughout the environment as a result of an ongoing, increasing, but also lavish use, of plastics over time and its inherent persistence. In contrast, there are almost no data that allow drawing conclusions about the evolution of plastic pollution in the environment over the past decades. This study investigates the MP load in blue mussels from the North and Baltic Sea archived by the German Environmental Specimen Bank in a time series covering almost 30 years. Samples were enzymatically and chemically oxidative digested for MP extraction and subsequent analyzed mass-quantitatively for nine common polymer clusters by pyrolysis gas chromatography-mass spectrometry. Seven polymer clusters were detected in mussel tissue. Summed MP levels were at ppm levels (<20 ÎÌg/g mussel, dry weight). North Sea samples reflected a gradual increase from the 1980s/90s to the 2000s whereas those from Baltic Sea showed consistently higher, rather constant MP levels similar to the North Sea site later than 2000. Polymer composition of both sites stood out by cluster (C) of C-PVC and C-PET at both sites. Mussels from Baltic Sea site had larger C-PE and C-PP proportions. Opposed polymer- and site-specific trends indicated both regional and trans-regional MP sources for different polymer clusters. The MP composition of mussels showed strong similarities with adjacent sediment and water samples. The study introduces a relevant dataset addressing the temporal development of MP pollution. It emphasizes a high indicative potential of environmental MP composition/loads received by mussels but raises the necessity on adequate control materials accompany such kind of studies. © 2022 Elsevier
The formation potential of contaminants diffusing from cross-linked polyethylene (PE-X) pipes and their impact on the odour of drinking water was determined. Three types of PE-X material, Pe-Xa, PE-Xb and PE-Xc, were extensively assessed by performing migration tests following EN 1420 and EN 12873-1. Migration waters were analysed for their threshold odour number (TON). The same samples were investigated by two gas chromatography-mass spectrometry methods: screening and olfactometry. Most of the PE-X materials failed the German regulation of TON <2 for cold water and TON <4 for warm water. PE-Xb material caused the strongest odour and also released the highest amount of contaminants. Metilox, 7,9-di-tert-butyl-1-oxaspiro(4,5)deca-6,9-diene-2,8-dione, 3,5-di-tert-butyl-4-hydroxybenzaldehyde and 2,6-di-tert-butyl-p-benzoquinone (2,6-DtBQ) were the most often detected substances leaching from the tested plastic materials. However, no odour was perceived for most of these substances. Methyl tert-butyl ether (MtBE) and 2-tert-butylphenol are believed to contribute to the sensory problem in the migration water among other substances such as tert-amyl methyl ether, 2,2,2,5-tetramethyltetrahydrofuran, toluene or xylene. In total ten specific descriptions characterized the odour of the individual contaminants: ethereal, fresh, solvent, sweet, fruity, floral, unsavoury, pungent, aromatic and chemical. Quelle: https://www.sciencedirect.com
The scientific and practical challenge of detecting microplastics (MPs) in the environment in a targeted and rapid manner is solved by innovative coupling of thermogravimetric analysis with mass spectrometric methods. Fast identification and quantitative determination of most thermoplastic polymers and elastomers is possible by using thermal extraction desorption gas chromatography-mass spectrometry (TED-GC-MS). © Authors
Das Projekt "Protocol for the evaluation of residues in industrial contaminated liquid effluents" wird vom Umweltbundesamt gefördert und von Fraunhofer-Institut für Toxikologie und Aerosolforschung durchgeführt. Objective: To perform the chemical analysis of compounds which are present in industrial effluents and important for their persistency, bio accumulative potential, toxicological and ecotoxicological activity. General Information: The project includes a global analysis on the samples followed by fractionation of the organic compounds into groups of different polarity by extraction at different pH's and with different materials and by further fractionation by HPLC, using for the analysis a series of powerful techniques, including LC-MS, GC-MS and NMR; a simple and cost-effective ecotoxicological characterisation of the samples and their fractions, using the most appropriate of a series of rapid screening tests, such as Microtox and the Daphnia Inhibitory Quotient (IQ) will be made. The project consists of three main tasks: -A multiple ecotoxicological approach for industrial effluents hazard evaluation. -Characterisation of the chemical composition of the effluent, and integration with the data from the first task. -Validation of the developed protocol. To develop and assess this general protocol and the individual elements of the approach, at least three authentic situations will be considered and liquid effluents of industrial origin will be studied. In particular, industries with different production and leachate from industrial wastes will be considered. Prime Contractor: Instituto di Richerche Farmacologiche Mario Negri; Milano; Italy.
Das Projekt "Flood risk in a changing climate (CEDIM)" wird vom Umweltbundesamt gefördert und von Karlsruher Institut für Technologie (KIT), Institut für Meteorologie und Klimaforschung, Department Troposphärenforschung durchgeführt. Aims: Floods in small and medium-sized river catchments have often been a focus of attention in the past. In contrast to large rivers like the Rhine, the Elbe or the Danube, discharge can increase very rapidly in such catchments; we are thus confronted with a high damage potential combined with almost no time for advance warning. Since the heavy precipitation events causing such floods are often spatially very limited, they are difficult to forecast; long-term provision is therefore an important task, which makes it necessary to identify vulnerable regions and to develop prevention measures. For that purpose, one needs to know how the frequency and the intensity of floods will develop in the future, especially in the near future, i.e. the next few decades. Besides providing such prognoses, an important goal of this project was also to quantify their uncertainty. Method: These questions were studied by a team of meteorologists and hydrologists from KIT and GFZ. They simulated the natural chain 'large-scale weather - regional precipitation - catchment discharge' by a model chain 'global climate model (GCM) - regional climate model (RCM) - hydrological model (HM)'. As a novel feature, we performed so-called ensemble simulations in order to estimate the range of possible results, i.e. the uncertainty: we used two GCMs with different realizations, two RCMs and three HMs. The ensemble method, which is quite standard in physics, engineering and recently also in weather forecasting has hitherto rarely been used in regional climate modeling due to the very high computational demands. In our study, the demand was even higher due to the high spatial resolution (7 km by 7 km) we used; presently, regional studies use considerably larger grid boxes of about 100 km2. However, our study shows that a high resolution is necessary for a realistic simulation of the small-scale rainfall patterns and intensities. This combination of high resolution and an ensemble using results from global, regional and hydrological models is unique. Results: By way of example, we considered the low-mountain range rivers Mulde and Ruhr and the more alpine Ammer river in this study, all of which had severe flood events in the past. Our study confirms that heavy precipitation events will occur more frequently in the future. Does this also entail an increased flood risk? Our results indicate that in any case, the risk will not decrease. However, each catchment reacts differently, and different models may produce different precipitation and runoff regimes, emphasizing the need of ensemble studies. A statistically significant increase of floods is expected for the river Ruhr in winter and in summer. For the river Mulde, we observe a slight increase of floods during summer and autumn, and for the river Ammer a slight decrease in summer and a slight increase in winter.
Das Projekt "Rahmenprojekt 1 - Teil B: Erfassung der Beschaffenheit von Roh- und Trinkwässern - Teil B" wird vom Umweltbundesamt gefördert und von ESWE-Institut für Wasserforschung und Wassertechnologie durchgeführt. Für eine fachgerechte wissenschaftliche Beurteilung einer Trinkwasseraufbereitung ist die Kenntnis der Roh- und Trinkwasserbeschaffenheit zwingend erforderlich. Ziel dieses Teilprojektes ist es, hierfür analytische Untersuchungen durchzuführen unter besonderer Berücksichtigung gesundheitsgefährdender Stoffe, die eine toxikologische oder endokrine Wirkung besitzen. Neben einer spezifischen Einzelstoffanalytik sollen aber auch Summen- und Gruppenparameter zur Charakterisierung der Wasserbeschaffenheit herangezogen werden, um einen möglichst vollständigen Überblick zu erhalten. 1. Auswertung vorhandener Analysenergebnisse, die im Rahmen des Teils A erfragt werden. 2. Überprüfung einzelner Parameter, insbesondere bei unplausiblen Daten. 3. Erstellung einer problemorientierten Liste abhängig von Land, Rohwasserart und Einzugsgebiet, wobei drei wesentliche Belastungsquellen berücksichtigt werden: Industrie, Landwirtschaft und menschliche Aktivitäten. 4. Durchführung von analytischen Untersuchungen nach adäquater Probenahme, und -Vorbereitung mittels u.a. GC/MS und HPLC/MS(MS). Die resultierenden Ergebnisse finden Verwertung im Rahmenprojekt Teil A und den Kernprojekten A bis D.
Das Projekt "Teil ICT" wird vom Umweltbundesamt gefördert und von Fraunhofer-Institut für Chemische Technologie durchgeführt. Ziel des Vorhabens ist es, das elektrochemische Verhalten von Vergällungsmitteln und ihren Einfluss auf die anodische Oxidation von Bioethanol zu untersuchen. Auf der Basis der Untersuchungen sollen Vergällungsmittel ausgewählt werden, die die Leistung einer Direkt-Ethanol-Brennstoffzelle nicht beeinflussen. Hiefür soll eine Auswahl von Vergällungsmitteln auf ihre elektrochemischen Eigenschaften an gängigen Elektrodenmaterialien untersucht werden. Dabei kommen eine Reihe von Methoden wie z.B. CV, DEMS, HPLC und GC-MS zum Einsatz. Ziel ist festzustellen ob die Vergällungsmittel umgesetzt werden, ob sie vergiftende Absorbate bilden und welche Produkte entstehen. Anhand der Ergebnisse sollen geeignete Vergällungsmittel ausgewählt werden. Das wesentliche Verwertungsziel ist die Vermarktung von Biobrennspiritus zum Einsatz in Brennstoffzellen durch die Südzucker. Die Bestimmung geeigneter Vergällungsmittel ist ein wichtiger Schritt, dem sich eine Standardisierung anschließen sollte. Seitens des ICTs ist ferner geplant durch die Veröffentlichung der Ergebnisse weitere Projekte im Bereich biogener Brennstoffe für Brennstoffzellen zu akquirieren.
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