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Eingeladener Vortrag
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Determination of elemental mass fractions in sediments plays a major role in evaluating the environmental status of aquatic ecosystems. Herewith, the optimization of a new total digestion protocol and the subsequent analysis of 48 elements in different sediment reference materials (NIST SRM 2702, GBW 07313, GBW 07311 and JMC-2) based on ICP-MS/MS detection is presented. The developed method applies microwave acid digestion and utilizes HBF4 as fluoride source for silicate decomposition. Similar to established protocols based on HF, HBF4 ensures the dissolution of the silicate matrix, as well as other refractory oxides. As HBF4 is not acutely toxic; no special precautions have to be made and digests can be directly measured via ICP-MS without specific sample inlet systems, evaporation steps or the addition of e.g. H3BO3, in order to mask excess HF. Different acid mixtures with and without HBF4 were evaluated in terms of digestion efficiency based on the trace metal recovery. The optimized protocol (5 mL HNO3, 2 mL HCL, 1 mL HBF4) allows a complete dissolution of the analyzed reference materials, as well as quantitative recoveries for a wide variety of certified analytes. Low recoveries for e.g. Sr, Ba and rare earth elements due to fluoride precipitation of HF-based digestions protocols, can be avoided by the usage of HBF4 instead. Based on the usage of high purity HBF4 all relevant trace, as well as matrix elements can be analyzed with sufficiently low LOQs (0.002 μg L−1 for U up to 6.7 μg L−1 for Al). In total, 34 elements were within a recovery range of 80%–120% for all three analyzed reference materials GBW 07313, GBW 07311 and JMC-2. 14 elements were outside a recovery range of 80%–120% for at least one of the analyzed reference materials.
The development of offshore wind turbines (WTGs) presents many challenges in terms of safe operation over extended periods of time. One of these is the corrosive environment towards metallic materials, which can lead to a loss of material thickness and thus to a deterioration of mechanical performances, especially the strength of infrastructures. This can be counteracted by painting and cathodic protection (CP). Much research has already been done in this area about inhibiting the corrosion process. However, gaps exist regarding free corrosion. This plays a greater role especially for time intervals during the installation of the systems and their maintenance, during which often no CP can be operated. This is especially true for areas where painting surfaces is impossible e.g., sediment areas. This problem is exacerbated by the different corrosion rates caused by the different zones (water and sediment), with their different amounts of dissolved oxygen.
This presentation deals with experiments in artificial seawater and sediment. Classical S355J2 steel samples in the form of coupons were fitted with welding wires that carried out the electrical contact to the outer side of the basin. Inside the basins, the specimens are stored in different zones like water and sediment which should simulate the foundation situation of monopiles. The mass loss was determined gravimetrically, elemental currents between specimens in water and sediment were measured and electrochemical investigations were carried out. The influences of the zones, based on different solved oxygen contents, and the rolling skin towards the corrosion behavior of the mild steel samples were determined in this work. Especially the influence of the sediment showed unexpected behavior, determined by electrochemical investigations. These results allow better conclusions to be drawn about the corrosion behavior of low alloy steels in offshore environments used in sediment and seawater, which cannot always be protected.
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.
Organotin compounds (OTCs) have been widely used in anti-fouling paints, pesticide formulations, and as stabilizers in polyvinyl chloride over the past century. In marine ecosystems, OTCs can cause severe damage to biodiversity, leading up to the extinction of vulnerable species. Due to the extensive use of tributyltin (TBT) as a biocide on ship hulls, it has been considered one of the most hazardous substances intentionally introduced into the aquatic environment. This resulted in a global ban on TBT-containing products in the 2000s. However, recent studies indicate the emerging presence of organotin pollutants.
OTCs are known to persist and accumulate in marine sediments, posing a long-term threat to the environment. These harmful substances can be set free and dispersed even after several decades. Therefore, analyzing sediment probes is imperative for a thorough monitoring of pollution. However, species-specific analysis of OTCs at required concentration levels in complex environmental matrices remains challenging. Chromatographic systems are commonly used for their analysis, but the required sample preparation is time-consuming and prone to contamination and analyte loss. The coupling of electrothermal vaporization and inductively coupled plasma-mass spectrometry (ETV/ICP-MS) demonstrates high potential as a rapid, convenient, and chemical-saving scanning tool for environmental samples.
This method enables the direct on-line fractionation of organic compounds from an inorganic fraction and provides element-specific detection at ultra-trace levels without complex sample preparation. Since OTCs are generally more toxic than ionic or elemental tin, analyzing them as a sum parameter is advantageous. Additionally, the determination of both organic and inorganic tin, rather than just organic tin, reveals valuable information about the fate of OTCs. The main challenge in obtaining accurate quantitative data using direct solid sampling techniques like as ETV/ICP-MS is applying a suitable calibration strategy. Our isotope dilution approach overcomes matrix effects in ETV/ICP-MS analysis and is compatible with commercial systems.
A method for the determination of the novel brominated flame retardant tetrabromobisphenol A bis(2,3-dibromopropylether), 1,1'-(isopropylidene)bis[3,5-dibromo-4-(2,3-dibromo-propoxy)-benzene] (TBBPA-dbpe), was developed. Technical TBBPA-dbpe was purified and the results of a thorough physical characterisation are reported. The application of APCI-MS is discussed and the fragmentation patterns are described. Quantification of TBBPA-dbpe was done by HPLC-DAD using external calibration. The validation of the method was accomplished using sediment and sewage sludge samples spiked with defined amounts of authentic TBBPA-dbpe. The average recovery rates of TBBPA-dbpe from spiked samples ranged from 35 to 91% (sediment) and from 57 to 98% (sewage sludge) depending on the respective extraction method. Pressurised fluid extraction (PFE) and fluidised bed extraction were superior to classical Soxhlet and sonication procedures and yielded recovery rates between 90 and 98% with relative standard deviations of 2%. The limits of detection (DTC), identification (ID) and determination (DTM) using HPLC-DAD were 10, 21 and 30 ng g-1 in sediment and 22, 44 and 72 ng g-1 in sewage sludge, respectively.
To combat climate change the share of renewable energy production must increase drastically. Offshore energy production – offshore wind and power-to-X – are crucial to achieving climate targets. However, the impact of these offshore constructions – wind turbines and production platforms – on the marine environment remains unclear in many aspects. Potential sources of chemical emissions are corrosion protection systems, remobilization of contaminants from old sediments during construction, the brine of desalination plants and increased shipping for maintenance and transportation. In order to minimize the environmental impact of renewable energies, close monitoring is essential. The goal of this project is the development of a monitoring concept for an offshore power-to-X production platform.
The pollution of marine, limnic and terrestrial environments with plastic waste and the potential impact especially on biota and humans has received increasing attention in recent years. Special focus is on particles smaller than 5 mm, the so-called microplastics. Consequently, possible regulations of emission and remediation efforts require sound information on the occurrence and fate of microplastics in the respective environmental compartments.
Microplastics (MP) differ from classical organic pollutants in biota or the environment in that they do not consist of clearly defined low-molecular weight compounds but of polymer particulates with varying sizes and chemical compositions. This leads to specific challenges regarding the analytical techniques to be employed for their identification and quantification.
Microplastics are defined as polymer particle in the size range between 1 µm and 5 mm and cover a wide range of polymers such as polyethylene, polypropylene, polystyrene and polyethylene terephthalate in variable geometric shapes. Properties relevant for environmental microplastics are polymer type, particle form and size distribution, surface morphology (aging status) and total mass fraction contained in a given sample. Polymer identification and particle size estimation using optical methods (IR and Raman spectroscopy) are time consuming and complicated by surface characteristics as a result of weathering, soiling, and microbial colonisation. Total mass fractions of MP in environmental samples can be determined by thermo-analytical methods.
There are currently no standardised methods for sampling, sampling preparation, or detection of MP in environmental samples. So far, qualitative and quantitative investigations are done by research institutes and have not reached the routine laboratory community. The near future will see harmonisation efforts of MP mass fraction determination in environmental matrices by thermo-analytical procedures.
The immediate need for reference materials during method development and comparison is outlined with regard to relevant matrix/polymer compositions, existing regulations and currently achievable detection limits. Examples for solid environmental matrix reference materials are discussed regarding the challenges encountered with matrices and polymer types as well as homogeneity testing and property value characterisation.
Das Ziel des Verbundforschungsvorhabens KKS-Gründung war die Entwicklung eines Monitoringsystems zur Erfassung von Korrosion an Gründungsstrukturen im Labormaßstab. Dafür war eine umfassende Bewertung und Beschreibung korrosionsbeeinflussender Faktoren und der Korrosionssysteme notwendig. Im Vorhaben KKS-Gründung wurde die Gründungsstruktur unterhalb der Wasserlinie betrachtet bis hin zum anaeroben Bereich im Sediment. Insbesondere der Sedimentbereich wurde bisher nur unzureichend betrachtet. Da die komplexen Mechanismen in der Sedimentzone noch nicht ausreichend wissenschaftlich untersucht wurden, mussten Möglichkeiten entwickelt werden, um diese zu bewerten.
Im Verbundforschungsvorhaben KKS-Gründung agierte die Bundesanstalt für Materialforschung und -prüfung (BAM) als Forschungsstelle. Die Hauptziele des Teilvorhabens der BAM waren die Bereitstellung einer Messumgebung für das von den Partnern entwickelte Monitoringsystem, die umfassende wissenschaftliche Beschreibung der Korrosionssysteme im Unterwasserbereich und Sediment sowie die Gewinnung von Messdaten zur Verifizierung und Überführung in die Simulation. Als Forschungsstelle war die BAM der Ansprechpartner für die Verbundpartner bei wissenschaftlichen Fragestellungen.
Die Hauptziele des Vorhabens wurden erreicht und es wurden grundlegende Erkenntnisse zum Korrosionsverhalten von Offshore-Stahl im Unterwasser und Sedimentbereich gewonnen. Darüber hinaus wurden wichtige Erkenntnisse zum Betrieb eines Laborcontainers und zur Nachstellung von Korrosionssystemen in Meerwasserbecken bei Verwendung von künstlichem Meerwasser und Sand als Sediment gewonnen. Eine Beschreibung und Bewertung der Korrosivität und ablaufender Reaktionen in den einzelnen Belastungszonen wurde mittels elektrochemischer und gravimetrischer Verfahren vorgenommen.