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Mikroplastik findet sich in Ozeanen, Seen, Flüssen und Bächen. Es kann in unserem Boden, in der Luft und sogar in Organismen nachgewiesen werden. Jedes Jahr werden weltweit Millionen Tonnen freigesetzt. Doch wo und wie landet Mikroplastik in der Umwelt? Und wie können wir diese winzigen Partikel nachweisen?
The latest ICP-MS technology - ICP-ToF (time of flight)-MS – enables the analysis of the multi-element fingerprint of individual cells. The interface between material and environmental analysis thus receives special attention, e.g., when considering corrosion processes. Microbiologically influenced corrosion (MIC) is a highly unpredictable phenomenon due to the influence of the environment, microbial communities involved and the respective electron source. However, the interaction pathway between cells and the metal surface remains unclear. The development of the MIC-specific ICP-ToF-MS analytical method presented here at the single cell level, in combination with the investigation of steel-MIC interactions, contributes significantly to progress in instrumental MIC analysis and will enable clarification of the processes taking place. For this, a MIC-specific staining procedure was developed. It allows the analysis of archaea at a single cell level and provides information about the interaction of the cells with the staining agent which is extremely scarce compared to other well characterized organisms. Additionally, the single cell ICP-ToF-MS is used for the analysis of archaea involved in MIC of steel. Hence, the possible uptake of individual elements from different steel samples is investigated - the information obtained will be used in the future to elucidate underlying mechanisms and develop possible material protection concepts, thus combining modern methods of analytical sciences with materials.
ICP-ToF (time of flight) MS enables the analysis of the multi-element fingerprint of single cells. The single cell ICP-ToF-MS is used in the presented poster for the analysis of archaea involved in microbiologically influenced corrosion (MIC) of steel. By means of sc-ICP-ToF-MS, the possible uptake of individual elements from the respective steel is investigated - the information obtained will be used in the future to elucidate underlying mechanisms and develop possible material protection concepts. The work combines modern methods of analytical sciences with materials.
Using nanofiber-like cell appendages, secreted proteins and sugars, bacteria can establish initial surface contact followed by irreversible adhesion and the formation of multicellular biofilms, often with enhanced resistance towards antimicrobial treatment and established cleaning procedures. On e.g. medical implants, in water supply networks or food-processing industry, biofilms can be a fertile source of bacterial pathogens and are repeatedly associated with persisting, nosocomial and foodborne infections. Nowadays, the emergence of resistances because of extensive usage of antibiotics and biocides in medicine, agriculture and private households have become one of the most important medical challenges with considerable economic consequences. In addition, aggravated biofilm eradication and prolonged cell-surface interaction can lead to increased biodeterioration and undesired modification of industrial and medical surface materials. Various strategies are currently developed, tested, and improved to realize anti-bacterial surface properties through surface functionalization steps avoiding antibiotics.
In this study, contact-less and aseptic large-area short or ultrashort laser processing is employed to generate different surface structures in the nanometer- to micrometer-scale on technical materials such as titanium-alloy and polyethylene terephthalate (PET). The laser processed surfaces were subjected to bacterial colonization studies with Escherichia coli test strains and analyzed with reflected-light and epi-fluorescence microscopy. Depending on the investigated surfaces, different bacterial adhesion patterns were found, ranging from bacterial-repellent to bacterial-attractant effects. The results suggest an influence of size, shape and cell appendages of the bacteria and – above all – the laser-processed nanostructure of the surface itself, emphasizing the potential of laser-processing as a versatile tool to control bacterial surface adhesion.
Monitoring von Mikroplastik
(2021)
Inter-pulse accumulation of heat could affect the chemical and morphological properties of the laser processed material surface. Hence, the laser pulse repetition rate may restrict the processing parameters for specific laser-induced surface structures. In this study, the evolution of various types of laser-induced micro- and nanostructures at various laser fluence levels, effective number of pulses and at different pulse repetition rates (1 – 400 kHz) are studied for common metals/alloys (e.g. steel or titanium alloy) irradiated by near-infrared ultrashort laser pulses (925 fs, 1030 nm) in air environment. The processed surfaces were characterized by optical and scanning electron microscopy (OM, SEM), energy dispersive X-ray spectroscopy (EDX) as well as time of flight secondary ion mass spectrometry (TOF-SIMS). The results show that not only the surface morphology could change at different laser pulse repetition rates and comparable laser fluence levels and effective number of pulses, but also the surface chemistry is altered. Consequences for medical applications are outlined.
Bacterial biofilms are multicellular communities adhering to surfaces and embedded in a self-produced extracellular matrix. Due to physiological adaptations and the protective biofilm matrix itself, biofilm cells show enhanced resistance towards antimicrobial treatment. In medical and industrial settings, biofilms on e.g. for implants or for surfaces in food-processing industry can be a fertile source of bacterial pathogens and are repeatedly associated with persisting, nosocomial and foodborne infections. As extensive usage of antibiotics and biocides can lead to the emergence of resistances, various strategies are currently developed, tested and improved to realize anti-bacterial surface properties through surface functionalization steps avoiding antibiotics. In this study, contact-less and aseptic large-area ultrashort laser scan processing is employed to generate different surface structures in the nanometer- to micrometer-scale on technical materials, i.e. titanium-alloy, steel, and polymer. The processed surfaces were characterized by optical and scanning electron microscopy and subjected to bacterial colonization studies with Escherichia coli test strains. For each material, biofilm results of the fs-laser treated surfaces are compared to that obtained on polished (non-irradiated) surfaces as a reference. Depending on the investigated surfaces, different bacterial adhesion patterns were found, suggesting an influence of geometrical size, shape and cell appendages of the bacteria and – above all – the laser-processed nanostructure of the surface itself.
In diesem Beitrag wird der Einfluss des Aktivkohleprodukts auf die Adsorption von Spurenstoffen aus Kläranlagenablauf gezeigt und diskutiert. Im zweiten Teil wird das Material Aktivkohle analytisch charakterisiert und die Eigenschaften systematisiert. Die gewonnenen Erkenntnisse werden mit Bezug zu Praxislösungen zusammengefasst.
As global demand for polymer products increases, so does the potential amount of leakage into the environment, known as macroplastic (> 1,000 µm) and microplastic particles (MP, 1 - 1,000 µm). To date, the environmental and health consequences are unclear and unpredictable, so robust MP monitoring data are needed to identify the sources, pathways and fate of these particles. Therefore, we developed the thermoanalytical method TED-GC/MS (thermal extraction desorption - gas chromatography/mass spectrometry), which uses polymer-specific thermal decomposition products for the detection of MP in environmental samples. It allows fast identification and the determination of MP mass contents, which is crucial for assessing of their potential effects and thus for legislation and monitoring.
For a better understanding of the TED-GC/MS, this presentation will provide the first methodological insights into systematic assessments of TED-GC/MS performance for MP detection in different environmental model matrices. Results of MP determination from real samples will underline the presentation and aspects of practical application will be addressed.
To harmonise the method, it is essential to assess different analytical performance parameters (e.g. recovery, signal quality or limit of detection, LOD) to ensure comparability of data. For this purpose, standard addition of different aquatic (e.g. suspended particulate matter, limnic sediment, activated sludge) and terrestrial samples (e.g. agricultural soil) were performed with non-biodegradable standard polymers (polyethylene, PE; polyethylene terephthalate, PET; polypropylene, PP; polymethyl methacrylate, PMMA; polystyrene, PS; styrene-butadiene rubber, SBR) as well as biodegradable polymers (polybutylene adipate terephthalate PBAT; polylactide, PLA) and analysed by TED-GC/MS. These results were then compared with the measurements of the neat polymers without matrix.
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).
Der Vortrag wurde im Rahmen der Abschlusskonferenz des Forschungsschwerpunktes "Plastik in der Umwelt" des BMBF gehalten. Er fasst die Ergebnisse des Verbundprojektes RUSEKU zusammen. Es wurde die Herstellung verschiedener Testmaterialien für die Mikroplastik (MP) Analytik beschrieben. Im weiteren geht es um verschiedene Ansätze MP kostengünstig und schnell zu detektieren, z.B. mit Nahinfrarotspektroskopie. Nanoplastik konnte mit der Transmissionselektronenmikroskopie sichtbar gemacht werden. Für die praxisnahe Beprobung von Gewässern wurde die Fraktionierte Filtration entwickelt. Integrale Beprobungen können mit dem Sedimentationskasten erfolgen. Als Beispiele für die Beprobung realer Gewässer wurde das urbane Abwassersystem Kaiserslautern, Getränkewasser und Waschmaschinenwasser gezeigt.
In this study, nanoscopic particles of magnesium Fluoride (MgF2) and calcium fluoride (CaF2) also known as nano metal fluorides (NMFs), were evaluated for their potential to improve wood durability. Even though these fluorides are sparingly soluble, their synthesis in the form of nano-sized particles turns them into promising candidates for wood preservation. Their distinct property of low-water solubility is proposed to maintain long-lasting protection of treated wood by reducing the leaching of fluoride. Analytical methods were used to characterize the synthesized NMFs and their distribution in treated wood specimens. Transmission electron microscopy images showed that these fluoride particles are smaller than 10 nm. In nano metal fluoride (NMF) treated specimens, aggregates of these particles are uniformly distributed in the wood matrix as confirmed with scanning electron microscopy images and their corresponding energy-dispersive X-ray spectroscopy maps. The fluoride aggregates form a protective layer around the tracheid walls and block the bordered pits, thus reducing the possible flow path for water absorption into wood. This is reflected in the reduced swelling and increased hydrophobicity of wood treated with NMFs. The biocidal efficacy of NMFs was tested against brown-rot fungi (Coniophora puteanaand Rhodonia placenta), white-rot fungus (Trametes versicolor), and termites (Coptotermes formosanus). The fungal and termite tests were performed in accordance with the EN 113 (1996) and EN 117 (2012) standards, respectively. Prior to fungal tests, the NMF treated wood specimens were leached according to the EN 84 (1997)standard. Compared to untreated specimens, the NMF treated wood specimens have a higher resistance to decay caused by brown-rot fungi, white-rot fungus, and termites. Although all NMF treatments in wood reduce the mass loss caused by fungal decay, only the combined treatment of MgF2 and CaF2 has efficacy against both brown-rot fungi and white-rot fungus. Similarly, wood treated with the combined NMF formulation is the least susceptible to attack by C. formosanus.It is proposed that combining MgF2 and CaF2changes their overall solubility to promote the release of fluoride ions at the optimal concentration needed for biocidal efficacy against fungi and termites. In this thesis, it was proven that even after leaching, sufficient fluoride was present to protect NMF treated wood from fungal decay. This shows that NMFs are robust enough for above ground contact outdoor applications of wood, where permanent wetness cannot be avoided according to Use Class 3.2, as per the EN 335 (2013) standard. Also, they pose a low risk to human health and the environment because they are sparingly soluble. Since NMFs significantly reduce the decay of wood, the CO2 fixed in it will be retained for longer than in unpreserved wood. Overall, the novel results of this study show the potential of NMFs to increase the service life of building materials made from non-durable wood.
Up to now, different analytical methods for single cell analysis exist focusing on key features such as size, shape, morphology and elemental composition. The combination of the latest ICP-MS techniques - ICP-ToF-MS - together with the latest developments in the field of sample delivery - micro droplet generator (MDG) – will allow a Deep insight into the composition and size of cells.
Microbiologically influenced corrosion (MIC) is an oxidation of metals affected by the presence or activity (or both) of microorganisms e.g. Shewanella Putrefaciens in biofilms on the surface of the corroding material. As this can happen for example in the soil on iron pipes of water pipes, in oil tanks or on steel sheet piling, there is great interest in MIC research, not only from various industrial sectors, but also from the environmental aspect.
Bei der Behandlung von Krebs mittels Strahlentherapie sollen Tumorzellen abgetötet werden ohne das umliegende gesunde Gewebe zu zerstören. Um Strahlentherapien für Patienten verträglicher zu machen, ist ein besseres Verständnis der zugrundeliegenden Prozesse auf der molekularen Ebene nötig. Dabei sind der Energieeintrag und die Streuprozesse der Strahlung in der Umgebung der DNA von besonderem Interesse. Durch Streuung von hochenergetischer Strahlung in Wasser werden besonders viele Sekundärelektronen mit niedriger Energie erzeugt. Zur Untersuchung der Schädigungseffizienz dieser Elektronen wurde ein Verfahren zur direkten Bestrahlung von Lösungen mittels Elektronen variabler Energien enwtickelt. Dies wurde durch einen neu entwickelten Probenhalter mit einer für Elektronen durchlässigen Nanomembran ermöglicht. Mit diesem können Bestrahlungen an DNA, Proteinen, und Zellen bei verschiedenen pH-Werten oder Salzkonzentrationen durchgeführt werden. Parallel dazu wurde der ortsabhängige Energieeintrag innerhalb des Wassers durch Elektronenstreusimulationen bestimmt. Diese neuartige Kombination von Experiment und Simulation ermöglicht die Bestimmung der Schaden-Dosis-Relation für Elektronenbestrahlung von biologischen Systemen unter realistischen physiologischen Bedingungen. So konnten für die genutzten Primärelektronen wie die mittlere letale Dosis, bei der 50 Prozent der DNA geschädigt sind, mit 1,7 Gy bestimmt. Ebenfalls wurde das für mikrodosimetrische Modellierungen und Betrachtungen der sogenannten Linear energy transfer (LET) Effekte, wichtige Verhältnis von DNA Einzelstrangbrüchen (SSB) zu Doppelstrangbrüchen (DSB) als SSB/DSB = 12/1 bestimmt. Mit Hilfe eines Modells für das Targetvolumen der DNA wurde der mittlere mikroskopische letale Energieeintrag berechnet als E1/2 = 6 ± 4 eV . Es wurde gefolgert, dass weniger als zwei Ionisationsprozesse im sensitiven Targetvolumen der DNA im Mittel zu einem Einzelstrangbruch führen. Diese Methode ist unabhängig von den Primärpartikel und geometrischen Bedingungen. Deshalb ermöglicht sie die Vergleichbarkeit experimenteller Systeme mit inhomogenen Energieverteilungen, welches sonst nicht gegeben ist. Des weiteren wurden die Strahlenschutzfunktionen des Zellschutzmoleküls Ectoines und sein Einfluss auf Wasser und Biomoleküle untersucht. Seine Schutzfunktion gegen ionisierende Strahlung wurde auf die Erhöhung des Streuquerschnitts niederenergetischer Elektronen und seine Eigenschaft als OH-Radikalfänger zurückgeführt. Aufbauend auf unseren Erkenntnissen finden in klinischen Arbeitsgruppen Untersuchungen zu Einsatzmöglichkeiten im Umfeld der Strahlentherapie statt.
Projektkennung Deutsche Forschungsgemeinschaft (DFG) - Projektnummer 245767821
Development and characterization of starch film and the incorporation of silver nanoparticles
(2020)
Starch is one of the biopolymers being used for bioplastic synthesis. For production, starch can be combined with different plasticizers, starches from different plant sources and even with nanomaterials to improve or to add film properties. The challenge of adding these, e.g. in the form of silver nanoparticles (AgNp) is to determine the concentration so as to avoid impairing the properties of the film, agglomeration or altering the visual characteristics of the film. In this study, a starch film synthesis route and the incorporation of silver nanoparticles has been proposed in order not to alter the properties of the film while maintaining the transparency and a clear colour of the starch film. The results showed that the proposed synthesis route is promising, efficient, reproducible, fast and the film has good mechanical properties.
This is the repository of all experimental raw data used in the Scientific Reports publication "Specific adsorption sites and conditions derived by thermal decomposition of activated carbons and adsorbed carbamazepine" by Daniel Dittmann, Paul Eisentraut, Caroline Goedecke, Yosri Wiesner, Martin Jekel, Aki Sebastian Ruhl, and Ulrike Braun.
It includes
- overview_measurements.xlsx and overview_measurements.ods containing a list of all TGA experiments (TGA, TGA-FTIR, TED-GC-MS, and ramp-kinetics)
- TED-GC-MS.zip containing gas chromatography-mass spectrometry experimtent files for the Chemstation and OpenChrom
- TGA.zip containing thermogravimetric analyses raw data on evolved gas analyses experiments (TGA-FTIR and TED-GC-MS)
- TGA_kinetics.zip containing thermogravimetric analyses raw data on decomposition kinetic experiments (ramp-kinetics)
- TGA-FTIR.zip containing Fourier-transform infrared spectroscopy series files for OMNIC
- XRF.zip containing x-ray flourescence data on elemental composition
Development and characterization of starch film and the incorporation of silver nanoparticles
(2020)
Starch is one of the biopolymers being used for bioplastic synthesis. For production, starch can be combined with different plasticizers, starches from different plant sources and even with nanomaterials to improve or to add film properties. The challenge of adding these, e.g. in the form of silver nanoparticles (AgNp) is to determine the concentration so as to avoid impairing the properties of the film, agglomeration or altering the visual characteristics of the film. In this study, a starch film synthesis route and the incorporation of silver nanoparticles has been proposed in order not to alter the properties of the film while maintaining the transparency and a clear colour of the starch film. The results showed that the proposed synthesis route is promising, efficient, reproducible, fast and the film has good mechanical properties.
There is growing interest in quantifying microplastics in environmental samples. This application note presents a thermal extraction desorption-gas chromatography/mass spectrometry (TED-GC/MS) method that is well suited to automation and increased sample throughput. The method is also able to detect all particle sizes in the sample as long as the limit of detection (LOD) is reached and allows analysis of larger samples of 15 to 25 mg or more. Samples were decomposed by thermogravimetric analysis (TGA), and the gaseous decomposition products were trapped on a solid-phase sorbent, followed by thermal desorption‑gas chromatography/mass spectrometry (TD-GC/MS) using an Agilent 5977B GC/MSD coupled to an Agilent 7890B GC. Target microplastic particle (MP) polymers were identified in environmental samples including surface water, finished compost, house dust, and drinking water. Quantification of MP polymers in environmental samples provided LODs of 0.06 to 2.2 μg, allowing the detection of MPs in trace amounts with sample weights of up to 1 g. Method repeatability was adequate for reliable quantification with RSDs of approximately 6 to 12%.
Fluorides are well-known as wood preservatives. One of the limitations of fluoride-based wood preservatives is their high leachability. Alternative to current fluoride salts such as NaF used in wood protection are low water-soluble fluorides. However, impregnation of low water-soluble fluorides into wood poses a challenge. To address this challenge, low water-soluble fluorides like calcium fluoride (CaF2) and magnesium fluoride (MgF2) were synthesized as nanoparticles via the fluorolytic sol−gel synthesis and then impregnated into wood specimens. In this study, the toxicity of nano metal fluorides was assessed by termite mortality, mass loss and visual analysis of treated specimens after eight weeks of exposure to termites, Coptotermes formosanus. Nano metal fluorides with sol concentrations of 0.5 M and higher were found to be effective against termites resulting in 100% termite mortality and significantly inhibited termite feeding. Among the formulations tested, the least damage was found for specimens treated with combinations of CaF2 and MgF2 with an average mass loss less than 1% and visual rating of “1”. These results demonstrate the efficacy of low water-soluble nano metal fluorides to protect wood from termite attack.
Eine umfangreich ausgestaltete Trinkwasseraufbereitung als Multibarrieren-System ist notwendig, wenn das Rohwasser direkt aus Fließgewässern entnommen wird (z. B. für das Mülheimer Verfahren). Eine der Barrieren wird, als gezielte Behandlungs- oder Sicherheitsstufe, oft als Filter mit granulierter Aktivkohle (GAK-Filter) realisiert. Ihre Standzeit kann bei geringer Wasserbelastung (DOC < 2 mg/L), z. B. bei der Landeswasserversorgung Langenau, bis zu 5 Jahre betragen. Bei Rohwasser mit höherem Organikgehalt (DOC > 7 mg/L), wie bei der Nordwasser in Rostock, wird hingegen mindestens alle drei Jahre die GAK in den Filterkolonnen ausgetauscht.
Die Rest-Adsorptionskapazität der GAK kann durch verschiedene Verfahren abgeschätzt werden, ist aber nach wie vor Gegenstand aktueller Forschung. Die weitergehende Charakterisierung der beladenen GAK kann hierbei helfen.
Auf dem Poster sollen erste Ergebnisse zu den in Langenau und Rostock eingesetzten Aktivkohlen präsentiert werden. Hierzu wurden die frischen und nach unterschiedlichen Laufzeiten beladenen GAK untersucht. Die Zusammensetzung der Anorganik und der adsorbierten Organik, welche mittels Zersetzungs¬gasanalyse charakterisiert wurde, zeigt deutliche Unterschiede. Bspw. nimmt der Calcium-Gehalt der GAK in Langenau kontinuierlich zu, wohingegen dieser in den Proben aus Rostock mit zunehmender Laufzeit zurückgeht. Umgekehrt verhält es sich mit der Organik: Die GAK aus Rostock zeigen Hinweise auf biologische Besiedelung, während diese in Langenau trotz längerer Filterlaufzeit auszubleiben scheint.
In this work the flexural rigidity of individual large diameter multi-walled carbon nanotubes (MWCNTs) was investigated. The bending modulus were obtained by detecting the resonance frequencies of mechanically excited cantilevered carbon nanotubes using the so-called dynamic scanning electron microscopy technique, and applying the Euler–Bernoulli beam theory. For the nanotubes studied, we determined a modulus of up to 160 GPa. This agrees with values reported by other authors for MWCNTs produced by catalytic chemical vapor deposition, however, it is 6-8 times smaller than values reported for single and multi-walled carbon nanotubes produced by arc-discharge synthesis. Toxicological studies with carbon nanotubes have been showing that inhaled airborne nanofibers that reach the deep airways of the respiratory system may lead to serious, asbestos-like lung diseases. These studies suggested that their toxicity critically depends on the fiber flexural rigidity, with high rigidity causing cell lesions. To complement the correlation between observed toxicological effects and fiber rigidities, reliable and routinely applicable measurement techniques for the flexural rigidity of nanofibers are required.
Tire wear particles (TW) are generated by the abrasions of tires on the road surface through traffic. These particles can be transported by air and surface runoff and might also infiltrate the soil and consequently affect terrestrial ecosystems. The estimated tire wear (TW) emissions are immense, with 1.33 106 t a-1 in Europe. Despite this, only little is known about the environmental contents or the fate of TW.
One reason for this knowledge gap is the challenging analysis of TW in environmental samples. Detection of TW with spectroscopic methods is problematic due to high fluorescence interferences caused by contained black carbon. One analytical approach is to use zinc (Zn), a typical additive in tires, as a specific marker for the quantification of tire wear. However, any Zn originating from the sample matrix must be separated beforehand and requires elaborate sample preparation.
Car tires consist partly of synthetic rubbers, such as styrene-butadiene-rubber (SBR). This SBR could be identified and quantified via Thermal-Extraction-Desorption-Gas Chromatography-Mass Spectrometry (TED-GC-MS). This newly developed and fast screening method allows the simultaneous detection of microplastics and TW mass contents and requires minimal to no sample preparation. Firstly the sample is thermally extracted in a thermobalance under a nitrogen atmosphere. The resulting specific decomposition products are sorbed on a solid phase adsorber, which is then transferred to a GC-MS via an autosampler, where the products are desorbed, separated and identified. Cyclohexenylbenzene is used as a specific marker for SBR.
Here we investigated top layer soil samples, collected at the roadside of highly frequented German highways. Samples were analyzed without sample preparation, and SBR was detected in all investigated samples in mass contents ranging from 67.2 to 2230 mg kg-1. A correlation between SBR and Zn content in the soil was confirmed, while the correlation between SBR and Corg was hardly pronounced. We successfully demonstrated the application of TED-GC-MS as a screening method for tire wear in soil samples.
The present study will discuss these analytical results in detail as well as sampling parameters like sampling depth and distance to the roadside, and the effect of the particle size on the particle transport by water runoff and air.
Biocide mitigation strategies of microbiologically influenced corrosion (MIC) in the oil and gas industry have been primarily used to eliminate the growths of sulfate-reducing microorganisms (SRM). However, methanogenic Archaea (MA) can also be highly corrosive by using iron as an electron source for methanogenesis. Because of the fundamental physiological differences between archaea and bacteria, responses of MA towards SRM-specific biocides cannot be deduced using SRM. Due to the lack of information available on the effect of biocides on corrosive MA, we selected THPS, glutaraldehyde, nitrate and perchlorate to compare against corrosive SRM.
Preliminary results showed that at low concentrations of THPS (0-10 ppm), growth of MA was not affected, methane production and corrosion rates (0.1 mm/yr) were comparable between the different THPS concentrations. On the contrary, the SRM strain showed decreased corrosion rates (0.18 mm/yr to 0.03 mm/yr) with increasing THPS concentrations. Further corrosion tests including electrochemical measurements of different biocides on the growth of MA and SRM will be conducted. Such knowledge not only provide important insights on the physiological response of MA to biocides but also contribute to more effective mitigation strategies that can be both economic and environmentally beneficial.
Microbiologically induced corrosion due to bacterial biofilms causes several problems in industrial systems, technical applications and in medicine. Prior to the formation of a biofilm on a substrate, planktonic cells attach on the surface. Hence, the properties of the surface play a key role in biofilm formation and are of great importance for the development of strategies to prevent bacterial attachment and biofilm formation.
This project aims at clarifying to which extent surface micro-/nanostructuring and chemical functionalization affects bacterial attachment and whether a synergistic combination of the two can be used to control bacterial adhesion. To answer these questions, model surfaces with regular patterns of 5-10 micrometers in size have been prepared, which provide distinct zones differing in terms of their chemistry or nano-roughness. This was achieved by micro contact printing of self-assembled monolayers with different functional groups and deposition of patterned ZnO nanorod arrays for studying the effect of surface chemistry and morphology, respectively. Typical contrasts studied were combinations of positively/negatively charged, hydrophobic/hydrophilic or flat/rough.
The attachment behavior of bacteria on tailored surfaces were studied in a flow chamber as a function of time. The strain Pseudomonas fluorescens SBW25 was chosen as a model organism. DNA-intercalating dyes such as Syto9 have a high affinity to adsorb on ZnO nanorods. To overcome this limitation a genetic modification was performed by introducing a gene which expresses a green fluorescent protein in P. fluorescens SBW25 enabling the quantitative evaluation of the flow chamber studies by means of fluorescence microscopy. Further analysis of the attachment behavior was performed by means of scanning electron microscopy.
The presentation will summarize the results of our systematic study on the role of individual parameters on bacterial attachment and highlight synergistic combinations, showing an inhibition or enhancing effect. As the investigations with model substrates enable a precise control of the surface parameters, this approach can be applied to different microorganisms and material systems to achieve a correlative description of bacterial adhesion on solid surfaces.
In arid sun-exposed environments, rock-inhabiting fungi dominate microbial communities on rock surfaces. Fungi are known to enhance rock weathering, although the exact mechanisms are not completely understood. These natural processes can be simulated by reproducible experimental systems. Particularly attractive are genetically amenable rock-weathering fungi, where certain traits can be knocked-out to identify weathering-relevant functions. Here, we studied the effect of the rock-inhabiting fungus Knufia petricola A95 and its melanin-deficient mutant (ΔKppks) on the weathering of a Fe-bearing olivine. We examined the olivine dissolution kinetics and looked at the olivine-fungus interface. For the former we inoculated olivine powder with the fungus in batch and mixed flow reactors and analysed the medium solution by ICP-OES, for the latter biofilm-covered olivine sections from flow-through reactors were analysed by FIB-TEM.
In general olivine dissolution was lower when olivine was incubated without fungi: the abiotic olivine dissolution rates were lowest and the surface of the abiotically reacted olivine sections showed no etching. Various chemical analyses show Fe (oxyhydr)oxide precipitation on top of the abiotically reacted olivine, indicating its role in inhibiting olivine dissolution. Both the wild type (WT) and ΔKppks solubilised and bound significant amounts of Fe released by olivine dissolution. Fe (oxyhydr)oxide precipitation was thus reduced, explaining the enhanced olivine dissolution in their presence. Particularly efficient at preventing Fe precipitation were attached WT cells: the inhibition of olivine dissolution almost completely disappeared. The attachment capacity of the WT is most likely caused by the production of WT-specific extracellular polymeric substances. Our presented experimental systems allowed the precipitation of Fe (oxyhydr)oxides and included a rock-inhabiting fungus and thus simulated weathering processes relevant to natural ecosystems.
Neuartige Materialien, die bekannte (Werk-)Stoffe mit neuen Funktionalitäten ausstatten, spielen eine zunehmend wichtige Rolle im Bereich der Materialforschung und -prüfung. Das Spektrum neuartiger Materialien reicht von der gezielten Oberflächenfunktionalisierung und -strukturierung makroskopischer Materialien, dünnen Beschichtungen bis hin zu mikro- und nanoskaligen Kompositmaterialien und funktionalen Materialien an der Schnittstelle zur Biologie, Biotechnologie, nachhaltige Energiespeicherung und Sensorik. Dabei bieten neuartige Materialien die Chance, Werkstoffe und Produkte mit erweiterter oder verbesserter Funktionalität zu erhalten und Sicherheit bereits im Designprozess zu berücksichtigen. Durch dieses breite Anwendungsspektrum und die Herausforderungen, die solche Materialien für die Sicherheit in Chemie und Technik mit sich bringen, sind diese in allen Themenfeldern der BAM repräsentiert (Material, Analytical Sciences, Energie, Infrastruktur und Umwelt).
Die Aufgaben der BAM erstrecken sich dabei von der Herstellung von Referenzmaterialien für Industrie, Forschung und Regulation, über die Erstellung von standardisierten Referenzverfahren für nachhaltige Messungen im Umwelt- und Lebenswissenschaftsbereich bis hin zur Bereitstellung von belastbaren und zitierbaren Referenzdaten. Durch die genaue Charakterisierung neuartiger Materialien können potentiell problematische Substanzen identifiziert und deren Risiken besser abgeschätzt werden. In diesem Beitrag werden einige aktuelle Beispiele aus diesen Bereichen vorgestellt.
Nach einer Übersicht zu den immer schneller aktualisierenden Rahmenbedingungen von Politik und Gesellschaft folgt eine Übersicht zu materialwissenschaftlichen Problemen des Recyclings von Kunststoffen. Lösungsansätze aus der Forschung reichen von einfacher Optimierung bis hin zur radikalen Neukonstruktion der polymeren Werkstoffe. Aus dem bereits möglichen Ansatz "performance-by-design" wird ein neuer Weg des "recycling-by-design" adressiert. Dies inkludiert methodisch eine skalenübergreifende Modellierung und die Depolarisation bis zum Monomer.
Seit einigen Jahren wird in den Medien viel über das Thema Mikroplastik (MP) diskutiert. Dabei wird häufig von einer großen Anzahl an MP-Partikeln in allen Bereichen der Umwelt, wie dem Wasser, dem Boden, der Luft und in Biota sowie über mögliche Gefahren ausgehend von MP, berichtet. Jedoch sind diese Studien häufig nicht untereinander vergleichbar, da verschiedene Konzepte der Probennahme, der Aufbereitung und unterschiedliche Detektionsverfahren verwendet werden. Um diesen Mangel an vergleichbaren und aussagekräftigen Daten zu beheben, wird aktuell versucht, eine Harmonisierung der Mikroplastikanalytik voranzutreiben. Neue, schnellere Methoden zur MP Quantifizierung wurden entwickelt. Gleichzeitig werden neue Strategien zur Probenahme und Probenvorbereitung konzipiert, da hier die Fehlerquellen besonders große Auswirkungen auf das Ergebnis haben.
In diesem Vortrag werden verschiedene Verfahren bezogen auf Probennahme, -vorbereitung und Analytik gezeigt und bezüglich ihres möglichen Ergebnisses diskutiert.
Im Vortrag wird die Problematik Mikroplastik eingeführt und ein Probenset aus dem Mittelmeer mit ersten Ergebnissen besprochen. Die Alterung von Polymeren im Umweltkontext sowie Möglichkeiten der Analyse von Polymeralterungsfortschritten werden diskutiert. Die thermoanalytische Methode mit Zersetzungsgasanalytik (TED-GC-MS) wird eingeführt und deren Einsatzmöglichkeiten in der Thematik umrissen.
Der Vortrag beschreibt den Entwicklungsprozess des Analysenverfahrens TED-GC-MS zur Bestimmung von Mikroplastikgehalten in Umweltproben im Rahmen des BMBF-Projektes MiWa. Die Funktionsweise, die Automatisierung und die Optimierung einzelner Geräteparameter und Leistungsdaten werden gezeigt. Untersuchungen des Einflusses von Probenmatrices werden dargestellt und die Ergebnisse einiger Messkampagnen und Ringversuche vorgestellt, die die Routinefähigkeit des Verfahrens dokumentieren.
Nanomaterials are present in our everyday life. Paint coats, sunscreens, catalysts and additives for tyres are good examples for the use of such materials in mass-market products. The problem of the safety of nanomaterials is recognized as a problem for health and environment, which lead to the special registration of nanomaterials according to an annex of REACH as of 2020. But a great problem for the risk assessment of nanomaterials that several factors could influence the hazardous nature of them. Additional to composition, crystal structure, size and shape the surface properties of such particles belong to these parameters for risk assesment. The reason for the relevance of the surface is obvious: the smaller the particle, the higher is the share of the surface. Additionally, the surface is the region of the particle which interacts with the surrounding which is another crucial factor for the understanding the effect of a nanomaterial on health and environment. In the OECD Testing Programme on Manufactured Nanomaterials exists consequently an Endpoint 4.30 Surface Chemistry in Chapter 4. PHYSICAL AND CHEMICAL PROPERTIES. In summary, there is obviously a need for a correlation between surface chemical analytic data and toxicity. To fill in this gap, we present surface analytic results obtained with X-ray photoelectron spectroscopy and Time-of-Flight Secondary Ion Mass Spectrometry and correlate them with cytotoxic data gain by high-throughput screening experiments. It must be noted, that these experiments were done at the same set of titania materials taken from the JRC (Joint Research Centre of the European Union) Nanomaterials Repository. As material TiO2 was chosen due to its widespread use in consumer products, e.g. paint coats and sunscreens. With this new approach a better understanding of the influence of surface properties on the toxicity can be expected leading to a better risk assessment of these materials.
The number of publications reporting the amount of microplastic (MP) all over the world increased rapidly. Methods used so far are very time consuming and not able to provide information on total contents. As harmonised sampling, sample preparation and analysis strategies are missing different studies can hardly be compared and quantitative data, including identification and mass contents of the polymers found, are missing. This leads to a lack of comprehensive understanding of MP occurrence, source and entry pathways into the environment.
We developed a method, Thermal Extraction/Desorption-Gaschromatography-Massspectrometry, as a fast screening method for MP analysis. Solid residues of water samples are heated up to 600 C under a N2 atmosphere without any sample preparation. The collected decomposition gases are separated in a gas chromatography system and detected in a mass spectrometer. Mass contents of the identified polymers can be calculated.
In this presentation we will show first results from the influent of the wastewater treatment plant Kaiserslautern (Germany) and its combined sewage system as possibly entry pathway. In order to determine the relevance of wastewater split streams analysis of grey water will be conducted. Samples are fractionally filtered by a sieve cascade with mesh sizes of 500, 100, 50 µm.
µ-FTIR spectroscopy is a widely used technique in microplastics research. It allows to simultaneously characterize the material of the small particles, fibers or fragments, and to specify their size distribution and shape. Modern detectors offer the possibility to perform two-dimensional imaging of the sample providing detailed information. However, datasets are often too large for manual evaluation calling for automated microplastic identification. Library search based on the comparison with known reference spectra has been proposed to solve this problem.
To supplement this ‘targeted analysis’, an exploratory approach was tested. Principal component analysis (PCA) was used to drastically reduce the size of the data set while maintaining the significant information. Groups of similar spectra in the prepared data set were identified with cluster analysis. Members of different clusters could be assigned to different polymer types whereas the variation observed within a cluster gives a hint on the chemical variability of microplastics of the same type. Spectra labeled according to the respective cluster can be used for supervised learning. The obtained classification was tested on an independent data set and results were compared to the spectral library search approach.
Plastics and rubber are used in many applications, such as packaging, building, construction and mobility. Due to their favourable properties like light weight, flexible processing and low costs their production and consequently their input into the environment has increased significantly over the last decades. In the environment, oxidation processes and mechanical abrasion lead to the decomposition of these plastics into small fragments, called microplastic (< 5 mm). By definition, microplastics only involve thermoplastics and duroplastics but elastomers made out of synthetic polymers (e. g. styrene butadiene rubber), modified natural polymers (e. g. natural rubber) and products of synthetic polymers (e. g. tires) are also part of the current microplastic discussion. The main entry pathway of rubber into the environment is the wear of used tire treads in road traffic. Lassen et al. showed that 60 % of the microplastic emissions in Denmark into the environment come from secondary microplastics generated by tires. Rain events can cause microplastic and rubber to get from the street into the street inlets. Depending on the sewage system, these waters are sometimes not cleaned in the sewage treatment plants and reach the surface waters untreated.
To analyse microplastic particles in samples, mainly FTIR or Raman spectroscopic methods are applied at present. Rubber or tire particles in environmental samples cannot be analysed by these methods, because the added carbon black leads to annoying absorption and fluorescent effects.
We developed a thermoanalytical method, the so-called TED-GC-MS (thermal extraction desorption gas chromatography mass spectrometry), which allows the simultaneous detection of microplastic and tire wear with almost no sample preparation in about 2.5 h. The TED-GC-MS is a two-step analytical method which consists of a thermobalance and a GC-MS system. Up to 50 mg of an environmental sample is heated up to 600 °C in a nitrogen atmosphere. During pyrolysis, between 300 and 600 °C polymer-specific decomposition products are produced and collected on a solid phase. Afterwards the substances are desorbed, separated and analysed using the GC-MS.
The aim of the present work is to present the TED-GC-MS as a time efficient screening method to quantify the industrial most relevant polymers in street run-off samples. Analytical challenges in the determination of polyethylene (PE), polypropylene (PP), polystyrene (PS), polyethylene terephthalate (PET) and polyamide (PA), polymethyl methacrylate (PMMA) and styrene-butadiene-rubber (SBR) as a component of tire wear are honestly discussed.
The study area is a 200 m long section of the Clayallee in Berlin, a representative typical urban catchment area. The road run-off in this section flows through the gullies directly into a sample chamber, which directs the runoff in an open channel to the rainwater sewer of this area. The sample chamber allows a sample to be taken directly from the road run-off without mixing with the run-off from other areas. The sample chamber is equipped with an automatic sampler. The automatic sampler is controlled by a conductivity sensor to detect the storm event at an early stage. The sensor gives the sampler a signal to start the sampling program when it gets in contact with water and reaches a certain conductivity threshold. The capacity of the sample container is 100 l and the maximum delivery of the automatic sampler is 2.8 l/min.
Afterwards, the water was pumped through various stainless-steel sieves with a diameter of approximately 20 cm and mesh widths of 500, 100, 50 μm. The obtained solids were steam sterilized, freeze-dried and measured with the TED-GC-MS.
The results of the TED-GC-MS-measurements are summarized in Figure 1. It shows the polymers which were detected in 1 mg of the dry masses of various street run off samples obtained during a period of 1.5 years. We detected PMMA, PS, PP, PE and SBR, as a component of tire wear in the samples. The quantification of the polymers leads to amounts of PS, PP, PE and SBR between 0 µg and 10 µg. PMMA was only detected in traces.
In diesem Beitrag wird gezeigt wie mit Thermogravimetrischen Analysen (TGA) Aktivkohleoberflächen charakterisiert werden können. Außerdem wie TGA mit Zersetzungsgasanalyse zur Untersuchung von Adsorbat-Systemen (Carbamazepin an drei verschiedenen Aktivkohlen) zur Aufklärung von Adsorptionszuständen genutzt werden kann.
Advanced wastewater treatment by the application of activated carbon is used to eliminate organic micropollutants in large scale wastewater treatment plants. However, underlying adsorption processes are unclear. On the one hand, compositions of wastewater differ and are very complex. On the other hand, activated carbons have physicochemical properties which impair investigations on adsorption mechanisms, since they are non-graphitic, non-graphitizable and have a highly disordered microstructure. This leads to their large surface areas and internal pore structure but also implies heteroatoms and functional groups. These are not easily accessible for research but affect the adsorption of organic micropollutants. Thermogravimetric analysis and evolved gas analysis can provide valuable insights into these kinds of systems. First, pyrolysis makes functional surface groups accessible, e.g. through decarboxylation, which facilitates characterisation of activated carbons. Second, adsorbates can be investigated by thermal desorption or decomposition, depending on the sorption conditions of the organic micropollutants. Single component systems as well as multi component systems with competing organic background matter are compared for various activated carbons. Surprising distinctions in the adsorption mechanisms will be presented.
Im Vortrag wird der Ansatz zur Aufklärung von Adsorptionsprozessen, die in der Wasserphase stattgefunden haben, mittels Thermogravimetrie und Zersetzungsgasanalyse vorgestellt.
Es wird allgemein gezeigt wie TGA zur Charakterisierung von Aktivkohleoberflächen genutzt werden kann und welche Unterschiede sich in verschiedenen Adsorbat-Systemen zeigen. Im Detail wird die thermische Zersetzung von adsorbiertem Carbamazepin an drei verschiedenen Aktivkohlen präsentiert.
Die ThermoExtraktionDesorption-Gaschromatografie-Massenspektrometrie (TED-GC-MS) ist die wichtigste Methode der BAM zur Analyse von Mikroplastikpartikeln in Umweltproben. Mit wachsendem Erfahrungsschatz traten Komplikationen auf, bei deren Bewältigung das Analysensystem verbessert werden konnte. Das Poster präsentiert u. a. die Verbesserung der Nachweisgrenzen sowie die Eliminierung von Kontaminationsquellen aus gängigen Probennahmeverfahren.
Der Vortrag beschäftigt sich mit den gängisten Methoden zur Probennahme, -vorbereitung und Detektion von Mikroplastik. Das Zusammenspiel von Fragestellung und Methode wird betont. Es wird auf das Dikussionspapier Analytik des BMBF-Forschungsschwerpunktes Plastik in der Umwelt besonders hingewiesen sowie Bemühungen zur Normierung der Methoden auf deutscher und internationaler Ebene dargestellt.
The ubiquitous presence of unwanted plastics in the environment, especially microscale particles, has been an issue in scientific studies and public debate in the last years. It is well known that oxidative degradation and subsequent fragmentation, caused by UV-radiation, oxidative aging and abrasion lead to the decomposition of larger plastic products into microplastics (MP). Possible effects of these MP on ecosystems are still unclear. Recent studies on MP findings are focused mainly on aquatic systems, while little is known about MP in terrestrial ecosystems.
A possible source of MP input into the soil is compost from domestic bio-waste. Inappropriate waste separation causes plastic fragments in the bio-waste, some of which end up in the compost. In Germany compost is used as fertilizer in agriculture, hence MP could enter the soil by this pathway. So far, there have been only a few studies on this object. For this reason, analysis of compost as a sink and source of MP in ecosystems is of high interest.
To estimate and monitor the MP content in compost and soil, fast and harmonised analytical methods are essential, which not only measure the polymer type and number of particles, but also the mass content. The most common spectroscopic methods are very time-consuming, often require complex sample preparation steps and cannot determine mass contents. Therefore, we used ThermoExtractionDesorption-GasChromatography-MassSpectrometry (TED-GC-MS) as a fast, integral analytical technique. The sample is pyrolyzed to 600°C in a nitrogen atmosphere and an excerpt of the pyrolysis gases is collected on a solid phase adsorber. Afterwards, the decomposition gases are desorbed and measured in a GC-MS system. Characteristic pyrolysis products can be used to identify the polymer type and determine the mass contents. This method is well established for the analysis of MP in water filtrate samples.
In the present work we optimized the TED-GC-MS method for compost and compost/soil matrix and very common polymers, such as polyethylene, polypropylene, polyethylene-terephthalate and polystyrene (sample mass, detection limits, interfering signals, etc.). Additionally, specific pyrolysis products of polymers used for bio-waste bags, such as polylactide (PLA) and polybutylenadipat-terephthalat (PBAT) had to be identified and evaluated.
First measurements were carried out on model and real samples from prepared mixtures and composting plant. The samples were sterilized, fractionated, filtered and dried. In addition, half of the sample material was treated with hydrogen peroxide to investigate a possible effect on detection.