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OECD Prüfrichtlinie zur Bestimmung der Partikelgröße und Anzahlgrößenverteilung von Nanomaterialien
(2021)
Abschlusspräsentation des Projektes "OECD Prüfrichtlinie zur Bestimmung der Partikelgröße und Anzahlgrößenverteilung von Nanomaterialien" - Projektteil Nanopartikel.
Es hat sich gezeigt, dass alle Methoden zur Bestimmung der Partikelgrößenverteilung Vor- und Nachteile haben. Es wird dringend empfohlen Größenverteilungen immer mit mindestens zwei unterschiedlichen Methoden zu bestimmen: Bildgebend und mit gute Anzahlstatistik.
Verschiedene Durchmesser wurden in der TG-PSD mit einem Indexsystem versehen, welches zukünftig Verwechslungen zwischen unterschiedlichen Durchmessern vermeiden soll.
Wird ein bestimmter Durchmesser benötigt (z.B. hydrodynamisch, aerodynamisch), muss die Methode passend gewählt werden. Eine Umrechnung von einem Durchmesser in einen anderen ist in der Regel fehlerbehaftet.
Es wurde ein einheitliches Reporting-System in der TG-PSD eingeführt.
Vorstellung der Ergebnisse bei der Entwicklung einer neuen OECD Prüfrichtlinie zur Bestimmung der Partikelgröße und Anzahlgrößenverteilung von Nanomaterialien. (Projektteil Fasern.)
Ergebnisse:
Abweichungen zwischen SEM and TEM insbesondere bei langen Fasern
Die Anwendung von TEM auf kurze Fasern < 5 µm beschränkt
Für SEM wurde keine signifikante Abhängigkeit der Bestimmung der Faserdurchmesser von der Pixelgröße der Aufnahmen festgestellt
Für TEM wurde eine Abhängigkeit der Bestimmung der Faserdurchmesser von der Pixelgröße festgestellt
Der Einfluss der Bildauswertenden auf die Varianz der Ergebnisse ist klein im Vergleich zu der gesamten Varianz.
Nanofasern können mit TEM und SEM bestimmt werden!
Vorstellung der Ergebnisse bei der Entwicklung einer neuen OECD Prüfrichtlinie zur Bestimmung der Partikelgröße und Anzahlgrößenverteilung von Nanomaterialien.
Ergebnisse:
Ideal sphärische Partikel sind gut und verlässlich mit vielen Methoden charakterisierbar.
Reale (Nicht ideale) Materialien sind gut charakterisierbar, wenn eine gewisse Homogenität und Stabilität vorliegt.
Stark inhomogene und stark agglomerierende Partikel liefern deutlich unterschiedliche Ergebnisse für verschiedene Methoden.
Partikel mit geringen Größenunterschieden lassen sich mit allen Methoden gut charakterisieren.
Partikel mit sehr deutlichen Größenunterschieden führen häufig zu einer Unterbewertung der kleineren Partikel.
Vollautomatische Partikeldetektion bei elektronenmikroskopischen Aufnahmen ist z.Zt. noch stark fehleranfällig und kann daher nicht empfohlen werden.
Es hat sich gezeigt, dass alle Methoden zur Bestimmung der Partikelgrößenverteilung Vor- und Nachteile haben. Es ist dringend zu empfehlen Größenverteilungen immer mit mindestens zwei unterschiedlichen Methoden zu bestimmen: Bildgebend und mit gute Anzahlstatistik.
Verschiedene Durchmesser wurden in der TG-PSD mit einem Indexsystem versehen, welches zukünftig Verwechslungen zwischen unterschiedlichen Durchmessern vermeiden soll.
Wird ein bestimmter Durchmesser benötigt (z.B. hydrodynamisch, aerodynamisch), muss die Methode passend gewählt werden. Eine Umrechnung von einem Durchmesser in einen anderen ist in der Regel fehlerbehaftet.
Es wurde ein einheitliches Reporting-System in der TG-PSD eingeführt.
In 1981 the OECD published the Test Guideline on Particle size and size distribution. This TG is still a valid document for the measurement of particles all over the world.
When nanomaterials gained importance, ISO set up a technical commitee for Nanotechnologies in 2005 and the OECD followed this step in 2006 with the Working Party on Manufactured Nanomaterials.
In the following years ISO and OECD published several documents about nanomaterials and the systematisation developed.
In 2017 it was finally clear that nanomaterials need to be adressed in another way than chemicals and in 2020 ECHA revised the REACH-Annexes accordingly and included nanomaterials.
Unfortunately there is a little problem with this: Only a few applicable test guidelines exit for the measurement of the nanomaterials. Several test guidelines date from 1981 and do not address nanomaterials.
The logical next step for the OECD would be to publish a series of test guidelines which are indeed currently prepared and will be shown in this talk.
Finally there is an additional need for the future of NM standardisation: Digitalisation.
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).
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.
Gypsum is widely used in the construction sector, and its worldwide consumption has been increasing now for several decades. Currently, the gypsum demand is met up to 60% by FGD gypsum (a by-product from coal-fired power plants) in Germany. The natural gypsum deposits cover the remaining gypsum demand. Due to national climate protection goals and the related shutdown of coal-fired power plants, the FGD gypsum supply will decrease significantly in the coming years and, therefore, other gypsum sources must be found.
Depending on the lifetime of the used gypsum products in the construction sector, an increase of gypsum in construction and demolition waste is to be expected. With regard to an upcoming shortage of gypsum, several approaches are being tested to recover gypsum from construction and demolition waste. Gypsum plasterboard recycling is already implemented on an industrial scale. Furthermore, new processes to recycle different types of gypsum products from construction and demolition waste are being examined. Of particular interest are different types of gypsum boards because they are well suited for selective dismantling. Therefore, they can be recovered comparatively free of impurities which is most important for the gypsum recycling.
In the research project “GipsRec 2.0”, funded by the Federal Ministry of Education and Research, recycling methods for gypsum fiberboards are being investigated. Additionally, the suitability of different types of synthetic gypsum as substitutes for FGD gypsum is being considered. Currently, the quantities of recycled gypsum are not sufficient with regard to the reduction of FGD gypsum. An increase of gypsum recycling should be achieved to narrow the future gypsum gap that will occur in the near future.
Antimicrobial surfaces have broad use in multiple settings including touch surfaces in hospitals, implanted devices, or consumer products. Their aim is to support existing hygiene procedures, and to help combat the increasing threat of antimicrobial resistance. However, concerns have been raised over the potential selection pressure exerted by such surfaces, which might drive the evolution and spread of antimicrobial resistance. In my presentation, I will highlight the risks and knowledge gaps associated with resistance on antimicrobial surfaces by different processes including evolution by de novo mutations and horizontal gene transfer, and species sorting of inherently resistant bacteria dispersed onto antimicrobial surfaces. The latter process has the potential to select for antibiotic resistance via cross-resistance between traits that confer resistance to both the antimicrobial surface coating and antibiotics. Conditions in which antibiotics and antimicrobial coatings are present simultaneously (e.g. implants) will lead to more complex interactions that can either result in the selection for or against antibiotic resistance. We mapped these interactions between several antimicrobials and antibiotics on growth and selection of Pseudomonas aeruginosa. We find prevalent physiological (i.e. synergy and antagonism) and evolutionary (i.e. cross-resistance and collateral sensitivity) combination effects. Understanding these interactions opens the door to tailor therapeutic interventions to select against resistance. In additions, we need new methods and translational studies that investigate resistance development to antimicrobial surfaces under realistic conditions. Therefore, I will present recent developments in our lab on the development of such a method based on existing efficacy standards.
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.
Quantitative chemical analysis of airborne particulate matter (PM) is vital for the understanding of health effects in indoor and outdoor environments and required by EU air quality regulations. Typically, airborne particles are sampled on filters, followed by lab-based analysis, e.g., with inductively coupled plasma mass spectrometry (ICP-MS). Within the EURAMET EMPIR AEROMET project, cascade impactor aerosol sampling was combined with on-site total reflection X-ray fluorescence (TXRF) spectroscopy. The study aimed at a proof of principles for this new mobile and on-size tool for the quantification of aerosol element compositions and element mass concentrations within short time intervals of less than 12 h. In a field campaign the method’s technical feasibility could be demonstrated. The TXRF results were traced back to a stationary, reference-free XRS setup in the laboratory of the German national metrology institute PTB at the BESSY II electron storage ring in Berlin, Germany. Simultaneous PM10-filter sampling, followed by standardized lab-based analysis, allowed for a comparison of the field campaign data of both methods. As Fig. 1 shows, the correspondence between PM10 filter sampling and ICP-MS, and on the other hand, cascade impactor sampling and TXRF is quite encouraging. However, for some of the analysed elements, e.g. V and Pb, the observed deviations are higher than expected and this highlights the fact, that spectral deconvolution strategies for TXRF on cascade impactor samples still need some improvement.
This work was supported by the EMPIR programme, co-financed by the Participating States and from the European Union’s Horizon 2020 research and innovation programme, through grant agreements 16ENV07 AEROMET and 19ENV08 AEROMET II
CF Pyro: Stofflich-energetische Verwertung von carbonfaserhaltigen Abfällen in der Pyrometallurgie
(2021)
Despite its contribution to tackling climate change by lightweight design, growing CFRP production also results in a global waste generation of 62 kt/a. Accordingly, the energy-intensive production process of carbon fibers (CF) necessitates sustainable recycling solutions.
Herein we will give an overview of current recycling processes, discuss their limitations and present a novel approach for safe treatment of CF unsuitable for material recovery . Our project CF Pyro examines feedstock recycling in pyrometallurgical processes, focusing on reactivity of CF, process stability and prevention of hazardous WHO fiber release. Besides fundamental experimental breakthroughs, their broader impact on circular economy will be presented.
The ISO 16000-6 standard describes a method for the determination of volatile organic compounds (VOCs) in indoor and test chamber air by sorbent-based active sampling, thermal desorption and gas chromatography coupled with mass spectrometry (GC/MS). It also gives directions to adapt this methodology to very volatile organic compounds (VVOCs). Indeed, toxicologically based guideline values are being implemented for these compounds and it becomes necessary to measure them. But a comprehensive and robust measurement method is lacking. Investigations on the use of gaseous standards, the suitability of chromatography columns, the suitable sorbent combinations and the water removal are required. The talk will highlight the points that need to be explored towards the standardisation of a suitable procedure and provide appropriate preliminary results.
Basic oxygen furnace slag (BOFS) is a by-product of the steelmaking process, of which about 10.4 Mt are produced annually in the European Union. Besides its predominant use in road construction, earthwork, and hydraulic engineering, it is also possible to use BOFS as a source material for Portland cement clinker.
The main difference in the chemical composition of BOFS from the chemical composition of Portland cement clinker is its high content of iron oxides (7-50 wt.%). In recent decades, many researchers have investigated the production of both Portland cement clinker and crude iron from BOFS via thermochemical reductive treatment. Carbothermal treatment of liquid BOFS causes reduction of iron oxides to metallic iron, which separates from the mineral phase due to its higher density.
In this study, German BOFS was reduced in a small-scale electric arc furnace using petrol coke as reducing agent. The produced low-iron mineral product was chemically similar to Portland cement clinker and contained the most important Portland cement mineral alite (Ca3SiO5) as main component. Besides alite, the mineral product contained other Portland cement clinker constituents such as belite (β-Ca2SiO4) and tricalcium aluminate (Ca3Al2O6).
The production of Portland cement clinker and crude iron from BOFS has economic and ecological benefits for both the cement and steel industry. Cement clinker from reduced BOFS may be used as a substitute for cement clinker from conventional cement production, thereby CO2 emissions will be reduced. The steel industry benefits from a high-value application for its by-products that avoids cost expensive landfilling and may even bring economic advantages. However, reductive treatment requires high temperatures and, for economic reasons, has to be carried out immediately after casting of the liquid BOFS, which is a logistical challenge for most steel plants. A cost-benefit analysis is therefore essential.
Basic oxygen furnace slags (BOFS) are a by-product of steel production. In 2016, 10.4 Mt of BOFS were produced in the European Union (EU). The main part of BOFS is used in road construction, earthwork and hydraulic engineering. A smaller part is returned to the metallurgical circle, used as fertilizer or landfilled. However, it is also possible to produce higher value products from BOFS. For example, many researchers have investigated the possibility of producing Portland cement clinker and crude iron from BOFS by a carbothermal post-treatment.
In this study, German BOFS was reduced in a small-scale electric arc furnace using petrol coke as reducing agent. The carbothermal treatment reduces the iron oxides in the BOFS to metallic iron, which accumulates at the bottom of the furnace by density separation. In addition to metallic iron, the process generates a mineral product rich in the tricalcium silicate solid solution alite. As the main constituent of Portland cement clinker, the hydraulic reactive mineral alite is of high economic importance.
In previous studies, the hydraulic reactivity of the mineral product was investigated by testing the compressive strength of blends with 70 wt.% ordinary Portland cement (OPC). Recent investigations focused on the hydraulic properties of the pure mineral product from the reduced BOFS. The heat of hydration of the mineral product was measured by isothermal calorimetry and compared with the heat of hydration of a synthetic low-iron slag and OPC. In addition, the formation of hydration products was investigated with differential scanning calorimetry (DSC) and x-ray diffraction analysis (XRD) on freeze-dried samples after defined curing times. The results of the calorimetric measurements indicate that the mineral product produced less heat of hydration and its reaction was delayed compared to the synthetic low-iron slag and OPC. Hydration products such as portlandite and calcium silicate hydrates (C-S-H) formed later and in lower amounts.
The production of a hydraulic material from BOFS by reductive treatment is of great interest to both the cement and steel industries. The substitution of cement clinker in OPC with a hydraulic material such as reduced BOFS leads to a reduction in greenhouse gas emissions from cement production. The steel industry benefits from an application for its by-products that avoids cost expensive landfilling and may even bring economic advantages. Furthermore, it may be possible to return the recovered crude iron to production.
Microbiologically Influenced Corrosion (MIC) is a phenomenon that is increasingly becoming a problem
for the society. MIC describes the negative effects a material can experience due to the presence of
microorganisms. In Europe, several research groups/ other industrial stakeholders are already dealing with
MIC. Unfortunately, the discussions are fragmented and the exchange of information is limited. A true
transdisciplinary approach is hardly ever experienced, although this would be logical for this
material/biology related challenge.
USA, Canada and Australia have strong networks, and develop methods, prevention measures and
standards, which Europe is forced to use, since nothing similar exists for a network and combined
knowledge to design them according to european standards. This makes Europe extremely dependent and,
in some cases, the potential measures or standards cannot been used because the suggested solutions
are prohibited by European laws (e.g. use of biocides).
Therefore, it is important to initiate a new European MIC-network. Europe needs to combine the efforts as
experts in different fields and develop prevention measures according to the European rules, in close
cooperation with industry and plant operators and owners of critical infrastructure. This COST Action will
provide the necessary interaction and communication, knowledge sharing, training of personnel and of
researchers of different disciplines. This will bring Europe to a leading role in this process, bringing ideas on
an equal level with other nations, considering the values which are important for Europe and attitudes (e.g.environmental protection) and representing greater protection for people, property and the environment.
The main aim and objective of the Action is to , in the context of MIC-research/control, encourage a
fluent/synergistic collaboration/communication, closing the gap between materials scientists, engineers,
microbiologists, chemists and integrity managers to encourage sufficient interaction between academia and
industry. This Action will create a common MIC-Network, including the important stakeholders.
In recent years, the fabrication of laser-generated surface structures on metals such as titanium surfaces have gained remarkable interests, being technologically relevant for applications in optics, medicine, fluid transport, tribology, and wetting of surfaces.
The morphology of these structures, and so their chemistry, is influenced by the different laser processing parameters such as the laser fluence, wavelength, pulse repetition rate, laser light polarization type and direction, angle of incidence, and the effective number of laser pulses per beam spot area.
However, the characterization of the different surface structures can be difficult because of constraints regarding the analytical information from both depth and the topographic artifacts which may limit the lateral and depth resolution of elemental distributions as well as their proper quantification. A promising technique to investigate these structures even at the nano-scale is Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS), a very surface sensitive technique that at the same time allows to perform depth-profiling, imaging and 3D-reconstruction of selected ion-sputter fragment distributions on the surface.
In this study we combine chemical analyses such as Energy Dispersive X-ray spectroscopy (EDX) and high-resolution scanning electron microscopy (SEM) analyses with ToF-SIMS to fully characterize the evolution of various types of laser-generated micro- and nanostructures formed on Ti and Ti alloys at different laser fluence levels, effective number of pulses and at different pulse repetition rates (1 – 400 kHz), following irradiation by near-infrared ultrashort laser pulses (925 fs, 1030 nm) in air environment or under argon gas flow.
We show how this combined surface analytical approach allows to evaluate alteration in the surface chemistry of the laser-generated surface structures depending on the laser processing parameters and the ambient environment.
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.
During iron and steel production, several by-products such as slags, dusts and sludges are generated in addition to pig iron and steel as primary products. While established recycling routes exist for slags, there are still considerable recycling problems for other residual materials, especially for filter dusts and sludges containing zinc and lead from waste gas purification. However, the high heavy metal contents make landfilling these dusts and sludges cost-intensive and ecologically problematic. In addition, the relatively high zinc and iron loads represent a valuable material potential, which can make reprocessing of the material with recovery of the zinc and iron loads as secondary raw materials ecologically as well as economically attractive. Against this background, a process is being developed in a cooperative project between Ferro Duo GmbH and the Federal Institute for Materials Research and Testing (BAM), in which the heavy metals (zinc, lead, cadmium, etc.) contained in the filter dusts and sludges are selectively converted into chlorides in a thermochemical process after the addition of a chlorine donor and evaporated at temperatures between 650 and 1100 °C. This process can be used to recover zinc and iron as secondary raw materials.
Experiments to date in a batch reactor show that >99% of the zinc and lead can be removed from the treated material. However, a continuous process is necessary for an economical process, which is why this process is transferred to a rotary kiln and relevant process parameters are identified and optimized. The results of these investigations will be presented here.