4 Material und Umwelt
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Monodisperse iron oxide nanoparticles as reference material candidate for particle size measurements
(2020)
In order to utilize and rationally design materials at the nanoscale the reliable characterization of their physico-chemical properties is highly important, especially with respect to the assessment of their environmental or biological impact. Furthermore, the European Commission’s REACH Regulations require the registration of nanomaterials traded in quantities of at least 1 ton. Powders or dispersions where 50% (number distribution) of the constituent particles have sizes ≤ 100 nm in at least one dimension are defined as nanomaterials. This creates a need for industrial manufacturers and research or analytical service facilities to reliably characterize potential nanomaterials. Currently, BAM is developing reference nanoparticles, which shall expand the scarce list of worldwide available nano reference materials certified for particle size distribution and will also target other key parameters like shape, structure, porosity or functional properties. In this respect, materials like iron oxide or titanium dioxide are considered as candidates to complement the already available silica, Au, Ag, and polystyrene reference nanoparticles.
The thermal decomposition of iron oleate precursors in high boiling organic solvents can provide large quantities of iron oxide nanoparticles that can be varied in size and shape.[1, 2] The presence of oleic acid or other hydrophobic ligands as capping agents ensures stable dispersion in nonpolar solvents. Such monodisperse, spherical particles were synthesized at BAM and pre-characterized by electron microscopy (TEM, SEM including the transmission mode STEM-in-SEM) and dynamic light scattering comparing cumulants analysis and frequency power spectrum.
1. REACH regulations and nanosafety concerns create a strong need for nano reference materials with diverse properties.
2. Iron oxide nanoparticles are under development as new candidate reference material at BAM.
3. Narrow particle size distribution confirmed by light scattering and electron microscopy.
Recycled fertilizers produced using processes for the recovery of phosphate from residual materials such as wastewater, sewage sludge and sewage sludge ashes show very good bioavailability, but it is still a product largely unknown to the market. The aim of CLOOP is therefore to document the properties and effects of such fertilizers through chemical, mineralogical and ecological analyses as well as analytical method development and pot and field plant growth trials.
Outotec focused on 3 points in CLOOP: Experimental campaigns, process simulations as well as economic analyses with focus on the AshDec process, respectively the design of a large-scale AshDec plant for phosphorus recovery. The laboratory scale trials as well as the semi-industrial scale campaign provided valuable insights into the operating parameters of the process and the plant. As a result, for example, the temperature range could be significantly lowered, and the additive addition reduced by approx. 20 %. They have further shown that the AshDec process is not susceptible to operating fluctuations and that the product can be consistently produced at high quality. With the selection of suitable operating parameters, heavy metals (As, Pb, Cd, (Zn)) can be removed. Within the campaign, about 1.5 t of fertilizer for the plant trials in CLOOP could be produced. An AshDec plant process was digitally created in simulation software, allowing valuable process parameters to be simulated at various operating parameters. On this basis, a full-scale plant was designed. The data obtained in the project were used for a detailed economic analysis including a sensitivity analysis. It was possible to show under which conditions this plant can be operated economically.
At BAM, the AshDec fertilizer was synthesized with different additives and then applied to plant experiments at Uni Bonn. The goal hereby was to check differences in plant uptake. Because of the promising results of AshDec synthesized with sodium-carbonate and because this AshDec version does not require special off gas treatment for sulfur recovery (compared to AshDec synthesized with sodium-sulfate), all project partners agreed on continuing working with this AshDec variation. It was then used as a raw P-source for formulating it into NPK-fertilizers, by granulation with ammonium-sulfate and straw ash as potassium source. These recycling fertilizers were applied to plant- and field experiments by project partners in Brazil (University of Sao Paulo) and Australia (University of Queensland). Furthermore, in leaching experiments, the solubility of phosphorus in AshDec was compared to triple super phosphate. The experiments were carried out on soils with a varying phosphorus buffering index. Results show, that the phosphorus form in AshDec is way less soluble in water. This indicates that AshDec has the potential for a so-called next generation fertilizer – a fertilizer which’s nutrients remain in the soil and supply the plant according to its needs. At the moment, this behavior gets examined more in depth in lysimeter experiments in cooperation with University of Technology Berlin.
The focus of KWB is the Life Cycle Assessment (LCA) of different NextGen fertilizers to evaluate the entire process chain from recovery to fertilizer application. The NextGen fertilizer is credited by the amount of plant available nutrients in the product, which replace nutrients from conventional fertilizer. The LCA covers N-struvite precipitation from municipal wastewater, K-struvite precipitation from industrial wastewater and the AshDec-product from sewage sludge. The LCA task is almost complete. It could be shown that struvite precipitation has comprehensive environmental benefits, mainly since positive side effects occur in sewage sludge treatment (e.g. reduced sludge volume). In principle, the energetic and ecological profile of the AshDec process compared to direct use of sewage sludge ash cannot be assessed as being generally beneficial or negative. Regarding the global warming potential, the Ashdec process shows that the expenses (e.g. energy, chemicals) cannot be covered by the P fertilizer credit. In contrast, the impact categories “terrestrial acidification potential”, and “freshwater eutrophication potential” show positive results as the credits for conventional fertilizer are higher than the burdens for the process.
At University Bonn, the standardized pot experiments were conducted with several AshDec variations, using ryegrass, soybean, and spinach on a slightly acidic sandy soil and an organic-free standard substrate. P-uptake and biomass production of different AshDec variations were generally like those of triple super phosphate and struvite, and clearly outperformed untreated sewage sludge ash and rock phosphate. Field trials in Australia and Brazil with sugarcane on acidic soils are still ongoing and results are expected by the end of 2021.
Conventional fertilisers have their disadvantages as nutrient release is not synchronised with the demand of plants. Several approaches of "next generation fertilisers" are aiming at controlled nutrient release. Recycling fertilisers are often not soluble in water but fully plant available. They are suitable raw materials for the production of new types of controlled release fertilisers.
A new sewage sludge ordinance was set in force in Germany in 2017 that makes phosphorus recovery from sewage sludge mandatory. The technological possibilities for P-recovery from waste water, sewage sludge and sewage sludge ash were presented.
The project ProMoAM is presented. The goal of the project is to evaluate which NDT techniques or combination of techniques is suited for in-situ quality assurance in additive manufacturing of metals. To this end, also 3d-data fusion and visualization techniques are applied. Additional ex-situ NDT-techniques are used as references for defect detection and quantification. Feasability studies for NDT-techniques that are presently not applicable for in-situ use are performed as well.
The presentation gives a brief overview of the whole project and the different involved NDT-techniques.
Microbiologically influenced corrosion (MIC) is a highly unpredictable process involving a complex group of microorganisms, including sulfate-reducing bacteria and methanogens. Standard laboratory MIC testing using static serum bottle enrichments is an easy but limited method, offering poor resolution on the biomineralization process of corrosion products. An example of this is the presumed corrosion product siderite by corrosive methanogens (Mi-MIC). Previous publications reported siderite was the sole corrosion product of M. maripaludis using metal coupons incubated under stationary conditions.
However, the formation of siderite is closely related to the surrounding environmental conditions, i.e. pH, CO2 concentration, flow and temperature. Thus, siderite as the sole corrosion product of Mi-MIC remain inconclusive and questionable. To study Mi-MIC effectively, a novel versatile multiport flow-column corrosion monitoring system (MFC) was developed. MFC allows sectional corrosion rate determination under flow conditions using different types of material, inoculum and packing material. MFC offers great flexibility, ease of operation and accurate corrosion measurements that can be combined with many other techniques. Using MFC, we studied multiple strains of methanogens and compared it with sulfate-reducing bacteria under neutral and low pH conditions. It was revealed by MFC that corrosive methanogens have equally high corrosion potential as sulfate-reducing bacteria. Additionally, siderite is not the dominant nor sole corrosion product of Mi-MIC. Thus, effective corrosion monitoring and establishing standard laboratory practices, i.e. incorporating MFC as part of regular testing process, will provide deeper understanding of MIC. This will allow further microbial electrophysiology understandings, contributing to effective mitigation strategy development.
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 influenced corrosion (MIC) is an expensive but unpredictable problem for the industries. The most well-known culprit for MIC is the sulfate-reducing microorganisms (SRM), such as members from the genus Desulfovibrio. It has been widely accepted that SRM can contribute significantly to MIC through the production of hydrogen sulfide (HS-) or in some cases a direct electron uptake from the metal surface. However, in a real environmental system, SRM is not exclusive and often involved with other microorganisms that may also contribute to MIC, such as methanogens.
Methanogenic archaea can produce methane (CH4) using H2+CO2, formate, methylated amines or acetate. Methanogens are highly abundant in the environment and many are found in very extreme conditions, such as high temperature and high salinity. Previous researches have demonstrated that methanogens are capable of MIC, though the specific mechanisms are still under investigation. In the oil and gas industry, methanogens are not considered as the main contributor for MIC since the corrosion rates are often too low. However, the tests for methanogen-induced MIC are usually performed at static conditions, which cannot represent the system accurately. Here, we developed a novel anaerobic system to evaluate the corrosion potential of methanogens under flow conditions. We will use the Methanococcus maripaludis KA1 strain, which was isolated from a crude oil tank, as the organism of interest. A separate system for Desulfovibrio alaskensis will be established for corrosion rate comparisons. Furthermore, we will study the synergistic effects of M. maripaludis and D. alaskensis on MIC under flow.
Harnessing near-chromosome level quality genomes to explore the evolution of termite immunity
(2023)
The phylogeny of the Blattodea boasts a wide degree of sociality spanning from solitary cockroaches to advanced ecosystem-dominating higher termite societies. The emergence of sociality in termites was associated with the acquisition of a diverse range of social structures. Previous work has found evidence for a caste-specific social defence system in termites leading to an immune system that may favour group over individual defence. While preliminary work suggests a correlation between social transitions and a reduction of immune gene family diversity, the lack of available high-quality termite genomes hampers complete knowledge of the true diversity of immune gene evolution across termite phylogeny. Here, we report on the sequencing and near-chromosome level assembly of 48 high-quality long-read-based genomes across major termite and cockroach sister-branch lineages. We investigate the diversity and evolutionary history of immune genes across genomes, focusing particular attention on correlations between immune gene evolution and transitions in sociality over termite phylogeny.
Insecta is one of the most diverse phyla in the animal kingdom, with species living in all types of habitats encountering an even greater diversity of pathogens and parasites. Defence strategies against such harmful threats led to a variety of molecular mechanisms, ecological shifts, and genetic innovations. Gene families underlying the molecular basis of the immune responses have evolved within the boundaries given by the species ecology. Here, we explore the evolution of some emblematic immune gene families throughout the Insecta phylum shedding light on remarkable genetic events such as gene duplication or gene loss. We followed a workflow based on the Hidden Markov model to search for immune genes in 55 high-quality genomes of insects. We highlight the emergence of group defence in social species as an ecological shift that released selection pressure on immune gene families notably in Blattodea. Further, we draw attention to certain gene families and the link between their diversity and the specificities of the species’ microbiota. Overall, we report data on immune gene diversity in insects.
The phylogeny of the Blattodea boasts a wide degree of sociality spanning from solitary cockroaches to advanced ecosystem-dominating higher termite societies. The emergence of sociality in the termites was associated with the acquisition of a diverse range of social structures and differential expression of specific gene network. Previous work has found evidence for a caste-specific social defence system in termites leading to an immune system that may favour group over individual defence. While preliminary work suggests a correlation between social transitions and a reduction of immune gene family diversity, the lack of available high-quality termite genomes hampers complete knowledge of the true diversity of immune gene evolution across termite phylogeny. Here, we report on the sequencing and assembly of 50 high-quality long-read-based genomes and 180 caste- and sex-specific brain transcriptomes across major termite and cockroach sister-branch lineage. We investigate the diversity and evolutionary history of immune genes across genomes, and the potential gene networks that have evolved with the emergence of termite sociality and some aspect of immune related behaviours.
The presentation gives an overview about the use of ecotoxicity testing in assessment of waste. Especially in cases with unknown composition this kind of test are useful. Recently, the assessment of the hazard property HP 14 "ecotoxicity" for the labelling of waste was published. The labelling procedure is explained in detail.
The presentation gives an overview about the use of ecotoxicity testing in assessment of waste. Especially in cases with unknown composition this kind of test are useful. Recently, the assessment of the hazard property HP 14 "ecotoxicity" for the labelling of waste was published. The labelling procedure is explained in detail.
The presentation gives an overview about the use of ecotoxicity testing in assessment of waste. Especially in cases with unknown composition this kind of test are useful. Recently, the assessment of the hazard property HP 14 "ecotoxicity" for the labelling of waste was published. The labelling procedure is explained in detail.
Fluorometric sensing is a versatile approach for trace analysis outside of the laboratory, requiring suitable sensor materials and their integration into sensing devices. The versatility of fluorophores as probes, especially in terms of the possibility to tailor their optical as well as their recognition properties by synthetic modifications in a wide range, renders them as superior active component for the preparation of optical sensing devices. Recent works at BAM in this field include, for example, the detection of nerve gas agents, illustrating impressively the aforementioned benefits of fluorophores in optical sensing applications.
In the interdisciplinary project presented here, we target hazardous gases such as ammonia, benzene, and hydrogen sulfide, next to others, which pose a major threat to human health and environmental safety and for which the availability of a sensitive and reliable detection method is highly desirable. The dyes presented follow a “turn-on” fluorescence schematic, which allows for the selective and sensitive detection of the respective gaseous analyte. The immobilization of the probe in polymeric matrices is then the next step toward the fabrication of a prototype device for molecular sensing. Further steps in the project include the assembly of instruments for test-atmosphere generation, the referencing of the sensor system, development and implementation of an optical setup, and the testing of the prototype device under laboratory conditions and in the field.
In this presentation, we give an overview over the recent developments on this topic in our groups. Highlights are hydrogen sulfide sensitive, BODIPY based transition metal complexes, which allow for a sensitive as well as selective detection of the toxic gas. In addition, we present a novel class of highly substituted BODIPY derivatives – pocket-BODIPYs – which are of a synthetically high versatility and can readily be modified to create pockets in the periphery of the molecule of defined geometries. This is illustrated on the successful encapsulation of benzene by a pocket-BODIPY derivative, confirmed by X-ray crystallographic analysis as well as by further spectroscopic and analytical methods.
Microbial contamination of fuels by fungi or bacteria poses risks such as corrosion and fuel system fouling, which can lead to critical problems in refineries and distribution systems and has a significant economic impact at every stage of the process. Many factors have been cited as being responsible for microbial growth, like the presence of water in the storage tanks. In fact, only 1 % water in a storage system is sufficient for the growth of microorganisms like bacteria or yeasts, as well as for the development of fungal biomass at the oil/water interface.
This work presents a rapid test for the accurate determination of genomic DNA from aqueous fuel extracts. The detection is based on the use of polystyrene-mesoporous silica core-shell particles onto which modified fluorescent molecular beacons are covalently grafted. These beacons contain in the hairpin loop a target sequence highly conserved in all bacteria, corresponding to a fragment of the 16S ribosomal RNA subunit. The designed single-stranded molecular beacon contained fluorescein as an internal indicator and a quencher in its proximity when not hybridized. Upon hybridization in presence of the target sequence, the indicator and the quencher are spatially separated, resulting in fluorescence enhancement. To perform the assay the developed particles were deposited on different glass fibre strips to obtain a portable and sensitive rapid test. The assays showed that the presence of genomic DNA extracts from bacteria down to 50–70 μg L–1 induced a fluorescence response. The optical read-out was adapted for on-site monitoring by fitting a 3D-printed case to a conventional smartphone, taking advantages of the sensitivity of the CMOS detector. Such embedded assembly enabled the detection of genomic DNA in aqueous extracts down to the mg L–1 range and represents an interesting step toward on-site monitoring of fuel contamination.
Innovation Network PerFluSan
(2020)
Per- and polyfluorinated alkyl substances (PFAS) are transferred into the environment as part of their broad industrial use, where they pose a problem due to their critical properties. The sustainable protection of people and the environment from this group of substances is an important task for the future. However, available PFAS removal and remediation processes are expensive and often inadequate. PerFluSan would like to make a relevant contribution to solve this problem by developing new PFAS remediation methods for soils and water, as well as innovative analytical methods for PFAS detection.
The long-term vision is to develop PerFluSan into a national contact point for the PFAS topic, which uses synergies between the PerFluSan actors to address all aspects of the problem holistically, sustainably and effectively.
Thermal Destruction of PFAS
(2023)
Thermal treatment processes are currently the only full-scale option for thedestruction of per- and polyfluoroalkyl substances (PFAS) in large waste streams. While all organic molecules including PFAS are susceptible to thermal destruction, their decomposition rates are controlled by process variables such as temperature, reaction atmosphere, and residence time. Concerns exist about the formation of products of incomplete destruction and their emission from hazardous waste incinerators. This talk will summarize the current stateof-the-art of thermal PFAS destruction, identify research needs, and showcase future research designed to address critical knowledge gaps.
Z02 is one of the three technically supporting projects at the CSMC. In collaboration with Z01 and Z03, it aims at bridging the gap between humanities and natural sciences and technology. To that purpose, we set up a laboratory with a range of high-end instruments, most of them mobile, allowing thorough non-destructive analysis of manuscripts. In addition to working on constantly improving the laboratory and the methods of analysis, a substantial part of our activities is dedicated to service, by supporting different research projects conducted at the center.
In this talk, we will present our equipment and the possibilities offered by the different techniques available regarding the different kinds of missions: typology and classification of inks, provenance studies, recovery of faded inscriptions and palimpsests, reconstruction of the history of manuscripts, authentication and dating. We will give a brief overview of our past and ongoing activities in the frame of the second phase of the CSMC. Finally, a selection of three projects will be presented in greater detail to highlight the possibilities of our laboratory and the diversity of missions which can be carried out:
- Support of project C08 on East Frankish manuscripts containing collections of formulae
- Identifying color materials applied in Muhammad Juki's Shahnamah with non-invasive combined methods
- Checking for the presence of metals in the Herculaneum papyri
Hundreds of papyrus rolls, carbonized during the 79CE eruption of Mount Vesuvius, were discovered in 1754 at Herculaneum. Sophisticated mechanical methods for unrolling the best-preserved scrolls have been applied, with varying success. However, such processes have been abandoned, to prevent risk from irremediable damage or loss and to preserve the integrity of the extremely fragile rolls. Following the development of X-ray based non-invasive techniques, attempts to virtually unroll the scrolls were made. The most common ink in Antiquity was carbon-based, and the main element of carbonized papyrus is carbon, making these investigations difficult. However, some attempts with synchrotron X-ray phase-contrast tomography (XPCT) were successful. Recently, the identification of antique inks containing metals raised hope that if some of the inks contain metal the rolls can be virtually unrolled using conventional CT- technique. We are presenting here the first results of a preliminary analysis, which aimed at identifying scrolls whose ink contains metals.
Z02 is one of the three technically supporting projects at the Centre for the Study of Manuscript Cultures (CSMC). In collaboration with the other two service projects, Z01 and Z03, it aims at bridging the gap between humanities and natural sciences and technology. To that purpose, we set up a laboratory with a range of high-end instruments, most of them mobile, allowing thorough non-destructive analysis of manuscripts. In addition to working on constantly improving the laboratory and the methods of analysis, a substantial part of our activities is dedicated to service, by supporting different research projects conducted at the centre. In this talk, we will present our equipment and the possibilities offered by the different techniques available regarding the different kinds of missions: typology and classification of inks, provenance studies, recovery of faded inscriptions and palimpsests, reconstruction of the history of manuscripts, authentication and dating. We will give a brief overview of our past and ongoing activities in the frame of the second phase of the CSMC. Finally, a selection of three projects will be presented in greater detail to highlight the possibilities of our laboratory and the diversity of missions which can be carried out.
Z02 is one of the three technically supporting projects at the Centre for the Study of Manuscript Cultures (CSMC). In collaboration with the other two service projects, Z01 and Z03, it aims at bridging the gap between humanities and natural sciences and technology. To that purpose, we set up a laboratory with a range of high-end instruments, most of them mobile, allowing thorough non-destructive analysis of manuscripts. In addition to working on constantly improving the laboratory and the methods of analysis, a substantial part of our activities is dedicated to service, by supporting different research projects conducted at the centre. In this talk, we will present our equipment and the possibilities offered by the different techniques available regarding the different kinds of missions: typology and classification of inks, provenance studies, recovery of faded inscriptions and palimpsests, reconstruction of the history of manuscripts, authentication and dating. We will give a brief overview of our past and ongoing activities in the frame of the second phase of the CSMC. Finally, a selection of projects will be presented in greater detail to highlight the possibilities of our laboratory and the diversity of missions which can be carried out.
The processing of laser-induced periodic surface structures (LIPSS) represents a simple and robust way for the nanostructuring of solids that allows creating a wide range of surface functionalities featuring applications in optics, tribology, medicine, energy technologies, etc. While the currently available laser and scanner technology already allows surface processing rates at the m2/min level, industrial applications of LIPSS are sometimes hampered by the complex interplay between the nanoscale surface topography and the specific surface chemistry. This typically manifests in difficulties to control the processing of LIPSS and in limitations to ensure the long-term stability of the created surface functions. This presentation aims to identify some unsolved scientific problems related to LIPSS, discusses the pending technological limitations, and sketches the current state of theoretical modelling. Hereby, it is intended to stimulate further research and developments in the field of LIPSS for overcoming these limitations and for supporting the transfer of the LIPSS technology into industry.
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.
The properties of nanomaterials are influenced not only by their chemical composition but also by physical properties (such as size, geometry and crystal structure). For the reliable determination and assessment of behaviour and effects of nanomaterials as well as for the determination of the exposure of humans and environment a comprehensive physical-chemical characterization of nanomaterials is essential. This is an important prerequisite to identify them as nanomaterials and to interpret and compare test results and - in future – to forecast interaction and effects of nanomaterials.
In 2006, the OECD launched a sponsorship program for the testing of nanomaterials in which 11 nanomaterials were thoroughly investigated using a variety of methods. The aim of the project was, among other things, to find out where problems occur and where there are gaps in the measurement and test procedures and where are changes required. An important outcome of the sponsorship program was the finding that the OECD Test Guidelines should in several cases be extended to the specific needs in testing of nanomaterials. The existing standardized test methods of the OECD for physical-chemical characterization have not been developed for nanomaterials in particular. A high demand for an extension of the test guidelines was identified. Germany complied with the OECD's request in 2017 and has agreed to extend the “Test Guideline on Particle Size Distribution / Fiber Length and Diameter Distributions Test Guideline” for Manufactured Nanomaterials (MN). UBA commissioned BAM and BAuA with the preparation of the Test Guideline. The aim of the project is the development of a harmonized test protocol for a valid and reproducible determination of particle size and size distribution which is one of the most relevant physical-chemical properties for MNs.
Different measuring methods provide different results for the size distribution of the particles. This is caused by the different measuring principles of the methods. Each method measures a specific parameter that ultimately determines particle size. First, the measured quantity differs for each method (Scattered light intensity, 2D image / projection, electric mobility, etc.). Second, the calculated diameters of the MN may differ (Feret Diameter, Area Projection, Mobility Diameter, Aerodynamic Diameter, Hydrodynamic Diameter). Third, a measuring method provides a size distribution which is measured either mass-based, surface-based or number-based. A conversion between the results requires additional parameters and thus possibly increases the measurement error.
In addition to the technical differences, the individual parameters are strongly influenced by the structure and material of the nanoparticles. For example, a surface functionalization can lead to very different results in the size distribution. The suitability of measurement methods differs with the material of the MN. As a result, two very different results can be measured for the particle size distribution using two different methods, which are nevertheless both correct. Several large projects in recent years therefore concluded that nanomaterials should be characterized by at least two complementary method. Imaging techniques are regarded as one of these methods for the characterization, the complementary methods are supposed to be statistical methods.
The different results for the size distribution of nanomaterials become problematic for the registration of new MN. A comparable and reproducible size distribution is a prerequisite for a standardized registration. In the future, the particle size distribution in the EU will also decide on the classification of a substance as a nanomaterial or as a non-nanomaterial. Especially in borderline cases, a standardized and comparable measurement methodology is therefore essential.
The intention of the presentation is to inspire a discussion on the needs and challenges for the digitalisation of SOPs. SOPs are available for the disciplines of physical-chemical characterisation, for toxicology, for environmental applications and for exposure applications. Furthermore the SOPs need to be integrated in the regulatory framework and need to be detailed enough for the digital processing. This is highlighted in this presentation.
This presentation was held in an OECD Webinar introducing the newly developed and published OECD TG 125 on particle size and size distribution. The presentation is explaining the structure if the TG 125 and addresses all included methods and methodologies in a short and understandable way for the broader public. The presentation includes sections about nano-particles and nano-fibres.
Simple particulate matter sensors are gaining popularity due to their low price, easy handling and good temporal resolution. In this presentation, we report on the performance of a Sharp optical PM sensor GP2Y1010AU0F, which costs less than 15 €.
The sensor is built around an infrared emitting diode (ILED) and a phototransistor detecting the light scattered from the aerosol particle. An electronic circuit shapes the detected light in a pulsed signal. The manufacturer advises sampling the output signal 280 microseconds after the ILED pulse. The measured output voltage is an indicator of dust concentration.
We have built two identical simple PM monitoring devices using Raspberry Pi 3 computer interfacing the PM sensor with Microchip’s MCP3002 ADC via SPI. The ADC is capable of more than 100 ksamples/s at 10-bit resolution. The Rpi3 was pulsing the sensor at 10Hz, digitizing and saving the data and sending the results wirelessly.
Sensor’s output pulse shape was sampled with 10 microsecond time steps and saved, thus making offline analysis possible. A time jitter of output pulses can be observed and suggests a peak fitting as a better approach to the signal readout compared to the single sampling at a fixed time after pulse triggering We compared both methods.
Generation of Cryomyces antarcticus mutants to explore the importance of DHN melanin for survival
(2023)
Cryomyces antarcticus, a cryptoendolithic melanized fungus endemic to Antarctica (phylum Ascomycota, class Dothideomycetes incertae sedis), has demonstrated high capability to survive extreme environmental conditions like those found in space (e.g., ionizing radiation, vacuum, microgravity), thus fueling fundamental astrobiological questions like “the search for life beyond Earth”. Its extraordinary resilience has been attributed to the presence of thick, highly melanized cell walls, which may contain both DHN and DOPA melanins. To better understand the contribution of DHN melanin to the overall resilience of C. antarcticus, we decided to generate melanin-deficient mutants by genetic engineering. For this, the melanin-PKS (polyketide synthase)- encoding ortholog was identified in the C. antarcticus CBS 116301 genome and used to design primers for re-sequencing of the capks1 locus in the strain CCFEE 515. Based on the genetic toolkit developed for the black fungus Knufia petricola, we designed a strategy for mutating capks1. Protoplasts of C. antarcticus CCFEE 515 were generated and co-transformed with a circular AMA-containing plasmid for expression and in-vivo assembly of Cas9 and two capks1-specific sgRNAs and a PCR-generated donor DNA i.e., a hygromycin resistance cassette flanked by ~75-bp-long sequences homologous to the capks1 locus. Transformation of C. antarcticus is challenging because of its very slow growth and uncertain gene copy number. It took six months from obtaining enough biomass for cell wall lysis to transferring the putatively resistant transformants for genotyping, but we eventually managed to generate three independent non-melanized (whitish) Δcapks1 mutants! We are now awaiting first complemented strains as ultimate genetic transformation control. They are considered to have a wild-type-like pigmentation due to the reintroduction of the wild-type capks1 into the Δcapks1 mutant.
This study focuses on the analysis of a corpus of manuscripts found in Fustat (medieval Cairo, Egypt) in the biggest medieval “archive” found until now: the Cairo Geniza. The giant collection of mostly Jewish documents has been attracting scholars’ attention a lot but so far, the material aspects of these documents seem to have been mainly neglected.
Application of scientific methods of analysis, especially X-Ray fluorescence characterization, contributes to our understanding of the materials used for production of manuscripts during the Middle ages.
Our corpus of the 11th century manuscripts comprises manuscripts written by scribes belonging to three Jewish communities that co-existed in Cairo during this period: the Karaites, the so-called Jerusalemites (or Palestinian) and the so-called Babylonians (or Iraqi), three different communities with different traditions and different leaders. The differences manifest themselves also in the paleographical properties of the manuscripts produced within each community. Can we extend the differences detected by the paleographical analysis to differences in composition of the writing materials and especially the composition of the inks? Or can we relate the differences in the composition to the manuscript type (legal, private...), or to another criterion. In this presentation, we offer answers to some of the questions using statistical analysis of the measurements results.
This study focuses on the analysis of a corpus of manuscripts found in Fustat (medieval Cairo, Egypt) in the biggest medieval “archive” found until now: the Cairo Geniza. The giant collection of mostly Jewish documents has been attracting scholars’ attention a lot but so far, the material aspects of these documents seem to have been mainly neglected.
Application of scientific methods of analysis, especially X-Ray fluorescence characterization, contributes to our understanding of the materials used for production of manuscripts during the Middle ages.
Our corpus of the 11th century manuscripts comprises manuscripts written by scribes belonging to three Jewish communities that co-existed in Cairo during this period: the Karaites, the so-called Jerusalemites (or Palestinian) and the so-called Babylonians (or Iraqi), three different communities with different traditions and different leaders. The differences manifest themselves also in the paleographical properties of the manuscripts produced within each community. Can we extend the differences detected by the paleographical analysis to differences in composition of the writing materials and especially the composition of the inks? Or can we relate the differences in the composition to the manuscript type (legal, private...), or to another criterion. In this presentation, we offer answers to some of the questions using statistical analysis of the measurements results.
The Cairo Genizah is a well-known “archive” discovered in the 19th century in Ben Ezra Synagogue in Fustat, a district in Old Cairo (Egypt), located south of the center of modern Cairo. The giant collection of mostly Jewish documents that vary in genres, languages and writing supports contains a large number of early medieval Hebrew manuscripts, mostly in fragmentary form. The larger part of the Cairo Genizah is stored today in the Cambridge University Library, containing about 200,000 fragments.
The Genizah provides sources for the literary, linguistic, historical studies of the various aspects Jewish and non-Jewish life. As the documents attest, at least two Jewish communities co-existed in Fustat up to 11th century: a so-called Babylonian and Palestinian. These communities had different leaders, different traditions and lived independently. The differences manifest themselves also in the paleographical properties of the manuscripts produced by each community.
Although Genizah manuscripts have attracted a great deal of scholarly attention, the material aspects of these documents seem to have been largely neglected. The current study aims to obtain information on the composition of the writing supports and the inks used, in order to obtain insights on trade, local production techniques and social structures.
Can we extend the differences detected by the paleographical analysis to differences in composition of the writing materials ? Can we relate the differences in the composition to a community, to the manuscript type (legal, private...), or to another criterion?
Results:
- Four types of inks were measured iron gall (vitriolic and non vitriolic), carbonic, mixed and vegetable inks.
- We need to start analyzing systematically the organic part of the inks.
- Great variety in the composition of the inks.
- No correlation between the type of ink used and any other criteria apart from a personal preference.
- Inks purchased by (some) scribes.
- Reconstruction of the chronology of writing and signing of certain legal documents.
- Comparison with documents written by the Muslim court.
In recent years the BAM has been focusing on the characterization of the writing materials of the medieval Torah scrolls. The challenge imposed by the study of this specific type of manuscript led to designing and building dedicated stages to ensure the safety of the scrolls during the analysis. Furthermore, the identification of multiple corrections executed in apparently identical inks required broadening the standard two-step protocol of near infrared reflectography and X-ray fluorescence to include multispectral imaging. This work has prepared the division to participate in the large collaborative project “To roll: Materialisierte Heiligkeit (Materialised Holiness)” based at the Free University, Berlin.
The presentation will demonstrate the aims of the studies, preliminary results and the strategies adopted by the division 4.5 of the BAM.
The Cairo Geniza is an “archive” discovered in the 19th century in Ben Ezra Synagogue in Fustat, a district in Old Cairo (Egypt). The collection of mostly Jewish documents that vary in genres, languages and writing supports contains a large number of early medieval Hebrew manuscripts.
The Geniza provides sources for the literary, linguistic, historical studies of the various aspects Jewish life. As the documents attest, at least two Jewish communities co-existed in Fustat up to 11th century: a so-called Babylonian and Palestinian. These communities had different leaders, different traditions and lived independently. The differences seem to manifest themselves also in the paleographical, codicological and some material properties of the manuscripts produced by each community.
The aim of this project is to compare the inks used in the Jewish documents depending on different variables: support (paper, parchment), purpose of the manuscript (legal, private, religious), provenance of the scribe. For the determination of the inks type and composition we had to choose non-invasive, non-destructive and portable techniques to analyze the corpus directly on-situ.
The analyses were carried out with a micro-X-ray spectrometer ArtTAX® (Bruker GmbH) and a digital stereomicroscope features built-in LED illumination at 395 nm and 940nm, Dino Lite.
We would like to stress that though the methods of material analysis listed above have been successfully employed in the field of cultural heritage and conservation including ancient and medieval manuscripts they have not yet been used to study fragments from the Cairo Genizah. Therefore, we believe that this research project is a pioneering study that will provide new insights into the history of Hebrew writing materials, their production techniques and materials and, thus, contribute new data to the field of Hebrew paleography.
In the 15th century, Persian manuscripts underwent significant and lasting changes. Possibly as a response to the import of tinted and gold-decorated paper from China, which was used for manuscript production in Greater Iran, Persian papers were also tinted and embellished with gold-decorated and marbled margins or frames. In a joint project between CSMC and the University of St Andrews, we aim to analyse papers and their decorations in Persian The analyses aim to determine the consistencies of papers, pigments and metals and the techniques used for their production and application. The support will be first described in its codicological characteristics such as dimensions, thickness, colour (expressed in colour coordinates), pattern left from the sieve (observed in transmitted light). The plant used as raw material in paper production will be studied by fibres analysis, while the sizing agents, the pigments, dyes and metals will be analysed by the application of several methods: in particular Reflectography, X-Ray Fluorescence and InfraRed, Raman and Visible Reflectance Spectroscopy. The results of the analyses will form an important resource for the material aspects of Persian manuscripts and be a starting point for establishing a first chronology of the materials and techniques used in Persian manuscript production. An example of the application of the techniques on the analysis of a fragment from a 15th c. Persian Manuscript will be provided.
Papyrus was in use in the Islamic world until the 11th century and few ink recipes collected from treatises about the art of the books are dedicated to this support. But papyrus was also burnt in order to obtain soot used as an ingredient for a particular type of ink (midād al-qarāṭīs). In this talk I will give an overview of the recipes – in particular those by ar-Rāzī –, their context and transmission in order to evaluate this double nature of papyrus, which is considered at the same time a writing support and a material to be recycled. Moreover, I will discuss what kinds of ink are most likely to be found, according to these literary sources, on Arabic manuscripts and documents written on papyrus and compare them to the typologies mentioned for paper and parchment. These results are the premises of a research project starting at the beginning of 2019, in which a number of dated fragments from several European institutions will be analysed with non-destructive techniques in order to establish a profile of the main writing media used in the early centuries of the Islamic Era.
Fifty shades of black: Typologies and terminology of black inks in the light of new discoveries
(2019)
The identification of the materials constituting an artefact is the basis of any correct conservation project. For this reason (among others) in the last 50 years analytical techniques have been applied to the study of manuscripts. Unfortunately, the scientific investigation of Arabic books is still uncommon, focusing mainly on single case studies of illuminated manuscripts where the black media used to write the text is largely overlooked. This lack of knowledge prompted a recent research in which black ink recipes have been collected from written Arabic sources, their feasibility has been assessed, and some of them have been reproduced. These samples were artificially aged and analysed through an array of analytical techniques, mostly non-invasive and non-destructive, in order to build a database of Arabic inks and their ingredients and to verify the detection limits of the equipment employed. Finally, the results were compared to the data collected from historical manuscripts.
In this talk I will focus on the ink typologies and the terminology (ancient and modern) used to describe them. In particular I will highlight how even the modern classification fails to capture the variety encountered in both recipes and manuscripts, particularly in the light of recent discoveries. I will address especially the terminological and conceptual issues of mixed inks – in the form of carbon inks and tannins, of carbon and iron gall inks, and of carbon and metallic salts –, iron gall inks made without vitriol and iron gall inks made with sources of tannins different from gall nuts.
Ink recipes from the islamic era: Texts, manuscripts, ink reproductions and scientific analyses
(2019)
Ink recipes can often be found in Arabic manuscripts. They may be included in treatises of diverse subjects – from handbooks for secretaries or calligraphers to books on arts and crafts, to alchemical and astrological essays. Recipes can also appear, with or without relation to the main text in the manuscript, in the form of lists or collections or even added in empty spaces as single entries. Why were these recipes written down? Were they used by the many professionals dealing with inks in their every-day work? Or were they part of the literary genre of adab with little or no practical application? To answer these questions a research project was set up: ink recipes have been collected from written Arabic sources, their feasibility has been assessed and some of them have been reproduced. These samples were artificially aged and analysed through an array of analytical techniques, most non-invasive and non-destructive, and the results compared to the data obtained by the application of the same analyses on concrete manuscripts. The codicological characteristics of the manuscripts have also been studied. My aim in this talk is to show how such an interdisciplinary approach could be beneficial for the study of material culture.
This talk will be divided into two parts. In the first part I will present the analytical techniques and the equipment used by the Centre for the Study of Manuscript Cultures that can be applied for the study of decorated papers. The analyses aim to determine the constituent materials of papers, pigments, dyes and metals and the techniques used for their production. I will focus in particular on the kind of information these techniques allow us to gather: through optical microscopy we conduct fibre analysis in order to identify the plant used as raw material in paper production while Reflectography, X-Ray Fluorescence and InfraRed, Raman and Visible Reflectance Spectroscopy are used to study the sizing agents, the pigments, dyes and metals. In the second part I will show some results obtained by the application of these techniques on a few Persianate manuscripts, dating between the 15th and 17th centuries, belonging to the corpus of Ilse Sturkenboom.
The Interdisciplinary Alchemist: Reproduction and Study of Black Inks from the Islamicate World
(2019)
The identification of the materials constituting an artefact is the basis of any correct conservation project, for this reason (among others) in the last 50 years analytical techniques have been applied to the study of manuscripts. Unfortunately, the scientific investigation of Arabic books is still uncommon, focusing mainly on single case studies, often producing unclear results, especially for black inks. This lack of knowledge prompted a recent research in which black ink recipes have been collected from written Arabic sources on bookmaking, their feasibility has been assessed, and finally some of them have been reproduced. These samples were artificially aged and analysed through an array of analytical techniques, mostly non-invasive and non-destructive, in order to build a database of Arabic inks and their ingredients and also to verify the detection limits of the portable equipment employed. In this talk I will present some instances of how this approach can help textual criticism, for example in evaluating variants and determining the competence of authors and compilers. At the same time the research highlights how much this scientific work depends on textual studies, especially concerning the identification of ingredients. Moreover, I will focus on some of the problematics I faced both during the textual interpretation and the actual reproduction of the recipes and how they influenced the results of the scientific analyses. In particular I’ll look into the role played by the degree of purity of the components and the function (real and perceived) of some of the ingredients.
In the 15th century, Persian manuscripts underwent significant and lasting changes. Possibly as a response to the import of tinted and gold-decorated paper from China, which was used for manuscript production in Greater Iran, Persian papers were also tinted and embellished with gold-decorated and marbled margins or frames. In a joint project between CSMC and the University of St Andrews, and in co-operation with the Golestan Palace Museum, we aim to analyse papers and their decorations in manuscripts in the holdings of the Golestan Palace Library. The analyses aim to determine the consistencies of papers, pigments and metals and the techniques used for their production and application. The support will be first described in its codicological characteristics such as dimensions, thickness, colour (expressed in colour coordinates), pattern left from the sieve (observed in transmitted light). The plant used as raw material in paper production will be studied by fibres analysis, while the sizing agents, the pigments, dyes and metals will be analysed by the application of several methods: in particular Reflectography, X-Ray Fluorescence and InfraRed, Raman and Visible Reflectance Spectroscopy. The results of the analyses will be published in an online database that will form an important resource for the material aspects of Persian manuscripts and be a starting point for establishing a first chronology of the materials and techniques used in Persian manuscript production.
EN 16516 sets the test method and requirements for the determination of emissions of Volatile Organic Compounds (VOCs) from building materials into indoor air. To address the quality control requirements for the class of semi-VOCs (SVOCs), VSL developed gaseous reference materials. A novel home-made dynamic gas mixture preparation system, operating according to ISO 6145-4 (continuous injection method), has recently been developed and validated. Thanks to the stable temperature control up to 100 oC, the system can prevent condensation of the SVOCs in air at indoor air concentration levels. The in-situ obtained SVOC gas standards can be sampled in sorbent tubes to obtain SVOC transfer standards. A study was performed to determine the optimal sorbent material and storage conditions. This study will be presented together with the results of the 2018 Round Robin test for emission test chamber measurements organised by BAM. Using the novel system, VSL prepared transfer standards with known amounts of VOCs and SVOCs for participants to evaluate their analytical performance.
Rock-inhabiting black fungi are adapted to survive extreme stresses such as radiation and lack of water and are thus able to colonise arid material surfaces like solar panels and marble monuments. Black fungi can typically grow as one of two cell types: depending on the environmental conditions, they are able to form yeast-like cells or hyphal filaments. Knufia petricola is one member of the rock-inhabiting black fungi which functions as a model reference species. As there is no mathematical model for biofilm formation of RIF, we are going to develop a model for K. petricola which describes fungal growth on the level of individual cells adn biofilm formation.
Corrosion is a very expensive and serious problem in the different industry sectors, eg. Petroleum-, On- and off-shore, infrastructure. It is estimated that 20% of all corrosion damage is caused by microorganisms or microbiologically influenced corrosion (MIC). Several microorganisms are known to cause corrosion, including sulfate-reducing bacteria, nitrate-reducing bacteria, methanogens etc. For several years, methanogens were regarded as a mild corroder (~0.065 mm/yr), largely due to a lack of detailed investigation on the corrosion mechanism under real-environment simulated conditions. Resulting in the common belief that siderite, a non-conductive compound, is the sole corrosion product (CP) of methanogen-induced MIC (Mi-MIC).
To simulate natural environmental conditions, we developed and introduced the multiport flow column system (MFC), a multi-sectional corrosion flow-cell. Using the MFC, we obtained ten times higher corrosion rates than previously reported. With a combination of several analytical techniques, such as ToF-SIMS, SEM-EDS and FIB-SEM, we found strong indication that siderite is not the sole corrosion product of Mi-MIC. The corrosion layers contained phosphorus, oxygen, magnesium, calcium and iron. The differences in the CP between static and dynamic environments demonstrated the impact of testing procedures on the corrosive potential of methanogens. To further verify and deepen our understanding of Mi-MIC, we are currently studying the influence of additional environmental parameters (e.g. pH, salinity, flow rate) on Mi-MIC.
Overall, results of this study will expand the current understanding of MIC from both analytical and mechanistic points of view, thus aiding the development of different mitigation strategies for various industry sectors.
Microbiologically influenced corrosion (MIC) is a now well-known challenge and affects industry, society and infrastructure. For a long time, the impact of methanogen-induced MIC (Mi-MIC) was underestimated. This was mainly due to the rather low published corrosion rates and the presumed corrosion product siderite, which is not electrically conductive. In our laboratory, we were able to show that this trivialization or underestimation of Mi-MIC was due to the nature of the testing. The static systems used so far do not provide environmentally relevant information about the corrosion rate and the corrosion product, especially for methanogens
To further illustrate the importance of the environment on the MIC process, we established a multiport flow column (MFC), to simulate the natural environment. With this method, and in contrast to published results using the static conditions, we obtained ten times higher corrosion rates. We analyzed the corrosion products with a combination of techniques, like ToF-SIMS, SEM-EDS and FIB-SEM, and found strong evidence that siderite is not the sole corrosion product of Mi-MIC. The corrosion layers contain phosphorus, oxygen, magnesium, calcium and iron and lacked on carbon-related species. It is hypothesized that methanogens may have influenced the nucleation process of siderite, converting bicarbonate into carbon dioxide for methanogenesis. This results in increased localized corrosion and reduced siderite formation. To verify and deepen our understanding of Mi-MIC, we are currently studying the influence of additional environmental parameters (e.g. pH, salinity, flow rate etc.) on Mi-MIC and the subsequent impacts on corrosion rates and the corrosion products.
Overall, results of this study will expand the current understanding of MIC from both analytical and mechanistic points of view, thus aiding the development of different mitigation strategies for various industry sectors.