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Organisationseinheit der BAM
- 6 Materialchemie (12)
- 1 Analytische Chemie; Referenzmaterialien (8)
- 6.3 Strukturanalytik (7)
- 4 Material und Umwelt (6)
- 7 Bauwerkssicherheit (6)
- 1.4 Prozessanalytik (5)
- 7.5 Technische Eigenschaften von Polymerwerkstoffen (5)
- 2 Prozess- und Anlagensicherheit (4)
- 8 Zerstörungsfreie Prüfung (4)
- 2.1 Sicherheit von Energieträgern (3)
- 4.0 Abteilungsleitung und andere (3)
- 6.6 Physik und chemische Analytik der Polymere (3)
- 5 Werkstofftechnik (2)
- 5.4 Multimateriale Fertigungsprozesse (2)
- 6.1 Oberflächen- und Dünnschichtanalyse (2)
- 6.5 Synthese und Streuverfahren nanostrukturierter Materialien (2)
- 8.1 Sensorik, mess- und prüftechnische Verfahren (2)
- 8.4 Akustische und elektromagnetische Verfahren (2)
- 1.2 Biophotonik (1)
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- 4.1 Biologische Materialschädigung und Referenzorganismen (1)
- 4.3 Schadstofftransfer und Umwelttechnologien (1)
- 4.4 Thermochemische Reststoffbehandlung und Wertstoffrückgewinnung (1)
- 4.5 Kunst- und Kulturgutanalyse (1)
- 7.4 Baustofftechnologie (1)
Subsurface granitic environments are scarce and poorly investigated. A multi-disciplinary approach was used to characterize the abundant moonmilk deposits and associated microbial communities coating the granite walls of the 16th Century Paranhos spring water tunnel in Porto city (north-west Portugal). It is possible that this study is the first record of moonmilk in an urban subsurface granitic environment. The morphology and texture, mineralogical composition, stable isotope composition and microbial diversity of moonmilk deposits have been studied to infer the processes of moonmilk formation. These whitish secondary mineral deposits are composed of very fine needle fibre calcite crystals with different morphologies and density. Calcified filaments of fungal hyphae or bacteria were distinguished by field emission scanning electron microscopy. Stable isotope analysis revealed a meteoric origin of the needle fibre calcite, with an important contribution of atmospheric CO2, soil respiration and HCO3 − from weathering of Ca-bearing minerals. The DNA-based analyses revealed the presence of micro-organisms related to urban contamination, including Actinobacteria, mainly represented by Pseudonocardia hispaniensis, Thaumarchaeota and Ascomycota, dominated by Cladosporium. This microbial composition is consistent with groundwater pollution and contamination sources of the overlying urban area, including garages, petrol stations and wastewater pipeline leakage, showing that the Paranhos tunnel is greatly perturbed by anthropogenic activities. Whether the identified micro-organisms are involved in the formation of the needle fibre calcite or not is difficult to demonstrate, but this study evidenced both abiotic and biogenic genesis for the calcite moonmilk in this subsurface granitic environment.
This work aims to address the technical aspects related to the thermodynamic characterization of natural gas mixtures blended with hydrogen for the introduction of alternative energy sources within the Power-to-Gas framework. For that purpose, new experimental speed of sound data are presented in the pressure range between (0.1 up to 13) MPa and at temperatures of (260, 273.16, 300, 325, and 350) K for two mixtures qualified as primary calibration standards: a 11 component synthetic natural gas mixture (11 M), and another low-calorific H2-enriched natural gas mixture with a nominal molar percentage x(H2) = 3 %.
Measurements have been gathered using a spherical acoustic resonator with an experimental expanded (k = 2) uncertainty better than 200 parts in 106 (0.02 %) in the speed of sound. The heat capacity ratio as perfect-gas gammapg, the molar heat capacity as perfect-gas Cp,m pg, and the second betaa and third gammaa acoustic virial coefficients are derived from the speed of sound values. All the results are compared with the reference mixture models for natural gas-like mixtures, the AGA8-DC92 EoS and the GERG-2008 EoS, with Special attention to the impact of hydrogen on those properties. Data are found to be mostly consistent within the model uncertainty in the 11 M synthetic mixture as expected, but for the hydrogen-enriched mixture in the limit of the model uncertainty at the highest measuring pressures.
Speed of sound is one of the thermodynamic properties that can be measured with least uncertainty and is of great interest in developing equations of state. Moreover, accurate models are needed by the H2 industry to design the transport and storage stages of hydrogen blends in the natural gas network. This research aims to provide accurate data for (CH4 + H2) mixtures of nominal (5, 10, and 50) mol-% of hydrogen, in the p = (0.5 up to 20) MPa pressure range and with temperatures T = (273.16, 300, 325, 350, and 375) K. Using an acoustic spherical resonator, speed of sound was determined with an overall relative expanded (k = 2) uncertainty of 220 parts in 10^6 (0.022%). Data were compared to reference equations of state for natural gas-like mixtures, such as AGA8-DC92 and GERG-2008.
Average absolute deviations below 0.095% and percentage deviations between 0.029% and up to 0.30%, respectively, were obtained. Additionally, results were fitted to the acoustic virial equation of state and adiabatic coefficients, molar isochoric heat capacities and molar isobaric heat capacities as perfect-gas, together with second and third acoustic virial coefficients were estimated. Density second virial coefficients were also obtained.
This work aims to address the technical concerns related to the thermodynamic characterization of gas mixtures blended with hydrogen for the implementation of hydrogen as a new energy vector. For this purpose, new experimental speed of sound measurements have been done in gaseous and supercritical phases of two binary mixtures of nitrogen and hydrogen using the most accurate technique available, i.e., the spherical acoustic resonator, yielding an experimental expanded (k = 2) uncertainty of only 220 parts in 106 (0.022%). The measurements cover the pressure range between (0.5 and 20) MPa, the temperature range between (260 and 350) K, and the composition range with a nominal mole percentage of hydrogen of (5 and 10) mol%, respectively.
From the speed of sound data sets, thermophysical properties that are relevant for the characterization of the mixture, namely the second βa and third γa acoustic virial coefficients, are derived. These results are thoroughly compared and discussed with the established reference mixture models valid for mixtures of nitrogen and hydrogen, such as the AGA8-DC92 EoS, the GERG-2008 EoS, and the recently developed adaptation of the GERG-2008 EoS, here denoted GERG-H2_improved EoS. Special attention has been given to the effect of hydrogen concentration on those properties, showing that only the GERG-H2_improved EoS is consistent with the data sets within the experimental uncertainty in most measuring conditions.
The publicly available document encapsulates the first version of the Catalogue of Services of the future EC4Safenano Centre (CoS 2019).
The CoS 2019 is structured in 12 Service Categories and 27 Service Topics, for each of the 12 categories considered. This architecture configures a 12 x 27 matrix that allows ordering the potential EC4Safenano offer in 324 types of services/groups of services.
Each type of service/group of services is described, in a simple and friendly way, by means of a specific service sheet: the EC4Safenano - Service Data Sheet (EC4-SDS). These EC4-SDSs allow structuring and summarizing the information of each service, providing the customer with a concise view of characteristics of the service and also the contact details with the service provider.
The CoS 2019 deploys a map of services consisting of a set of 100 EC4-SDSs, covering 7 of the 12 Service Categories and 17 of the 27 Service Topics.
The harmonization of services is visualized as a future necessary step in EC4Safenano, in order to strengthen the offer and provide added value to customers with a growing offer of harmonized services in future versions of the CoS.
The information contained in this document is structured in 3 main sections, as follows:
• Catalogue structure. This section describes in short the main characteristics of the CoS 2019.
• Catalogue content. This section represents the core part of the document and encapsulates the set of 100 SDSs displaying the offer proposed by the CoS 2019.
• Online Catalogue. This section describes the resources implemented by EC4Safenano to facilitate the on-line consultation of the CoS 2019 by customers and other interested parties.
The Scythica Vindobonensia, the new fragments on Gothic incursions into Roman provinces in the Balkans in the middle of the third century AD that were revealed some years ago in a Greek palimpsest at the Austrian National Library in Vienna (ÖNB), are commonly considered as one of the most important additions of the last decades to the corpus of texts from classical Antiquity. Tere is a high degree of confdence among scholars in supposing that the fragments come from the lost work Scythica written in Greek by the third-century historian P. Herennius Dexippus (Δέξιππος) of Athens. The new fragments have hence also been called Dexippus Vindobonensis. In his Scythica, Dexippus recorded wars of the Romans with the Goths (and other tribes) whom he called Scythians.
The work had been hitherto known only from excerpts and quotes by later authors. Eight pages of a Byzantine manuscript copy of the ancient text have survived hidden underneath the visible surface of the last four parchment folios of the Vienna manuscript Historicus graecus 73, f. 192r -195v4. The copy is written in a Greek calligraphic minuscule which has been estimated by palaeographers to be of the middle or the second half of the eleventh century. In the thirteenth century, the text (on each of the eight pages arranged in one column, with 30 lines per page) was washed of the parchment and the valuable material made from animal skin was re-used for Christian texts. The new writing largely covered the faded remnants of the original text. It thus became hidden from the human eye for more than seven hundred years. Its discovery by Jana Grusková, a classical philologist specialized in the transmission of Greek texts, resulted from a systematic review of all Greek palimpsests kept at the Austrian National Library in Vienna at the beginning of the twenty-first century and a detailed examination of the four folios in 2007-20097.
Recent DNA-based studies have shown that the built environment is surprisingly rich in fungi. These indoor fungi – whether transient visitors or more persistent residents – may hold clues to the rising levels of human allergies and other medical and building-related health problems observed globally. The taxo¬nomic identity of these fungi is crucial in such pursuits. Molecular identification of the built mycobiome is no trivial undertaking, however, given the large number of unidentified, misidentified, and technically compromised fungal sequences in public sequence databases. In addition, the sequence metadata required to make informed taxonomic decisions – such as country and host/substrate of collection – are often lacking even from reference and ex-type sequences. Here we report on a taxonomic annotation workshop (April 10–11, 2017) organized at the James Hutton Institute/University of Aberdeen (UK) to facilitate reproducible studies of the built mycobiome. The 32 participants went through public fungal ITS bar¬code sequences related to the built mycobiome for taxonomic and nomenclatural correctness, technical quality, and metadata availability. A total of 19,508 changes – including 4,783 name changes, 14,121 metadata annotations, and the removal of 99 technically compromised sequences – were implemented in the UNITE database for molecular identification of fungi (https://unite.ut.ee/) and shared with a range of other databases and downstream resources. Among the genera that saw the largest number of changes were Penicillium, Talaromyces, Cladosporium, Acremonium, and Alternaria, all of them of significant importance in both culture-based and culture-independent surveys of the built environment.
DICONDE in der ZfP
(2023)
DICONDE (Digital Imaging and Communication in Non-Destructive Evaluation) ist ein offener internationaler Standard zur Speicherung und zum Austausch industrieller Prüfdaten und prozessbezogener Informationen. Der DICONDE-Standard definiert sowohl die Semantik für eine strukturierte Speicherung von Daten als auch die netzwerkbasierte Kommunikation zwischen zwei Endpunkten. Damit lassen sich viele Vorgänge von Prüfprozessen digital und sicher abbilden und gleichzeitig normative Anforderungen wie eine Rückführbarkeit zum Prüfer und Prüfobjekt sowie eine Reproduzierbarkeit von Prüfergebnissen erfüllen.
DICONDE (Digital Imaging and Communication in Non-Destructive Testing) is an open international standard for storing and exchanging industrial test data and process-related information. The DICONDE standard defines both the semantics for structured storage of data and the network-based communication between two endpoints. This allows many test processes to be mapped digitally and securely, while at the same time meeting normative requirements such as traceability to the tester and test object and reproducibility of test results.
High Speed, High Resolution imaging spectrometers based on pnCCDs for XRF and XRD applications
(2016)
For many years pnCCDs have been well known as X-ray detectors for spectroscopic imaging in many fields of science: X-Ray Fluorescence analysis (XRF), X-ray Diffraction (XRD) with light sources in large accelerator facilities as well as with laboratory light sources or with X-rays from celestial sources in X-ray astronomy. A brief introduction in GEXRF (Grazing Emission XRF) measurements with a laboratory laser produced plasma source will be given, PIXE (Particle Induced X-ray Emission) measurements and D2XRF (Double Dispersive X-Ray Fluorescence) and Slicing experiments with pnCCDs coupled to polycapillary optics performed at the BESSY synchrotron will be shown. Energy-dispersive Laue diffraction with ultra-hard X-rays for the analysis of defects in metals will conclude the overview of spectroscopic X-ray imaging measurements in the field of structure and dynamics of matter.
In a color X-ray camera spatial resolution is achieved by means of a polycapillary optic conducting X-ray photons from small regions on a sample to distinct energy dispersive pixels on a CCD matrix. At present, the resolution limit of color X-ray camera systems can go down to several microns and is mainly restricted by Pixel dimensions. The recent development of an efficient subpixel resolution algorithm allows a release from pixel size, limiting the resolution only to the quality of theoptics. In this work polycapillary properties that influence the spatial resolution are systematized and assessed both theoretically and experimentally. It is demonstrated that with the current technological Level reaching one micron resolution is challenging, but possible.
Purpose – This purpose of this paper is to report about the temperature distribution in metal and ceramic powder beds during 3D printing. The differing powders are thoroughly characterized in terms of thermal conductivity, thermal diffusivity, emissivity spectra and density.
Design/methodology/approach – The temperature distribution was measured in a 3D printing appliance (Prometal R1) with the help of thin thermocouples (0.25 mm diameter) and thermographic imaging. Temperatures at the powder bed surface as well as at differing powder bed depths were determined. The thermal conductivity, thermal diffusivity and emissivity spectra of the powders were measured as well. Numerical simulation was used to verify the measured temperatures.
Findings – The ceramic powder heated up and cooled down more quickly. This finding corresponds well with numerical simulations based on measured values for thermal conductivity and thermal diffusivity as well as emissivity spectra. An observed color change at the metal powder has only little effect on emissivity in the relevant wavelength region.
Research limitations/implications – It was found that thermocouple-based temperature measurements at the powder bed surface are difficult and these results should be considered with caution.
Practical implications – The results give practitioners valuable information about the transient temperature evolution for two widely used but differing powder systems (metal, ceramic). The paramount importance of powder bed porosity for thermal conductivity was verified. Already small differences in thermal conductivity, thermal diffusivity and hence volumetric heat capacity lead to marked differences in the transient temperature evolution.
Originality/value – The paper combines several techniques such as temperature measurements, spectral emissivity measurements, measurements of thermal conductivity and diffusivity and density measurements. The obtained results are put into a numerical model to check the obtained temperature data and the other measured values for consistency. This approach illustrates that determinations of surface temperatures of the powder beds are difficult.
Accurate and reliable detection of subsea Pipeline corrosion is required in order to verify the integrity of the pipeline. A laboratory trial was conducted with a representative pipe sample. The accurate measurement of the wall thickness and corrosion was performed with high energy X-rays and a digital detector array. A 7.5 MV betatron was used to penetrate a stepped pipe and a welded test pipe of 3 m length and 327 mm outer diameter, with different artificial corrosion areas in the 24 mm thick steel wall. The radiographs were taken with a 40 x 40 cm² digital detector array, which was not large enough to cover the complete pipe diameter after magnification. A C-arm based geometry was tested to evaluate the potential for automated inspection in field. The primary goal was the accurate measurement of wall thickness conforming to the standard. The same geometry was used to explore the ability of a C-arm based scanner in asymmetric mode for computed tomography (CT) measurement, taking projections covering only two thirds of the pipe diameter. The technique was optimized with the modelling Software aRTist. A full volume of the pipe was reconstructed and the CT data set was used for reverse engineering, providing a CAD file for further aRTist simulations to explore the technique for subsea inspections.
n this study, two green synthesis routes were used for the synthesis of Ag/ZnO nanoparticles, using cassava starch as a simple and low-cost effective fuel and Aloe vera as a reducing and stabilizing agent. The Ag/ZnO nanoparticles were characterized and used for bacterial dis-
infection of lake water contaminated with Escherichia coli (E. coli). Characterization indicated the formation of a face-centered cubic structure of metallic silver nanoparticles with no insertion of Ag into the ZnO hexagonal wurtzite structure. Physicochemical and bacteriological analyses described in “Standard Methods for the Examination of Water and Wastewater” were used to evaluate the efficiency of the treatment. In comparison to pure ZnO, the synthesized Ag/ZnO nanoparticles showed high efficiencies against Escherichia coli (E. coli) and general coliforms present in the lake
water. These pathogens were absent after treatment using Ag/ZnO nanoparticles. The results indicate that Ag/ZnO nanoparticles synthesized via green chemistry are a promising candidate for the treatment of wastewaters contaminated by bacteria, due to their facile preparation, low-cost synthesis,and disinfection efficiency.
Service life of geosynthetics made of polyolefin materials is mainly limited by oxidative degradation. Durability of polyolefin products depend on formulation, morphology resulting from manufacturing, design and particularly on the antioxidants used. Although the fundamental oxidative reactions are known, the complex effect of geosynthetic characteristics and external influences mean that durability assessments require practical tests.
The assessment of oxidative durability involves exposure to accelerating conditions as well as the material characterisation with respect to the state of stabilisation and/or degradation (e.g. by tensile testing and/or oxidation induction time).
The autoclave test developed by BAM for durability assessments of polyolefin geosynthetics is based on the simultaneous application of moderately elevated temperatures (up to 80 degrees Celsius) and elevated oxygen pressures (up to 5.0 MPa) in combination with a surrounding aqueous medium. Thus this test method provides several advantages in comparison to conventional oven testing, especially with respect to test duration, impact of surrounding environment and the potential to differentiate and rank oxidative resistance between products of very different dimensions (surface/volume) and stabilisation.
In view of the increasing demand for durability assessments of geosynthetic products with lifetimes significantly exceeding 25 years, the contribution is focused on practical aspects concerning implementation and optimisation of test procedures, conditions and evaluation of results. Furthermore, advanced approaches based on multiple exposure conditions will also be included and corresponding calculations of expected service life in typical applications will be evaluated with respect to significance and repeatability. Thereby involved standards and recommendations - such as EN ISO 13438, Part C or EAG-EDT - are considered.
Whenever geosynthetics are used to reinforce or stabilise infrastructural elements such as road- and railways, bridge abutments, run- and taxiways on airports or to protect coastlines of canals and other steep slopes they may be exposed to cyclic loads. Therefore, a reduction factor for dynamic effects on the geosynthetic tensile strength has been included into the calculation of the Long Term Design Strength (LTDS). An approach to assess the behaviour of geosynthetics is to adopt Woehler- or Smith graphs and Haigh-diagrams for polymers. This is because an endurance limit for polymers, which defines an infinite life under a defined cyclic load, has not been seen so far. A huge amount of mechanical testing is needed to predict the behaviour of geosynthetics against this particular background.
To reduce these efforts while getting an indication of the cyclic effect on geosynthetics, a combined method of mechanical and chemical analysis has been developed. The pure tensile strength tests to determine the residual strength after cyclic stress has been amended by IR-spectroscopy and Differential Scanning Calorimetry (DSC). In this context the chain change model of PET has been proven as valid for cyclic loads as well, which helps to define the endurance limit of materials made out of PET. For polyolefins such as PP and PE, a limit for the maximum alternating load has been identified at the point of the stress strain graph where the actual and the numerical stress of a material diverge from each other. Cyclic tensile strength tests have been carried out in a hydraulic test frame. The test parameters have been set to simulate the service life of a railway bed trafficked by high speed trains (ICE).
A multiproxy approach to evaluate biocidal treatments on biodeteriorated majolica glazed tiles
(2016)
The Fishing House located on the grounds of the Marquis of Pombal Palace, Oeiras, Portugal, was built in the 18th century. During this epoch, Portuguese gardens, such as the one surrounding the Fishing House, were commonly ornamented with glazed wall tile claddings. Currently, some of these outdoor tile panels are covered with dark colored biofilms, contributing to undesirable aesthetic changes and eventually inducing chemical and physical damage to the tile surfaces. Phylogenetic analyses revealed that the investigated biofilms are mainly composed of green algae, cyanobacteria and dematiaceous fungi. With the aim of mitigating biodeterioration, four different biocides (TiO2 nanoparticles, Biotin® T, Preventol® RI 80 and Albilex Biostat®) were applied in situ to the glazed wall tiles. Their efficacy was monitored by visual examination, epifluorescence microscopy and DNA-based analysis. Significant changes in the microbial community composition were observed 4 months after treatment with Preventol® RI 80 and Biotin® T. Although the original community was inactivated after these treatments, an early stage of re-colonization was detected 6 months after the biocide application. TiO2 nanoparticles showed promising results due to their self-cleaning effect, causing the detachment of the biofilm from the tile surface, which remained clean 6 and even 24 months after biocide application.
A metrological approach to improve accuracy and reliability of ammonia measurements in ambient air
(2016)
The environmental impacts of ammonia (NH3) in ambient air have become more evident in the recent decades, leading to intensifying research in this field. A number of novel analytical techniques and monitoring instruments have been developed, and the quality and availability of reference gas mixtures used for the calibration of measuring instruments has also increased significantly. However, recent inter-comparison measurements show significant discrepancies, indicating that the majority of the newly developed devices and reference materials require further thorough validation. There is a clear need for more intensive metrological research focusing on quality assurance, intercomparability and validations. MetNH3 (Metrology for ammonia in ambient air) is a three-year project within the framework of the European Metrology Research Programme (EMRP), which aims to bring metrological traceability to ambient ammonia measurements in the 0.5–500 nmol mol−1 amount fraction range. This is addressed by working in three areas: (1) improving accuracy and stability of static and dynamic reference gas mixtures, (2) developing an optical transfer standard and (3) establishing the link between high-accuracy metrological standards and field measurements. In this article we describe the concept, aims and first results of the project.
In diesem Verbundvorhaben werden standardisierte Messverfahren für hybride Gemische erarbeitet, die der Bestimmung sicherheitstechnischer Kenngrößen des Explosionsschutzes dienen. Unter einem hybriden Gemisch wird dabei ein mehrphasiges System aus Brenngas oder brennbarem Dampf, sowie Luft und brennbarem Staub verstanden. Die Veröffentlichung der Ergebnisse erfolgt in einem Abschlussbericht und als DIN-Spezifikation (DIN SPEC). Diese DIN SPEC versetzt Prüfinstitute und Industrie in die Lage, Explosionsgefahren beim Betrieb technischer Anlagen mit hybriden Gemischen einzuschätzen und damit Prozesse sowohl sicherer als auch effizienter zu steuern. Dieses Projekt wird im Rahmen des WIPANOProgramms (Wissens- und Technologietransfer durch Patente und Normen) vom BMWi gefördert.
Polymers with intrinsic microporosity (PIMs) are gaining attention as gas separation membranes. Nevertheless, they face limitations due to pronounced physical aging. In this study a covalent organic framework containing λ5-phosphinine moieties, CPSF-EtO were incorporated as a nanofiller (concentration range 0-10 wt%) into a PIM-1 matrix forming dense films with a thickness of ca. 100 μm. The aim of the investigation was to investigate possible enhancements of gas transport properties and mitigating effects on physical aging. The incorporation of the nanofiller occurred on aggregate level with domains up to 100 nm as observed by T-SEM and confirmed by X-ray scattering. Moreover, the X-ray data show that the structure of the microporous network of the PIM-1 matrix is changed by the nanofiller.
As the molecular mobility is fundamental for gas transport as well as for physical aging, the study includes dielectric investigations of pure PIM-1 and PIM-1/CPSF-EtO mixed matrix membranes to establish a correlation between the molecular mobility and the gas transport properties. Using the time-lag method the gas permeability and the permselectivity were determined for N2, O2, CH4 and CO2 for samples with variation in filler content. A significant increase in the permeability of CH4 and CO2 (50 % increase compared to pure PIM-1) was observed for a concentration of 5 wt% of the nanofiller. Furthermore, the most pronounced change in the permselectivity was found for the gas pair CO2/N2 at a filler concentration of 7 wt%.
This work reports new experimental data on densities and viscosities of (CO2 + n-pentane) and (CO2 + n-hexane) mixtures at high pressures and temperatures. The densities were measured by a vibrating-tube densimeter with an expanded uncertainty (k = 2) smaller than 1.8 kg/m3 at six isotherms (from 273.15 K to 373.15 K), twelve pressures starting at 5 MPa up to 100 MPa, and at six CO2 molar compositions (from 0 to 0.6). The viscosities were measured by a vibrating-wire viscometer with the corresponding relative expanded uncertainty (k = 2) smaller than 0.016 at five isotherms (from 273.15 K to 373.15 K), twelve pressures (from 5 MPa up to 100 MPa), and at two CO2 molar compositions (0.1 and 0.3). The densities were fitted by the semiempirical Tammann-Tait equation for density data and the Vogel-Fulcher-Tammann (VFT) equation for viscosity data, respectively. The Groupe Européen de Recherches Gazières (GERG-2008) equation of state was also applied for modelling the densities. Over-all robustness and reliability of the Perturbed-Chain Statistical Association Fluid Theory (PC-SAFT) and its critical point-based modification (CP-PC-SAFT) were examined. Accuracies of the Modified Yarranton-Satyro (MYS) coupled with CP-PC-SAFT and the NIST Reference Fluid Thermodynamic and Transport Properties Database (REFPROP 10) in predicting the viscosities were evaluated.
Examples of XRF and PIXE imaging with few microns resolution using SLcam® a color X-ray camera
(2015)
We present results of recent development of the color X-ray camera, type SLcam®, allowing detection of X-ray images with few microns resolution. Such spectral resolution is achieved with the use of high-quality polycapillary optics combined with sub-pixel resolution. Imaging of Siemens star resolution test chart reveals that the resolution limit of SLcam® can go down to nearly 5µm. Several real sample examples of measurements carried out at the laboratory, synchrotron, and particle-induced X-ray emission beamlines are shown. This is the first time SLcam® is used as particle-induced X-ray emission detector.
Bundling analytical capacities to understand phase formation in recycling of functional materials
(2019)
Transitioning from combustion engine-driven transportation to e-mobility demands a paradigm shift – from a system geared to maximize energy efficiency (i.e. fuel consumption) to a system that may be constrained by the availability of high technology (critical) metals required for electrical energy storage systems and drives. In the wake of these developments efforts in securing new resources of these metals from recycling of end-of-life products are increasing steadily.
Recycling of Li-Ion batteries has recently been evaluated. The results pinpoint to a critical need for understanding slag Formation and its dependence on metal components like Mn under extreme conditions. This will allow researchers to predict optimal Operation setting and to react quickly to changing market demands (which may be Li or Co at one point but may also shift to Ni or rare earth elements (REE)). The long-term goal is to control the formation of specific phases in slags allowing for a Maximum yield of elements of interest and optimal recovery in the separation processes that follows. The combination of data on the physical micro structure and local chemistry of the multi-Phase products during and after processing will help to understand and derive thermodynamic and kinetic data on its formation.
In this paper we are giving an overview on the analytical challenges and approaches to provide robust data on local element concentration and species (especially Mn which is a common component of next generation Li-ion batteries cathodes), spanning the dimensions from the nanometer scale to the bulk material. The complementary interactions of X-rays and electrons make them ideal probes to collect Interface and “in-depth” information. Before- and -after studies as well as in situ structural changes and Phase (trans)formation, changes in elemental and elemental species (e.g. oxidation state) distribution may be tracked by X-ray diffraction (XRD), X-ray fluorescence microscopy and X-ray Absorption spectroscopy. The application of such advanced analytical tools will not only provide essential clues during early lab-based experiments towards the development of new recycling technologies, but may also be deployed for on-line and in-line monitoring of industrial processes.
The development of earth-abundant catalysts for selective electrochemical CO2 conversion is a central challenge. Cu-Sn bimetallic catalysts can yield selective CO2 reduction toward either CO or formate. This study presents oxide-derived Cu-Sn catalysts tunable for either product and seeks to understand the synergetic effects between Cu and Sn causing these selectivity trends. The materials undergo significant transformations under CO2 reduction conditions, and their dynamic bulk and surface structures are revealed by correlating observations from multiple methods—X-ray absorption spectroscopy for in situ study, and quasi in situ X-ray photoelectron spectroscopy for surface sensitivity. For both types of catalysts, Cu transforms to metallic Cu0 under reaction conditions. However, the Sn speciation and content differ significantly between the catalyst types: the CO-selective catalysts exhibit a surface Sn content of 13 at. % predominantly present as oxidized Sn, while the formate-selective catalysts display an Sn content of ≈70 at. % consisting of both metallic Sn0 and Sn oxide species. Density functional theory simulations suggest that Snδ+ sites weaken CO adsorption, thereby enhancing CO selectivity, while Sn0 sites hinder H adsorption and promote formate production. This study reveals the complex dependence of catalyst structure, composition, and speciation with electrochemical bias in bimetallic Cu catalysts.
In the quest for finding the ideal synchrotron-radiation-induced imaging method for the investigation of trace element distributions in human bone samples, experiments were performed using both a scanning confocal synchrotron radiation micro X-ray fluorescence (SR-mXRF) (FLUO beamline at ANKA) setup and a full-field color X-ray camera (BAMline at BESSY-II) setup. As zinc is a trace element of special interest in bone, the setups were optimized for its detection. The setups were compared with respect to count rate, required measurement time and spatial resolution. It was demonstrated that the ideal method depends on the element of interest. Although for Ca (a major constituent of the bone with a low energy of 3.69 keV for its K alpha XRF line) the color X-ray camera provided a higher resolution in the plane, for Zn (a trace element in bone) only the confocal SR-µXRF setup was able to sufficiently image the distribution.
The color X-ray camera SLcam® is a full-field, single photon detector providing scanning-free, energy and spatially resolved X-ray imaging. Spatial resolution is achieved with the use of polycapillary optics guiding X-ray photons from small regions on a sample to distinct energy dispersive pixels on a charged-coupled device detector. Applying sub-pixel resolution, signals from individual capillary channels can be distinguished. Therefore, the SLcam® spatial resolution, which is normally limited to the pixel size of the charge-coupled device, can be improved to the size of individual polycapillary channels. In this work a new approach to a sub-pixel resolution algorithm comprising photon events also from the pixel centers is proposed. The details of the employed numerical method and several sub-pixel resolution examples are presented and discussed.
Two-dimensional covalent organic frameworks (COFs) based on phosphinine and thiophene building blocks have been synthesized with two different side groups. The materials are denoted as CPSF-MeO and CPSF-EtO where CxxF correspond to the covalent framework, whereas P and S are related to heteroatoms phosphorous and sulfur. MeO and EtO indicate the substituents, i.e. methoxy and ethoxy.
Their morphologies were studied by scanning electron microcopy and X-ray scattering. The absence of crystalline reflexes in the X-ray pattern reveal that both materials are amorphous and can be considered as glasses. Furthermore, N2 adsorption measurements indicate substantial Brunauer–Emmett–Teller (BET) surface area values pointing to the formation of three-dimensional pores by stacking of the aromatic 2D layer. An analysis of the porosity of both COFs showed a mean radius of the pores to be of ca. 4 nm, consistent with their chemical structure. The COFs form nanoparticles with a radius of around 100 nm. The thermal behavior of the COFs was further investigated by fast scanning calorimetry. These investigations showed that both COFs undergo a glass transition. The glass transition temperature of CPSF-EtO is found to be ca. 100 K higher than that for CPSF-MeO. This large difference in the glass transition is discussed to be due to a change in the interaction of the COF sheets induced by the longer ethoxy group. It might be assumed that for CPSF-EtO more individual COF sheets assemble to larger stacks than for CPSF-MeO. This agrees with the much larger surface area value found for CPSF-EtO compared to CPSF-MeO. To corroborate the results obtained be fast scanning calorimetry dielectric measurements were conducted which confirm the occurrence of a dynamic glass transition. The estimated temperature dependence of the relaxation rates of the dielectric relaxation and their absolute values agrees well with the data obtained by fast scanning calorimetry. Considering the fragility approach to the glass transition, it was further found that CPSF-MeO is a fragile glass former whereas CPSF-EtO behaves as a strong glass forming material. This difference in the fragility points also to distinct differences in the interaction between the 2D COF molecules in both materials.
Weltweit werden etwa 80–85 % aller abgebauten Rohphosphate für die Produktion von Düngemitteln verwendet. Bei noch steigendem Bedarf an Phosphor (P) geht man derzeit davon aus, dass die weltweiten P-Reserven noch über 200 Jahre ausreichen. Um den P-Vorrat langfristig abzusichern, sollte der in Reststoffen enthaltene Phosphor möglichst umfänglich genutzt werden. Dieser Forderung trägt das von der Bundesregierung 2012 erstmals beschlossene Deutsche Ressourceneffizienzprogramm ProgRess Rechnung. Rohphosphat wird auch seitens der Europäischen Kommission aufgrundseiner ökonomischen Bedeutung und des unsicheren Angebots als „kritischer Rohstoff“ eingestuft. Vor diesem Hintergrund hat die Bundesregierung in der Verordnung zur Neuordnung der Klärschlammverwertung vom 27. September 2017 in Deutschland eine verpflichtende technische Rückgewinnung von Phosphor für Abwasserbehandlungsanlagen ab einer Ausbaugröße von 100.000 Einwohnerwerten (12 Jahre nach Inkrafttreten der Verordnung) bzw. ab einer Ausbaugröße von über 50.000 Einwohnerwerten (15 Jahre nach Inkrafttreten der Verordnung) vorgeschrieben. Die Verordnung enthält keine Vorgaben hinsichtlich der anzuwendenden Technologie bei der Phosphorrückgewinnung. Ausgenommen von der Rückgewinnungspflicht sind Klärschlämme mit niedrigen Phosphorgehalten (weniger als 20 Gramm Phosphor je Kilogramm Klärschlamm-Trockenmasse). Auch die im Jahre 2017 verabschiedeten neuen Rechtsvorschriften für die Düngung verlangen zukünftig einen nachhaltigen und ressourceneffizienten Umgang mit Nährstoffen bei der landwirtschaftlichen Erzeugung und schränken die P-Zufuhr insbesondere auf hoch versorgten Böden ein (Düngeverordnung vom 26. Mai 2017). Dies wird zu einem mehr am Pflanzenbedarf orientierten und ggf. vermehrt überbetrieblichen Einsatz von wirtschaftseigenen Düngern führen. Um den politischen und gesetzlichen Anforderungen gerecht zu werden, müssen einerseits wirksame und kosteneffiziente technische Verfahren zum P-Recycling (weiter)entwickelt werden. Andererseits müssen die Recyclingprodukte die Anforderungen für eine direkte Verwendung in der Landwirtschaft oder als Rohstoff für die Herstellung von Düngemitteln erfüllen. In dem vorliegenden Standpunkt wird zunächst der potenzielle Beitrag von Reststoffen zur Deckung des P-Bedarfs in der deutschen Pflanzenproduktion geschätzt. Für die wichtigsten Reststoffe werden technische Verfahren zur P-Rückgewinnung bzw. Aufarbeitung skizziert. Auf Basis der Anforderungen der Landwirtschaft bzw. der Düngemittelindustrie
an die P-Recyclingprodukte werden deren Herstellungsverfahren bewertet. Schließlich wird der Regelungs- und Forschungsbedarf formuliert.
The biogenesis of iron–sulfur (Fe/S) proteins entails the synthesis and trafficking of Fe/S clusters, followed by their insertion into target apoproteins. In eukaryotes, the multiple steps of biogenesis are accomplished by complex protein machineries in both mitochondria and cytosol. The underlying biochemical pathways have been elucidated over the past decades, yet the mechanisms of cytosolic [2Fe-2S] protein assembly have remained ill-defined. Similarly, the precise site of glutathione (GSH) requirement in cytosolic and nuclear Fe/S protein biogenesis is unclear, as is the molecular role of the GSH-dependent cytosolic monothiol glutaredoxins (cGrxs). Here, we investigated these questions in human and yeast cells by various in vivo approaches. [2Fe-2S] cluster assembly of cytosolic target apoproteins required the mitochondrial ISC machinery, the mitochondrial transporter Atm1/ABCB7 and GSH, yet occurred independently of both the CIA system and cGrxs. This mechanism was strikingly different from the ISC-, Atm1/ABCB7-, GSH-, and CIA-dependent assembly of cytosolic–nuclear [4Fe-4S] proteins. One notable exception to this cytosolic [2Fe-2S] protein maturation pathway defined here was yeast Apd1 which used the CIA system via binding to the CIA targeting complex through its C-terminal tryptophan. cGrxs, although attributed as [2Fe-2S] cluster chaperones or trafficking proteins, were not essential in vivo for delivering [2Fe-2S] clusters to either CIA components or target apoproteins. Finally, the most critical GSH requirement was assigned to Atm1-dependent export, i.e. a step before GSH-dependent cGrxs function. Our findings extend the general model of eukaryotic Fe/S protein biogenesis by adding the molecular requirements for cytosolic [2Fe-2S] protein maturation.
We present a systematic study on the effect of surface ligands on the luminescence properties and colloidal stability of β-NaYF4:Yb3+,Er3+ upconversion nanoparticles (UCNPs), comparing nine different surface coatings to render these UCNPs water-dispersible and bioconjugatable. A prerequisite for this study was a large-scale synthetic method that yields ~2 g per batch of monodisperse oleate-capped UCNPs providing identical core particles. These ~23 nm sized UCNPs display an upconversion quantum yield of ~0.35% when dispersed in cyclohexane and excited with a power density of 150 W cm-2, underlining their high quality. A comparison of the colloidal stability and luminescence properties of these UCNPs, subsequently surface modified with ligand exchange or encapsulation protocols, revealed that the ratio of the green (545 nm) and red (658 nm) emission bands determined at a constant excitation power density clearly depends on the surface chemistry. Modifications relying on the deposition of additional (amphiphilic) layer coatings, where the initial oleate coating is retained, show reduced non-radiative quenching by water as compared to UCNPs that are rendered water-dispersible via ligand exchange. Moreover, we could demonstrate that the brightness of the upconversion luminescence of the UCNPs is strongly affected by the type of surface modification, i.e., ligand exchange or encapsulation, yet hardly by the chemical nature of the ligand.
Several glazed ceramic fragments (XVIth to XVIIIth centuries) from two production centers in Portugal (Coimbra and Lisbon) were the object of this study. The ones from Coimbra comprise two sets of samples: faiences and tiles. The ones from Lisbon are only tiles (azulejos, in Portuguese). The three main divisions of such pieces are the ceramic support (body), glaze and surface decoration. The system decoration/glaze is not easy to investigate, due to the high heterogeneity resulting from the mixing procedures and firing temperatures used. Moreover, the ability of the pigment to diffuse into the base glaze varies depending on the composition of both the pigment and the glaze in terms of fusibility. In order to raster these effects, high resolution techniques are required. In this work, synchrotron micro-X-ray fluorescence (µ-XRF) analysis was performed to monitor the profiles of the characteristic elements from the colors used and the glaze in well prepared cross-sections of the samples. Key elements are: Co for blue, Mn for purple, Cu for green, Sb for yellow, Pb for the glaze and Fe for the body. The major difference observed is that faiences have glaze thicknesses between 150 and 200 µm and tiles have glaze thicknesses between 350 and 400 µm. Furthermore, in faiences all the pigments except the yellow ones are well dispersed into the glassy matrix, while in tiles, all of them are just partially diffused throughout the glaze. However, differences between the tiles from Coimbra and Lisbon were observed. In the samples from Lisbon, a higher intake from the pigment throughout the glaze is observed.
A research project is described involving a comparison of different non-destructive test methods for concrete bridges. A cooperative test series was started with the aim to compare and evaluate the performance and benefits of the latest technical developments in this field. For this purpose test specimens with localized defects were produced. Different modifications of radar, ultrasonic-echo and impact-echo methods were investigated. Including two- and three- dimensional reconstruction models. The experiments were accompanied by numerical simulation of the propagation of sound waves and microwaves. The results showed that the radar and the ultrasonic methods were efficient tools to locate the tendon ducts accurately if the reinforcing bars were not to narrowly spaced. The ultrasonic imaging methods were capable of identifying injection and compaction faults in a blind test. The good performance of the impact-echo method with regard to locating tendon ducts which was claimed in several publications could not be validated in the present investigations. The simulation models provided valuable information on how to improve the experimental test program and its evaluation.
Die Empfindlichkeit von Eindring- und Magnetpulverprüfungen (PT, MT) hängt unter anderem von der Eignung und der Qualität der Prüfmittel ab (für PT bezeichnet als Eindringsystem). Die Ermittlung der Empfindlichkeit erfolgt an Kontrollkörpern mit natürlichen und künstlichen Inhomogenitäten durch Ermittlung der Anzeigenerkennbarkeit als Maß für die Eignung. Die europäischen Normen spezifizieren die Anforderungen an die Prüfmittel für Typen-, Chargen- und Betriebsprüfungen nach pr EN ISO 3452-2 für PT und EN ISO 9934-2 für MT. Dieser Beitrag beschreibt die Ermittlung der Empfindlichkeit von Prüfmitteln sowie deren Qualifizierung bei der Typenprüfung. Die vorgeschlagenen Verfahren wurden durch experimentelle Untersuchungen validiert, bei denen ein Bildverarbeitungssystem zur Ermittlung der Anzeigenerkennbarkeit verwendet wurde. Im Hinblick auf die Qualifizierung der Prüfmittel wird die Zuverlässigkeit der Verfahren diskutiert.
Apparently that the type testing procedure should be conducted under the conditions ensuring reproducibility of its outcomes. We investigated various factors effecting upon the reproducibility. To obtain quantitative characteristics of indications visibility the image-processing hard-and software were used. It was established that there are two main groups of these factors. The first depends on the differences between various test panels, which are used for type testing. The second one concerns the reproducibility of some stages of penetrant testing procedure (excess penetrant removing and developer application). The recommendations to increase the reproducibility of type testing are developed and illustrated experimentally.
The determination of penetrant system sensitivity as a part of type testing should be conducted ensuring reproducibility of the result. We investigated some factors effecting the reproducibility. To obtain quantitative characteristics of indications visibility, an image processing system was used [1]. We used 3 different sets of reference blocks (rb1, rb2, rb3) corresponding to type 1 of EN ISO 3452-3 [2]. Two fluorescent penetrants with different sensitivities and the same wet solvent developer were used.
It was established that the reproducibility of type testing is influenced by mainly two principal factors. First there are the differences between reference blocks. Second one concerns the reproducibility of penetrant testing procedure, especially excess penetrant removal and developer application.
According to EN ISO 3452-3 a reference block for determination of sensitivity level of fluorescent penetrants consists of a set of three nickel-chrome plated panels with 10, 20 and 30 µm plating thickness. Transverse cracks are made in each panel by stretching the panels in the longitudinal direction and width to depth ratio of the cracks should be approximately 1/20. Each panel presents a certain sensitivity level, which is characterised by the level of visibility of the indication. The highest level 3 corresponds to the panel with 10 µm thickness plating. Each panel is cut longitudinally (perpendicular to the crack) so that 2 sheets (panels A and B) with nearly the same cracks will be produced. These panels A and B of a reference block are used for relative evaluation, for example to compare sensitivities of two penetrants. It is considered that the application of the same penetrant to both panels with subsequent adequate development results in the same visibility of the indications on these panels.
Quantitative correlations between the abilities of the reference blocks used for determining of the sensitivity were obtained in our investigations. We used the relations between the measured values of light-fluxes from the indications of similar comparing areas on two panels. These indications correspond to certain cracks parts of the same total length on both comparing areas. The relations of the steps between the panel are responsible for the definition of the sensitivity groups. From our investigations it follows that the steps of the different sets are different. Besides it was established that the indications visibility for the same penetrant applied on different reference blocks might have a considerable difference depending on the penetrant sensitivity: the higher penetrant sensitivity, the smaller is such a difference between the steps 30/20 and 20/10. For example, for rb3 the relations 30/20 and 20/10 for lower sensitive penetrant (I1) reached factor 3 comparing with factor 2 for higher sensitive penetrant (I2).
Some results of the comparison between the 3 sets (rb1, rb2, rb3) investigations are summarised in Table 1 with rb1 as a reference.
This paper focuses on the preparation and characterization of crystalline thin films of rare-earth-doped sesquioxides (Y2O3, Lu2O3) grown by pulsed laser deposition on single-crystal (0001) sapphire substrates. X-ray diffraction measurements show that the films with thicknesses between 1 nm and 500 nm were highly textured along the 111 direction. Using Rutherford backscattering analysis, the correct stoichiometric composition of the films was established. The emission and excitation spectra of europium-doped films with a thickness 100 nm look similar to those of the corresponding crystalline bulk material, whereas films with a thickness 20 nm show a completely different emission behavior.