Filtern
Erscheinungsjahr
Dokumenttyp
- Zeitschriftenartikel (105)
- Beitrag zu einem Tagungsband (29)
- Beitrag zu einem Sammelband (15)
- Sonstiges (10)
- Posterpräsentation (2)
- Buchkapitel (1)
- Vortrag (1)
- Preprint (1)
- Forschungsbericht (1)
Sprache
- Englisch (135)
- Deutsch (29)
- Mehrsprachig (1)
Schlagworte
- Synchrotron (13)
- XRF (12)
- Gel-type electrolytes (9)
- BAMline (8)
- Gold (8)
- Gelartige Elektrolyte (7)
- Archaeometry (6)
- Synchrotron radiation (6)
- Zinc coatings (6)
- Color X-ray camera (5)
Organisationseinheit der BAM
- 6 Materialchemie (15)
- 1 Analytische Chemie; Referenzmaterialien (14)
- 6.3 Strukturanalytik (12)
- 7 Bauwerkssicherheit (12)
- 1.4 Prozessanalytik (7)
- 7.5 Technische Eigenschaften von Polymerwerkstoffen (7)
- 2 Prozess- und Anlagensicherheit (6)
- 2.1 Sicherheit von Energieträgern (6)
- 1.5 Proteinanalytik (5)
- 4 Material und Umwelt (5)
Paper des Monats
- ja (1)
Eingeladener Vortrag
- nein (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.
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.
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.
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.
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.
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.
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.
Compact pnCCD-based X-ray camera with high spatial and energy resolution: a color X-ray camera
(2011)
For many applications there is a requirement for nondestructive analytical investigation of the elemental distribution in a sample. With the improvement of X-ray optics and spectroscopic X-ray imagers, full field X-ray fluorescence (FF-XRF) methods are feasible. A new device for high-resolution X-ray imaging, an energy and spatial resolving X-ray camera, is presented. The basic idea behind this so-called 'color X-ray camera' (CXC) is to combine an energy dispersive array detector for X-rays, in this case a pnCCD, with polycapillary optics. Imaging is achieved using multiframe recording of the energy and the point of impact of single photons. The camera was tested using a laboratory 30 µm microfocus X-ray tube and synchrotron radiation from BESSY II at the BAMline facility. These experiments demonstrate the suitability of the camera for X-ray fluorescence analytics. The camera simultaneously records 69696 spectra with an energy resolution of 152 eV for manganese Kα with a spatial resolution of 50 µm over an imaging area of 12.7 × 12.7 mm². It is sensitive to photons in the energy region between 3 and 40 keV, limited by a 50 µm beryllium window, and the sensitive thickness of 450 µm of the chip. Online preview of the sample is possible as the software updates the sums of the counts for certain energy channel ranges during the measurement and displays 2-D false-color maps as well as spectra of selected regions. The complete data cube of 264 × 264 spectra is saved for further qualitative and quantitative processing.
We present a new high resolution X-ray imager based on a pnCCD detector and a polycapillary optics. The properties of the pnCCD like high quantum efficiency, high energy resolution and radiation hardness are maintained, while color corrected polycapillary lenses are used to direct the fluorescence photons from every spot on a sample to a corresponding pixel on the detector. The camera is sensitive to photons from 3 to 40 keV with still 30% quantum efficiency at 20 keV. The pnCCD is operated in split frame mode allowing a high frame rate of 400 Hz with an energy resolution of 152 eV for Mn Kα (5.9 keV) at 450 kcps. In single-photon counting mode (SPC), the time, energy and position of every fluorescence photon is recorded for every frame. A dedicated software enables the visualization of the elements distribution in real time without the need of post-processing the data. A description of the key components including detector, X-ray optics and camera is given. First experiments show the capability of the camera to perform fast full-field X-Ray Fluorescence (FF-XRF) for element analysis. The imaging performance with a magnifying optics (3×) has also been successfully tested.
A new setup is presented which enables simultaneous wide- and small-angle X-ray scattering (WAXS/SAXS) and Raman spectroscopic experiments during the synthesis of Mo-based mixed oxide catalyst precursors at the µ-spot beamline at the Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung (BESSY). Furthermore, we report about the separate monitoring of the same reactions under comparable conditions by simultaneous combined ATR/UVvis/Raman spectroscopic measurements. For testing the performance of both experimental setups two syntheses were described comprising the precipitation of metal molybdates by mixing solutions of metal nitrates and ammonium heptamolybdate. Additionally, the effect of H3PO4 admixture on precipitation was investigated. The combined evaluation of spectroscopic and WAXS/SAXS data allows the discrimination between different molybdate species appearing in solution and precipitate. Furthermore, these molybdate species could be assigned to separate phases of different crystallinity.
A set of ten calibration materials based on acrylonitrile-butadiene-styrene terpolymer (ABS) containing the elements Br, Pb, Cd, Cr, and Hg was produced in order to control polymer samples in regard to the restriction on the use of certain hazardous substances (RoHS) directive. The materials were produced with respect to the special demands of X-ray fluorescence analysis (XRF) and inductively coupled plasma mass spectrometry in combination with laser ablation (LA-ICP-MS).
The mass fractions of all elements were 0-1500 mg/kg and the materials were produced as granulates and solid discs with a diameter of 40 mm and thicknesses of 1, 2, and 6 mm. It could be shown that the signals measured by XRF strongly depend on the thickness of polymeric samples.
Macroscopic homogeneity was assessed with XRF measuring a total of 180 samples. The microscopic homogeneities were determined for a material with average elemental mass fractions with the aid of synchrotron radiation (SR) µ-XRF and LA-ICP-MS. Sufficient macroscopic and microscopic homogeneities for all elements could be achieved. It was observed that organic additives show a better homogeneity than oxides.
XRF and LA-ICP-MS were successfully calibrated with the new materials. Limits of detection were in the range of 0.4-22 mg/kg for XRF and 2.3-26.8 mg/kg for LA-ICP-MS. The materials are considered as candidate reference materials (RM) by the Federal Institute of Materials Research and Testing (BAM, Germany).
During the processing of superconducting Nb3Sn wire, several intermediate intermetallic phases including a previously encountered Cu-Nb-Sn phase show up. The yet unknown crystal structure of this phase is now identified by a combination of different experimental techniques and database search to be of the hexagonal NiMg2 type with a proposed composition of about (Nb0.75Cu0.25)Sn2. The structure determination started from an evaluation of the lattice parameters from EBSD Kikuchi patterns from quenched material suggesting hexagonal or orthorhombic symmetry. A database search then led to the hexagonal NiMg2 type structure, the presence of which was confirmed by a Rietveld analysis on the basis of high energy synchrotron X-ray powder diffraction data. Assuming a partial substitution of Nb in orthorhombic NbSn2 by Cu, the change of the valence electron concentration provokes a structural transformation from the CuMg2 type for NbSn2 to the NiMg2 type for (Nb0.75Cu0.25)Sn2. In the previous literature the (Nb0.75Cu0.25)Sn2 phase described here has occasionally been referred to as Nausite.
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.
At the core of luminescence color and lifetime Tuning of rare earth doped upconverting nanoparticles (UCNPs), is the understanding of the Impact of the particle architecture for commonly used sensitizer (S) and activator (A) Ions. In this respect, a series of core@Shell NaYF4 UCNPs doped with Yb3+ and Ho3+ ions are presented here, where the same dopant concentrations are distributed in different particle architectures following the scheme: YbHo core and YbHo@..., ...@YbHo, Yb@Ho, Ho@Yb, YbHo@Yb, and Yb@YbHo core-Shell NPs. As refealed by quantitative steady-state and time-resolved luminescence studies, the relative spatial Distribution of the A and S ions in the UCNPs and their protection from surface quenching has a critical Impact on ther luminescence characteristics. Although the increased amount of Yb3+ Ions boosts UCNP Performance by amplifying the Absorption, the Yb3+ ions can also efficiently dissipate the energy stored in the material through energy Migration to the surface, thereby reducing the Overall energy Transfer Efficiency to the activator ions. The results provide yet another proof that UC Phosphor chemistry combined with materials Engineering through intentional core@shell structures may help to fine-tune the luminescence Features of UCNPs for their specific future applications in biosensing, bioimaging, photovoltaics, and Display technologies.
REALight ‐ Leichtgranulate und REA‐Gips aus feinkörnigen sulfatbelasteten Bau‐ und Abbruchabfällen
(2023)
Ziel des Projekts REALight ist die Entwicklung einer Referenzanlage zur Herstellung von Leichtgranulaten (leichte Gesteinskörnungen) aus Bau‐ und Abbruchabfällen und zur Gipsrückgewinnung. Als Rohstoffe werden bisher ungenutzte oder auf niedrigem Niveau eingesetzte Bau‐ und Abbruchabfälle und industrielle Nebenprodukte verwendet. Als Produkte werden leichte Gesteinskörnungen hergestellt. Die Sulfatabtrennung durch eine thermische Zersetzung bildet die Grundlage für die zusätzliche Gewinnung von Rauchgasentschwefelungs‐Gips (REA‐Gips). Das Projekt wird im Rahmen der Fördermaßnahme „Ressourceneffiziente Kreislaufwirtschaft – Bauen und Mineralische Stoffkreisläufe (ReMin)” gefördert. ReMin ist eine Maßnahme zur Umsetzung des BMBF‐Forschungskonzepts „Ressourceneffiziente Kreislaufwirtschaft” als Teil der BMBF Strategie „Forschung für nachhaltige Entwicklung – FONA”. Ziel der Förderung ist es, den Ausbau der Kreislaufwirtschaft voranzutreiben. Im Mittelpunkt steht dabei die Bauwirtschaft mit ihrer hohen Nachfrage nach Rohstoffen und gleichzeitig großen Mengen an anfallenden mineralischen Abfällen. Am Projekt REALight sind 12 Partner aus verschiedenen Bereichen der Baustoffherstellung und ‐anwendung, Abfallaufbereitung, Verfahrenstechnik sowie Forschung und Entwicklung beteiligt.
Flexible polyurethane foams with densities of 40 ± 2 kg m−3 were prepared by combining different ecofriendly fillers such as layered double hydroxides (LDH) and kraft lignin (a byproduct of the pulp and paper industry) with a phosphorous polyol (E560) in order to study their effect on the mechanical performance and fire behavior of the foams. Two series of foams were prepared, some containing lignin or LDH separately, and some with a combination of both: one of the series was prepared without E560 (0E foam series) and the other with 5 parts per hundred of E560 polyol (5E series). The use of fillers resulted in increased viscosity of the reactive mixture, requiring higher blowing agent content in order to hold the density of the foams constant. It was observed that urea phase segregation was favored in the series of 0E foams due to their lower viscosity than the 5E series. This had consequent effects on the resilience, compression force deflection and compression set of these foams. In terms of fire behavior it was observed that while the limiting oxygen index decreased, cone calorimeter results showed that the combination of lignin, LDH and E560 decreased the heat release of the foams. In addition, the combination of fillers and E560 contributed to increase the viscosity of the pyrolysis products, preventing the dripping of the molten polymer, which is a key factor in flame propagation towards adjacent objects in fire scenarios.
In this work, a cost-effective optofluidic system is proposed and preliminary experimental results are presented. A microfluidic channel monolithically integrated into a photonic integrated circuit technology is used in conjunction with a cyclic olefin copolymer (COC) substrate to provide fluidic in- and output ports. We report on initial experimental results as well as on the simple and cost-effective fabrication of this optofluidic system by means of micro-milling.
Condensation particle counters (CPCs) are widely used for the measurement of aerosol particle number concentrations in the size range from approximately 3 nm to 3 μm. For an SI-traceable calibration of the size-dependent counting efficiency, which is advisable on a regular basis and required in several applications, Faraday cup aerosol electrometers (FCAEs) are considered to be a suitable SI-traceable reference.While the volumetric aerosol inlet flowrate and the electrical current measurement in FCAEs can be related to respective SI references, inter-comparison exercises for FCAEs are still performed on a regular basis to establish reliable uncertainty budgets and to further investigate the influences of designs and operational parameters on comparability. This is strongly demanded in the international community of metrological institutes and aerosol calibration facilities around the world, which provide CPC calibrations. In the present study, the performance of FCAEs was investigated,using Ag test aerosol particles with a 30 nm particle diameter by varying the inlet flowrates from 0.5 l min−1 to 4 l min−1. From our experimental results, significant deviations were observed in FCAE currents at sample flowrates smaller than 1.5 l min−1. It is recommended that these discrepancies should be quantified before an FCAE is used for CPC calibration at low sample flowrates and small particle sizes in the sub-30 nm size range.
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.
Phoenician ivory objects (8th century B.C., Syria) from the collections of the Badisches Landesmuseum, Karlsruhe, Germany, have been studied with full field X-ray fluorescence microimaging, using synchrotron radiation (SR-FF-microXRF). The innovative Color X-ray Camera (CXC), a full-field detection device (SLcam), was used at the X-ray fluorescence beamline of the ANKA synchrotron facility (ANKA-FLUO, KIT, Karlsruhe, Germany) to noninvasively study trace metal distributions at the surface of the archeological ivory objects. The outstanding strength of the imaging technique with the CXC is the capability to record the full XRF spectrum with a spatial resolution of 48 µm on a zone of a size of 11.9 × 12.3 mm² (264 × 264 pixels). For each analyzed region, 69696 spectra were simultaneously recorded. The principal elements detected are P, Ca, and Sr, coming from the ivory material itself; Cu, characteristic of pigments; Fe and Pb, representing sediments or pigments; Mn, revealing deposited soil minerals; Ti, indicating restoration processes or correlated with Fe sediment traces; and Au, linked to a former gilding. This provides essential information for the assessment of the original appearance of the ivory carvings. The determined elemental maps specific of possible pigments are superimposed on one another to visualize their respective distributions and reconstruct the original polychromy and gilding. Reliable hypotheses for the reconstruction of the original polychromy of the carved ivories are postulated on this basis.
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.
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.
Sixteen Ayyubid-Mamluk glazed pottery sherds were analyzed in order to identify and characterize the elemental composition to determine their provenance. The tested sherds were collected from the historical site of Karak Castle, southern Jordan.
Chemical analysis for the sixteen samples has been carried out using Synchrotron Radiation X-ray Fluorescence Spectrometry (SR-XRF) Technique. Furthermore, the semiquantitative analysis of the elements Fe – Cu – Zn – Br – Rb – Sr – Y – Zr – Nb – Mo – Pd – Ag – Cd and Pb has been performed for the samples based on Principal Component Analysis (PCA) and hierarchical Cluster Analysis with Bray-Curtis in order to define grouping of different glazed pottery by obtaining information on their similarity and clustering. The results of chemical analysis provided persuasive evidence that the Karak Castle pottery sherds have at least three different sources of provenance.
A new high-resolution detector setup for neutron imaging has been developed based on infinity-corrected optics with high light collection, combined with customized mounting hardware. The system can easily be installed, handled and fitted to any existing facility, avoiding the necessity of complex optical systems or further improved electronics (CCD). This is the first time optical magnification higher than 1:1 has been used with scintillator-based neutron detectors, as well as the first implementation of infinity corrected optics for neutron imaging, achieving the smallest yet reported effective pixel size of 3.375 µm. A novel transparent crystal scintillator (GGG crystal) has been implemented with neutrons for the first time to overcome limitations of traditional powder scintillators (Li6/ZnS, Gadox). The standardized procedure for resolution measurements with the Modulation Transfer Function (MTF) is summarized to facilitate comparison between instruments and facilities. Using this new detector setup, a resolution of 14.8 µm with a field of view of 6 mm × 6 mm has been achieved while maintaining reasonable count times. These advances open a wide range of new possible research applications and allow the potential for additional future developments.
In situ secondary ion mass spectrometry (SIMS) analyses of δ7Li, Li/Ca, and Mg/Ca were performed on five synthetic aragonite samples precipitated from seawater at 25°C at different rates. The compositions of δ7Li in bulk aragonites and experimental fluids were measured by multicollector inductively coupled plasmamass spectrometry (MC-ICP-MS). Both techniques yielded similar δ7Li in aragonite when SIMS analyses were corrected to calcium carbonate reference materials. Fractionation factors α7Li/6Li range from 0.9895 to 0.9923, which translates to a fractionation between aragonite and fluid from -10.5‰ to -7.7‰. The within-sample δ7Li range determined by SIMS is up to 27‰, exceeding the difference between bulk δ7Li analyses of different aragonite precipitates. Moreover, the centers of aragonite hemispherical bundles (spherulites) are enriched in Li/Ca and Mg/Ca relative to spherulite fibers by up to factors of 2 and 8, respectively. The Li/Ca and Mg/Ca ratios of spherulite fibers increase with aragonite precipitation rate. These results suggest that precipitation rate is a potentially important consideration when using Li isotopes and elemental ratios in natural carbonates as a proxy for seawater composition and temperature.
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.
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.
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.
Optical filters and fabrics are important parts of laser safety equipment such as goggles and curtains. A choice of these materials with varying absorption spectra is investigated with respect to their resistance to Ti:sapphire femtosecond laser radiation (800 nm wavelength, 1 kHz repetition rate). Pulse durations down to 30 fs and multiple-pulse irradiation conditions are employed to evaluate technically relevant damage thresholds. The ablation threshold fluences of the absorbing filters are comparable to those observed for transparent materials with 30-fs-pulses. These investigations together with scanning electron microscopy of the surface morphology after laser treatment provide insight into the interaction mechanism of the short pulses with the materials.
Besonders in beweglichen Weichenteilen, wie z.B. Zungen und beweglichen Herzstückspitzen ist die Detektion von Rissen, die zum Bruch des Bauteils führen können, von außerordentlicher Bedeutung. Wegen der komplizierten geometrischen Randbedingungen muß der Schienenprüfzug hier seinen Prüfkopfträger anheben. Aus diesem Grund werden diese Bereiche regelmäßig durch eine manuelle Ultraschallprüfung überwacht. Da auch sehr kleine Anrisse im Oberflächenbereich interessant sind, soll das bereits vorhandene Prüfverfahren durch ein Wirbelstrom-Handprüfsystem so erweitert werden, daß eine sichere Detektion in den gefährdeten Bereichen möglich ist. Aufbau und Wirkungsweise des Wirbelstrom-Handprüfsystems werden erläutert.
Damage experiments of absorbing filters (Schott BG18 and BG36) were performed with Ti:sapphire laser pulses with durations from 30 fs to 340 fs (800 nm, 1 kHz) in air. The direct focusing technique was employed under single- and multi-pulse irradiation conditions. Ablation threshold fluences were determined from a semi-logarithmic plot of the ablation crater diameter vs. laser fluence. The damage threshold fluence decreases for shorter pulse durations. In the investigated pulse duration range, the measured multi-pulse ablation threshold fluences are practically similar to those of undoped glass material (~1 Jcm-2). That means that the multi-pulse ablation threshold is independent on the doping level of the filters. For more than 100 pulses per spot and all pulse durations applied, the threshold fluence saturates. This leads to technically relevant damage threshold values in the femtosecond laser pulse duration domain.
Commercially available absorption filters (Schott BG18 and BG36) were investigated with respect to their single- and
multi-pulse ablation threshold using laser pulses from a Ti:Sapphire laser in the range between 30 and 340 fs. It could be
observed, that the threshold fluence decreases for shorter pulse durations. The similarity of the measured multi-pulse
threshold fluences with those of undoped glass material (around 1 J/cm^2 for a pulse duration of 30 fs) suggests that, for
very short pulses, the threshold is independent on the doping level and therefore, linear absorption does not significantly
contribute to laser-induced damage. For >100 pulses per spot and all pulse durations applied, the threshold fluences
saturate. This independence on the number of applied pulses leads to technically relevant damage threshold values.
The market of the penetrant systems is increasing every year. A sensitivity of the penetrant systems is one of the main criteria for a customer. Therefore the importance of reliable result of the determination of penetrant systems sensitivity is increasing as well. It was established in our experiments that repeating the procedure of type testing in accordance with ISO EN 3452-2, in many cases one can obtain rather variable results for the sensitivity level. The goal of our investigations was to establish the principal factors, influencing upon the result of penetrant system type testing. Our results show that the values of the duration of such penetrant inspection technological stages as penetrant and developer applications may be considerably lower than the values recommended by ISO EN 3452-2 for the type testing. At the same time the character of the procedure's realisation of excess penetrant removal and developer application strongly influences upon the type testing results. Some recommendations for obtaining more reliable results of the determination of penetrant system sensitivity are worked out and proposed. ©2002 American Institute of Physics.
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.
Femto- and nanosecond laser ablation of polymethylmethacrylate (PMMA) and PMMA doped with a linear absorber was
investigated in the infrared spectral region. Ablation thresholds were determined and incubation phenomena were identified. The
degree of incubation was calculated employing a phenomenological model. The influence of the pulse duration on the
machining quality of the polymers was examined. The presence of an absorbing chromophore is not a prerequisite for a
controllable fs-laser structuring in contrast to the ns-treatment. Surface swelling always accompanied ablation.
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.
Ablation experiments employing Ti:sapphire laser pulses with durations from 30 to 340 fs (centre wavelength 800 nm, repetition rate 1 kHz) were performed in air. Absorbing filters (Schott BG18 and BG36) served as targets. The direct focusing technique was used under single- and multi-pulse irradiation conditions. Ablation threshold fluences were determined from a semi-logarithmic plot of the ablation crater diameter versus laser fluence. The threshold fluence decreases for a shorter pulse duration and an increasing number of pulses. The multi-pulse ablation threshold fluences are similar to those of undoped glass material (~1 J cm-2). That means that the multi-pulse ablation threshold is independent on the doping level of the filters. For more than 100 pulses per spot and all pulse durations applied, the threshold fluence is practically constant. This leads to technically relevant ablation threshold values.
Textile, aluminium and polyethylene used as components in laser protection curtains were investigated with respect to their ablation behaviour. Employing 33-fs pulses (800 nm wavelength, 1 kHz repetition rate), ex situ geometrical measurements of the ablation cavities and in situ acoustic investigations with a microphone were performed to determine the ablation thresholds in the single- and multi-pulse cases. The acoustical method proved advantageous for complex surface morphologies and/or single laser pulse interactions. Incubation phenomena can be observed for all the materials studied. Technically relevant multi-pulse ablation thresholds are presented and are compared with the single-pulse (1-on-1) irradiation.
Validation of non-destructive testing methods is necessary to create a common basis where different systems can be compared and their applications and limitations be identified. This can be achieved through comparing the measurements taken by several systems used for a common diagnostic purpose under practical but controlled testing conditions. Well-designed small and large laboratory or field specimens promise such conditions.
The special concrete specimen (LCS) at BAM was constructed for validation purposes, in particular, to be used for evaluating the performance of echo methods. The thickness of the specimen is varying and it contains carefully designed built-in faults, such as voids, honeycombs and tendon ducts with various degrees of grouting defects. Since the geometry and condition of the defects are known, it can be used to compare the performance of radar, ultrasonic, impact-echo. The research was conducted within the Research group FOR384, sponsored by the German Research Society DFG.
Für die zerstörungsfreie Prüfung großer Betonbauwerke unter dem Aspekt der Analyse von Spannkanälen hat sich die Ultraschalltechnik in den letzten Jahren als geeignete Methode herausgestellt, da sowohl die Messtechnik insbesondere die Ultraschallwandler als auch die numerischen Auswerteverfahren in einem Stadium sind, das es erlaubt, größere Messflächen und damit größere Volumina zu beschallen und abzubilden. Mit Hilfe der Modellierung der Ausbreitung elastischer Wellen in komplexen Medien können praxisrelevante Problemstellungen untersucht werden, auch unter dem Aspekt, Testkörper zu planen oder gar zu ersetzen. Durch die Auswertung der Phase der Rekonstruktion eines Streuvorgangs können Fehlstellen klassifiziert und damit Aussagen über die Bauwerkssicherheit signifikant objektiviert werden. Die Methoden werden, im Hinblick auf eine ganzheitliche Sichtweise von skalaren und polarimetrischen Abbildungsverfahren mit Unterstützung der Modellierung und der anschließenden Klassifizierung durch Phasenanalyse, an ausgewählten Beispielen erläutert.
For nondestructive testing of concrete buildings under the aspect of tendon duct analysis, ultrasonic testing has proven to be a suitable method, as both the measuring technique in particular the acoustic sensors and the numerical methods allow the insonification and imaging of larger surfaces and volumes. With the aid of numerical modelling of elastic wave propagation in complex media real life problems can be examined with the goal to design or even to replace test specimen. By determination of the phase of an imaged scattering event, defects can be classified, and the prediction of the integrity of buildings can be significantly objectified. The methods are explained for selected examples in an integral way with respect to scalar and polarimetric imaging algorithms supported by modelling and subsequent classification through phase analysis.
Results of a round-robin experiment in multiple-pulse LIDT measurement with ultrashort pulses
(2004)
The influence of different laser pulse lengths on the removal of a polymer layer from metal substrates was investigated. As model systems, doped poly(methylmetacrylate) (PMMA) on titanium and tungsten substrates were selected.
The ablation threshold and irradiation spot morphology of titanium and tungsten were compared for femtosecond (fs) and nanosecond (ns) laser irradiation and different pulse numbers. Nanosecond laser treatment resulted in a non-homogeneous surface morphology for both titanium and tungsten substrates. Femtosecond irradiation of tungsten revealed a homogeneous ablation spot with little changes in the surface morphology. For titanium, the formation of columnar structures within the irradiation spot was observed.
Two different dopant concentrations were used for PMMA to achieve an equal linear absorption coefficient for the femto- and nanosecond laser wavelengths of 790 and 1064 nm. The best results were achieved for the removal of doped PMMA by femtosecond laser irradiation, where only a minimal modification of the metal surface was detected. In the case of nanosecond laser exposure, a pronounced change of the structure was observed, suggesting that damage-free cleaning of the selected metal may only be possible using femtosecond laser pulses. Different experimental parameters, such as laser fluence, pulse repetition rate and sample speed were also investigated to optimize the cleaning quality of doped PMMA from tungsten substrates with femtosecond laser pulses.
Minimum explosion concentration (MEC) of three agriculture dusts and two coal dusts was studied via a 20-L explosion chamber to reveal the role of gaseous inhibitors. Both active method (CO2 diluting air) and passive method (CO2 replacing O2) were used. The TG and DTG thermal analysis tests were conducted to study the pyrolysis and combustion characteristics of dust samples. An alternative explosion criterion based on combustion duration time was used to determine MEC, and compared with the standardized overpressure method. Under 10-kJ ignition condition, as oxygen mole fraction (XO2) decreased from 21% to 10%, MEC of agriculture dusts and coal dusts respectively increased by around 5 times and 2 times. The active inerting method with a lower N2/CO2 ratio was found to have a better suppression effect on the explosion of the five carbonaceous dusts because the blend has a higher specific heat and a lower oxygen diffusion rate.
Minimum ignition temperature of dust clouds (MITC) was studied experimentally and theoretically in different atmospheres. Three carbonaceous dusts were tested in both air and O2/CO2 atmospheres with CH4 mole fraction from 0 to 2%. Results showed that the ignition risk of the three dusts significantly increases (decrease of MITC by ~100 ℃) with increasing XO2 from 21% to 50%, but significantly decreases replacing N2 in air with CO2. The inhibition effect of CO2 on MITCs could be diminished by increasing XO2 or adding CH4. The addition of small amount of CH4 has different effects on the MITCs of different dust samples, following the opposite order of volatile matter content: anthracite>bituminous coal>starch. Two modified steady-state ignition models, considering the density of mixture gas and dust cloud, XO2 and its diffusivity, were developed to interpret the experimental observations. The analysis revealed that the global heterogeneous ignition model suits well for the hybrid mixtures of anthracite or bituminous coal dusts. In contrast, the proposed global homogeneous ignition model was found to be only valid for the pure starch dust, and the extra CH4 addition could strongly affect the ignition process of starch, particularly in O2/CO2 atmospheres with higher XO2.
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.
Gaseous inhibitors are used in many industries for the explosion prevention of combustible dusts, mitigating the potential hazard to humans, properties and environments. This work experimentally and theoretically studied the inerting effect of gaseous inhibitors on the ignition process of dust clouds in O2/N2/CO2 atmospheres, with an emphasis on the role of the CO2/N2 ratio. 10 different combustible carbonaceous dusts were selected, including grain dust, biomass dust and coal dust. Experimental results showed that the inhibition effect of CO2/N2 is closely related to the ignition mechanism of dust clouds. Specifically, a higher ratio of CO2/N2 yields a stronger inhibition effect on the ignition process of dust samples with relatively low volatile matter contents predominated by heterogeneous ignition. In addition, two novel steady-state ignition mechanism models were developed to interpret the experimental observations. Maxwell-Stefan equations were used to describe the diffusivity in the ternary O2/N2/CO2 gas mixtures. The analytical results were in good agreement with the experimental data of the minimum ignition temperature of dust cloud (MITC) in oxygen-lean atmospheres. The mechanism modelling can be used to estimate the critical ignition temperature of all carbonaceous dust clouds with a wide range of volatile matter content under different inert atmospheres, which will provide a reference for the explosion hazard assessment of dust posed by a hot surface in the process industries.
This contribution will show that gel-type electrolytes influence protective layers on zinc coatings considerably less than typical bulk electrolytes. Different zinc coatings are investigated, their naturally formed protective layers are electrochemically characterized and corrosion relevant values are determined by using a gel pad based on polysaccharide. From the results it is evident that gel-type electrolytes represent a viable and promising field in corrosion research.
Die drei Beispiele zerstörungsfreier Prüfungen an Spannbetonbrücken zeigen unterschiedliche Problemstellungen und deren Lösung mit unterschiedlichen Ansätzen.
Allen drei Beispielen gemeinsam ist die Verwendung kommerzieller Geräte. Diese werden von verschiedenen Anbietern bereitgestellt. Eine weitere Gemeinsamkeit ist, dass die Grundgeräte durch zusätzliche Maßnahmen ergänzt. Erst dann ist der gewünschte Untersuchungserfolg sicher gestellt.
Im ersten Beispiel wurde die vom Auftraggeber geforderte Präzision dadurch erreicht, dass systematische Voruntersuchungen stattfanden. Die Übertragung der Lokalisierung direkt auf die Betonoberfläche stellte sicher, dass keinen Informationsverluste an die nachfolgenden Aufgaben auftraten.
Das zweite Beispiel zeigt den Nutzen von Automatisierung und Kombination von Verfahren. Damit können dem Auftraggeber die notwendigen Angaben über Einbauteile mit großer Detaitreue und leicht verständlicher Visualisierung aufbereitet werden. Der abschließende Bericht zeigt, wie vorhandene Auswertungen sinnvoll durch noch in der Forschung befindliche Ansätze bereichert werden.
Insgesamt ist die zerstörungsfreie Prüfung in der Lage, an Brücken preisrelevante Fragestellungen zu lösen. Voraussetzung hierfür ist eine sorgfältig geplante Vorgehensweise und ein sicheres Verständnis der Grundlage der eingesetzten Geräte und Auswertungsschritte.
The incorporation of colloidal quantum dots (QDs) into solid matrices, especially ionic salts, holds several advantages for industrial applications. Here, we demonstrated via absolute measurements of photoluminescence quantum yields (PL-QY) that the photoluminescence of aqueous CdTe QDs can be considerably increased upon incorporation into a salt matrix with a simple crystallization procedure. Enhancement factors of up to 2.8 and a PL-QY of 50 to 80%, both in NaCl crystals and incorporated in silicone matrices, were reached. The fact that the achievable PL enhancement factors depend strongly on PL-QY of the parent QDs can be described by the change of the dielectric surrounding and the passivation of the QD surface, modifying radiative and nonradiative rate constants. Time-resolved PL measurements revealed noncorrelating PL lifetimes and PL-QY, suggesting that weakly emissive QDs of the ensemble are more affected by the enhancement mechanism, thereby influencing PL-QY and PL lifetime in a different manner.
In the determination of the provenance of gold in archaeological artifacts, trace elements are more significant than the main components. Several minute fragments of natural Carpathian gold-placer and primary-and some very small (a few milligrams) fragments of archaeological items were studied using micro Synchrotron Radiation X-Ray Fluorescence (micro SR-XRF) at the BESSY Synchrotron Facility in Berlin, Germany. The goal of the study was to identify the trace elements characterizing Carpathian gold, looking especially at Sn, Sb, Pb and Te, and to determine if the gold in the archaeological items is native or refined. Applications to the authentication and provenance of nine Dacian gold bracelets, koson coins and two Bronze Age items are presented.
A Large Aperture UltraSonic (LAUS) system has been designed and built for testing thick concrete structures. The scalable system consists of twelve ultrasonic units, each hosting 32 individual shear wave transducers with mechanical dry point contact (DPC) to the concrete surface. The twelve units are attached to the concrete surface using a vacuum case which holds them in place during operation. Each LAUS unit can be placed individually depending on the surface condition and optimal ultrasonic condition, e.g. rebar position. Air pressure is supplied to each unit through an air hose. The following extended abstract is a short version of an article to be published in the special edition of ASCE JIS that will describe the outline of the system, the principle of functioning, the data processing and adapted reconstruction calculation based on SAFT as well as the system performance during first applications.
A comparative study on the performance of digital detector systems for high energy applications
(2014)
For cast components reaching or exceeding total material thicknesses of 150mm, high energy sources such as linear accelerators or Betatrons are required in order to obtain reasonable exposure times. In this study, the performance of digital detector systems, involving imaging plates (IP) and digital detector arrays (DDA), was evaluated with respect to the testing class B requirements as formulated in the standard EN ISO 17636-2. As a reference, traditional radiographic film and a Cobalt-60 source was used. With film exposures, testing class B was achieved with Co-60 and Betatron (7.5 MV) at longer exposure times. The preliminary results show that the testing class B was not obtained with the examined digital detector arrays (DDA) and the high resolution imaging plates (IP) , even at 40, 60 and 80 minutes exposure time with a 7.5 MV Betatron. Class A was achieved using high resolution imaging plates with optimized metal filters between object and IPs and a high resolution DDA with intermediate Cu filters. Class A was also achieved applying a DDA with lower basic spatial resolution than required by Table B.13 of EN ISO 17636-2, but using the compensation principle as described in this standard. The next generation of digital detector arrays might potentially be able to obtain class B performance with the expected spatial resolution and sensitivity improvements.
Shading Effects in SR-TXRF: Calculations and Experimental Visualization using a Color X-ray Camera
(2014)
Recent results from a three-year multi-disciplinary project on Ancient Egyptian gold jewellery revealed that items of jewellery from the Middle Kingdom to the New Kingdom were manufactured using a variety of alluvial gold alloys. These alloys cover a wide range of colours and the majority contain Platinum Group Elements inclusions. However, in all the gold foils analysed, these inclusions were found to be absent. In this work a selection of gilded wood and leather items and gold foil fragments, all from the excavations by John Garstang at Abydos (primarily from Middle Kingdom graves), were examined using Scanning Electron Microscopy-Energy Disperse Spectroscopy (SEM-EDS), X-Ray Fluorescence (µXRF), Particle Induced X-Ray Emission (µPIXE) and Double Dispersive X-Ray Fluorescence (D²XRF). The work allowed us to characterise the composition of the base-alloys and also to reveal the presence of Pt at trace levels, confirming the use of alluvial gold deposits. Corrosion products were also investigated in the foils where surface tarnish was visually observed. Results showed that the differences in the colour of corrosion observed for the foils are related not only to the thickness of the corrosion layer but also to a multi-layer structure containing the various corrosion products.
Bright emitters with photoluminescence in the spectral region of 800–1600 nm are increasingly important as optical reporters for molecular imaging, sensing, and telecommunication and as active components in electrooptical and photovoltaic devices. Their rational design is directly linked to suitable methods for the characterization of their signal-relevant properties, especially their photoluminescence quantum yield (Φf). Aiming at the development of bright semiconductor nanocrystals with emission >1000 nm, we designed a new NIR/IR integrating sphere setup for the wavelength region of 600–1600 nm. We assessed the performance of this setup by acquiring the corrected emission spectra and Φf of the organic dyes Itrybe, IR140, and IR26 and several infrared (IR)-emissive Cd1-xHgxTe and PbS semiconductor nanocrystals and comparing them to data obtained with two independently calibrated fluorescence instruments absolutely or relative to previously evaluated reference dyes. Our results highlight special challenges of photoluminescence studies in the IR ranging from solvent absorption to the lack of spectral and intensity standards together with quantum dot-specific challenges like photobrightening and photodarkening and the size-dependent air stability and photostability of differently sized oleate-capped PbS colloids. These effects can be representative of lead chalcogenides. Moreover, we redetermined the Φf of IR26, the most frequently used IR reference dye, to 1.1 × 10-3 in 1,2-dichloroethane DCE with a thorough sample reabsorption and solvent absorption correction. Our results indicate the need for a critical reevaluation of Φf values of IR-emissive nanomaterials and offer guidelines for improved Φf measurements.
The interest in (micro)porous systems is greater than ever before with microporous polymers finding application in areas such as gas storage/separation and catalysis. In contrast to the vast majority of publications on microporous polymers seeking ever higher values for surface area or uptake capacity for a particular gas, this work presents a means to render a microporous system responsive to electromagnetic stimuli. The incorporation of a diarylethene (DAE) derivative in the backbone of a polymer of intrinsic microporosity (PIM) produces a microporous system that exhibits photochromism as proven by UV–vis absorption and NMR studies. In the resulting DAE-PIM, surface area is not a fixed unalterable property but can be influenced by the external and nondestructive stimulus light in a reversible manner. Furthermore, in combination with Matrimid, free-standing membranes can be produced that display light-switchable diffusivity and permeability for carbon dioxide and oxygen. In this way, material scientists are offered the potential to employ only one system that can assume several states with different properties for each.
Ein neuer Ansatz bei elektrochemischen Korrosionsuntersuchungen kann durch den Einsatz von gelartigen Elektrolyten als Alternative zu wässrigen Prüfelektrolyten beschritten werden. Gelartige Elektrolyte ermöglichen minimalinvasive Untersuchungen an natürlich gebildeten Zinkdeckschichten. Dadurch können korrosionsrelevante Kennwerte ermittelt werden, die Aussagen zur Deckschichtbildung und zur Stabilität der gebildeten Deckschichten unter verschiedenen klimatischen Bedingungen erlauben. In diesem Beitrag wird anhand verschiedener Deckschichtzustände an Zink der Mehrwert von Untersuchungen mit gelartigen Elektrolyten für die Korrosionsforschung verdeutlicht.
Limitations are encountered regarding the electrolyte when studying atmospheric corrosion reactions on materials that form protective layers on their surface or tend to passivate. For example, the reconstruction of a thin wet film, as well as the interpretation of electrochemical measurements in so-called bulk solutions (a "mass" of electrolyte), often proves to be difficult in view of corrosion behavior under atmospheric conditions. A new approach to this problem in corrosion research includes the use of gel-type electrolytes as an alternative to bulk electrolytes. Gel-type electrolytes form a thin wet film on the surface of the material, whereby the naturally formed protective layer is affected similar to atmospheric conditions and can be examined in an almost non-destructive way. Through electrochemical instrumentation specific values such as polarization resistances and corrosion currents can be determined providing information on kinetics of surface layer formation and stability of surface layers formed under the influence of a thin wet film. Thus, new test methods can be developed that supply a better understanding of corrosion processes in specific atmospheres.
In this article different zinc coatings and aluminium alloys were investigated, their naturally formed protective layers were electrochemically characterized and corrosion relevant values were determined by using a gel pad based on polysaccharide. Corrosion relevant values allowed the differentiation of various coating systems and could describe the current protective effect provided by the coating. It is shown that gel-type electrolytes influence protective layers and coatings considerably less than corresponding bulk electrolytes and that an atmospheric wet film is approached by these test conditions. From the results it is evident that gel-type electrolytes represent a viable and promising field in corrosion research.
In the presentation different zinc coatings are presented and investigated. Their naturally formed protective layers are electrochemically characterized and corrosion relevant values are determined by using a gel pad based on polysaccharide. The corrosion relevant values allow the differentiation of various zinc coating systems and can describe the current protective effect provided by the coating. It is shown that gel-type electrolytes influence protective layers and coatings considerably less than corresponding bulk electrolytes. From the results it is evident that gel-type electrolytes represent a viable and promising field in corrosion research.
Korrosionsuntersuchungen mit gelartigen Elektrolyten an natürlich gebildeten Zinkdeckschichten
(2016)
Ein neuer Ansatz bei elektrochemischen Korrosionsuntersuchungen kann durch den Einsatz von gelartigen Elektrolyten als Alternative zu wässrigen Prüfelektrolyten beschritten werden. Gelartige Elektrolyte ermöglichen minimalinvasive Untersuchungen an natürlich gebildeten Zinkdeckschichten.
Dadurch können korrosionsrelevante Kennwerte ermittelt werden, die Aussagen zur Deckschichtbildung und zur Stabilität der gebildeten Deckschichten erlauben. In diesem Beitrag wird anhand verschiedener Deckschichtzustände an Zink der Mehrwert von gelartigen Elektrolyten für die Korrosionsforschung verdeutlicht.
A new approach to the assessment of the corrosion behaviour of zinc coatings under atmospheric conditions can be achieved using gel-type electrolytes as an alternative to standard aqueous test electrolytes. Gel-type electrolytes allow minimally invasive corrosion investigations on zinc coatings. They also provide the possibility to carry out corrosion investigations onsite. By using gel-type electrolytes corrosion-relevant characteristic values such as corrosion currents and polarization resistances can be determined. These allow to describe the formation and the stability of the formed corrosion product layers under various climatic conditions. With this knowledge, a prediction of the zinc coating life cycle is possible. In this contribution, the value of gel-type electrolytes for corrosion research on zinc coatings is presented.
In accordance with IAEA SSR-6 para 306 a management system shall be established and implemented to ensure compliance with the relevant provisions of the IAEA regulations. BAM has issued an update of the guideline: the BAM-GGR 011. The new revision describes necessary quality assurance measures for design, manufacture, testing, documentation, use, maintenance and inspection of packagings for package designs requiring competent authority approval for the transport of radioactive material.
The measures can be categorised as system-related and design-related. They are independently approved and monitored by the German competent authority BAM and its authorised expert (BAM/T). The qualification of the organisation applying for the design approval certificate is reviewed in the context of the design approval procedure. The quality assurance measures for manufacture consist of three main steps. Pre-assessment of manufacturing documents such as quality plans, specifications etc., Manufacturing inspections according the pre-assessed documents and inspection before commissioning including documentation review. Periodic inspections during operation as well as relevant specifications for use and maintenance ensure that the properties specified in the approval certificate are preserved over the package life time. Special provisions for the return on
experience regarding operational feedback for design, manufacture, use, maintenance and inspection are given. Special focus shall be given here to the rearranged and meanwhile established system of manufacturing inspections. This includes more transparent roles for a) the Producers authorised inspection 11282 representative, b) the independent inspection expert (S), acting on behalf of the manufacturer with acceptance of BAM, and c) BAM or its authorised expert (BAM/T). Additional attention shall be drawn to the management of deviations during manufacturing and provisions for maintenance and periodic inspections.
To better study the impact of nanoparticles on both in vitro and in vivo models, tissue distribution and cellular doses need to be described more closely. Here silver nanoparticles were visualized in alveolar macrophages by means of synchrotron radiation micro X-ray fluorescence spectroscopy (SR-μXRF) with high spatial resolution of 3 × 3 μm2. For the spatial allocation of silver signals to cells and tissue structures, additional elemental labeling was carried out by staining with eosin, which binds to protein and can be detected as bromine signal with SR-μXRF. The method was compatible with immunostaining of macrophage antigens. We found that the silver distribution obtained with SR-μXRF was largely congruent with distribution maps from a subsequent laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) of the same tissue sites. The study shows a predominant, though not exclusive uptake of silver into alveolar macrophages in the rat lung, which can be modeled by a similar uptake in cultured alveolar macrophages. Advantages and limitations of the different strategies for measuring nanoparticle uptake at the single cell level are discussed.
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.
Bei elektrochemischen Untersuchungen von atmosphärischen Korrosionsreaktionen an deckschicht- und passivschichtbildenden Werkstoffen stößt man elektrolytseitig an Grenzen. So erweisen sich sowohl das Nachempfinden eines dünnen Feuchtfilms als auch die Interpretation von elektrochemischen Messungen in so genannten Bulk-Lösungen (eine „Masse“ an Elektrolyt) hinsichtlich des Korrosionsverhaltens unter atmosphärischen Bedingungen häufig als schwierig. Eine neue Herangehensweise an diese Problemstellung in der Korrosionsforschung beinhaltet den Einsatz von gelartigen Elektrolyten als Alternative zu den Bulk-Elektrolyten. Gelartige Elektrolyte bilden einen dünnen Feuchtfilm auf der Werkstoffoberfläche aus, wodurch die natürlich gebildete Deckschicht ähnlich wie an Atmosphäre beeinflusst wird und nahezu zerstörungsfrei untersucht werden kann. Durch eine elektrochemische Instrumentierung können geeignete Kennwerte wie Polarisationswiderstände und Korrosionsströme ermittelt werden, die Aussagen zur Kinetik der Deckschichtbildung und zur Stabilität der gebildeten Deckschichten unter Einwirkung eines dünnen Feuchtfilms ermöglichen.
Anhand von auf Polysaccharid basierenden Gelpads werden im vorliegenden Beitrag verschiedene Zinkschichtsysteme und Aluminiumlegierungen untersucht, die natürlich gebildeten Deckschichten elektrochemisch charakterisiert und korrosionsrelevante Kennwerte bestimmt. Die ermittelten Kennwerte erlauben eine Differenzierung verschiedener Schichtsysteme und beschreiben die momentane Schutzwirkung der Deckschichten unter atmosphärischen Bedingungen.
For the assessmentand for monitoring of timber structures there are numerous promising methods that enable the quantitative description of the current condition of construction elements or parts of a structure. This concerns material properties like modulus of elasticity, moisture content and density as well as structural properties like dynamic characteristics, localization of inhomogeneities, cracks, and biological attack. During the work in COST Action FP 1101, since 2012 the capability of experimental methods are discussed and compared. This covers electrical and electromagnetic wave methods (resistivity, microwave, Radar, X-Ray), elastic waves (ultrasound, pile testing) and mechanical testing (static and dynamic). Describing and collecting the use of the experimental methods for monitoring purposes was the objective of working group 3 "Monitoring of Timber Structures" of the COST Action. Monitoring capabilities will extend the use of timber structures to further applications in civil engineering. So far, no standard exists but collections of application examples and review papers representing the state of the art. From there needs for further developments regarding monitoring and NDT methods for timber structures can be identified and these are described in this paper.
The key objective of this work is to create a comprehensive comparison between experimental analysis methods for detecting crosslinking reaction in EVA encapsulant material during PV module fabrication process. Several analytical methods, spanning from classical gel content extraction measurements over different thermo-analytic and mechanical approaches to spectroscopic analysis as Thermally Stimulated Current (TSC), have been investigated as to their ability to reveal the crosslinking state of ethylene vinyl acetate (EVA). The basic results show that TSC complements perfectly other thermal analysis methods like as Differential Scanning Calorimetry (DSC), Dynamic Mechanical Thermal Analysis (DMTA) to determine fundamental properties of EVA such as molecular mobility characteristics and also to monitor the crosslinking reaction. Exothermic peak as revealed by DSC analysis can be used to estimate the crosslinking rate of EVA during PV module encapsulation process as fast quality control test. ------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
L'objectif principal de ce travail est de permettre une meilleure compréhension entre les différentes techniques analyses expérimentales pour détecter la réaction de réticulation au niveau de lencapsulant Ethylène-Vinyle Acétate (EVA), durant le process de fabrication d'un module PV. Plusieurs méthodes d'analyse, allant du test classique d'extraction du taux de gel aux différentes techniques d'analyses thermomécaniques ainsi que les techniques d'analyse de spectroscopie comme le courant stimulé thermiquement (TSC), ont été étudiés pour permettre de révéler le phénomène de la réaction de réticulation de l'encapsulant l'EVA. Les résultats de base montrent que la TSC complète parfaitement d'autres méthodes d'analyses thermiques comme la calorimétrie différentielle à balayage (DSC), l'analyse mécanique dynamique (DMTA) pour déterminer les propriétés fondamentales de l'EVA. Ces techniques permettent de déterminer les caractéristiques relatives à la mobilité moléculaire et aussi pour mieux mettre en évidence la réaction de réticulation. Le pic exothermique comme révélé par l'analyse par DSC, peut être utilisé pour estimer le taux de réticulation de l'EVA au cours du process d'encapsulation du module PV comme un test rapide de contrôle de qualité.
In this paper, we present and validate the concept of an autonomous aerial robot to reconstruct tomographic 2D slices of gas plumes in outdoor environments. Our platform, the so-called Unmanned Aerial Vehicle for Remote Gas Sensing (UAV-REGAS), combines a lightweight Tunable Diode Laser Absorption Spectroscopy (TDLAS) gas sensor with a 3-axis aerial stabilization gimbal for aiming at a versatile octocopter. While the TDLAS sensor provides integral gas concentration measurements, it does not measure the distance traveled by the laser diode’s beam nor the distribution of gas along the optical path. Thus, we complement the set-up with a laser rangefinder and apply principles of Computed Tomography (CT) to create a model of the spatial gas distribution from a set of integral concentration measurements. To allow for a fundamental ground truth evaluation of the applied gas tomography algorithm, we set up a unique outdoor test environment based on two 3D ultrasonic anemometers and a distributed array of 10 infrared gas transmitters. We present results showing its performance characteristics and 2D plume reconstruction capabilities under realistic conditions. The proposed system can be deployed in scenarios that cannot be addressed by currently available robots and thus constitutes a significant step forward for the field of Mobile Robot Olfaction (MRO).
Elastomers are used in almost all areas of industrial applications, such as tires, engine mounts, bridge bearings, seals or coatings. During their use in operation, they are exposed to different environmental influences. These include, in particular, climatic factors such as air oxygen, high temperatures, light (UV radiation) and the influence of media (e.g. oils, fuels). A very important result of these factors is the chemical ageing of elastomers. In this case, the elastomer degenerates and changes its chemical structure in the aged regions, which leads to an irreversible change in the material properties in connection with the reduction in its usability. In this paper, chemical ageing of nitrile butadiene rubber (NBR) is investigated. Especially in case of thermo-oxidative ageing at elevated operating temperatures, the ageing processes run inhomogeneously. These effects are known as diffusion-limited oxidation (DLO) and are associated with the diffusion–reaction behaviour of atmospheric oxygen with the elastomer network. For these reasons, NBR samples are artificially aged in air and subjected to different experimental methods, which are presented and discussed. Additional results from inhomogeneous mechanical tests and permeation tests indicate the causes of the DLO-effect, show the influence of chemical ageing and are subsequently used for parameter identification in relation to the diffusion–reaction equation. A continuum-mechanical modelling approach is also presented here, which describes the finite hyperelasticity, diffusion–reaction processes as well as chemical degradation and reformation of the elastomer network. This multifield problem leads to a system of partial and ordinary differential equations and constitutive equations and is solved within the finite element method.
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.
Ein neuer Ansatz bei elektrochemischen Korrosionsuntersuchungen kann durch den Einsatz von gelartigen Elektrolyten als Alternative zu wässrigen Prüfelektrolyten beschritten werden. Gelartige Elektrolyte ermöglichen minimalinvasive Untersuchungen an natürlich gebildeten Zinkdeckschichten. Dadurch können korrosionsrelevante Kennwerte ermittelt werden, die Aussagen zur Deckschichtbildung und zur Stabilität von atmosphärisch gebildeten Deckschichten erlauben. In diesem Beitrag wird anhand verschiedener Untersuchungen an Reinzink der Mehrwert von gelartigen Elektrolyten für die Korrosionsforschung und -prüfung verdeutlicht. Darüber hinaus werden neue Erkenntnisse zur Deckschichtbildung von Zink unter atmosphärischen Bedingungen vorgestellt.
The development of organic coatings for corrosion protection is an elaborate process with a multitude of often interminable investigations and tests of protection properties. Electrochemical methods support the processes of development to a great extent and help to understand mechanisms of action and failure. They are usually carried out on applied coating systems with a completed formulation. An examination possibility is presented in this publication that enables the characterization of waterbased coatings with different formulation variations in the liquid (aqueous) state with the aid of electrochemical noise technique. Thus, selection of binders, pigments, and other additives is supported essentially and made more efficient in a very early Phase of formulation development. The paper shows that a unique insight into the dynamic processes of a metal in contact with an aqueous coating dispersion is possible using the example of the development of zinc-free corrosion-inhibiting pigments for waterbased coatings. In addition, it is presented in which way the results correlate with the performance of applied coatings.
The paper presents a new method for the determination and evaluation of tafel factors using gel-type electrolytes and electrochemical frequency modulation technique (EFM). This relatively new electrochemical method offers the possibility to determine both polarization resistances and tafel factors within one measurement and in short measuring intervals. Starting from a comprehensive parameter study it is shown that a direct relationship between the two values exists that can be described mathematically. This contribution presents the determined tafel factors for the system gel-type electrolyte/zinc and discusses their applicability and their limits.
The paper presents a new method for the determination and evaluation of tafel factors using gel-type electrolytes and electrochemical frequency modulation technique (EFM). This relatively new electrochemical method offers the possibility to determine both polarization resistances and tafel factors within one measurement and in short measuring intervals. Starting from a comprehensive parameter study it is shown that a direct relationship between the two values exists that can be described mathematically. This contribution presents the determined tafel factors for the system gel-type electrolyte/zinc and discusses their applicability and their limits.
Magura Cave, north-western Bulgaria, possesses valuable rock-art paintings made with bat guano and dated from the period between the Eneolithic and Bronze Ages. Since 2008, the Art Gallery is closed to the general public in order to protect the paintings from vandalism, microclimatic changes caused by visitors and artificial illumination, and the consequent growth of fungi and phototrophs. Nevertheless, some tourist visits are allowed under the supervision of cave managers. This study provides the first scientific report on cultivable fungal assemblages dwelling different substrata in the Art Gallery. A total of 78 strains, belonging to 37 OTUs (Ascomycota 81%, Zygomycota 13%, Basidiomycota 5%), were isolated in the study. This fungal diversity was clearly dominated by Penicillium (50% of strains) and Aspergillus (13%). The most relevant visible fungal colonies were detected in sediments rich in bat guano, where, besides Penicillium, other guanophilic fungi such as Mucor, Mortierella, Trichosporon and Trichoderma were dominant. Conversely, scarce fungi were detected on rock surface of painted walls. Based on the biocide susceptibility assay, octylisothiazolinone (OIT) and benzalkonium chloride (BAC) were effective inhibiting the in vitro growth of dominant fungal species in Magura Cave, when applied at concentrations ranged from 100 to 1,000 mg/L. These data provide a valuable knowledge about Magura fungi, and exemplify a type of preliminary test that may be conducted before planning any biocide treatment. However, considering the irreversible effects of biocides on the ecological balance in caves, and the low fungal contamination in painted walls of Magura Cave, there is no reason to use conventional biocides in this cave. Further studies, monitoring microbial communities and microclimatic parameters, should be conducted to improve the knowledge on microbial ecology in Magura Cave and possible human impacts, as well as to allow the early detection of potential microbial outbreaks.
In this paper, we present an autonomous aerial robot to reconstruct tomographic 2D slices of gas plumes in outdoor environments. Our platform, the so-called Unmanned Aerial Vehicle for Remote Gas Sensing (UAV-REGAS) combines a lightweight Tunable Diode Laser Absorption Spectroscopy (TDLAS) sensor with a 3-axis aerial stabilization gimbal for aiming on a versatile octocopter. The TDLAS sensor provides integral gas concentration measurements but no information regarding the distance traveled by the laser diode's beam or the distribution of the gas along the optical path. We complemented the set-up with a laser rangefinder and apply principles of Computed Tomography (CT) to create a model of the spatial gas distribution from these integral concentration measurements. To allow for a rudimentary ground truth evaluation of the applied gas tomography algorithm, we set up a unique outdoor test environment based on two 3D ultrasonic anemometers and a distributed array of 10 infrared gas transmitters. We present first results showing the 2D plume reconstruction capabilities of the system under realistic conditions.
Elektrochemisches Rauschen von unlegiertem Stahl in wasserbasierten Bindemittel-Pigment-Gemischen
(2017)
Die Entwicklung von Beschichtungen für den Korrosionsschutz ist ein aufwändiger Prozess mit einer Vielzahl von oftmals langwierigen Untersuchungen und Prüfungen der Schutzeigenschaften.
Elektrochemische Methoden unterstützen die Entwicklungsprozesse in hohem Maße und helfen beim Verstehen von Wirk- und Schadensmechanismen. Sie werden meistens an fertig formulierten und applizierten Beschichtungssystemen vorgenommen. Es wird eine Untersuchungsmöglichkeit vorgestellt, bei der sich wasserbasierte Beschichtungsstoffe in unterschiedlichen Formulierungsvarianten bereits im flüssigen Zustand mit Hilfe des elektrochemischen Rauschens charakterisieren lassen. Damit ist es möglich, bereits in einer sehr frühen Phase der Formulierungsentwicklung die Auswahl von Bindemitteln, Pigmenten und weiteren Zusatzstoffen entscheidend zu unterstützen und effizienter zu gestalten. Am Beispiel der Entwicklung von zinkfreien Korrosionsschutzpigmenten für wasserbasierte Beschichtungen
wird gezeigt, dass ein einzigartiger Einblick in die dynamischen Prozesse bei Kontakt eines Metalls mit der wässrigen Beschichtungsdispersion möglich ist und wie dies mit der Performance der Beschichtungen korreliert.
Ein neuer Ansatz bei elektrochemischen Korrosionsuntersuchungen kann durch den Einsatz von gelartigen Elektrolyten als Alternative zu wässrigen Prüfelektrolyten beschritten werden. Gelartige Elektrolyte ermöglichen minimalinvasive Untersuchungen an natürlich gebildeten Zinkdeckschichten. Dadurch können korrosionsrelevante Kennwerte ermittelt werden, die Aussagen zur Deckschichtbildung und zur Stabilität der gebildeten Deckschichten erlauben. In diesem Beitrag wird anhand verschiedener Deckschichtzustände an Zink der Mehrwert von gelartigen Elektrolyten für die Korrosionsforschung verdeutlicht.
Electrochemical tests, hardness measurements, and microstructure analysis are performed to study the influence of austenitizing, quenching, and tempering parameters on the corrosion resistance of the martensitic stainless steel grade X50CrMoV15 (1.4116). Different heat treatment states were studied using an adapted EPR-Test to evaluate the chromium distribution and depletion caused by the formation and dissolution of chromium rich carbides. The EPR results were correlated with pitting corrosion behavior, demonstrating the strong effect of heat treatment parameters on the susceptibility of martensitic stainless steels to corrosion phenomena.
Inelastic incoherent neutron time-of-flight scattering was employed to investigate the low-frequency vibrational density of states (VDOSs) for a series of glassy Janus-poly(tricyclononenes), which consist of a rigid main chain and flexible alkyl side chains. Here, the length of the flexible side chains was systematically varied from propyl to octyl. Such materials have potential applications as active separation layers in gas separation membranes as a green future technology, especially for the separation of higher hydrocarbons. From the morphological point of view, the Janus polynorbornenes undergo a nanophase separation into alkyl side chain-rich nanodomains surrounded by a rigid polynorbornene matrix. Here, the influence of the nanophase-separated structure on the low-frequency VDOS is investigated from a fundamental point of view. The low-frequency VDOSs of these Janus polynorbornene show excess contributions to the Debye type VDOS known as the Boson peak (BP) for all side chain lengths. Due to the high incoherent scattering cross-section of hydrogen, most of the scattering comes from the alkyl side chain-rich domains.
Compared to conventional glass-forming materials, in the considered Janus polynorbornenes, the BP has a much lower intensity and its frequency position is shifted to higher values. These experimental results are discussed in terms of the nanophase-separated structure where the alkyl chain-rich domains were constrained by the surrounding matrix dominated by the rigid backbone. With increasing alkyl chain length, the size of the alkyl chain-rich domains increases. The frequency position of the BP shifts linearly to lower frequencies with the size of these nanodomains estimated from X-ray measurements. The obtained results support the sound wave interpretation to the BP
Im deutschen Eisenbahnnetz sind ca. 80 Millionen Spannbetonschwellen verbaut. Analog zu anderen Bauwerken werden Wpannbetonschwellen regelmäßig visuell inspiziert. Die Rissbildung ist bei diesen Inspektionen ein Kriterium für die Schädigung einer Spannbetonschwelle. Durch Rissbildung kann es passieren, dass Betonschwellen ihre Nutzungsdauer nicht erreichen.
A facile approach for the synthesis of monodisperse gold nanoparticles with radii in the range of 7 to 20 nm is presented. Starting from monodisperse seeds with radii of 7 nm, produced in the first step, the addition of a defined amount of additional precursor material permits distinct size regulation and the realization of predicted nanoparticle sizes. These information were derived from ex- and in situ investigations by comprehensive small angle X-ray scattering (SAXS), X-ray absorption near edge structure (XANES) and UV-Vis data to obtain information on the physicochemical mechanisms. The obtained mechanisms can be transferred to other seeded growth processes. Compared to similar approaches, the presented synthesis route circumvents the use of different reducing or stabilizing agents. The size of resulting nanoparticles can be varied over a large size range presented for the first time without a measurable change in the shape, polydispersity or surface chemistry. Thus, the resulting nanoparticles are ideal candidates for size dependence investigations.
A collaborative trial involving 16 participants from nine European countries was conducted within the NORMAN network in efforts to harmonise suspect and non-target screening of environmental contaminants in whole fish samples of bream (Abramis brama). Participants were provided with freeze-dried, homogenised fish samples from a contaminated and a reference site, extracts (spiked and non-spiked) and reference sample preparation protocols for liquid chromatography (LC) and gas chromatography (GC) coupled to high resolution mass spectrometry (HRMS). Participants extracted fish samples using their in-house sample preparation method and/or the protocol provided. Participants correctly identified 9-69% of spiked compounds using LC-HRMS and 20-60% of spiked compounds using GC-HRMS. From the contaminated site, suspect screening with participants’ own suspect lists led to putative identification of on average ~145 and ~20 unique features per participant using LC-HRMS and GC-HRMS, respectively, while non-target screening identified on average ~42 and ~56 unique features per participant using LC-HRMS and GC-HRMS, respectively. Within the same sub-group of sample preparation method, only a few features were identified by at least two participants in suspect screening (16 features using LC-HRMS, 0 features using GC-HRMS) and non-target screening (0 features using LC-HRMS, 2 features using GC-HRMS). The compounds identified had log octanol/water partition coefficient (KOW) values ranging from -9.9 to 16 and mass-to-charge ratio (m/z) of 68 to 761 (LC-HRMS and GC-HRMS). A significant linear trend was found between log KOW and m/z for the GC-HRMS data. Overall, these findings indicate that differences in screening results are mainly due to the data analysis workflows used by different participants. Further work is needed to harmonise the results obtained when applying suspect and non-target screening approaches to environmental biota samples.
"Ullmann's Encyclopedia of Industrial Chemistry" is the benchmark reference in chemistry and chemical and life science engineering, covering inorganic and organic chemicals, advanced materials, pharmaceuticals, polymers and plastics, metals and alloys, biotechnology and biotechnological products, food chemistry, process engineering and unit operations, analytical methods, environmental protection, and much more.
The present article is part of the topic collection "Environmental Protection and Industrial Safety". It covers plant and process safety, focusing on hazardous materials and process conditions.
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%.