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Eingeladener Vortrag
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Der Implant-Test nach ISO 17642-3 gehört zur Gruppe der fremdbeanspruchten Kaltrisstests, bei dem eine äußere Beanspruchung auf einen zylindrischen Stab (Implant-Probe) definiert aufgebracht wird. Mit dieser Kaltrissprüfung wurde vergleichende Analysen zur Kaltrissempfindlichkeit der modernen hochfesten Feinkornbaustähle S960MC und S960QL durchgeführt.
This work focuses on the question if the bubble test prescribed in the Dangerous Goods Regulations has sufficient sensitivity to detect leakage rates which could result in the formation of explosive atmospheres during transport. The sensitivity of the bubble test is not directly comparable with other leak testing methods because of its different flow conditions.
Therefore, a normalized minimum detectable leakage rate under Helium test conditions is calculated for the bubble test. This sensitivity of the bubble test under reference conditions is compared with limit leakage rates for a worst-case transport scenario. The sensitivity of the bubble test is not sufficient to prove the limit leakage rates for 6-L packagings. The Formation of explosive vapour-air-mixtures cannot be excluded. Therefore, more sensitive leak testing methods should be considered for smaller packaging design types.
19th and 20th centuries glass paint layers consist of a colour body and a colourless lead silicate flux, in which borax or boric acid was added as further component to improve the paint ability and to reduce the firing temperature for multiple layers of paint. Model glasses were used in laboratory tests to investigate the stability of glass paints with additions of boron oxide. To determine boron in paint layers, a LIBS-system with pulsed NdYAG-laser was used.
For metal-based additive manufacturing, sensors and measuring systems for monitoring of the energy source, the build volume, the melt pool and the component geometry are already commercially available. Further methods of optics, spectroscopy and non-destructive testing are described in the literature as suitable for in-situ application, but there are only a few reports on practical implementations.
Therefore, a new BAM project aims to develop process monitoring methods for the in-situ evaluation of the quality of additively manufactured metal components. In addition to passive and active thermography, this includes optical tomography, optical emission and absorption spectroscopy, eddy current testing, laminography, X-ray backscattering and photoacoustic methods. These methods are used in additive manufacturing systems for selective laser melting, laser metal deposition and wire arc additive manufacturing. To handle the sometimes huge amounts of data, algorithms for efficient preprocessing are developed and characteristics of the in-situ data are extracted and correlated to defects and inhomogeneities, which are determined using reference methods such as computer tomography and metallography. This process monitoring and fusion of data of different measurement techniques should result in a significant reduction of costly and time-consuming, destructive or non-destructive tests after the production of the component and at the same time reduce the production of scrap.
Here, first results of simultaneous measurements of optical emission spectroscopy and thermography during the laser metal deposition process using 316L as building material are presented. Temperature values are extracted from spectroscopic data by fitting of blackbody emission spectra to the experimental data and compared with results from a thermographic camera. Measurements with and without powder flow reveal significant differences between welding at a pristine metal surface and previously melted positions on the build plate, illustrating the significant influence of the partial oxidation of the surface during the first welding process on subsequent welding. The measurement equipment can either be mounted stationary or following the laser path. While first results were obtained in the stationary mode, future applications for online monitoring of the build of whole parts in the mobile mode are planned.
This research was funded by BAM within the focus area Material.
High-density polyethylene becomes optically transparent during tensile drawing when previously saturated with diesel fuel. This unusual phenomenon is investigated as it might allow conclusions with respect to the material behavior. Microscopy, differential scanning calorimetry, density measurements are applied together with two scanning X-ray scattering techniques: wide angle X-ray scattering (WAXS) and X-ray refraction, able to extract the spatially resolved crystal orientation and internal surface, respectively. The sorbed diesel softens the material and significantly alters the yielding characteristics. Although the crystallinity among stretched regions is similar, a virgin reference sample exhibits strain whitening during stretching, while the diesel-saturated sample becomes transparent. The WAXS results reveal a pronounced fiber texture in the tensile direction in the stretched region and an isotropic orientation in the unstretched region. This texture implies the formation of fibrils in the stretched region, while spherulites remain intact in the unstretched parts of the specimens. X-ray refraction reveals a preferred orientation of internal surfaces along the tensile direction in the stretched region of virgin samples, while the sample stretched in the diesel-saturated state shows no internal surfaces at all. Besides from stretching saturated samples, optical transparency is also obtained from sorbing samples in diesel after stretching.
The investigation of the long-term performance of sealing systems employed in containers for radioactive waste and spent nuclear fuel is one research focus area for division 3.4 “Safety of Storage Containers” at the Bundesanstalt für Materialforschung und -prüfung (BAM). Our investigations comprise investigations on metallic and elastomeric seals and covers experimental investigations to get a database on the component/material behaviour, work on analytical descriptions and numerical analysis. Our aim is to understand the long-term behaviour of the sealing systems for evaluation of their performance during possible extended interim storage and subsequent transportation.
The investigation of the long-term performance of sealing systems employed in containers for radioactive waste and spent nuclear fuel is one research focus area for division 3.4 “Safety of Storage Containers” at the Bundesanstalt für Materialforschung und -prüfung (BAM). Our investigations comprise investigations on metallic and elastomeric seals and covers experimental investigations to get a database on the component/material behaviour, work on analytical descriptions and numerical analysis. Our aim is to understand the long-term behaviour of the sealing systems for evaluation of their performance during possible extended interim storage and subsequent transportation.
It is a well-known story that copolymers beside their molar mass distribution (MMD) can exhibit a functionality type distribution (FTD), a copolymer composition distribution (CCD), a monomer sequence distribution (MSD) and additionally different topologies within one sample. Nowadays a wide range of different analytical separation techniques and multi-detection possibilities are available.
The challenge consists in a clever combination of these techniques coordinated with the heterogeneity to be investigated.
A number of applications will be presented from e.g. topology elucidation of branched EO-PO “academic” copolymers to copolymer composition of partially broadly distributed progressively tailored “industrial relevant” copolymers consisting of e.g. polyamides, polycarbonates and polysiloxanes.
Multidimensional separation techniques will be demonstrated with focus on mass spectrometric detection techniques (ESI-/MALDI-TOF-MS) coupled online or semi-online to prior separation.
The use of secondary building materials can meet the requirements of sustainability in several ways: the extended time availability of primary raw materials and, thereby, the protection of natural ressources as well as the conservation of landfill sites. Regarding the predicted decrease of gypsum supply in Germany, particularly the recycling of gypsum (calcium sulfate) is of growing importance. Currently, the gypsum demand is fulfilled (at least 60%) by gypsum as side product from coal-fired power plants (FGD Gypsum). Germany’s natural gypsum deposits fulfil the remaining gypsum demand. Due to national climate protection goals the gypsum supply from coal power plants will decrease significantly in the future.
In addition, the content of sulfates in other secondary building materials, in particular in recycled concrete aggregates, should be minimized for quality reasons. Separated gypsum can be used in gypsum production if the high quality requirements for recycled gypsum are met. Accordingly, there have been significant advancements in the processing of gypsum residues in the last years. Since almost all processing steps in the recycling process are associated with environmental impacts, an evironmental evaluation of the use of recycled gypsum as a substitute in gypsum production has to be carefully conducted.
The presentation focusses on the techniques for generating recycled gypsum from gypsum plaster boards, the related quality requirements and a comprehensive environmental evaluation of the complete process.
Nanocomposites based on MgAL layered double hydroxides (LDH) and an epoxy resin were prepared and investigated by a combination of complementary methods. As epoxy resin Bisphenol A diglycidyl ether (DGEBA) was used with Diethylenetriamine as curing agent. The LDH was modified with taurine, which acts as an additional crosslinking agent due to its amine groups. The epoxy resin was cured in a presence of the nanofiller, which was added to the system in various concentrations. X-ray scattering, by combination of SAXS and WAXS was used to characterize the morphology of the obtained nanocomposites. These investigations show that the filler is distributed in the matrix as small stacks of ca. 10 layers. The molecular dynamics of the system, as probe for structure, was investigated by broadband dielectric spectroscopy. In addition to the - and -relaxation (dynamic glass transition), characteristic for the unfilled materials, a further process was found which was assigned to localized fluctuations of segments physically adsorbed or chemically bonded to the nanoparticles. The dielectric -relaxation is shifted to higher temperatures for the nanocomposites in comparison to the pure material but depends weakly on the content of nanoparticles. Further, for the first time Flash DSC was employed to a thermosetting system to investigate the glass transition behavior of the nanocomposites. The heating rates were converted in to relaxation rates. For low concentrations of the nanofiller the thermal data overlap more or less with that of the pure epoxy. For higher concentrations the thermal data are shifted significantly to higher temperatures. This is discussed in terms the cooperativity approach to the glass transition.
Localized patches are a cost- and time-effective method for repairing fiber-reinforced polymer (FRP) sandwich wind turbine rotor blade shells. To increase the understanding of their effect on the fatigue of the blades, this study examines the effect of various layup methods of localized repair patches on the structural integrity of composite sandwich structures. Manufactured with the vacuum-assisted resin infusion (VARI) process, the shell test specimens are produced as a curved structure with glass fiber reinforced polymer (GFRP) sandwiching a polyvinyl chloride (PVC) foam core. Patch repairs are then introduced with varying layup techniques, and material properties are examined with cyclic fatigue tests. The transition region between patch and parent material is studied in greater detail with finite element method (FEM) simulations, with a focus on the effect of fiber orientation mismatch. Damage onset, crack development, and eventual failure are monitored with in-situ non-destructive testing methods to develop a robust understanding of the effects of repair concepts on material stiffness and strength.
This presentation describes the testing methods used to determine the thermal properties of insulation materials and mechanical properties of materials used for the load-bearing structure for pressure tanks (up to 4 bar) and cryogenic liquids (LNG, -162 °C at atmospheric pressure). Goal is to design a transportation tank that does not exceed 4 bars (relative) within 10 h, starting at atmospheric pressure. PUR-foam is a suitable material for the insulation. A 12,5 l small scale tank prototype reached 4 bar (relative) within 87 minutes, which is, regarding the influence of the size, a satisfying result. The mechanical properties change significantly at cryogenic temperatures. The bending modulus is similar at first, but decreases at a certain point by 2/3. However, the maximum stress is much higher and could not be reached within this testing setup.
Rationale: Boron (B) is an essential micronutrient in plants and its isotope variations are used to gain insights into plant metabolism, which is important for crop plant cultivation. B isotope variations were used to trace intra‐plant fractionation mechanisms in response to the B concentration in the irrigation water spanning the
range from B depletion to toxic levels.
Methods: A fully validated analytical procedure based on multi‐collector inductively coupled plasma mass spectrometry (MC‐ICP‐MS), sample decomposition and B Matrix separation was applied to study B isotope fractionation. The Validation was accomplished by establishing a complete uncertainty budget and by applying reference materials, yielding expanded measurement uncertainties of 0.8‰ for pure boric acid solutions and ≤1.5‰ for processed samples. With this validated procedure SI traceable B isotope amount ratios were determined in plant reference materials for the first time.
Results: The B isotope compositions of Irrigation water and bell pepper samples suggest passive diffusion of the heavy 11B isotope into the roots during low to high B concentrations while uptake of the light 10B isotope was promoted during B depletion, probably by active processes. A systematic enrichment of the heavy 11B isotope in higher located plant parts was observed (average Δ11Bleaf‐roots = 20.3 ± 2.8‰ (1 SD)), possibly by a facilitated transport of the heavy 11B isotope to growing Meristems by B transporters.
Conclusions: The B isotopes can be used to identify plant metabolism in Response to the B concentration in the irrigation water and during intra‐plant B transfer. The large B isotope fractionation within the plants demonstrates the importance of
biological B cycling for the global B cycle.
Im 2. Teil des Artikels zu den Untersuchungen zum Einfluss von Rohrleitungsverzweigungen auf die Wirksamkeit von Deflagrationsrohrsicherungen (s. a. [1]) werden die Ergebnisse der visuellen Beobachtungen des Reaktionsverlaufes sowie die Belastungen der Flammendurchschlagsicherung (s. Bild 1) bei unterschiedlichen Einbaubedingungen in den Vordergrund gestellt. Gegenübergestellt wird die Belastungssituation der Flammensperre in einer geraden und einer verzweigten Rohrleitung. Ausdrücklich wurden Einbaubedingungen gewählt, die nicht Normgerecht [2] sind. Verwendet wurde dafür eine speziell gefertigte Deflagrationsrohrsicherung, die eine Beobachtung des Reaktionsverlaufs im Bereich der spiralförmig gewickelten Metallbänder erlaubt. Zusätzlich wurde im geschützten Bereich in der Rohrleitung eine Kamera installiert, die die Belastungssituation bei den einzelnen Versuchen dokumentierte. Die Ergebnisse bestätigen sehr eindrucksvoll, dass die Belastungssituation der Deflagrationsrohrsicherung sich in Abhängigkeit von der Konfiguration der Rohrleitung entscheidend ändert.
The European Joint Programme on Radioactive Waste Management (EURAD) has been launched to coordinate activities on agreed priorities of common interest between European partners. The main actions include scientific and technical activities on radioactive waste characterization and processing, interim storage of radioactive waste as well as predisposal and disposal solutions. As part of the programme, the work package on Spent Fuel Characterization and Evolution until Disposal (SFC) was proposed and accepted by the European Commission. The objectives of this work package include the development of beyond-state-of-the-art characterization techniques for spent nuclear fuel during its evolution from reactor unloading until disposal, the understanding of the spent fuel performance during prolonged storage, transport and emplacement in a deep geological repository, the understanding of the behaviour of fuel, cladding, pellet-cladding interaction and ageing effect under normal and postulated accident scenarios until disposal, and contributions to operational safety concepts for fuel handling at spent nuclear fuel packaging facilities.
The knowledge of transformation pathways and identification of transformation products (TPs) of veterinary drugs is important for health, food and environmental matters. Monensin (MON) is an ionophore antibiotic widely used to cure and prevent coccidiosis by chicken especially in broiler farming. Residues can be found in food products (chicken and eggs) and in the environment (manure, soil, water). Several transformation processes can alter the parent compound MON, ranging from biotransformation in living organism to biotic/abiotic and microbial processes in environmental matters.
The main objective of this work was to investigate the potential of electrochemistry (EC) to simulate oxidative transformation processes of MON and to predict TPs. An electrochemical reactor was used consisting of a flow-through cell with a glassy carbon working electrode. Derived TPs were analyzed by online coupling of EC and high-resolution mass spectrometry (HRMS) and LC/HRMS offline measurements. Among the generated TPs already known as well as unknown TPs of MON could be found.
Additionally, MON was subjected also to other transformation experiments like metabolism tests with rat microsomes or the pH-dependent hydrolysis. As a result, different targeted and suspected TPs could be identified by analysis with LC/HRMS.
An overview of detected/identified TPs from this study will be presented in comparison to literature known metabolites and TPs.
This textbook fulfills its dedication of being the “essential reference for the field, featuring protocols, analysis,fundamentals and the latest advances” of impedance spectroscopy to its readers. It really provides an insight in all facets of this powerful technique.
It should not be missed in the bookshelf of electrochemists and all other interested researchers and engineers who want to be on the current state of this technique.
This talk presents a new application for high-spatial resolution eddy current testing (ET) with magneto resistive (MR) sensor arrays. With rising popularity and availability of additive manufacturing (AM), companies mainly in the aerospace sector, set high requirements on quality control of AM parts, especially produced with selective laser melting (SLM). Since it was shown that those parts are prawn to flaws like pores or cracks, every part needs to be tested. Therefore, NDT Methods, like ET, could help to characterize SLM parts. Research on ET has shown, that offline ET with high spatial resolution MR sensor arrays is possible and that flaws as small as 50 µm could be detected while significantly reducing testing time. In this talk a first approach on automated online ET method for testing SLM parts is proposed. An approach with hundreds of MR sensor is made to maintain spatial resolution and short testing times. Classic signal conditioning methods are used to reduce cost and complexity while maintaining high testing bandwidths. The proposed idea enables further research on automated generation of testing reports, process control or automated flaw curing.
To arrive to sustainable hydrogen-based energy solutions, the understanding of water-splitting catalysts plays the most crucial role. Herein, state-of-the-art hypotheses are combined on electrocatalytic active metal sites toward the oxygen evolution reaction (OER) to develop a highly efficient catalyst based on Earth-abundant cobalt and zinc oxides.
The precursor catalyst Zn0.35Co0.65O is synthesized via a fast microwaveassisted approach at low temperatures. Subsequently, it transforms in situ from the wurtzite structure to the layered γ-Co(O)OH, while most of its zinc leaches out. This material shows outstanding catalytic Performance and stability toward the OER in 1 m KOH (overpotential at 10 mA cm−2 ηinitial = 306 mV, η98 h = 318 mV). By comparing the electrochemical results and ex situ analyses to today’s literature, clear structureactivity correlations are able to be identified. The findings suggest that coordinately unsaturated cobalt octahedra on the surface are indeed the active centers for the OER.
Laser-induced periodic surface structures (LIPSS, ripples) are a universal phenomenon that can be observed on almost any material after the irradiation by linearly polarized laser beams, particularly when using ultrashort laser pulses with durations in the femtosecond to picosecond range.
During the past few years significantly increasing research activities have been reported in the field of LIPSS, since their generation in a single-step process provides a simple way of nanostructuring and surface functionalization towards the control of optical, mechanical, biological, or chemical surface properties. In this contribution the mechanisms of formation and current applications of LIPSS are reviewed, including the colorization of technical surfaces, the control of surface wetting properties, the mimicry of the natural texture of animal integuments, the tailoring of surface colonization by bacterial biofilms, the advancement of medical pacemakers, and the improvement of the tribological performance of nanostructured metal surfaces.
Up to now, oriented surface crystallization phenomena are discussed controversially, and related studies are restricted to few glasses. The vast majority of previous work does not consider possible effects of surface preparation and surrounding atmosphere. Moreover, very few observations of surface crystal orientation were made on separately grown crystals.
The aim of our project is to advance the basic understanding of oriented surface crystallization, e.g. whether preferred orientation of surface crystals results from oriented nucleation or reorientation mechanisms during early crystal growth. In both cases, crystal orientation may reflect the orientation of the glass surface or that of anisotropic active surface nucleation sites. Therefore, we focus on orientation of surface crystals separately growing under controlled conditions.
First results on diopside (MgCaSi2O6) and walstromite (BaCa2Si3O9) crystals growing from 18BaO·22CaO·60SiO2 and MgO·CaO·2SiO2 glass surfaces, respectively, indicate that different orientation mechanisms may occur.
Neighbored walstromite crystals were found to gradually reorient themselves when they are going to impinge each other during stepwise isothermal treatments (log η = 4,5 Pa*s) of polished glass samples. Nevertheless, no preferred crystal orientation was evident for separate crystals.
For diopside crystals growing from polished glass surfaces (1 μm diamond lapping foil), strong preferred orientation was observed for 3.5 to 85 min annealing at 850 °C. Electron Backscatter Diffraction (EBSD) studies showed that the c-axis of surface crystals is oriented parallel to the glass surface and that separated diopside crystals as small as 600 nm are already oriented. Studies on glass surfaces, polished with diamond lapping foils starting from 16 μm down to 1 μm grain, revealed that crystal orientation may scatter arround this preferential orientation and that this scatter progressively decreases with decreasing polishing grain size.
Glass powders are promising candidates for manufacturing a broad diversity of sintered materials like sintered glass-ceramics, glass matrix composites, glass bonded ceramics or pastes. Powder processing, however, can substantially affect sinterability, e.g. by promoting surface crystallization. On the other hand, densification can be hindered by gas bubble formation for slow crystallizing glass powders. Against this background, we studied sintering and foaming of silicate glass powders with different crystallization tendency for wet milling and dry milling in air, Ar, N2, and CO2 by means of heating microscopy, DTA, Vacuum Hot Extraction (VHE), SEM, IR spectroscopy, XPS, and ToF-SIMS. In any case, foaming activity increased significantly with progressive milling. For moderately milled glass powders, subsequent storage in air could also promote foaming. Contrarily, foaming could be substantially reduced by milling in water and 10 wt% HCl. Although all powder compacts were uniaxially pressed and sintered in air, foaming was significantly affected by different milling atmosphere and was found most pronounced for milling in CO2 atmosphere. Conformingly, VHE studies revealed that foaming is mainly driven by carbonaceous species, even for powders milled in other gases. Current results of this study thus indicate that foaming is caused by carbonaceous species trapped on the glass powder surface.
Metal-organic frameworks (MOFs) are suitable materials for gas storage of small molecules due to their nanoporous, crystalline structure. The extensively studied MOF HKUST-1 consist of Cu(II)-dimers in a paddlewheel structure, with 1,3,5-benzenetricarboxylic acid (BTC) as organic linker. Instability to humidity remains an issue for many types of MOFs, and for HKUST-1, it has been found that exposure to water vapor creates a surface barrier which reduces the gas uptake rate.
Near-ambient pressure XPS (NAP-XPS) is a promising method for investigations of the stability and interaction of HKUST-1 with various gas molecules. The oxidation state of copper can be monitored before, during and after exposure to various gases. This does not only provide information on the stability of the MOFs, but also on the interaction with the gas molecules and the reversibility of the processes.
NAP-XPS measurements of HKUST-1 exposed to methanol, pyridine and water vapor were performed with EnviroESCA, a laboratory NAP-XPS instrument developed by SPECS. Cu 2p, O 1s and C 1s core level spectra were acquired in pressure ranging from 10-5 to 8 mbar to assess the oxidation state of copper and the stability of the organic linker. HKUST-1 does not show interaction with pyridine, but there are indications of copper-reduction upon exposure to methanol and water vapor. Radiation induced damage is considered and two different approaches for determining the ratio of Cu(I) to Cu(II) will be discussed.
Experimenting on MAUS
(2019)
Everything SAXS
(2019)
For the purpose of increasing payload and reduce freight cost, lightweight composite tank containers used for Transportation have been progressively developed during the last years. Compared to conventionally produced cylindrical steel tanks, the fiber-reinforced solutions allow greater flexibility in the tank design. Despite a number of further material-related benefits of fiber-reinforced composites as non-conductive and non-magnetic behavior as well as corrosion resistance and high strength, the optimization of their thermal degradation properties during combustion is still a challenge. To improve the fire performance of lightweight composite containers, special intumescent fire protection coatings can be applied onto the outside tank surface. This paper presents fire tests on glass-fiber-reinforced plastic transport tanks with complex geometries sheltered with different surface-applied fire protection systems. To evaluate the fire resistance of the tank structures, a fiber optic monitoring system was developed. This system is based on distributed temperature measurements using high-Resolution optical backscatter reflectometry and pointwise reference measurements using fiber Bragg gratings. Thereby, all the fiber optic sensors were directly integrated in the composite layer structure of the tanks. The focus of the presented work is on the demonstration of capability of fiber optic monitoring system in such high-temperature application. Moreover, the fiber optic measurements provide new insights into the efficiency of intumescent coating applied for fire protection of fiber-reinforced plastic transport tanks.
The presented results gained within the project "CoFi-ABV - Consequences of tank failure" give detailed insights into the potential consequences of tank failure of commercial 11 kg propane cylinders and the LPG tank installed in a car in case of a misfunction of the safety device. In comprehensive test campaigns performed on the Test Site for Technical Safety of BAM (BAM TTS), 15 off-the-shelf propane bottles and three passenger cars with a LPG tank were exposed to an intensive fire. Sensors and measurement equipment were used to gain data (temperature, pressure, dynamic overpressure, thermal radiation, video data) enabling an analysis of the consequences of tank failure and for the continuous monitoring of the experiments.
Laser-induced plasmas are widely used in many areas of science and technology; examples include spectrochemical analysis, thin film deposition, material processing, and even jet propulsion. Several topics will be addressed. First, general phenomenology of laser-induced plasmas will be discussed. Then, a chemical model will be presented based on a coupled solution of Navier-Stokes, state, radiative transfer, material transport, and chemical (Guldberg-Waage) equations. Results of computer simulations for several chemical systems will be shown and compared to experimental observations obtained by optical imaging, spectroscopy, and tomography. The latter diagnostic tools will also be briefly discussed.
The transformation of a base-catalyzed, mechano-assisted Knoevenagel condensation of mono-fluorinated benzaldehyde derivatives (p-, m-, o-benzaldehyde) with malonodinitrile was investigated in situ and in real time. Upon milling, the para-substituted product was found to crystallize initially into two different polymorphic forms, depending on the quantity of catalyst used. For low catalyst concentrations, a mechanically metastable phase (monoclinic) was initially formed, converting to the mechanically stable phase (triclinic) upon further grinding. Instead, higher catalyst concentrations crystallize directly as the triclinic product. Inclusion of catalyst in the final product, as evidenced by mass spectrometric analysis, suggests this complex polymorphic pathway may be due to seeding effects. Multivariate analysis for the in situ Raman spectra supports this complex formation pathway, and offers a new approach to monitoring multi-phase reactions during ball milling.
In this study, an Impulse Response Function analysis of pile response to sine-sweep excitation by a low cost, portable Shaker was used to identify defects in piles. In straightforward impact-echo methods, echoes from the pile toe and defects are visible in the time domain measurements. However, these echoes are not present in the time domain records of piles subjected to sine-sweep excitations, due to interactions between the input and output signals. For this reason, the impulse response function in the time domain has been calculated and is able to identify the echoes from pile impedance changes. The proposed methodology has been evaluated both numerically and experimentally. A one-dimensional pile-soil interaction system was developed, and a finite difference method used to calculate the pile response to sine-sweep excitation. The numerical simulations indicate that impulse response measurements with a synthesized logarithmic, sine-sweep excitation could be an effective tool for detecting defects in piles. The methodology was further tested with field trials on 6 cast in situ concrete test piles including 1 intact pile and 5 defective piles subjected to sine-sweep excitations by a shaker. In 5 of the 6 cases the echoes from the pile toe could be identified in the deconvoluted waveforms—the impulse Response functions. Damage detection is more difficult and dependent on the selection of the optimal regularization parameter. Further research and optimization of the deconvolution process is needed to evaluate the effectiveness compared to standard pile integrity testing methods.
The 44th Meeting of the Versailles Project on Advanced Materials and Standards (VAMAS) Steering Committee has just taken place at NIST in Boulder (CO, USA). BAM participates with significant contributions in Technical Working Areas on nanoparticle and surface chemistry characterization, but also has positioned itself to new global material challenges and trends in the developement of advanced materials and their characterization, such as thermal properties, self-healing materials, and micro- and nanoplastic.
The subject of damage localization is an important issue for Structural Health Monitoring (SHM) particularly in mechanical or civil structures under ambient excitation. In this paper, the statistical subspacebased damage localization method has been applied on a benchmark application, namely a 1/200 scale model of the Saint-Nazaire Bridge, which is a cable-stayed bridge located on the Loire River near the river’s mouth. The employed damage localization method combines data-driven features with physical parameter information from a finite element model in statistical tests, avoiding typical ill-conditioning problems of FE model updating. Damage is introduced in the mockup for cable failures on some of the 72 cables. The purpose of the experiment is to assess the capability of damage assessment methods to find a cable failure.
The Stochastic Dynamic Damage Locating Vector (SDDLV) approach is a vibration-based damage localization method based on both a finite element model of a structure and modal parameters estimated
from output-only measurements in the damage and reference states. A statistical version of the Approach takes into account the inherent uncertainty due to noisy measurement data. In this paper, the effect of temperature fluctuations on the performance of the method is analyzed in a model-based approach using a finite element model with temperature dependent parameters. Robust damage localization is carried out by rejecting the temperature influence on the identified modal parameters in the damaged state. The algorithm is illustrated on a simulated structure.
Within the presented research project, experimental and numerical investigations were performed to develop a thin-shelled, modular, mobile element system made of a micro-reinforced ultra-high-performance ductile concrete (DUCON®). Material parameters were experimentally determined to adapt the material model within the numerical analysis applying the Drucker-Prager relationship. Afterwards, for validation of the numerical models, quasi-static and high-velocity impact tests were performed on plate-like structures. Finally, a suitable geometry of transportable barrier elements will be designed, which provides a maximum of resistance against impact by a minimum of weight and a maximum of mobility.
The antibacterial features of natural pine/spruce rosin are well established, yet the functionality in various thermoplastics has not been surveyed. This work focuses on the processing of industrial grade purified rosin mixed with polyethylene (PE), polypropylene (PP), polylactic acid (PLA), polyamide (PA) and corn starch based biopolymer (CS). Homopolymer masterbatches were extrusion-compounded and melt-spun to form fibres for a wide range of products, such as filters, reinforcements, clothing and medical textiles. Due to the versatile chemical structure of rosin, it was observed compatible with all the selected polymers. In general, the rosin-blended systems were shear-thinning in a molten condition. The doped fibres spun of PE and PP indicated adequate melt-spinning capability and proper mechanical properties in terms of ultimate strength and Young's modulus. The antibacterial response was found dependent on the selected polymer. Especially PE with a 10 wt% rosin content showed significant antibacterial effects against Escherichia coli DH5α and Staphylococcus aureus ATCC 12598 when analysed in the Ringer's solution for 24 h.
Solidification cracking of metals is a well-researched topic in the field of welding science. A material’s susceptibility to solidification cracking can be tested using numerous different specialized test procedures, one of which is the Modified Varestraint-/Transvarestraint test (MVT). It was developed at BAM in 1982 and is internationally standardised. Over the decades, this test has been extensively used to characterise the solidification cracking resistance of many different materials.
The present study was conducted to further investigate the influences of the standardised MVT testing parameters, as well as the characteristics of evaluation methods on the results. Several different high alloyed martensitic LTT (low transformation temperature) filler materials, CrNi and CrMn type, were used. In previous pilot studies, these alloys have shown a rather distinctive solidification cracking behaviour (Fig. 1). During testing, energy input per unit length and bending speed were varied (especially the latter is usually kept at standard values), in addition to the most commonly altered factor - total deformation.
First, the effects of different process parameter sets on the solidification cracking response were measured using the standard approach - microscopic analysis of the specimen surface. It was found that not all parameter changes had the expected outcome. For the Cr8Ni6 and Cr11Mn5 filler materials, influences of energy input per unit length and welding speed were in direct opposition.
In order to investigate those apparent contradictions, µCT scans of MVT specimens were made. The results consistently show sub surface cracking, to significant, yet varying extents. Different primary solidification types were found using WDX-analysis, an aspect that is believed to be the main difference between the CrNi- and CrMn-type materials and their cracking characteristics.
Results show that when it comes to testing of modern high-performance alloys, one set of standard MVT testing parameters might not be equally suitable for all materials. Also, to properly accommodate different solidification types, sub-surface cracking has to be taken into account.
Feuchte, insbesondere in Form von Flüssigwasser, stellt in Baustoffen ein hohes Schadenspotential dar. Um mit zerstörungsfreier Prüfung mögliche Risikostellen zu lokalisieren und Präventionsmaßnahmen zu ergreifen, sind Kenntnisse über das Porengefüge und Feuchtetransportmechanismen im Baustoff erforderlich. Eine wesentliche Problematik besteht derzeit in der Erfassung und Quantifizierung von Feuchteverteilungen bei Teilsättigung.
Wir verfolgen derzeit einen Ansatz, mittels Nuklear Magnetischer Resonanz (NMR) in Korrelation mit relativen Luftfeuchtmessungen den Flüssigwasseranteil bei Teilsättigung zu ermitteln. Mit Protonen-NMR lassen sich Relaxationszeiten von Wasserstoffprotonen in Abhängigkeit von ihrer Bindungsart und ihrer Umgebung - z. B. Porenstruktur und -größe - erfassen. Allerdings lässt sich bei Materialien mit sehr breiten Porengrößenverteilungen nicht klar differenzieren, ob kurze Relaxationszeiten durch größere teilgesättigte oder kleinere vollgesättigte Poren verursacht werden. Für die Korrelation mit der relativen Luftfeuchte im Baustoff erfolgt zunächst eine künstliche Regulierung im Klimaschrank. Durch einen neuentwickelten Ansatz von Hillerborg lassen sich dann bei jeder Luftfeuchte die adsorbierten Wasserschichtdicken und der Porensättigungsgrad für die vorhandenen Porengrößen berechnen. Mithilfe des berechneten Porensättigungsgrades lässt sich eine genauere Analyse der zeitlichen Entwicklung von Relaxationszeitenverteilungen (insbesondere bei Trocknungs- und Aufsättigungsprozessen) vornehmen. Somit sollen erstmals Aussagen zu kürzeren Relaxationszeiten bei teilgesättigten Porensystemen, die beispielsweise auch eine multimodale Porengrößenverteilung aufweisen, getroffen werden können.
In dieser Arbeit wird die Kombination aus NMR und der relativen Luftfeuchte an sehr porösen Dämmplatten aus Kalziumsilikat, die zur Wärmedämmung sowie der Entgegenwirkung von Schimmelbildung eingesetzt werden, angewendet. Untersucht werden 28 Proben à 6 Gruppen, die von unterschiedlichen Herstellern stammen bzw. unterschiedlich hergestellt wurden.
We demonstrate the use of a 3D printed radial collimator in X-ray powder diffraction and surface sensitive grazing incidence X-ray diffraction. We find a significant improvement in the overall Signal to background ratio of up to 100 and a suppression of more than a factor 3⋅10⁵ for undesirable Bragg reflections generated by the X-ray “transparent” windows of the sample environment.
The background reduction and the removal of the high intensity signals from the windows, which limit the detector’s dynamic range, enable significantly higher sensitivity in experiments within sample environments such as vacuum chambers and gas- or liquid-cells. Details of the additively manufactured steel collimator geometry, alignment strategies using X-ray fluorescence, and data analysis are also briefly discussed. The flexibility and affordability of 3D prints enable designs optimized for specific detectors and sample environments, without compromising the degrees of freedom of the diffractometer.
Der steigende Einsatz von Holz-Kunststoff-Verbundwerkstoffen (Wood Plastic Composite, WPC) erfordert das Wissen um seine spezifischen Eigenschaften, insbesondere dem Brand risiko.
Dabei können Flammschutzmittel die Entflammbarkeit, Wärmeabgabe und die Brandausbreitung des Materials verringern.
Deshalb sind der gezielte und effiziente Einsatz und die Kenntnis über die Wirkungsweise der Flammschutzmittel im WPC für den Brandschutz von enormer Bedeutung. Dazu gehört auch die Rauchentwicklung im Brandfall. Rauch beeinflusst aufgrund seiner Toxizität und seiner Sichttrübung die Fluchtmöglichkeit der betroffenen Personen. In der Rauchkammer nach ISO 5659-2 wird die Rauchentwicklung von flachen Werkstoffproben ermittelt. Die Rauchgastoxizität bzw. die Rauchgaszusammensetzung wird mithilfe der FTIR (Fourier Transformierte Infrarot)-Spektroskopie ermittelt. Frei werdende Partikel schädigen die Atemorgane und beeinflussen damit auch die Fluchtfähigkeit von Personen im Brandfall. Aussagen zur Partikelemission können mithilfe eines an die Rauchkammer gekoppelten Partikelanalysators getroffen werden. Im Rahmen dieser Arbeit wurden verschiedene flammgeschützte WPC-Systeme hinsichtlich ihres Rauchverhaltens in der Rauchkammer untersucht. Die Ergebnisse zu emittierten toxischen Gasen, Partikeln und zur Rauchentwicklung werden vorgestellt und in Abhängigkeit von den eingesetzten Flammschutzmitteln im WPC diskutiert.
Leitungswasserschäden nahmen im Jahr 2016 mit rund 2,6 Milliarden Euro den größten Posten bei Gebäudeversicherungen ein. Die Bestimmung und Lokalisierung des Schadensausmaßes ist dabei ein erster wichtiger Schritt, um die erforderlichen Sanierungsarbeiten abschätzen und effizient vornehmen zu können. Hierfür sind Radar und Neutronensonden bereits etablierte Verfahren. Für verlässliche Aussagen zum quantitativen Feuchtegehalt eines Baustoffes werden jedoch zerstörende Sondierungsbohrungen zur Kalibrierung der aufgenommenen Daten benötigt. Dieser hohe zeitliche und finanzielle Aufwand soll zukünftig durch den parallelen Einsatz der genannten Messverfahren verhindert werden. In der durchgeführten Studie wurden Estrichprobekörper auf Zement- und Anhydritbasis mit variablen Dicken und Festigkeiten hergestellt und deren Austrocknung mit Radar und Neutronensonde über einen Zeitraum von 90 Tagen beobachtet. Als Referenzverfahren zur Ermittlung des Feuchteverlaufs dienten die gravimetrische Darr- und chemische Calcium-Carbid-Methode, welche an kleineren Schwesterproben der gleichen Charge angewendet wurden. Kontinuierliche Wägungen der größeren Probekörper gaben hierbei Aufschluss über den durch Austrocknung schwindende Wasseranteil. Aus dem aufgenommen Radardatensatz konnten anschließend markante Signalmerkmale im Zeit- und Frequenzbereich extrahiert und deren Zusammenhang zum Feuchtegehalt der Estrichtypen untersucht werden. Hierbei wurden gängige Methoden aus der Literatur zur Feuchtemessung mit Radar angewandt, wobei die Kombination dieser und das Hinzuziehen der Neutronensonde mittels Datenfusion zu einem höheren Informationsgehalt beiträgt. Somit kann eine zerstörungsfreie Quantifizierung des Feuchteschadens an schwimmenden Fußbodenaufbauten vorgenommen werden
Flame retardants (FR) are inevitable additives to many plastics. Halogenated organics are effective FRs but are controversially discussed due to the release of toxic gases during a fire or their persistence if landfilled. Phosphorus-containing compounds are effective alternatives to halogenated FRs and have potential lower toxicity and degradability. In addition, nitrogencontaining additives were reported to induce synergistic effects with phosphorus-based FRs. However, no systematic study of the gradual variation on a single phosphorus FR containing both P−O and P−N moieties and their comparison to the respective blends of phosphates and phosphoramides was reported. This study developed general design principles for P−O- and P−N-based FRs and will help to design effective FRs for various polymers. We synthesized a library of phosphorus FRs that only differ in their P-binding pattern from each other and studied their decomposition mechanism in epoxy resins. Systematic control over the decomposition pathways of phosphate (PO(OR)3), phosphoramidate (PO(OR)2(NHR)), phosphorodiamidate (PO(OR)(NHR)2), phosphoramide (PO(NHR)3), and their blends was identified, for example, by reducing cis-elimination and the formation of P−N-rich char with increasing nitrogen content in the P-binding sphere. Our FR epoxy resins can compete with commercial FRs in most cases, but we proved that the blending of esters and amides outperformed the single molecule amidates/diamidates due to distinctively different decomposition mechanisms acting synergistically when blended.
Die Identifizierung von Transformationsprodukten (TPs) von Tierarzneimittelwirkstoffen ist wichtig für Gesundheit, Lebensmittel und Umwelt. Monensin (MON) gehört zu den Ionophoren Antibiotika und wird genutzt zum Schutz und zur Behandlung von Kokzidiose bei Geflügel, vorwiegend prophylaktisch in der Geflügelmast. Rückstände können in tierischen Produkten (Geflügel und Eier) aber auch in der Umwelt (Tiermist, Gewässer, Böden) gefunden werden. Verschiedene Transformationsprozesse können auftreten, beginnend bei der Biotransformation in lebenden Organismen bis hin zu biotischen und abiotischen Prozessen in der Umwelt.
Die Kopplung von Elektrochemie und Massenspektrometrie, kurz EC/HRMS, als rein instrumenteller Ansatz zur Simulation von Transformationsprodukten ist seit vielen Jahren in der pharmazeutischen Forschung etabliert. Hierbei wird mithilfe einer elektrochemischen Durchflusszelle der oxidative Metabolismus einer Substanz simuliert und zugleich analysiert. Unter Verwendung von EC/HRMS und LC-HRMS wurde MON elektrochemisch bei Potentialen bis zu 2.5 V vs Pd/H2 oxidiert und die entstehenden TPs mit Metabolismustests mit Rattenlebermikrosomen verglichen. Als Ergebnis wurden verschiedene TPs von MON gefunden und Strukturvorschläge wurden erstellt. Ein Überblick über die detektierten und identifizierten TPs wird dargestellt.
Gegenüber dem Neubauentwurf können bei der Bewertung von bestehender Bausubstanz Sicherheitsreserven genutzt werden, da Unsicherheiten, die beim Bau auftreten können, besser bekannt oder nicht mehr vorhanden sind. Können solche Unsicherheiten genauer bewertet werden, z. B. durch die Feststellung der genauen Lage der Spannglieder bei einer Spannbetonbrücke, so können Sicherheitsbeiwerte reduziert werden, ohne dass es dabei zu Auswirkungen auf das normativ festgelegte Zuverlässigkeitsniveau kommt. Mittlerweile sind Prüfmethoden an Bauwerken wirtschaftlich einsetzbar und auch so leistungsfähig, dass die für die Tragfähigkeit und Gebrauchstauglichkeit wesentlichen Parameter identifiziert werden können. Ein wesentlicher Punkt ist hierbei die Integration derartiger Messergebnisse in Rechenmodelle, die für die Nachrechnung des Bauwerks verwendet werden. Dies können sowohl semiprobabilistische Rechenmodelle als auch vollprobabilistische Modelle sein. Bei semiprobabilistischen Methoden können aus den Messergebnissen Teilsicherheitsbeiwerte berechnet und abgeleitet werden, die dann in den bekannten Nachweisformaten gemäß den Eurocodes und der Nachrechnungsrichtlinie berücksichtigt werden. Bei vollprobabilistischen Nachweisen können die Messdaten in Form von Verteilungsdichtefunktionen mit gemessenen Variationskoeffizienten direkt in das Rechenmodell eingehen. In einer dreiteiligen Aufsatzreihe werden die Messverfahren und die Nutzung der Ergebnisse bei der Nachrechnung vorgestellt. Der vorliegende Teil 1 zeigt die Möglichkeiten des Einsatzes von zerstörungsfreien Prüfverfahren und bewertet deren Leistungsfähigkeit. Messen heißt wissen. Dieses Wissen spiegelt die Realität wider und soll den Tragwerksplaner bei der Entscheidungsfindung über die Sicherheit und Zuverlässigkeit von Bestandsbauwerken unterstützen.
Leitungswasserschäden nahmen im Jahr 2016 mit rund 2,6 Milliarden Euro den größten Posten bei Gebäudeversicherungen ein. Die Bestimmung und Lokalisierung des Schadensausmaßes ist dabei ein erster wichtiger Schritt, um die erforderlichen Sanierungsarbeiten abschätzen und effizient vornehmen zu können. Hierfür sind Radar und Neutronensonden bereits etablierte Verfahren. Für verlässliche Aussagen zum quantitativen Feuchtegehalt eines Baustoffes werden jedoch zerstörende Sondierungsbohrungen zur Kalibrierung der aufgenommenen Daten benötigt. Dieser hohe zeitliche und finanzielle Aufwand soll zukünftig durch den parallelen Einsatz der genannten Messverfahren verhindert werden.
In der durchgeführten Studie wurden Estrichprobekörper auf Zement- und Anhydritbasis mit variablen Dicken und Festigkeiten hergestellt und deren Austrocknung mit Radar und Neutronensonde über einen Zeitraum von 90 Tagen beobachtet. Als Referenzverfahren zur Ermittlung des Feuchteverlaufs dienten die gravimetrische Darr- und chemische Calcium-Carbid-Methode, welche an kleineren Schwesterproben der gleichen Charge angewendet wurden. Kontinuierliche Wägungen der größeren Probekörper gaben hierbei Aufschluss über den durch Austrocknung schwindende Wasseranteil.
Aus dem aufgenommen Radardatensatz konnten anschließend markante Signalmerkmale im Zeit- und Frequenzbereich extrahiert und deren Zusammenhang zum Feuchtegehalt der Estrichtypen untersucht werden. Hierbei wurden gängige Methoden aus der Literatur zur Feuchtemessung mit Radar angewandt, wobei die Kombination dieser und das Hinzuziehen der Neutronensonde mittels Datenfusion zu einem höheren Informationsgehalt beiträgt. Somit kann eine zerstörungsfreie Quantifizierung des Feuchteschadens an schwimmenden Fußbodenaufbauten vorgenommen werden
In this paper, we introduce a nano aerial robot swarm for Indoor Air Quality (IAQ) monitoring applications such as occupational health and safety of (industrial) workplaces. The robotic swarm is composed of nano Unmanned Aerial Vehicles (UAVs), based on the Crazyflie 2.0 quadrocopter, and small lightweight Metal Oxide (MOX) gas sensors for measuring the Total Volatile Organic Compound (TVOC), which is a measure for IAQ. An indoor localization and positioning system is used to estimate the absolute 3D position of the swarm similar to GPS. A test scenario was built up to validate and optimize the swarm for the intended applications. Besides calibration of the IAQ sensors, we performed experiments to investigate the influence of the rotor downwash on the gas measurements at different altitudes and compared them with stationary measurements. Moreover, we did a first evaluation of the gas distribution mapping performance. Based on this novel IAQ monitoring concept, new algorithms in the field of Mobile Robot Olfaction (MRO) are planned to be developed exploiting the abilities of an aerial robotic swarm.
In this paper, we introduce a nano aerial robot swarm for Indoor Air Quality (IAQ) monitoring applications such as occupational health and safety of (industrial) workplaces. The robotic swarm is composed of nano Unmanned Aerial Vehicles (UAVs), based on the Crazyflie 2.0 quadrocopter, and small lightweight Metal Oxide (MOX) gas sensors for measuring the Total Volatile Organic Compound (TVOC), which is a measure for IAQ. An indoor localization and positioning system is used to estimate the absolute 3D position of the swarm similar to GPS. A test scenario was built up to validate and optimize the swarm for the intended applications. Besides calibration of the IAQ sensors, we performed experiments to investigate the influence of the rotor downwash on the gas measurements at different altitudes and compared them with stationary measurements. Moreover, we did a first evaluation of the gas distribution mapping performance. Based on this novel IAQ monitoring concept, new algorithms in the field of Mobile Robot Olfaction (MRO) are planned to be developed exploiting the abilities of an aerial robotic swarm.
Als Ausgangspunkt für i-TRIBOMAT schließen vier renommierte Institutionen in Europa, darunter die BAM, ihre Test- und Analytik-Methoden zusammen. Es entsteht ein Testfeld aus weit über 100 Tribometern mit den entsprechenden, analytischen Kapazitäten. Alle Ergebnisse fließen in eine harmonisierte Datenbank, die tribologische Erkenntnisse mit Materialeigenschaften ebenso zugänglich macht, wie Hinweise auf ökologische und gesundheitliche Verträglichkeiten. Diese Datenbank bildet zusätzlich das Rückgrat einer Vielzahl von Modellierungsmethoden, die die Entwicklungszeiten von der Idee bis zum marktreifen Produkt deutlich verkürzen sollen. Alle diese Möglichkeiten sollen über eine europaweit agierende, zentrale Kontaktstelle zur Verfügung gestellt werden.
Compatibility of polymeric materials with heating oil/biodiesel blends at different temperatures
(2019)
Materials compatibility is a major concern whenever the fuel composition is changed. The question arises of whether polymeric materials are resistant to heating oil with admixtures of 10 % biodiesel (B10) and 20 % biodiesel (B20).
The polarity of biodiesel increases its solvency and facilitates permeation and extrac-tion. Solvation, swelling and/or extraction lead to changes in the physical properties and chemical changes of polymeric materials.
The objective of this research was to determine the resistance of frequently used sealing materials such as FKM, EPDM, CR, CSM, NBR, IIR, VMQ, FVMQ, PA and PUR in up to four-year aged B10 for 84 days at 20 °C, 40 °C and 70 °C.
The polymeric materials: ACM, FKM, HNBR, PA, PE; POM, PUR and PVC were ex-posed to B20 for 84 days at 40°C and 70°C in another research project.
Mass, tensile strength, breaking elongation and Shore hardness A (D) of the test specimens were determined before and after the exposure for 84 (42) days in the heating oil blends B10 and B20.
There is not determined a threshold for the reduction in tensile properties and Shore hardness in the international standards. Therefore, a threshold of 15 % was deter-mined for the evaluation of the compatibility.
Measurements of the variations in mass, tensile properties and Shore hardness after exposure of the polymers in non-aged and aged heating oil B10 showed clearly that FKM, FVMQ and PA were the most resistant materials in B10. The elastomers CR, CSM, EPDM, IIR, NBR and VMQ were generally not resistant to B10. Damage to the materials increased with higher test temperatures and the age of B10.
FKM, POM and PVC showed high compatibility in B20 at 40°C and 70 °C. ACM, HNBR and PA were evaluated as resistant in B20 at 40 °C but not at 70°C.
Small-scale variations in mineral chemistry, textures, and platinum group element (PGE) mineralization were investigated in the Lower and Middle Group chromitite layers LG6, LG6a, MG1, MG2, and MG2 II from vertical drill core profiles at the Thaba mine in the northwestern limb of the Bushveld Complex. We present detailed geochemical profiles of chromite composition and chromite crystal size distribution curves to shed light on the processes of chromite accumulation and textural modification as well as mineralization. Multiple samples within each layer were assayed for PGE concentrations, and the respective platinum group mineral association was determined by mineral liberation analysis (MLA).
There is strong evidence for postcumulus changes in the chromitites. The crystal size distribution curves suggest that the primary chromite texture was coarsened by a combination of adcumulus growth and textural equilibration, while compaction of the crystal mush played only a minor role. Mineral compositions were also modified by postcumulus processes, but because of the very high modal amount of chromite and its local preservation in orthopyroxene oikocrysts, that phase retained much primary information. Vertical variations of chromite composition within chromitite layers and from one layer to another do not support the idea of chromite accumulation from crystal-rich slurries or crystal settling from a large magma chamber. Instead, we favor a successive buildup of chromitite layers by repeated injections of relatively thin layers of chromite-saturated magmas, with in situ crystallization occurring at the crystal mush-magma interface. The adcumulus growth of chromite grains to form massive chromitite required addition of Cr to the layers, which we attribute to downward percolation from the overlying magma.
The PGE concentrations are elevated in all chromitite layers compared to adjacent silicate rocks and show a systematic increase upward from LG6 (avg 807 ppb Ir + Ru + Rh + Pt + Pd + Au) to MG2 II (avg 2,062 ppb).
There are also significant internal variations in all layers, with enrichments at hanging and/or footwalls. The enriched nature of chromitites in PGEs compared to host pyroxenites is a General feature, independent of the layer thickness. The MLA results distinguish two principal groups of PGE mineral associations: the LG6, LG6, and MG1 are dominated by the malanite series, laurite, and PGE sulfarsenides, while the MG2 and MG2 II layers are characterized by laurite and PGE sulfides as well as Pt-Fe-Sn and PGE-Sb-Bi-Pb alloys. Differences in the PGE associations are attributed to postcumulus alteration of the MG2 and MG2 II layer, while the chromitites below, particularly LG6 and LG6a, contain a more pristine association.
Ultraschallmessverfahren werden seit Langem erfolgreich für Prüfaufgaben im Bauwesen eingesetzt. Die dauerhafte Überwachung und frühzeitige Erkennung von Schäden an komplexen Neubauten und alternder Infrastruktur kann mittels Ultraschall-Transmissionsmessungen und speziellen Auswertemethoden, wie z. B. Korrelationverfahren und Codawelleninterferometrie, realisiert werden. Für die Dauerüberwachung wurde ein kompaktes System entwickelt, das Ultraschall-Messdaten erfassen und ins Internet auf einen FTP-Server übertragen kann. Es können hierbei alle angeschlossenen Prüfköpfe für jede Messung wahlweise als Sender oder Empfänger geschaltet werden. Es wurden Vorverstärker entwickelt, bei denen die Versorgung mit Strom über die Messleitung erfolgt. Dadurch können die Verstärker nahe am Prüfkopf positioniert werden. Durch Änderungen in den Ultraschall-Signalen können Schädigungen des Bauteils, wie z.B. Risse, in Echtzeit erkannt werden.
To exploit application fields beyond packaging for biodegradable materials, flame retardancy and increased mechanical strength are usually required. This work focuses on the flammability of a thermoplastic starch/polyester blend reinforced with natural fibers derived from Mexican industry processes wastes, such as keratin fibers from the tannery industry, coconut fibers (coconut industry), and agave tequilana fibers and henequen fibers from tequila industry. Different fiber contents as well as combinations of varying contents of aluminum trihydroxide, expandable graphite, aluminum diethylphosphinate or ammonium polyphosphate are investigated. It is the goal to propose sustainable waste fibers as adjuvants improving the flame retardancy. This work provides the proof of principle for sustainable biodegradable flame retarded biocomposites.
In recent years superglassy polymers exhibiting intrinsic microporosity established a new perspective for a number of applications, especially for gas separation membranes as These polymers Combine extremely high permeabilities with attractive selectivities. The essential factor governing the structure Formation in the solid film or layer is either a contorted rigid Backbone (polymers of intrinsic microporosity - PIMs) or extremely bulky side groups (polynorbornenes and polytricyclonenenes).
For a deeper understanding of both types of such high-Performance polymers for gas separation membranes and their further development broadband dielectric spectroscopy (BDS) can provide a substantial contribution.
BDS addresses molecular relaxations characterizing the dynamics of the solid polymer as a major factor determining the gas transport properties but also the physical aging behavior which is an essential issue for such polymers.
BDS is applied on PIMs where fluctuations of molecular dipoles connected to the backbone can be directly monitored. Furthermore, also polynorbornenes were investigated which carry no dipole moment in their repeat unit - the high resolution of modern equipment allows for the detailed analysis also for very small dielectric losses originating from partially oxidized moieties or marginal catalyst residues.
Additionally, from interfacial polarization phenomena, such as Maxwell-Wagner-Sillars (MWS) polarization due to blocking of charge carriers at internal interfacial boundaries on a mesoscopic length scale, valuable information on the intrinsic microporosity and its changes induced by physical aging can be obtained.
Finally, also conductivity can be characterized in detail in such polymeric systems revealing contributions of interactions of aromatic moieties (π-π-stacking) or the drift motion of charge carriers. These features also determine the structure formation in the solid state.
Some critical discussion of the state of the art of uncertainty evaluationin Instrumented Indentation Testing IIT
Nowadays the Instrumented Indentation Testing (IIT), in the nano range often named as nano indention, is one of the most commonly used methods to determine the mechanical properties of materials in the micro and nano range. This method is already extensive standardized in ISO 14577 part 1-4. In the past, the application of this standard in testing praxis shows that the established values have an excellent precision.If an uncertainty is calculated, the range of values within which the true value is asserted to lie with some level of confidencewill be known. In part 1 of ISO 14577 [1] two methods for evaluation of the uncertainty in IIT are mentioned:
Method 1 for determining uncertainty considers only those uncertainties associated with the overall measurement performance of the testing machine with respect to the reference blocks.
Method 2calculates a combined uncertainty from individual contributions. These may be grouped into random and systematic uncertainties.
Both methods will be described in detail using examples from the dailyexperimental praxis. The comparabilityof both methods will be critically discussed. Finally, it will be showedhow the calculated uncertaintiescan be used for performancetests and product specifications.
Acknowledgement
This work was performed under the support of the EMPIR project 17NRM05Advancing measurement uncertainty̶ comprehensiveexamples for key international standards
References
[1] ISO 14577 part 1 (2017)
The lecture traces the origins of paper, the manufacture and the spread from China to the Middle East and Europe.
Though technological progress considerably affected each step of the manufacture of paper, the essence of the invention remains unchanged until today. The process of manufacturing handmade paper can be divided into a number of steps:
- choosing the raw material (e.g. cellulose from wood, cotton, rags)
- beating and grinding the fibres into small pieces
- producing a liquid pulp of the desired texture
- treating the pulp with various additives
- filling the pulp suspension into a paper mould
- draining the water
- pressing and drying to get the actual sheet
- various post-production treatments
We will see how the manufacturing process is reflected in the properties of the paper and its degradation. A special attention will be paid to the instrumental analysis for identification of the paper types. Also watermark play an important role in the studies of the manuscripts. A short overview will be offered at the ends of the lecture.
Inks and pigments
(2019)
The writing materials used in various cultures and epochs can be divided into two groups. The first comprises materials that write themselves, producing script by rubbing their own material off onto the writing surface. It includes charcoal, graphite, chalk, raddle, and metal styluses. Depending on the material and consistency, these are cut or pressed to make styluses and then used for writing.
The second group comprises all coloring liquids that are applied to the writing surface with a quill, pen, or printing block. It includes inks made from dye solutions (for example, tannin inks) and those made from pigment dispersions (for example, sepia, soot, and bister inks). The latter are sometimes also rubbed as pastes into letters incised into the writing surface, where they increase visual contrast.
Due to the variety of recipes and the natural origin of raw materials, there is a wide range of different components and impurities in writing materials.
Soluble inks (Tinten)
Soluble inks are based mainly on dyes forming a water solution. Colored inks were manufactured with different plant or insect dyes (e.g. Brazil wood, kermes). To stabilize the volatile material, the dyes were mixed with a mordant (e.g., alum).
Brown plant inks – best-known as blackthorn or Theophilus’ inks – are usually produced from the blackthorn bark and wine. In the early European Middle Ages, inks of this kind were widely used in the production of manuscripts in monasteries. Usually, they are light brown, so sometimes small amounts of iron sulfate were added, which led to what was called an “imperfect” iron gall ink. The difference between “classic” iron gall ink and such imperfect ink is therefore not clear: the distinction is not possible, especially with the naked eye.
Dispersion inks (Tuschen)
According to its generic recipe, one of the oldest black writing materials is produced by mixing soot with a binder dissolved in a small amount of water. Thus, along with soot, binders such as gum arabic (ancient Egypt) or animal glue (China) are among the main components of soot inks. From Pliny’s detailed account of the manufacture of various soot-based inks, we learn that, despite its seeming simplicity, producing pure soot of high quality was not an easy task in Antiquity. Therefore, we expect to find various detectable additives that might be indicative of the time and place of production. One such carbon ink requires the addition of copper sulfate . The experimental discovery of this ink in 1990 led to a misleading expression “metal ink” that is sometimes found in the literature.
Colored dispersion inks based on pigments such as orpiment, cinnabar, or azurite have been known since Antiquity. Natural or artificially produced minerals are finely ground and dispersed in a binding medium. As in soot inks, water-soluble binders such as gum arabic or egg white were used.
Iron gall ink (Eisengallustinten)
Iron gall inks are a borderline case between these two groups. They are produced from four basic ingredients: galls, vitriol as the main source of iron, gum arabic as a binding media, and an aqueous medium such as wine, beer, or vinegar. By mixing gallic acid with iron sulfate, a water-soluble ferrous gallate complex is formed; this product belongs to the type “soluble inks”. Due to its solubility, the ink penetrates the writing support’s surface, making it difficult to erase. Exposure to oxygen leads to the formation of insoluble black ferric gallate pigment, i.e., “dispersion ink”.
Natural vitriol consists of a varying mixture of metal sulfates. Since for ink making it was obtained from different mines and by various techniques, inks contain many other metals, like copper, aluminum, zinc, and manganese, in addition to the iron sulfate. These metals do not contribute to color formation in the ink solution, but possibly change the chemical properties of the inks.
Parchment
(2019)
This lecture will present history of parchment based on written sources and chemical examination of antique, medieval and modern parchment.
Our studies of the Dead Sea Scrolls writing surfaces show that they can be divided roughly into three groups: leather, parchments of a light tint, and those of various shades of brown. The latter ones are invariably tanned, whereas the middle group is characterized by the presence of various inorganic salts. Some of the pale parchments, among them the Temple Scroll (11Q19), are remarkably similar to medieval European parchment. Therefore we have formulated the working theory that in the Judaea of the Hellenistic period two different parchment-making traditions existed side by side: an ‘eastern’ one (represented by the tanned parchments of Qumran, closely resembling Aramaic documents from the fifth century BC, and a ‘western’ one (represented by the untanned/lightly tanned ones similar to early Christian Greek parchments).
This division has found support during our studies of the Geniza fragments, in which Babylonian and Palestinian traditions seem to follow the “eastern” and “western” technologies, respectively.
Natural sciences play auxiliary role in the studies of manuscripts. The success of their contribution depends strongly on the formulation of the question and the choice of the methods to obtain the requested answer. Therefore, one should try to go beyond the understanding of the basic principles of the scientific analysis.
We will start with a glance at the basic principles of the techniques used in the material science for determination of the elemental composition (X-ray emission) and molecular composition (FTIR & Raman). We will move then to the bench and mobile equipment commonly used in the field of cultural heritage. At the end we will choose a question to be answered and design an ideal experiment that will be modified according to the limitations dictated by on-site conditions.
In the ateliers in the afternoon we will
a) compare two XRF devices that differ in their spatial resolution;
b) use a high resolution microscope (Keyence) to obtain a close look at writing surfaces and materials;
c) we will learn to determine the type of the inks with the help of another microscope (DinoLite AD413T-12V), a usb microscope with visible, UV and NIR illumination;
d) we will learn to use FTIR-ATR device for determination of the type of the writing surface;
e) We will use mobile Raman device for identification of pigments.
The evolution and socio-geographic distribution of writing inks from Late Antiquity to the Middle Ages are one of the foci of our investigative work at the Bundesanstalt für Materialforschung und -prüfung (BAM) in Berlin and the Centre for the Study of Manuscript Cultures, Hamburg University.
This presentation will examine the inks used by Jews in the in different geographical zones try to correlate the results of the material analysis with written records and existing traditions. We will compare the inks proposed by Maimonides, who lived in 12th-century Egypt, with the considerations of Rashi, who lived in 11th-century northern France, and see that they both advocated use of the inks commonly known and produced in their respective regions. It is Maimonides who proposes to add tannins to the soot inks, but rejects the metallic salt, both of which were practices that were well attested in contemporary Arabic recipes for making ink. In contrast, Rashi was favourable to employing the plant inks in use in contemporary Northern Europe.
While studying the socio-geographic history of inks, division 4.5 of the Bundesanstalt für Materialforschung und Prüfung (BAM) together with the Centre for the Study of Manuscript Cultures (CSMC) in Hamburg has developed a non-invasive protocol for ink analysis. It consists of a primary reflectographic screening to determine the type of the ink (soot, tannin or iron-gall) and a subsequent in-depth analysis using several spectroscopic techniques: X-ray fluorescence (XRF), Infrared and Raman spectroscopies. The first of them, XRF elemental analysis aims at establishing the unique fingerprints of inks containing metals or trace elements in carbon inks. In addition, we use Raman analysis to identify so-called mixed inks, an ink category that received little attention so far. Finally, with the help of IR spectroscopy we obtain information about the ink binders.
Our research aims primarily at recreating a socio-geographic history of inks, parchment, and papyrus and includes the comparative analysis of the writing materials of the Dead Sea Scrolls, ink and papyrus in Ancient and Hellenistic Egypt, and inks in documents from various contemporary medieval communities in Fustat (first nucleus of Cairo) as well as other medieval Jewish and Armenian communities.
The presentation shows the panorama of historic inks and our attempt to follow up the transition of the inks from those based on soot to the iron-gall inks commonly used in the Middle Age.
Heute stimmen die meisten Gelehrten und Historiker darin überein, dass die Höhlen von Qumran eine Essener-Bibliothek beherberg-ten. Über ihren Ursprung, sowie die Herkunft der einzelnen Schriften, wird noch immer rege debattiert. Der aktuelle Beitrag präsentiert detaillierte Lösungsansätze zu Klärung der Provenienzfrage der Schriftrollen von Qumran.
Our study is dedicated to non-destructive characterization of the support and the inks of the DSS.
To that aim we use micro-XRF, 3D- SY-XRF, different IR methods including synchrotron radiation based reflectance spectroscopy, optical and electron microscopy.
The lecture discusses advantages and the shortcomings of the non-destructive testing approach.
While studying the history of inks, division 4.5 of the BAM (Bundesanstalt für Materialforschung und Prüfung) together with the Centre for the Study of Manuscript Cultures in Hamburg has developed a protocol for ink analysis. It consists of a primary screening to determine the type of the ink, and a subsequent in-depth analysis using several spectroscopic techniques. One of them, X-ray Fluorescence (XRF) aims primarily at establishing the fingerprints of inks containing metals, making it possible to distinguish among different inks.
Our research aims primarily at recreating a socio-geographic history of inks, parchment, and papyrus and includes the comparative analysis of the writing materials of the Dead Sea Scrolls, ink and papyrus in Ancient and Hellenistic Egypt, and inks in documents from various contemporary medieval communities in Fustat (first nucleus of Cairo) as well as other medieval Jewish and Armenian communities.
The presentation shows the panorama of historic inks and our attempt to follow up the transition of the inks from those based on soot to the iron-gall inks commonly used in the Middle Age.
Sunlight, the major source of energy, drives life but in excess it provokes UV-induced DNA damage, accumulation of reactive oxygen species, desiccation, osmotic stresses and so on. Biological strategies to survive excess light include protection, avoidance and active utilisation. Phototrophic organisms including cyanobacteria, green algae and plants use all three strategies. Fungi occupying phototrophic niches may profit from the surplus photosynthetic products which also obliges them to cope with the same light-induced stresses. One way of handling these stresses would be to use similar signalling pathways to sense the presence and to interact with their phototrophic partners. Obviously, the levels of adaptation and responses to light will depend on the environment as well as fungal genotype and phylogenetic position. Black fungi – a polyphyletic group – accumulate the dark pigment DHN melanin in their cell walls and often occupy light-flooded habitats from phyllosphere to rock surfaces. Here we compare two sequenced melanised fungi of different lifestyles in their response to light.
The Leotiomycete Botrytis cinerea is an aggressive pathogen that primarily infects the above-ground parts of plants. It possesses large numbers of photoreceptors that respond to a broad spectrum of light. As a consequence, light controls morphogenesis in which it induces conidiation for disease spreading and represses sclerotial development for survival and/or sexual recombination. Cellular components involved in photo-perception and regulation of morphogenesis, stress responses and virulence have been identified and appear to regulate propagation, survival and infection. These include phytochromes, a group of photoreceptors which are particularly enriched in the Leotiomycetes and that mediate coordinated responses to light and elevated temperatures. Assuming that photo-regulation may be equally important for fungi that live in mutualistic relationships with phototrophs either by forming composite organisms or biofilms, we investigate the role of light in the rock-inhabiting Eurotiomycete Knufia petricola. Like other black yeasts, K. petricola grows slowly, does not form specialised reproductive structures and constitutively produces DHN melanin as well as carotenoids. Combining K. petricola with the cyanobacterium Nostoc punctiforme, we developed a model system for studying biofilm formation and bio-weathering. A genetic toolbox to manipulate this model system is being developed. K. petricola strain A95 possesses ten putative photoreceptors, more than found in filamentous Eurotiomycetes suggesting that light plays an important role for abiotic and biotic interactions in extremo-tolerant and symbiosis-capable fungi.
The rotation of the Earth causes a day/night cycle that is characterized by changing light and temperature conditions. Fungi actively sense the environmental light conditions to induce protective mechanisms against the light-associated stresses and to regulate development. Since fungi adapted to habitats with different light regimes, the complexities of their ‘visual’ systems and photoresponses may vary significantly. Fungi that are associated with plants experience a special light regime because the host seeks optimum light conditions for photosynthesis – and the fungus must cope with them. Moreover, fungi living under the canopy are confronted with an altered spectrum enriched for green and far-red light. Plants sense light to coordinate growth and morphogenesis: a low red:far-red ratio indicates the presence of competitors (shading by other plants) and triggers the shade avoidance response which is accompanied by increased susceptibility to nectrophic pathogens.
Botrytis cinerea, the causal agent of gray mold diseases on many plant species in moderate climate zones (high humidity, temperatures around 20°C, seasons), exhibits striking photoresponses accompanied by a broad action spectrum and a high number of photoreceptors. Light is the most important factor controlling morphogenesis: it induces conidiation for disease spreading (summer cycle) and represses sclerotial development for survival and/or sexual recombination (winter cycle). In the past years, we identified several cellular components involved in photoperception and regulation of photomorphogenesis and virulence indicating that the same signaling pathways are of relevance for both processes, propagation and infection. Notably, we recognized the role of the phytochromes (red/far-red light sensors) for coordinated responses to light and elevated temperatures (photo-/thermomorphogenesis) – similar to the function of Arabidopsis PhyB. BcPHY2-like thermosensors are likely restricted to the Leotiomycetes, which include several plant pathogens of the moderate climate zones.
Chemical effects during the formation of femtosecond laser-induced periodic surface structures
(2019)
The processing of laser-induced periodic surface structures (LIPSS, ripples) on metals and semiconductors in ambient air is usually accompanied by superficial oxidation effects – a fact that is widely neglected in the current literature. In this contribution, chemical, structural, and mechanical alterations in the formation of femtosecond LIPSS are characterized by a variety of surface analytical techniques, including energy dispersive X-ray analyses (EDX), X-ray photoelectron spectroscopy (XPS), micro Raman spectroscopy (µ-RS), and depth-profiling Auger electron microscopy (AEM). Alternative routes of electrochemical and thermal oxidation allow to qualify the relevance of superficial oxidation effects on the tribological performance in oil lubricated reciprocating sliding tribological tests (RSTT). It is revealed that the fs-laser processing of near-wavelength sized LIPSS on metals leads to the formation of a few hundreds of nanometers thick graded oxide layers, consisting mainly of amorphous oxides. Regardless of reduced hardness and limited thickness, this nanostructured surface layer efficiently prevents a direct metal-to-metal contact in the RSTT and may also act as an anchor layer for specific wear-reducing additives contained in the used engine oil.
Composite-Druckgefäße für den Gefahrguttransport sowie für Wasserstoff- und Erdgasfahrzeuge bestehen aus einem lasttragenden Composite und einer gasdichten, metallischen oder polymeren Barriereschicht (Liner). Zur Untersuchung des Alterungsverhaltens solcher Composite-Druckgefäße wurde in der BAM das interdisziplinäre Themenfeldprojekt COD-AGE durchgeführt. Ziel des Projektes war die Entwicklung von Methoden und Modellen zur Beschreibung und Bestimmung des Alterungsverhaltens von Carbonfaser-Compositen am Beispiel von Druckgefäßen, um eine bessere Vorhersage der Alterung und der sicheren Gebrauchsdauer zu ermöglichen. Ein Schwerpunkt in diesem Projekt war die Bereitstellung geeigneter ZfP-Methoden. Dabei ging es sowohl um versuchsbegleitende Prüfungen, als auch um die mögliche Entwicklung von Prüfeinrichtungen für den späteren praktischen Gebrauch.
In dem Vortrag werden Prüfergebnisse der alterungsbegleitenden Wirbelstromprüfung an Composite-Druckgefäßen vorgestellt.
In Alterungsversuchen wurden Druckgefäße aus einem ca. 4 mm dicken Aluminiumliner und ca. 8 mm dicker CFK-Ummantelung untersucht. Typisches Einsatzgebiet solcher Druckgefäße sind Atemschutzgeräte der Feuerwehr. Die Druckgefäße wurden sowohl mit konventioneller Wirbelstromtechnik von außen und von innen als auch mit hochfrequenter Wirbelstromtechnik von außen geprüft. Es konnten sowohl Beschädigungen des metallischen Liners, als auch Strukturen des CFK-Geflechts nachgewiesen werden. Eine besondere mechanische Herausforderung bestand in der Prüfung der Innenseite der Liner, da hier eine zylindrische Fläche mit einem Innendurchmesser von 150 mm durch einen Zugang von nur 15 mm Durchmesser geprüft werden muss.
Composite-Druckgefäße für den Gefahrguttransport sowie für Wasserstoff- und Erdgasfahrzeuge bestehen aus einem lasttragenden Composite und einer gasdichten, metallischen oder polymeren Barriereschicht (Liner). Zur Untersuchung des Alterungsverhaltens solcher Composite-Druckgefäße wurde in der BAM das interdisziplinäre Themenfeldprojekt COD-AGE durchgeführt. Ziel des Projektes war die Entwicklung von Methoden und Modellen zur Beschreibung und Bestimmung des Alterungsverhaltens von Carbonfaser-Compositen am Beispiel von Druckgefäßen, um eine bessere Vorhersage der Alterung und der sicheren Gebrauchsdauer zu ermöglichen. Ein Schwerpunkt in diesem Projekt war die Bereitstellung geeigneter ZfP-Methoden. Dabei ging es sowohl um versuchsbegleitende Prüfungen, als auch um die mögliche Entwicklung von Prüfeinrichtungen für den späteren praktischen Gebrauch.
In dem Vortrag werden Prüfergebnisse der alterungsbegleitenden Wirbelstromprüfung an Composite-Druckgefäßen vorgestellt.
In Alterungsversuchen wurden Druckgefäße aus einem ca. 4 mm dicken Aluminiumliner und ca. 8 mm dicker CFK-Ummantelung untersucht. Typisches Einsatzgebiet solcher Druckgefäße sind Atemschutzgeräte der Feuerwehr. Die Druckgefäße wurden sowohl mit konventioneller Wirbelstromtechnik von außen und von innen als auch mit hochfrequenter Wirbelstromtechnik von außen geprüft. Es konnten sowohl Beschädigungen des metallischen Liners, als auch Strukturen des CFK-Geflechts nachgewiesen werden. Eine besondere mechanische Herausforderung bestand in der Prüfung der Innenseite der Liner, da hier eine zylindrische Fläche mit einem Innendurchmesser von 150 mm durch einen Zugang von nur 15 mm Durchmesser geprüft werden muss.
Dissolved water has major impact on the physical and chemical properties of phosphate glasses. In the present study we have investigated the structural response to water incorporation for glasses in the system Li2O–MgO–Al2O3–P2O5.
Glasses containing 0–8 wt% H2O were synthesised at 500 MPa confining pressure in internally heated gas pressure vessels at 1323 K (LMP, Al-poor glass) and 1423 K (LMAP, Al-enriched glass). Water contents of glasses were determined by pyrolysis and subsequent Karl-Fischer titration (KFT) and/or by infrared spectroscopy. Density varies nonlinearly with water content implying large structural changes when adding up to 2 wt% H2O to the dry glass. Glass Transition temperatures measured by differential thermal analysis (DTA) continuously decrease with water content. The trend can be explained by depolymerisation of the phosphate network. Near-infrared spectroscopy shows that even in Al poor glasses only a minority of dissolved water is present as H2O molecules, but the largest amount is present as OH Groups formed by hydrolysis of P–O–P bonds. The network is stabilised by aluminium which is predominantly six-coordinated in these glasses as shown by 27Al MAS NMR spectroscopy. With increase of Al in the glasses, breaking up of the Phosphate network through hydrolysis is depressed, i.e. much lower OH Contents are formed at same total water content.
Network depolymerisation upon addition of H2O is evident also from 31P MAS NMR spectroscopy. While Phosphate tetraheda are crosslinked by two to three bridging oxygen in dry glasses, diphosphate Groups are dominant in glasses containing 8 wt% H2O.
Computational methods for lifetime prediction of metallic components under high-temperature fatigue
(2019)
The issue of service life prediction of hot metallic components subjected to cyclic loadings is addressed. Two classes of lifetime models are considered, namely, the incremental lifetime rules and the parametric models governed by the fracture mechanics concept. Examples of application to an austenitic cast iron are presented. In addition, computational techniques to accelerate the time integration of the incremental models throughout the fatigue loading history are discussed. They efficiently solve problems where a stabilized response of a component is not observed, for example due to the plastic strain which is no longer completely reversed and accumulates throughout the fatigue history. The performance of such an accelerated Integration technique is demonstrated for a finite element simulation of a viscoplastic solid under repeating loading–unloading cycles.
Entwicklung eines luftgekoppelten Ultraschall-Echo-Prüfverfahrens mittels fluidischer Anregung
(2019)
In vielen technischen Bereichen werden Ultraschallverfahren zur zer-störungsfreien Werkstoffprüfung eingesetzt. Dabei wird ein Schallpuls von einem Prüfkopf in ein Prüfobjekt eingebracht. Der Puls kann unter anderem durch Membra-nen oder Piezoelemente erzeugt werden und wird in der Regel durch direkten Kontakt oder über ein Koppelmittel an das Objekt übertragen. Luftgekoppelter Ultraschall spielt in kommerziellen Anwendungen bisher eine untergeordnete Rolle, da die Dif-ferenz der akustischen Impedanzen von Luft und Festkörpern immense Verluste beim Übergang des Schallsignals hervorruft.
In diesem Beitrag soll ein neuartiges Anregungsprinzip vorgestellt werden, mit dem ein Großteil dieser Verluste vermieden wird. Anstelle eines Festkörpers soll mit Hilfe einer fluidischen Düse Druckluft zur Signalerzeugung eingesetzt werden. In die-ser Düse wird eine selbsterhaltende Strömungsinstabilität erzeugt, die einen Schall-puls von bis zu 100 kHz hervorruft, sodass der Impedanzverlust in die Umgebungsluft entfällt. Da die charakteristische Frequenz eines fluidisch generierten Pulses maßgeb-lich von der Bauform der Düse und dem anliegenden Druck abhängt, lässt sich mittels einer geeigneten Strömungsregelung ein breiter Frequenzbereich zur Abtastung nut-zen. Die so emittierten Pulse werden auf das Prüfobjekt gerichtet und die reflektierten Signale mit einem Laservibrometer an der Oberfläche des Objekts im Echo-Verfahren abgetastet. Von drei signalmindernden Materialübergängen bei gewöhnlichem luftge-koppeltem Ultraschall bleibt in dem hier vorgeschlagenen Messystem lediglich die Grenzfläche von Luft zu Prüfkörper, sodass eine höhere Signalausbeute als bisher er-wartet werden kann.
Measurement of elemental composition of Fe1-xNix and Si1-xGex alloy thin films by EMPA and µ-XRF
(2019)
It was demonstrated in the past that the electron probe microanalysis (EPMA) can be applied to determine accurately both elemental composition and thickness of thin films by using the dedicated software package for thin film analysis Stratagem. A relatively small number of film materials such as pure metallic films of platinum and nickel, binary alloys of Fe-Ni, and Pt-Ni-Co ternary alloy films has been reported in literature as working successfully. Further, the software can be applied ‘inversely’, i.e., by feeding it with the thickness of the film and using the determined mass coating, one can easily calculate the film density, which for porous layers leads us to the true film porosity.
The present study repeats measurements on an already tested system of Fe-Ni thin films on silicon and reports for the first-time results of analysis on Si-Ge thin films deposited on a non-conductive aluminium oxide substrate. Standard-based and standardless EPMA (with EDS) results were used in combination with Stratagem for the quantification.
Further, X-ray fluorescence analysis (XRF) can be used for the determination of elemental composition and thickness of such films as well. In this case, XRF with a μ-focus X-ray source (μ-XRF) attached to a SEM was applied. For quantification, a fundamental parameter (FP) approach has been used to calculate standard-based and standardless results. Compared to EPMA, XRF has a larger information depth and a higher elemental sensitivity because of a generally lower background.
Both thin film systems have been chosen as samples of an international round robin test (RRT) organised in the frame of standardisation technical committee ISO/TC 201 ‘Surface chemical analysis’, under the lead of KRISS. The main objective of the RRT is to compare the results of atomic fractions of Fe1-xNix and Si1-xGex alloy films obtained by different surface Analysis techniques, such as X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), and secondary ion mass spectrometry (SIMS) applied in the depth-profiling operation mode.
Five samples of different atomic fractions of each thin film system, i.e., Fe1-xNix and Si1-xGex, have been grown by ion beam sputter deposition on silicon and Al2O3 wafers, respectively. Reference FeNi and SiGe films with well-known elemental composition and thickness have been also supplied for standard-based analysis. The atomic fractions of all the samples including the references have been certified by RBS (Rutherford backscattering spectrometry) and ICP-AES (inductively coupled plasma atomic emission spectroscopy).
An analysis has been presented pertaining to the use of a convex
bottom tank shape instead of an elliptical, for a road tanker.
Two analyses have been made, concerning the static and the dynamic
relative performance expectations of such tank shape when compared
with the elliptical shape performance.
The outputs of both analyses suggest that the level of average benefit
due to using the proposed shape, is around 10%, with a maximum
benefit observed in the dynamic performance in the case of the
minimum fill level.
Correlation between static and dynamic outputs. Manufacturing.
The potential benefits to the roll stability of a road tanker, derived from using a convex-bottom tank, instead of a concave-bottom one, are assessed. The convex-bottom tank consists of a modified elliptical figure to which the concave bottom is substituted by a convex one. The concave-bottom consists of an elliptical shape. Static and dynamic analyses are performed, for which the proposed shape revels enhancements on the order of 10%. The static rollover stability factor, and the lateral load transfer ratio, are used as performance measures for the static and the dynamic analysis, respectively. The dynamic analysis derives from a simplified model, for which the sloshing mass is substituted by a calibrated simple pendulum. Other potential benefits of the proposed tank shape are discussed, including a reduction in the aerodynamic drag, and a longer life for the vehicle components.
Longitudinal Load transfer light sensitivity to cargo type, fill level and the impact distance.
Maximum sloshing effect for the case of the lowest fill level 12
while for half fill level the sloshing cargo performs as a dynamic damper, with a maximum effect of 6 in the case of medium impact input
The sloshing effect for the highest fill level yielded a mixed output, with the maximum impact distance producing a positive but moderate effect.
The interaction between the sloshing cargo and the carrying vehicle has been predominantly studied from the perspective of road safety, aiming at characterizing the effects of cargo motion on both, the lateral stability of the vehicles and the respective braking performance. In this regard, one main issue is to objectively clarify the potential effects of the sloshing cargoes, when compared with solid or non-sloshing cargoes. While there are abundant theoretical studies about the comparative effects of one substance and the other on the vehicle performance, only few experimental studies have been reported with that approach. In this paper, the outputs from an experimental study involving the longitudinal load transfer of sloshing and non-sloshing cargoes, is presented. The longitudinal load transfer is characterized in this paper on the basis of the moment of the reaction forces at the wheel-support interface, with respect to the impact spot. Results suggest that for one-quarter fill level, the sloshing cargo produces an amplification of the performance measure (12% maximum) while at half fill level the sloshing cargo damps the outputs (6.31 % reduction), while at high fill levels, the sloshing effect is mixed, as a function of the impact input, from -1.1% at low impact distance, to +6.6 for large impact distance.
The occurrence of microplastic particles (MP) in nearly each environmental compartment but especially in water is well documented in an increasing amount of publication within the last few years. However, a comprehensive understanding of MP occurrence, sources and pathways in the environment as well as effects of MP on the environment is still unclear. Many of the studies are not compatible, because they used different sampling, sample preparation and detection techniques, resulting in a very broad variation and very different dimension of archived results. Hence a useful avoiding strategy for reduction the MP entry in the environment is not possible. Furthermore, the existing methods are often very time consuming, need user knowledge and labour force, which is often not acceptable for the routine monitoring of an action or sanction.
The call for harmonised methods become loud and louder and promising efforts are done in this area. However, the scientific discussion is often focus on advantages and disadvantages of detection tools and sample preparation, less initiative is given to the sampling strategy. That is a pity, because every environmental scientist knows, a good analytical result depend on a good sampling strategy.
The sampling of water seems on the first view easy because the sampling process include already an up concentration of the MP by means of sieves and filters. However, this filtering of water is often limited by filter cake on the sieves, consisting of high amount of natural particular matter. Hence often a small water volume is filtered, which will not own a representative amount of trait carriers or complex sieves cascades are used, which need a high technical equipment.
Recently we presented a fast thermoanalytical method for the detection of polymers fractions in water samples. This method, thermo-extraction desorption gas chromatography mass spectrometry (TED-GC-MS) can analyse MP in water filtrates without sample preparations within 2-3 hours. Advantageous is the additional analysis of rubber particles from tires beside the MP. In order to come even faster we now start to develop new sampling strategies, which should be use for different water systems. It is intended to reduce the effort in the field and to elongate times for sampling to obtain a representatives result without random effects.
In the present presentation we will show first result using a sedimentation box for sampling of MP from surface water. Advantages and disadvantages will be discussed and comparison to data from conventional fractionated filtration will be given.
Simulational tools are applied to investigate the physical properties of nanoparticles.
For the description of radioactive gold nanoparticles, particles scattering simulations are performed with the Geant4 monte carlo simulation toolkit.
The temperature dependent behaviour of the magnetization dynamics of different magnetic nanoparticles are simulated with the object oriented micormagnetic framework (OOMMF).
Microbeam analysis data are of continuously improving quality, this owing mainly to developments in instrumentation (hardware and software) and computer performance. The knowledge and skills of the operators must be also kept correspondingly updated. To be deemed as technically competent, the laboratories must be accredited according to an accreditation scheme, mostly following ISO/IEC 17025.
International standards are able to provide requirements, specifications, guidelines or characteristics of methods, instruments or samples with the final goal that these can be used consistently in accredited laboratories. In the field of electron microscopy and microbeam Analysis standardisation and metrology are terms that are encountered rather seldom at major conferences and scientific publications. Several ISO standards already published and used successfully by a large part of the electron microscopy and microbeam analysis community. For example, file formats such as EMSA/MSA for spectral-data exchange or tagged image file format (TIFF) for SEM images; procedures for the specification of X-ray spectrometers, the specification of certified reference materials (CRMs), and for measurement of average grain size by electron backscatter diffraction (EBSD); and guidelines for calibrating image magnification in SEM or TEM. A main task of ISO technical committee TC 202 ‘Microbeam Analysis’ is to identify feasible projects/proposals needed to be developed into new international standards, particularly in respect to recent technology, such the silicon drift detector (SDD).
As far as the metrological aspects are regarded, The International Bureau of Weights and Measures (BIPM) through the Consultative Committee for the Amount of Substance (CCQM) is concerned with the metrological aspect in Chemistry and Biology. In particular, the Surface Analysis Working Group (SAWG) assists in identifying and establishing inter-laboratory work to test the consistency as well as to improve the traceability of spatially resolved chemical surface analysis at the micro and nanoscale. Examples of recent projects on quantitative microbeam analysis at low energies, such as the quantification of light elements such as carbon and nitrogen will be presented.
The significant sources of measurement uncertainty will be emphasized. These are: quality of the unknown and the reference materials used, the quantification model, instrumental parameters like take-off-angle, spectrometer efficiency, and particularly the beam current. The crucial importance of working with uniform and well-defined measurement and data evaluation protocols will be discussed in compliance with the ISO document “Guide to the expression of uncertainty in measurement (GUM)”.
Another international platform where pre-standardisation work can be organised is VAMAS (Versailles Project on Advanced Materials and Standards). International collaborative Projects aim at providing the technical basis for harmonised measurements, testing, specifications, and standards to be further developed at ISO level. One key point of VAMAS activities is constituted by inter-laboratory comparisons for high-quality data. In the field of microbeam analysis, the technical working area (TWA) 37 Quantitative Microstructural Analysis deals with corresponding projects. Good ideas, e.g., on analysis at low energies, are particularly encouraged by directly contacting the author. Support and guidance will be supplied.
Porous materials play an important role in several fields of technology, especially for energy applications like photovoltaics, electrolysis or batteries. The activity of porous films is affected by properties like porosity, film thickness, chemical composition of the material, as well as the crystallinity of the framework. The complex morphology of such porous films constitutes a challenge even for modern analytical techniques and requires new approaches employing the combination/complementation of data of different analytical methods. In this contribution, we characterise thin mesoporous iridium-titanium mixed oxide film properties by electron probe microanalysis (EPMA) with energy-dispersive X-ray spectroscopy (EDS) at an SEM.
Mesoporous iridium oxide - titanium oxide (IrOx-TiOx) films were prepared via dip-coating of a solution containing a triblock-copolymer as structure-directing agent, an iridium precursor as well as a titanium precursor in ethanol. IrOx-TiOx films were synthesized with different amounts of iridium and calcined in air. The SEM micrographs reveal for all films the achievement of a well-ordered mesoporous structure and homogeneous films with thicknesses between 67 nm and 152 nm.
For the determination of film elemental composition and porosity, EPMA can be used as part of a combined SEM/EDS/STRATAGem analysis. Elemental compositions and mass depositions (in μg cm-2) of IrOx-TiOx films were calculated with the thin film analysis Software STRATAGem via k-values measured with SEM/EDS. Pure bulk Ir, TiO2 and Si were measured as references. The average density of the films was obtained from the mass Deposition and the film thickness as measured by cross-section SEM. The porosity was then extracted from the measured average film density divided by a theoretical bulk density. The latter is calculated from the weight fractions of IrOx and TiOx as determined with STRATAGem and the bulk mass densities of IrO2 and TiO2 (rutil) from literature.
The fitting results of the k-values from the STRATAGem software, which are in fair agreement with the measured k-values.
The application of the SEM/EDS/STRATAGem approach for accurate porosity determination on pure mesoporous TiOx films and pure porous IrOx films has been recently demonstrated.
The porosities of pure IrOx, TiOx and mixed IrOx-TiOx films in this study have been determined. The contribution will assess in detail the advantages and limitations of the combined SEM/EDS/STRATAGem analysis for the morphology and porosity of thin metal oxide films. Moreover, the comparison with other measurement techniques and the combination of datasets from multiple measurements will be discussed.
Cancer cell lipid class homeostasis is altered under nutrient-deprivation but stable under hypoxia
(2019)
Background: Cancer cells modify the balance between fatty acid (FA) synthesis and uptake under metabolic stress, induced by oxygen/nutrient deprivation. These modifications were shown to alter the levels of individual triglyceride (TG) or phospholipid sub-species. To attain a holistic overview of the lipidomic profiles of cancer cells under stress we performed a broad lipidomic assay, comprising 244 lipids from six major classes. This assay allowed us to perform robust analyses and assess the changes in averages of broader lipid-classes, stratified on the basis of saturation index of their fatty-acyl side chains.
Methods: Global lipidomic profiling using Liquid Chromatography-Mass Spectrometry was performed to assess lipidomic profiles of biologically diverse cancer cell lines cultivated under metabolically stressed conditions.
Results: Neutral lipid compositions were markedly modified under serum-deprived conditions and, strikingly, the cellular level of triglyceride subspecies decreased with increasing number of double bonds in their fatty acyl chains.
In contrast and unexpectedly, no robust changes were observed in lipidomic profiles of hypoxic (2% O2) Cancer cells despite concurrent changes in proliferation rates and metabolic gene expression.
Conclusions: Serum-deprivation significantly affects lipidomic profiles of cancer cells. Although, the levels of individual lipid moieties alter under hypoxia (2% O2), the robust averages of broader lipid classes remain unchanged.
It was demonstrated in the past that the electron probe microanalysis (EPMA) can be applied to determine accurately both elemental composition and thickness of thin films by using the dedicated software package for thin film analysis Stratagem. A relatively small number of film materials such as pure metallic films of platinum and nickel, binary alloys of Fe-Ni, and Pt-Ni-Co ternary alloy films has been reported in literature as working successfully. Further, the software can be applied ‘inversely’, i.e., by feeding it with the thickness of the film and using the determined mass coating, one can easily calculate the film density, which for porous layers leads us to the true film porosity.
The present study repeats measurements on an already tested system of Fe-Ni thin films on silicon and reports for the first-time results of analysis on Si-Ge thin films deposited on a non-conductive aluminium oxide substrate. Standard-based and standardless EPMA (with EDS) results were used in combination with Stratagem for the quantification.
Further, X-ray fluorescence analysis (XRF) can be used for the determination of elemental composition and thickness of such films as well. In this case, XRF with a μ-focus X-ray source (μ-XRF) attached to a SEM was applied. For quantification, a fundamental parameter (FP) approach has been used to calculate standard-based and standardless results. Compared to EPMA, XRF has a larger information depth and a higher elemental sensitivity because of a generally lower background.
Both thin film systems have been chosen as samples of an international round robin test (RRT) organised in the frame of standardisation technical committee ISO/TC 201 ‘Surface chemical analysis’, under the lead of KRISS. The main objective of the RRT is to compare the results of atomic fractions of Fe1-xNix and Si1-xGex alloy films obtained by different surface Analysis techniques, such as X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), and secondary ion mass spectrometry (SIMS) applied in the depth-profiling operation mode.
Five samples of different atomic fractions of each thin film system, i.e., Fe1-xNix and Si1-xGex, have been grown by ion beam sputter deposition on silicon and Al2O3 wafers, respectively. Reference FeNi and SiGe films with well-known elemental composition and thickness have been also supplied for standard-based analysis. The atomic fractions of all the samples including the references have been certified by RBS (Rutherford backscattering spectrometry) and ICP-AES (inductively coupled plasma atomic emission spectroscopy).
The test material EDS-TM001 together with an accompanying software package, “EDX spectrometer check”, have been made available in 2009 by BAM to be employed by EDS (energy-dispersive X-ray spectrometer) users to check the performance of an EDS attached to the SEM. Particularly for test laboratories operating under accreditation schemes like ISO/IEC 17025, a periodical control of the critical instrumental parameters in end-user laboratories is required. With EDS-TM001 or EDS-TM002 (second generation) test material, this periodical check is simplified to the acquisition of only one 10 kV spectrum. The software “EDX spectrometer check” is destined to evaluate automatically this spectrum and determine the performance of the EDS in terms of energy resolution and calibration, as well as possible alteration of low-energy Efficiency due to detector contamination. Energy resolution can be compared with the specified values according to the international ISO standard ISO 15632:2012. EDS-TM is a synthetic material consisting of a 6 μm thick layer of C, Al, Mn, Cu and Zr deposited on a steel (in case of EDS-TM001) or silicon (in case of EDS-TM002) substrate. The chemical composition of EDS-TM was chosen such as to give nearly equal intensities of the low energy lines in a 10 kV spectrum, thus, making it very sensitive against spectrometer efficiency changes. Meanwhile, about 150 laboratories use the EDS-TM001 or EDS-TM002 test material for the periodical check of their EDS. A detailed description of the test material and software together with examples of application was published recently. New results and gained experiences will be presented as well. When the FWHM of the X-ray lines in the EDS-TM spectrum are determined, the spectrum background must be subtracted accurately. The applied physical background subtraction procedure is robust and takes into account the transmission of the detector window. While the previous version considers only Moxtek AP windows, the new version includes selection of silicon Nitride window and the case of windowless detector. Moreover, the new version allows importing of spectra in Bruker spx-format and EMSA/MSA files from EDAX TEAM software.
Windowless detectors have been also tested demonstrating long-term stability after repeated heating and cooling cycles. In this case, the appropriate Background subtraction is decisive for accurate detector characterization. Detailed results will be presented.
The use of high-fired gypsum as binder for masonry and joint mortars or stuccowork in Central Europe in the Early and High Middle Ages was a regional specific as it depended on local gypsum deposits. The calcination technology possible at the time resulted in an assemblage of calcium sulphate phases dehydrated to different degrees and partly thermally damaged accessory minerals of the raw gypsum. Not hydrated clusters of firing products preserved in the binder matrix are a typical feature of such mortars. A novel Raman microspectroscopic approach, providing access to the burning history of individual anhydrite grains, was applied to samples from medieval South Tyrolean stucco decorations and sculptures. Beyond that, Raman microspectroscopy was employed for tracing and visualising pyrometamorphic reactions in natural impurities of the kiln run. In the discussed examples mineral thermometry indicates process temperatures above 800°C: the breakdown of magnesium-rich chlorite led to the formation of forsterite Mg2SiO4, while the thermal decomposition of dolomite CaMg(CO3)2 to periclase MgO and lime CaO yielded – after hydration and carbonation – magnesite MgCO3, CaCO3 polymorphs and magnesian calcite. Hydration of periclase in the mixed gypsum paste containing sulphate ions also resulted in magnesium sulphate hydrates, here identified in the form of hexahydrite MgSO4·6H2O. Lower burning temperatures left the accessory minerals in their pristine form, but can be traced by measuring the spectra of individual anhydrite crystals in grains of firing products and evaluating Raman band widths. Throughout the present study, calcination temperatures ranging from approx. 600°C to 900°C were determined.
Früh- bis spätmittelalterliche Stuckausstattungen bilden ein regionales, da an Gips-vorkommen korreliertes kunsttechnologisches Spezifikum. Aufgrund der beschränkten Kontrollmöglichkeiten über die in einem Meiler oder Feldofen herrschenden Parameter charakterisiert mittelalterliche Hochbrandgipse ein Phasengemisch aus Calciumsulfat-Hydratstufen und thermisch mehr oder weniger stark geschädigten Nebenbestandteilen aus der Gipslagerstätte. Die Analyse mittelalterlicher Hochbrandgipse erfordert die genaue Kenntnis der Bildungs- und Stabilitätsbereiche der Phasen im System CaSO4–H2O. Gips CaSO4 x 2 H2O entwässert beim Brennen über Halbhydrat CaSO4 x 0.5 H2O zu Anhydrit III CaSO4, welches schließlich in den für mittelalterliche Hochbrandgipse relevanten Anhydrit II (AII) übergeht. Für diesen wurden aufgrund der Abbindeeigenschaften drei bis vor kurzem nicht spektroskopisch unterscheidbare Sub-Phasen postuliert: Anhydrit II schwerlöslich (300-500°C, AII-s), unlöslich (500-700°C, AII-u) und Estrichgips (> 700°C, AII-E). Anhydrit I ist nur über 1180°C stabil.
Mittels strukturanalytischer Methoden wie Röntgenbeugung (XRD) und Raman-Spektroskopie lassen sich nur die verschiedenen Hydratstufen sowie AIII, AII und AI eindeutig aufgrund unterschiedlicher Kristallstrukturen identifizieren. Ein neues auf Raman-mikrospektroskopischer Bildgebung basierendes Verfahren ermöglicht den Nachweis verschiedener Brenntemperaturen aufgrund der Auswertung von Raman-Bandenbreiten von AII, welche ein Maß für die mit steigender Brenntemperatur zunehmende Kristallinität der Anhydritkörner sind.
Die Anwendung dieser Methode sowie der Nachweis pyrometamorpher Umwandlun-gen von Begleitmineralien aus dem Gipsstein als Mineralthermometer zur Bestimmung von Brenntemperaturen wird anhand von Proben früh- und spätmittelalterlicher Skulpturen und Stuckdekorationen aus Südtirol diskutiert. Außerdem wird gezeigt, wie die Analyse solch komplexer Materialien Rückkopplungen in die Analytische Chemie erzeugen kann, da zur erfolgreichen Analytik eine Möglichkeit zur reproduzierbaren Bestimmung von Ramanbandenbreiten und der Korrektur instrumentenabhängiger Verbreiterung gefunden und optimiert werden musste.
Damit sollten überzeugende Belege dafür erbracht werden können, dass die Komplexität des monomineralischen Bindemittels Gips bezüglich der je nach Brandbedingungen unterschiedlichen Eigenschaften und insbesondere bezüglich der Herausforderungen an die Analytische Chemie häufig unterschätzt wird.