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Eingeladener Vortrag
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The hepatotoxin phomopsin A (PHO-A), a secondary metabolite mainly produced by the fungus Diaporthe toxica, occurs predominantly on sweet lupins. Along with the growing interest in sweet lupins for food and feed commodities, concerns have been raised about fungal infestations, and consequently, about the determination of PHO-A.
High performance liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) represents the most suitable analytical technique for sensitive and selective detection of mycotoxins including PHO-A. However, isotopic labeled substances are needed as internal standards for a reliable and convenient quantification.
As no isotope standard for PHO-A is currently available, a biosynthesis of fully 15N6-labeled PHO-A was established by cultivation of D. toxica on defined media containing Na15NO3 and 15N-labeled yeast extract as the only nitrogen sources. The identity of 15N6-PHO-A was confirmed by high resolution mass spectrometry.
The new 15N6-labeled standard will facilitate the method development for PHO-A including a more accurate quantification by LC-MS/MS.
Austenitic stainless steels provide a beneficial combination of chemical and mechanical properties and have been used in a wide field of applications for over 100 years. Further improvement of the chemical and mechanical properties was achieved by alloying nitrogen. But the solubility of N within the melt is limited and can be increased in substituting Ni by Mn and melting under increased pressure. In order to avoid melting under pressure and decrease production costs, a part of N can also be substituted by C. This leads to austenitic high interstitial steels (AHIS). Within the solution annealed state strength and ductility of AHIS is comparable or even higher of those of AHNS and can be further improved by cold working. Unfortunately the endurance limit does not follow this trend as it is known from cold-worked austenitic CrNi steels. This is due to the differences of the slip behavior which is governed by the stacking fault energy as well as other near field effects. Construction components operating under cyclic loads over long periods of time cannot be considered being free of voids or even cracks. Thus the crack propagation behavior is of strong interest as well. This contribution presents the tensile, fatigue, crack propagation and fracture toughness properties of AHNS and AHIS in comparison to those of CrNi-steels. The differences are discussed in relation to microstructural characteristic as well as their alterations under cyclic loading.
In Betonbauteilen unter gleichzeitiger zyklischer Beanspruchung und externer Alkalizufuhr ist die Gefahr von Schäden infolge oder unter Mitwirkung einer Alkali-Kieselsäure-Reaktion (AKR) besonders hoch. Dies betrifft insbesondere Fahrbahndecken, bedingt durch den zunehmenden Schwerlastverkehr und den winterlichen Auftrag des Enteisungsmittels NaCl. Speziell die Rolle einer mechanischen Vorschädigung des Betons infolge der Verkehrsbeanspruchungen auf den Ablauf einer AKR ist dabei aber noch nicht in ausreichendem Umfang geklärt. Ein Teil der dazu seit 2012 durchgeführten Untersuchungen im Rahmen der DFG-Forschergruppe 1498 soll im Folgenden vorgestellt werden. Es zeigte sich, dass eine AKR in definiert mechanisch vorgeschädigten Betonprobekörpern mit alkalireaktiven Gesteinskörnungen und unter äußerer Alkalizufuhr vor allem früher beginnt als in äquivalenten Probekörpern ohne Vorschädigung. Grund dafür ist das schnellere und tiefere Eindringen von Wasser und insbesondere gelöstem NaCl in den Beton, wodurch Na-Ionen als Reaktionspartner für eine AKR früher und langfristig auch in größerer Menge verfügbar sind.------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
In concrete elements, simultaneously subjected to cyclic loadings and external alkalis, the risk for damages caused by or under participation of an alkali-silica reaction (ASR) is particularly high. This concerns especially concrete pavements due to the increasing heavy load traffic and the wintry application of NaCl deicer. Notably the role of a mechanical pre-damage of concrete caused by traffic loadings on the course of the ASR is largely unclear. A part of the investigations that has been conducted since 2012 into this issue within the scope of the DFG (German research foundation) funded research group 1498 shall be introduced in the following. It was evident that an ASR in defined mechanically pre-damaged concrete prisms with alkali-reactive aggregates and under an external supply of alkalis started earlier than in equal prisms without a pre-damage. The reason for this is the faster and deeper ingress of water and particularly of dissolved NaCl into the concrete, by what Na ions as reaction partner for an ASR are available earlier and, in the long-term, in greater amounts too.
Die "Empfehlungen für die Beförderung gefährlicher Güter, Handbuch über Prüfungen und Kriterien" ergänzen die "Empfehlungen für die Beförderung gefährlicher Güter, Modellvorschriften" und das "Global harmonisierte System zur Einstufung und Kennzeichnung von Chemikalien (GHS)". Sie enthalten Kriterien, Prüfmethoden und –verfahren, die angewendet werden sowohl für die Einstufung gefährlicher Güter nach den Vorschriften der Teile 2 und 3 der Modellvorschriften als auch für Chemikalien, von denen nach dem GHS physikalische Gefahren ausgehen.
Bright emitters with photoluminescence in the spectral region of 800–1600 nm are increasingly important as optical reporters for molecular imaging, sensing, and telecommunication and as active components in electrooptical and photovoltaic devices. Their rational design is directly linked to suitable methods for the characterization of their signal-relevant properties, especially their photoluminescence quantum yield (Φf). Aiming at the development of bright semiconductor nanocrystals with emission >1000 nm, we designed a new NIR/IR integrating sphere setup for the wavelength region of 600–1600 nm. We assessed the performance of this setup by acquiring the corrected emission spectra and Φf of the organic dyes Itrybe, IR140, and IR26 and several infrared (IR)-emissive Cd1-xHgxTe and PbS semiconductor nanocrystals and comparing them to data obtained with two independently calibrated fluorescence instruments absolutely or relative to previously evaluated reference dyes. Our results highlight special challenges of photoluminescence studies in the IR ranging from solvent absorption to the lack of spectral and intensity standards together with quantum dot-specific challenges like photobrightening and photodarkening and the size-dependent air stability and photostability of differently sized oleate-capped PbS colloids. These effects can be representative of lead chalcogenides. Moreover, we redetermined the Φf of IR26, the most frequently used IR reference dye, to 1.1 × 10-3 in 1,2-dichloroethane DCE with a thorough sample reabsorption and solvent absorption correction. Our results indicate the need for a critical reevaluation of Φf values of IR-emissive nanomaterials and offer guidelines for improved Φf measurements.
Critical review of the determination of photoluminescence quantum yields of luminescent reporters
(2015)
A crucial variable for methodical performance evaluation and comparison of luminescent reporters is the photoluminescence quantum yield (Φ pl). This quantity, defined as the number of emitted photons per number of absorbed photons, is the direct measure of the efficiency of the conversion of absorbed photons into emitted light for small organic dyes, fluorescent proteins, metal–ligand complexes, metal clusters, polymeric nanoparticles, and semiconductor and up-conversion nanocrystals. Φ pl determines the sensitivity for the detection of a specific analyte from the chromophore perspective, together with its molar-absorption coefficient at the excitation wavelength. In this review we discuss different optical and photothermal methods for measuring Φ pl of transparent and scattering systems for the most common classes of luminescent reporters, and critically evaluate their potential and limitations. In addition, reporter-specific effects and sources of uncertainty are addressed. The ultimate objective is to provide users of fluorescence techniques with validated tools for the determination of Φ pl, including a series of Φ pl standards for the ultraviolet, visible, and near-infrared regions, and to enable better judgment of the reliability of literature data.
Two-color double-fs-pulse experiments were performed on silicon wafers to study the temporally distributed energy deposition in the formation of laser-induced periodic surface structures (LIPSS). A Mach-Zehnder interferometer generated parallel or cross-polarized double-pulse sequences at 400 and 800 nm wavelength, with inter-pulse delays up to a few picoseconds between the sub-ablation 50-fs-pulses. Multiple two-color double-pulse sequences were collinearly focused by a spherical mirror to the sample. The resulting LIPSS characteristics (periods, areas) were analyzed by scanning electron microscopy. A wavelength-dependent plasmonic mechanism is proposed to explain the delay-dependence of the LIPSS. These two-color experiments extend previous single-color studies and prove the importance of the ultrafast energy deposition for LIPSS formation.
Development of a multi-VOC reference material for quality assurance in materials emission testing
(2015)
Emission test chamber measurement is necessary to proof building materials as sources of volatile organic compounds (VOCs). The results of such measurements are used to evaluate materials and label them according to their potential to emit harmful substances, polluting indoor air. If only labelled materials were installed indoors, this would improve indoor air quality and prevent negative impacts on human health. Because of the complex testing procedure, reference materials for the quality assurance are mandatory. Currently, there is a lack of such materials because most building products show a broad variation of emissions even within one batch. A previous study indicates lacquers, mixed with volatile organic pollutants, as reproducible emission source for a wide range of substances. In the present study, the curing of the lacquer-VOC mixture inside micro-chambers was optimised. Therefore, the humidity and the chamber flow were varied. Typical indoor air pollutants with a wide range of volatilities, for example, styrene, n-hexadecane, dimethyl and dibutyl phthalate were selected. It turned out that, under optimised curing parameters inside the micro-chamber, their emission can be reproduced with variations of less than 10 %. With this, a next important step towards a reference material for emission testing was achieved.
Fukuda et al. published a paper (Scripta Mater. 68 (2013) 984–987) in which they claimed to be able to determine the isothermal nature of the martensitic transformation in a Ti–Ni alloy. They analyzed the evolution of electrical resistance during isothermal holding stages and concluded that the variations were a consequence of the isothermal transition between austenite and martensite. In the following we will demonstrate that the discussed data do not allow the interpretation presented and that the isothermal nature is not proved.
Sulphurous additives for polystyrene: Influencing decomposition behavior in the condensed phase
(2015)
The thermal decomposition behaviour of polystyrene (PS) containing sulphur and phosphorus additives was investigated, using thermogravimetry coupled with Fourier transform infrared spectroscopy (TGA-FTIR). It was found that the additives influence the decomposition process of the polymer in the condensed phase, resulting in a decrease in styrene monomer formation and an increase in styrene oligmer derivatives. Via reference measurements with binary mixtures it was found that the presence of sulphur additives influences the radicalic decomposition process of PS. In combination with quantum chemical calculations it was concluded that this is due to the formation of radicals that abstract hydrogen from the polymer matrix at lower temperatures, disfavouring the radicalic decomposition pathway leading to styrene.
The effect of structural constriction on molecular mobility is investigated by broadband dielectric spectroscopy (BDS) within three types of molecular arrangements: monomers, oligomers and self-assembled monolayers (SAMs). While disordered monomers exhibit a variety of cooperative and local relaxation processes, the constrained nanodomains of oligomers and highly ordered structure of monolayers exhibit much hindered local molecular fluctuations. Particularly, in SAMs, motions of the silane headgroups are totally prevented whereas the polar endgroups forming the monolayer canopy show only one cooperative relaxation process. This latter molecular fluctuation is, for the first time, observed independently from other overlapping dielectric signals. Numerous electrostatic interactions among those dipolar endgroups are responsible for the strong cooperativity and heterogeneity of the canopy relaxation process. Our data analyses also revealed that the bulkiness of dipolar endgroups can disrupt the organization of the monolayer canopy thus increasing their ability to fluctuate as temperature is increased.
An approach is presented to model elastic waveguides of arbitrary cross-section coupled to infinite solid media. The formulation is based on the scaled boundary-finite element method. The surrounding medium is approximately accounted for by a dashpot boundary condition derived from the acoustic impedances of the infinite medium. It is discussed under which circumstances this approximation leads to sufficiently accurate results. Computational costs are very low, since the surrounding medium does not require discretization and the number of degrees of freedom on the cross-section is significantly reduced by utilizing higher-order spectral elements.
Epoxy carbon-fibre prepreg, Hexcel Type 6376 HTS, was investigated using Dynamic Mechanical Analysis (DMA). The DMA characteristic parameters are storage modulus E', loss modulus E' and loss factor tanδ. These parameters are ideally suited to observe the vitrification, referred to as glass transition, resulting from the cross-linking reaction. Detection of the cure state may also be achieved by determining the momentary glass transition temperature of partially cured samples. The consequent use of a multi-frequency measuring regime was used to derive the apparent activation energy for the glass transition process. Different temperature programs were also applied to monitor the curing process directly, as well as to investigate the different states of incomplete cure reached in preceding curing steps. The intention was to provide better understanding of the consequences of an interrupted autoclave curing process and to use DMA to detect the cure state achieved. With DMA, the continuation of an incomplete curing process also can be monitored. DMA measurements up to 300 °C showed, furthermore, that the final glass transition temperature was reduced by thermal degradation at high temperatures.
ISO standards for gas cylinders made from aluminum alloys generally require heat treatment after the forming process. Such heat treatment is a costly part of the manufacturing process. Particularly due to increasing international trade, market-surveillance authorities need simple and reliable methods to field-test cylinders for proper heat treating. By the present contribution the difference in strength of heat-treated and non-heat-treated gas cylinders is exemplarily shown and several material analysis methods are investigated for their suitability as field tests.
This article presents an analytical approach for simulation of ultrasonic diffracted wave signals from cracks in two-dimensional geometries based on a novel Huygens–Fresnel Diffraction Model (HFDM). The model employs the frequency domain far-field displacement expressions derived by Miller and Pursey in 2D for a line source located on the free surface boundary of a semi-infinite elastic medium. At each frequency in the bandwidth of a pulsed excitation, the complex diffracted field is obtained by summation of displacements due to the unblocked virtual sources located in the section containing a vertical crack. The time-domain diffracted wave signal amplitudes in a general isotropic solid are obtained by standard Fast Fourier Transform (FFT) procedures. The wedge based finite aperture transducer refracted beam profiles were modelled by treating the finite dimension transducer as an array of line sources. The proposed model is able to evaluate back-wall signal amplitude and lateral wave signal amplitude, quantitatively. The model predicted range-dependent diffracted amplitudes from the edge of a bottom surface-breaking crack in the isotropic steel specimen were compared with Geometrical Theory of Diffraction (GTD) results. The good agreement confirms the validity of the HFDM method. The simulated ultrasonic time-of-flight diffraction (TOFD) A-scan signals for surface-breaking crack lengths 2 mm and 4 mm in a 10 mm thick aluminium specimen were compared quantitatively with the experimental results. Finally, important applications of HFDM method to the ultrasonic quantitative non-destructive evaluation are discussed.
A software prototype is developed for assessing and updating the reliability of single-cell prestressed concrete box girders subjected to chloride-induced reinforcement corrosion. The underlying system model consists of two integrated sub-models: a condition model for predicting the deterioration state of the box girder and a structural model for evaluating the overall system reliability. The condition model is based on a dynamic Bayesian network (DBN) model which considers the spatial variation of the corrosion process. Inspection data are included in the calculation of the system reliability through Bayesian updating on the basis of the DBN model. To demonstrate the effect of partial inspections, the software prototype is applied to a case study of a typical highway bridge with six spans. The case study illustrates that it is possible to infer the condition of uninspected parts of the structure due to the spatial correlation of the corrosion process.
First developments of a new test to evaluate the fire behavior of photovoltaic modules on roofs
(2015)
A new test for photovoltaic (PV) modules exposed to an external fire source on roofs is proposed, and first results are presented. This is a simplification of the standards commonly in use for testing PV modules as roofing parts, roofing components or building components. Most of the tests required different fire scenarios and the use of burning brands such as wood cribs. In our study we proposed replacing wooden burning brands with a propane burner, the output of which is close to the one that can be observed in the burning of wooden cribs 500 g and 2 kg in size. The fire behavior was assessed by measuring smoke evolution, burning drips, flaming debris, and the time to burn-through of monocrystalline, polycrystalline and amorphous silicon panels. Two different configurations of the burner were tested, with the fire source on the top of the module or under the tilted module, respectively. The fire behavior of the modules was dependent on the burner output (16 to 46 kW), but also on the construction type of the panel (glass/glass or glass/plastic sheet) and on the position of the fire source (top or bottom). These preliminary tests for further development of the procedure yielded encouraging results for the evaluation of PV panels on roofs.
The aim of this study was the development of a low volume air sampling strategy for biocides and polychlorinated biphenyls (PCB) at low air change rates in modern, air-tight showcases as they are present in museums. Lindane, pentachlorophenol, dichlofluanid, tolyfluanid, isodrin, p,p-dichlorodiphenyl trichloroethane and permethrin were the biocides and PCB 28 and PCB 153 were the PCBs studied, all of which are semi volatile organic compounds (SVOC). Their occurrences in the museum environment originate from various sources e.g. preventive treatment of organic exhibits or organic building materials. Exhibits are long-term exposed to these pollutants due to storing in showcases or other storage equipment at low air change rates. To achieve air sampling under the aforementioned conditions the influences of temperature, air circulation, air change rate and relative humidity on the emission behavior of the selected biocides and PCBs had to be determined. This was carried out with pre-soaked wood samples in low volume air sampling experiments using 27 L test showcases and 23 L and 24 L emission test chambers and also diffusive sampling with glass as the sampling material.
The pore structure of lightweight granules made from masonry rubble was studied in order to better understand their engineering properties. Thermally and hydrothermally hardened granules were tested. Analysis by ESEM, mercury porosimetry and sorption methods yield important insight into their microstructure. The thermal granules are characterised by partly melted vitreous areas and large internal macropores that are connected via narrow throats. They show a marginal specific surface area along with a hydrophobic behaviour. In contrast, the hydrothermal granules have an accessible mesoporous system containing plate-like and ink-bottle pores. The shape of their water isotherms depending on the granules CaO content is sensitive to the morphology of calcium silicate hydrate phases (CSH). The hysteresis changes from a narrow loop that closes at low pressures, which can be attributed to coarser more crystalline CSH, to a large triangular-shaped loop along with a low pressure hysteresis, which is characteristic for fine fibre-like CSH with ink-bottle and plate-like pore morphologies. Granules with fibre-like CSH have the higher specific surfaces areas but those with more crystalline CSH show stronger physisorption of water molecules.
The aim of the joint project ViPQuali (Virtual Product Qualification) was to describe a components ageing behaviour in a given environment, by numerical simulation.
Having chosen polypropylene (PP) as the material, which does not show sensitivity to moisture, the relevant weathering parameters of the doseresponse functions could be limited to spectral irradiance and temperature.
In artificial irradiation tests, for PP plates of varied stabiliser content, spectral sensitivity as well as temperature dependence of irradiation-caused crack formation was quantified. For that purpose, samples were exposed both to artificial weathering tests at various constant temperatures and to spectrally resolved irradiation. The temperature dependence could be modelled by an Arrhenius fit. For fitting the spectral sensitivity, a plateau function was chosen. Subsequently, the stabiliser content was parameterised and extrapolated.
The formed dose–response functions were incorporated into a Computational Fluid Dynamics (CFD) software program, simulating the environment of a sample within a Phoenix-exposed IP/DP (Instrument Panel/Door Panel box) box, based on sun position and weather conditions, including radiation interactions. Observed local effects as well as the general ageing advance of PP hats are compared with respect to simulation and experiment.
Resulting from this project, for this most simple example of PP of varied stabiliser content, the time to failure can be estimated for each weathering exposure environment with known time-resolved irradiance and temperature conditions.