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Eingeladener Vortrag
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Effective cleanup of groundwater contaminated with radionuclides using permeable reactive barriers
(2015)
The mining of natural resources always causes environmental impacts such as land use, large quantities of waste, destruction of habitat, impairment of groundwater regime, and quite possibly contamination of soil, water, or air (Dudka and Adriano 1997). The environmental impact of mining cannot be estimated easily. The concept of total material requirement (TMR) is an attempt to quantify the environmental impact of materials. TMR is the sum of domestic and imported primary natural resources and their hidden flows (Adriaanse et al. 1997). Hidden flows are often not considered in environmental analyses because they are attributed with no cost. However, overburden from mining, earth moving for construction, and soil erosion are major sources of ecological damage. From the mining of minerals to the final products, a number of process steps take place (exploration, mine site development, extraction, milling, washing, concentration, smelting, refining, fabrication), each step being connected to other input flows such as energy or other resources. The hidden flows for metals related to metal ore mining have been investigated by Halada et al. (2001). Table 9.1 lists the data for some metals, together with the data for some other minerals and fuels. The TMR in the United States in the 1990s was between 80 and 100 tonnes per capita; in the European Union (EU-15) approximately 50 tonnes per capita (Bringezu 2002).
In order to assess the anisotropy-related uncertainties of relatively determined photoluminescence quantum yields (ΦPL) of molecular emitters and luminescent nanomaterials, we compared ΦPL values measured without and with polarizers using magic angle conditions and studied systematically the dependence of the detected emission intensity on the polarizer settings for samples of varying anisotropy. This includes a dispersion of a spherical quantum dot (QD) with an ideally isotropic emission, a solution of a common small organic dye in a fluid solvent as well as dispersions of elongated quantum dot rods (QDR) with an anisotropic luminescence and a small organic dye in a rigid polymeric matrix, as ideally anisotropic emitter. Our results show that for instruments lacking polarizers, anisotropy-related measurement uncertainties of relative photoluminescence quantum yields can amount to more than 40%, with the size of these systematic errors depending on the difference in emission anisotropy between the sample and the standard.
Mit einer neuartigen analytischen Zentrifuge können Klebverbindungen, Beschichtungen und Kompositwerkstoffe untersucht werden. Die Idee der Wissenschaftler an der BAM Bundesanstalt für Materialforschung und -prüfung: Die Proben müssen nicht mehr eingespannt, sondern nur noch eingesteckt werden. Durch das einfache Einstecken der Prüfkörper ist eine sehr schnelle Beladung möglich. Zudem können bis zu acht Proben gleichzeitig unter identischen Bedingungen geprüft werden. Konventionelle Zugprüfmaschinen waren und sind nur in der Lage, einen (eingespannten) Probekörper zu testen. Das von BAM-Forschern bereits 2004 zum Patent angemeldete Funktionsprinzip wurde seitdem von der Berliner LUM GmbH als Lizenznehmer zum marktreifen Produkt weiterentwickelt.
Radiologic evaluation techniques are nondestructive testing (NDT) used to detect the bulk of explosives and contraband materials in large objects. As compared to conventional low-energy (<450 key) X-ray imaging, high-energy (>1 MeV) digital X-ray radiography is required for the NOT of large containers because of the need for high penetration through thick materials, sensitivity, and the ability to distinguish between low-and high-Z materials. Mobile, high-energy, and high-resolution radiologic techniques are useful to detect contraband and threat materials in digital radiographic images of containers with complex packing. This paper presents a mobile, high-energy X-ray radiographic technique for the in-field nondestructive inspection of cargo containers. The developed experimental technique consisted of a betatron as a high-energy (7.5 MeV) X-ray source and a high-resolution (400 mu m) matrix detector for the digital X-ray imaging. In order to evaluate the detection efficiency and image quality of the measurement technique, a test specimen was proposed that was made of a 3 mm thick steel container with an inner dimension of 60 x 30 x 40 cm(3) comprising different low-and high-Z materials. Image quality indicators were used to assess the essential image quality parameters such as image basic spatial resolution, effective attenuation coefficient, and signal-to-noise ratio (SNR). Experimental investigations were performed on a 6.1 m sea freight container with mockup dangerous materials in complex packing. Preliminary experimental results showed that the proposed technique was able to distinguish between liquids and solids, as well as detect contraband materials. Furthermore, a remarkable SNR of 400 was achieved in the measured digital X-ray images. The influence of temperature on X-ray radiation dose rate at different X-ray energies was also investigated. Finally, important applications of the proposed technique in the context of maritime security are discussed.
In den Untersuchungen zum Zündvermögen von Filmeffektzündern wurde nachgewiesen, dass diese einen Plastiksprengstoff auf Basis von PETN nicht zu einer detonativen Umsetzung anregen können. Die Erfüllung der grundlegenden Sicherheitsanforderung (ESR) des Anhanges 1 der Richtlinie 2013/29/EG und die Kategorisierung als pyrotechnischer Gegenstand für Theater (T2) kann somit als gegeben angesehen werden, da der verwendete Explosivstoff zur Gruppe der sensibelsten Sprengstoffe (Initiierung mit geringen Zündenergien) gehört. Es wurde weiterhin nachgewiesen, dass der Untemassertest nach DIN EN 13763 Teil 15 aussagekräftige Ergebnisse liefert, welche die Fähigkeit von Filmeffektzündern und vergleichbaren pyrotechnischen Gegenständen bestätigen respektive widerlegen, einen Sekundärsprengstoff zu zünden (eine Detonation zu initiieren).
Für eine allgemeine Einschätzung des Zündvermögens von Filmeffektzündern und vergleichbaren pyrotechnischen Gegenständen ist ein Grenzbereich für ein äquivalentes Zündvermögen in g PETN auf Basis der Experimente mit dem o. g. Unterwassertest bestimmt worden. Filmeffektzünder und vergleichbare pyrotechnische Gegenstände sind nicht in der Lage, einen Sekundärsprengstoff zur Detonation anzuregen, wenn das aus dem Unterwassertest ermittelte äquivalente Zündvermögen unter 0,25 g PETN liegt.
Auswirkungen von Ermüdungsbeanspruchungen auf Struktur und Eigenschaften von Fahrbahndeckenbeton
(2015)
Ausgehend von der Zielsetzung der DFG-Forschergruppe 1498, die Einflüsse auf den AKR-Schädigungsprozess in Fahrbahndecken aus Beton grundlegend zu klären, sind zwei aufeinander aufbauende Untersuchungsschwerpunkte Gegenstand dieses Beitrags. Im ersten Schwerpunkt wurden die prüftechnischen Voraussetzungen für die Charakterisierung der Degradation und damit der Rissbildung im Fahrbahndeckenbeton durch die Vorschädigung infolge von Ermüdungsbeanspruchungen geschaffen. Realisiert wurde dies durch die Implementierung und Optimierung eines Monitoringsystems im zyklischen 4-Punkt-Biegeversuch zur simultanen Erfassung der Rissbildung im großformatigen Schwingbalken. Zusätzlich wurde die Röntgen-3D-Computertomografie für die hochauflösende räumliche quantitative Rissanalyse in den Bohrkernen aus den Schwingbalken ohne und mit Vorschädigung weiterentwickelt. Im zweiten Untersuchungsschwerpunkt wurde mittels vielfältiger Experimente an kleinformatigen Probekörpern aus dem Schwingbalken gezeigt, dass durch die Ermüdungsbeanspruchung die bruchmechanischen Materialkennwerte des Betons zum Teil eine signifikante Veränderung erfahren. Based on the objective of the DFG (German research foundation) funded research group 1498 to clarify the influences on the ASR damage process, this paper deals with two focuses of investigation. In the first focus the technical requirements for the characterisation concerning the degradation and the formation of cracks in concrete pavements by the pre-damage as a result of fatigue loading were created. This was realized by the implementation and the optimisation of a monitoring system in the cyclic four point bending test to capture simultaneously the formation of cracks in the beam under sinusoidal bending load. In addition, the X-ray 3D-computed tomography was enhanced for the high-resolution quantitative spatial crack analysis in the drilling cores extracted of the beam under sinusoidal bending load without and with a pre-damage. Building on the first focus, in the second focus of investigation a significant change of the fracture-mechanical properties of the concrete as a result of fatigue loading has been demonstrated in numerous experiments using small specimens extracted from the beam under sinusoidal bending load.
This paper presents a new X-ray backscatter technique (XBT) for non-destructive imaging of aerospace materials with only a single-sided access. It uses a special twisted slit collimator to inspect the whole object by changing the viewing direction of the X-ray backscatter camera. For the first time, the X-ray backscatter measurements were conducted using high-energy (>500 keV) X-ray sources. Experiments were performed on thick complex structured aluminium components, stringers and honeycomb structures to validate the applicability of the present technique to image small changes in the material properties and also to detect low-density material inclusions. In order to reduce the inspection time from hours to several seconds and to improve the image quality of the X-ray backscatter image, the backscattered signals were measured using a digital detector array with high spatial resolution (200 µm). The influence of the energy of the X-ray source and the slit width of the camera on the X-ray backscatter image were also investigated. In the proposed technique, the whole object is irradiated by an un-collimated X-ray beam resulting in a low image acquisition time of 3 min that facilitates the use of XBT for the real time NDT&E of aerospace materials.
Sicherstellung des Korrosionsschutzes durch werkstoffgerechte Verarbeitung nichtrostender Stähle
(2015)
The ground vibrations, which are generated by trains on different tracks, have been calculated by finite-element boundary-element models. The ballasted track is modelled in detail by the finite element method. The infinite soil is modelled by the boundary element method as a homogeneous or layered half-space. The track-soil system is coupled to a simple rigid mass model of the vehicle so that the vehicle-track interaction is completely included. Transfer functions are calculated in frequency domain without and with vehicle-track interaction, the compliance of the track and the mobilities of the soil at different distances from the track. Finally, the ratios between the ground vibration amplitudes with and without mitigation measures are calculated to quantify the effectiveness of the mitigation measures.
Tracks with under-sleeper pads have been investigated in a wide parameter study for the RIVAS project. The main parameters that influence the reduction of ground vibration are the stiffness of the under-sleeper pad, the mass and the width of the sleeper. The softest sleeper pad yields the best reduction of the ground vibration. The influence of the sleeper mass is not so strong, as the characteristic frequency is ruled by the mass of the sleeper and the mass of the wheelset as well.
Behavior of dust/air mixtures is very complex and difficult to predict since it depends on material properties as well as boundary conditions. Without other influences airborne particles deposit due to gravity but the time it takes for total deposition as well as easiness of resurrection depends very much on the specific dust sample and the boundary conditions. It still lacks a complete understanding of all interacting reasons and one approach is using experimentally determined characteristics, one is named dustiness.
Dustiness is the tendency of dust to form clouds and to stay airborne. Dustiness is determined with two basic principles, which are light attenuation and ratio of filled-in and measured mass. Assessment of dustiness of industrial powders has been done for a long time regarding work place safety. Dustiness is used there to determine inhalable fraction and to evaluate health risks. Lately it became interesting in dust explosion protection as well. Dustiness could be used to optimize determination of zones, adaption of venting area and/or for positioning of suppression systems.
Dustiness can be useful in many ways but is not a physical property of dusts, therefore it depends on material properties such as density, particle size distribution, shape and water content as well as boundary conditions or determination method. This makes it very difficult to compare dustiness for different techniques and apparatuses and determination method as well as results should be considered carefully. This work gives an overview of existing standards, recent research and suggests improvements to the new dustiness as proposed for dust explosion protection.
Pd/TiO2 coatings with template-controlled mesopore structure as highly active hydrogenation catalyst
(2015)
Micro-structured reactors offer excellent mass and heat transport capabilities and can therefore sustain very high reaction rates and space–time-yields also for highly exothermic catalytic reactions. However, such high rates cannot be reached when the reactors are coated or filled with conventional catalysts powders. We present a strategy for the direct synthesis of highly active wall-coated supported catalysts via co-deposition of a pore template (here micelles formed from PEO-b-PPO-b-PEO) and a precursors for the metal oxide (TiCl4) along with a compatible precursor for the active metal (PdCl2). The obtained catalytic coatings possess a template-controlled open pore structure and excellent mechanical stability. Moreover, the active metal is highly dispersed and well-distributed across the coating also at high Pd loadings. The corresponding high activity along with rapid mass transfer enabled by the open pore system results in the best space–time-yields in the gas-phase hydrogenation of butadiene reported so far in literature for a supported catalyst.
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.
Für Spannstähle muss im Rahmen der Überwachung die Beständigkeit gegenüber Spannungsrisskorrosion nach DIN EN ISO 15630-3 nachgewiesen werden. Die Stähle werden hierbei entweder einer konzentrierten Ammoniumthiocyanatlösung oder einer verdünnten Lösung, die eher die Verhältnisse in der Baupraxis wiedergibt, ausgesetzt. In den vergangenen Jahren gab es an Spannstäben der Festigkeitsklasse St 950/1050 immer wieder Probleme mit dem Erreichen der erforderlichen Standzeiten in der konzentrierten Lösung. Der Ringversuch sollte nun klären, inwieweit Unsicherheiten hinsichtlich der Zuverlässigkeit und Aussagekraft der Ergebnisse von Spannungsrisskorrosionsprüfungen bestehen. Außerdem sollten die Prüfanweisungen, die Prüfeinrichtungen sowie die Vor-Ort-Inspektion der Prüfstände kritisch beurteilt werden, um eventuell vorhandene versuchstechnische Probleme zu identifizieren und ggf. zu beheben.
Basics of statistic
(2015)
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.
The adsorption of porphyrin derivatives on a Au(111) surface was studied by scanning tunneling microscopy and spectroscopy at low temperatures in combination with density functional theory calculations. Different molecular appearances were found and could be assigned to the presence of single gold adatoms bonded by a coordination bond underneath the molecular monolayer, causing a characteristic change of the electronic structure of the molecules. Moreover, this interpretation could be confirmed by manipulation experiments of individual molecules on and off a single gold atom. This study provides a detailed understanding of the role of metal adatoms in surface–molecule bonding and anchoring and of the appearance of single molecules, and it should prove relevant for the imaging of related molecule–metal systems.
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.
We present a systematic study on the effect of surface ligands on the luminescence properties and colloidal stability of β-NaYF4:Yb3+,Er3+ upconversion nanoparticles (UCNPs), comparing nine different surface coatings to render these UCNPs water-dispersible and bioconjugatable. A prerequisite for this study was a large-scale synthetic method that yields ~2 g per batch of monodisperse oleate-capped UCNPs providing identical core particles. These ~23 nm sized UCNPs display an upconversion quantum yield of ~0.35% when dispersed in cyclohexane and excited with a power density of 150 W cm-2, underlining their high quality. A comparison of the colloidal stability and luminescence properties of these UCNPs, subsequently surface modified with ligand exchange or encapsulation protocols, revealed that the ratio of the green (545 nm) and red (658 nm) emission bands determined at a constant excitation power density clearly depends on the surface chemistry. Modifications relying on the deposition of additional (amphiphilic) layer coatings, where the initial oleate coating is retained, show reduced non-radiative quenching by water as compared to UCNPs that are rendered water-dispersible via ligand exchange. Moreover, we could demonstrate that the brightness of the upconversion luminescence of the UCNPs is strongly affected by the type of surface modification, i.e., ligand exchange or encapsulation, yet hardly by the chemical nature of the ligand.
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.