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Eingeladener Vortrag
- nein (985)
Original equipment manufacturers (OEMs) and end-users perceive 'Zero Wear' differently. The 'Zero Wear' approach will be put into a general relation for different applications and illuminated by individual paths, either based on monolithic materials, thin film coatings or alternative base oils, featuring triboactive materials and lubricious oxides for tribological engine components and dry running foil bearings or specific DLC, ta-C and novel Zirconium-based thin film coatings for concentrated contacts above FZG 14 and alternative engine oils (NoSAP & bio-no-tox). The associated tribometric test equipments for these examples will also be detailed.
Exclusion from Class 1
(2011)
UN 6(d) Test Results
(2011)
Inspired by the globule arc technique a new electrothermal vaporization inductively coupled plasma optical emission spectrometry (ETV-ICP OES) method was developed for the analysis of high-purity copper materials. The performance of the method was investigated for the analytes Ag, Al, As, Bi, Cd, Co, Cr, Fe, Mg, Mn, Ni, P, Pb, S, Sb, Se, Si, Sn, Te, Ti, Zn and Zr. ETV parameters were optimized regarding the release of the analytes, the transport efficiency and the quality of analytical results in terms of precision, trueness and power of detection. The influence of CCl2F2, CHClF2, C2H2F4 and CHF3 as gaseous halogenation modifiers was investigated. A sufficient in situ analyte matrix separation was achieved by using CHF3 as halogenating reagent avoiding a high matrix input from the molten copper sample into the ETV system and the plasma. A complete release from the samples was obtained for all investigated analytes except Se and Te. Acceptable results for the determination of the trace elements Ag, Al, As, Bi, Cd, Co, Cr, Fe, Mg, Mn, Ni, P, Pb, S, Sb, Si, Sn, Ti, Zn and Zr in high-purity copper were achieved. The method includes a preceding sample preparation step of oxidizing the surface of copper samples which results in a significantly enhanced sensitivity. In addition to the calibration with copper samples, the feasibility of the calibration with liquid multi-element solutions was investigated. Except for Ag, Mg and Ni all analytes could be analyzed using aqueous calibration solutions. The trueness of the method was tested by the determination of analyte contents of certified reference materials. Limits of quantification ranging from 0.6 ng g-1 to 29 ng g-1 were achieved. The developed direct solid sampling method is time and cost effective and well suited for the characterization of high-purity copper materials. The method can be automated to a large extent and is applicable for processes accompanying analyses. In contrast to all other investigated trace elements, Se and Te were not released from the matrix at measurable levels under the used conditions. The determination of these elements is still under investigation and will be reported in a succeeding publication.
Different types of lasers are used nowadays for a number of technological Solutions, Modem high power solid-state lasers with high brightness of Radiation like Fiber or disc lasers find ever more applications in welding technology. Apart from the replacement of the CC>2-iasers traditionaHy used fcr these purposes, they provide new technological possibilities of metal treatment, such as using industrial robots and remote welding with high power laser radiation. The possibility of flexible optical fiber delivery of the radiation to any point gives a great technological advantage and permits welding processes to be realized with complicated weld seam geomelries and different positions using a minimum of additional fixtures. The short wavelength of the high power solid state lasers (1.07 ’m) causes another advantage. The coefflcient of inverse 170
Bremsstrahlung absorption from free electrons in plasma for such radiation is about 100 times lower than for the COi-iaser radiation. Owing to this fact, using the solid state lasers allows it to avoid a negative influence of the welding plume.
However, a short wavelength can lead to another kind of laser Radiation attenuation, which is connected with the formation of a cloud consisting of small metal particles that absorb and scatter laser radiation. This cloud arises due to the condensation of hot metal vapor by flying out from the deep Penetration channel and broadening in relatively cold atmosphere over the metal Surface.
Some theoretical and experimental approaches were made in advance in Order to estimate the influence of the Condensed particles on laser radiation and welding quality.
In this paper a systematic study including the determination of the Cloud size and its dynamical characteristics is presented. The results were obtained within the scope of the first stage of the metal vapor condensation process Investigation during welding with high power fiber lasers.
Coda wave interferometry is a recent analysis method now widely used in seismology. It uses the increased sensitivity of multiply scattered elastic waves with long travel-times for monitoring weak changes in a medium. While its application for structural monitoring has been shown to work under laboratory conditions, the usability on a real structure with known material changes had yet to be proven. This article presents experiments on a concrete bridge during construction. The results show that small velocity perturbations induced by a changing stress state in the structure can be determined even under adverse conditions. Theoretical estimations based on the stress calculations by the structural engineers are in good agreement with the measured velocity variations.
Dealing with first corrosion screening experiments to predict the reliability and safety of Germanys first Carbon Capture and Storage site in the northern Bassin of Germany, northwest of the Capital Berlin, laboratory experiments have been established to simulate the particular conditions at T=60 °C, highly saline aquifer water similar to 'Stuttgart Aquifer', but only at ambient pressure. With mounting 2 independent full 2-grade titanium autoclave systems (running up to 250 bar and 300 °C) pressures up to p=100 bar are possible. In 2010 a specific corrosion chamber of 2-grade titanium working up to 100 °C, flowing aqui fer water with different gas mixtures was designed to fit to a high cycle fatigue testing machine. Long term fatigue experiments simulating fatigue crack growth under corrosive environments will soon start. These experiments may not only help engineering a CCS site, but results can be used to improve the maintenance of geothermal energy production sites, especially moved parts such as pumps and shafts.
The CCS technique involves the compression of emission gasses in deep geological layers. To guarantee the safety of the site, CO2-corrosion of the injection pipe steels has to be given special attention when engineering CCS-sites. To get to know the corrosion behaviour samples of the heat treated steel 1.72252CrMo4, used for casing, and the stainless injection-pipe steel 1.4034 X46Cr13 were kept at T=60 °C and ambient pressure as well as p=100 bar for 700 h - 8000 h in a CC 2-saturated synthetic aquifer environment similar to possible geological on-shore CCS-sites in the northern German Basin. The isothermal corrosion behaviour obtained by mass gain of the steels in the gas phase, the liquid phase and the intermediate phase gives surface corrosion rates around 0.1 to 0.8 mm/year at ambient pressure and much lower about 0.02 to 0.2 mm/year at 100 bar where the CO 2 is in its supercritical state. Severe pit corrosion with pit heights around 4.5 mm are only located on the 42CrMo4 steel. Main phase of the continuous complicated multi-layered carbonate/oxide structure is siderite FeCO 3 in both types of steel.
Honeycombs/compaction faults occur in the concrete structures due to improper solidification of the concrete, which may reduce the strength of the concrete and also act as a passage for the water/acids that further corrodes the reinforcements. This paper explores about the acoustic pulse-echo techniques for the detection of honeycomb defects in a laboratory specimen located at the Federal Institute for Materials Research and Testing (BAM), Berlin. Since concrete is an inhomogeneous medium, the defect Signals are masked by the material noise due to large amount of scattering/ reflections of acoustic waves. A filtering method using the discrete wavelet transforms is applied on the ultrasonic time Signals for the better localization of defects.
The main wood degraders in aerobic terrestrial ecosystems belong to the white- and brown-rot fungi, where their biomass can be created on wood decay only. However, total sulfur (S) concentration in wood is very low and only little is known about the different sulfur compounds in wood today. Sulfur-starved brown-rot fungi Gloeophyllum trabeum and Oligoporus placenta were incubated on sterilized pine wood blocks whereas Lentinus cyathiformis and the white-rot fungi Trametes versicolor were incubated on sterilized beech wood blocks. After 19 weeks of incubation, the S oxidation status was analyzed in wood, in degraded wood, and in biomass of wood-degrading fungi by synchrotron based S K-edge XANES, and total S and sulfate were quantified. Total sulfur and sulfate content in pine wood blocks were approximately 50 and 1 µg g-1, respectively, while in beech wood approximately 100 and 20 µg g-1 were found, respectively. Sulfur in beech was dominated by sulfate-esters. In contrast, pine wood also contained larger amounts of reduced S. Three out of four selected fungi caused a reduction of the S oxidation state in wood from oxidized S (sulfate-ester, sulfate) to intermediate S (sulfonate, sulfoxide) or reduced S (thiols, e.g., proteins, peptides, enzyme cofactors). Only O. placenta shifted thiol to sulfonate. Growth experiments of these fungi on selective minimal media showed that in particular cysteine (thiol), sulfonates, and sulfate enhanced total mycelium growth. Consequently, wood-degrading fungi were able to utilize a large variety of different wood S sources for growth but preferentially transformed in vivo sulfate-esters and thiol into biomass structures.
The presently active standards on Computed Radiography (CR) need a major revision. It was observed by many users that the image quality for class B of EN 14784-2 is not achievable under the same exposure conditions as used for film exposure. A mathematical model was developed and tested, which allows the calculation of the image quality, proven by image quality indicators (IQI), depending on the fixed pattern noise and the efficiency of the used imaging plate (IP) scanner system. All tested IP scanner systems provide a fixed correlation between the measured signal/noise ratio (SNR) and the grey values in the digital images. The maximum achievable SNRmax depends on the fixed pattern noise of the plate (high dose limit). Depending on the exposure dose an optimum visibility of IQIs can be predicted by calculation and measured considering the attenuation coefficient for calculation of the contrast/noise ratio (CNR). The diameter of the just visible wire is proportional to 1/sqrt(CNR). The optimum tube voltage for best visibility of IQIs and maximum CNR depend on the exposure dose. The optimum tube voltage for best visibility is achieved only at exposures with high dose. A dose dependant optimal tube voltage was not observed for film radiography.
Digital image analysis
(2011)
Comparatiye digital analysis was performed on the five moon drawings from the New York copy of the Sidereus Nuncius and the copperplate etchings printed in the Graz and Florence copies. The sequences of figures for the drawings on pages 8r, 9v and lOv demonstrate the process of digitally enhancing the black material on the drawings, isolating that material and then overlaying it on the etchings. Using an image editing program (Image Pro® Plus by Media Cybernetics) the black material on the drawings and the letterpress-printed text were isolated and segmented from the brown drawing media. As shown in Figs. 4, 6 and 8, the isolation was possible and the black material clearly overlaps the demarcation line in the drawings. To compare the drawn and printed images of each moon, the images were laid on top of each other with Adobe Photoshop® (Adobe Systems). In these images, the printed text was used for alignment and scale. By decreasing the opacity of the image on top, the lines of each image were compared. This technique revealed an almost one-to-one correlation between the demarcation line in the drawing (as indicated by the black material) and that on the etching. In each case, the similarities and concurrences by far outnumbered the minor deviations in line. One precondition of this work was that all the photographs be at the same angle, plane-parallel, so that the drawings could be compared with the etchings. A slight aberration in the plane could distort the geometry of the illustrations. Rectification of the image plane was carried out by means of the program metigo® MAP 2.2 (Fokus GmbH Leipzig). To validate the method, photographs from the same detail of the New York copy taken with different photographic cameras and different Parameters were rectified with metigo® MAP and compared in Adobe Photoshop®. The overlay of these photographs shows a good correlation in the layout of the lettering and moon figures with only small aberrations. The distribution of the black material on the drawings can be followed as clearly in the rectified photographs as in the unrectified photographs, the information is the same.
Biozide & Kulturgüter
(2011)
COORAL Teilprojekt MINIRISK
(2011)
Deliberate and accidental exposure of the ecosystem including humans to nanoparticles becomes inevitable as nanomaterials are increasingly used. In biological fluids, biomolecules associate with nanoparticles, leading to the formation of a dynamic biomolecule “corona” that critically defines the biological identity of the particle. As the bio-physical properties of such a decorated particle often differ significantly from those of the formulated particle a detailed characterization of nanoparticles in biological environments becomes increasingly important though, nevertheless also technically challenging. Here, we introduce experimental methods currently employed for nanoparticle characterization, present examples underlining the complexity of the nano-bio interface, and discuss the need for further technical and conceptual developments. A deep and mechanistic bio-physical understanding of the nano-bio interface is a challenge but also fundamental prerequisite for future applications in nanobiology, nanomedicine and nano(eco)toxicology.
Bericht aus dem Akkreditierungsbeirat: Ermittlungsprozess, ermittelte Regeln und weiteres Vorgehen
(2011)
Instrumented measurements on radioactive waste disposal containers during experimental drop testing
(2011)
In context with disposal container safety assessment of containers for radioactive waste the German Federal Institute for Materials Research and Testing (BAM) performed numerous drop tests in the last years. The tests were accompanied by extensive and various measurement techniques especially by instrumented measurements with strain gages and accelerometers. The instrumentation of a specimen is an important tool to evaluate its mechanical behavior during impact. Test results as deceleration-time and strain-time functions constitute a main basis for the validation of assumptions in the safety analysis and for the evaluation of calculations based on finite-element methods. Strain gauges are useful to determine the time dependent magnitude of any deformation and the associated stresses. Accelerometers are widely used for the measuring of motion i.e. speed or the displacement of the rigid cask body, vibration and shock events. In addition high-speed video technique can be used to visualize and analyze the kinematical impact scenario by motion analysis. The paper describes some selected aspects on instrumented measurements and motion analysis in context with low level radioactive waste (LLW) container drop testing
Instrumented Measurements on Radioactive Waste Disposal Containers During Experimental Drop Testing
(2011)
CCQM (Consultative Committee for Amount of Substance - Metrology in Chemistry) is an international body of the Meter Convention (BIPM) established as a framework of National Metrology Institutes running inter-laboratory of comparisons to demonstrate the international comparability of chemical measurements, with traceability to international or national reference standards. In 2003 the surface analysis working group (SAWG) was established at CCQM and since then several inter-laboratory comparisons in the field of EPMA have been carried out. In many cases the EPMA results deviated significantly from each other and the expanded uncertainties were greater than expected. Both methods EDS and WDS were employed. However, light elements such as carbon and nitrogen were the major elements analyzed and it is known that the corresponding lowenergy characteristic X-ray lines are more challenging to quantify by EPMA than the higher energy lines of elements with higher atomic numbers. Moreover, the standards selected and their qualities were variable, the quantification models were different, and the acquisition parameters were not specified sufficiently in the analysis instructions.
It is a latent wish of any SEM/EDS (scanning electron microscope with an energy dispersive spectrometer) analyst to “see more” of the analyzed specimen, i.e. to improve the existing analytical figures of merit.
One key issue are the relatively poor limits of detection (not below 0.1 mass-%) provided by energy dispersive X-ray spectrometry (EDX) with the conventional electron excitation (ED-EPMA). This is a consequence of relatively low peak-to-background ratios and reduced energy resolution when compared to wavelength dispersive spectrometry (WD-EPMA). Recent technological developments make possible to equip the SEM with a wavelength dispersive spectrometer (WDS), so that
significantly better energy resolution can be attained. Also a relative new product that can be easily attached to a SEM/EDS system is a micro-focus X-ray source. Hence, it is possible to perform (micro-focus) X-ray fluorescence spectrometry (μ-XRF) and take advantage of the enhanced peak-to-background ratios (well suited for trace analysis). However, there are also some disadvantages: an increased measurement time and excitation with a high current in the 10s of nA range are usually required for WDS. μ-XRF provides more bulk information and poor limits of detection for light elements. By combining the advantages of these analytical techniques “seeing more” becomes possible.
Simple procedures for specifying and checking the performance of energy dispersive X-ray spectrometers (EDS) have been since 2002 available in form of the international standard ISO 15632:2002 [1]. When specifying their spectrometers all major EDS manufacturers refer meanwhile to this standard. Main spectrometer parameters such as energy resolution can be determined as recommended in there. Just several years ago the Si-Li detector has been the mostly widespread type of detector. Since four-five years, silicon drift detector (SDD) EDS providing comparable (in many cases even better) energy resolutions at much higher count rates than the conventional Si-Li’s have got the breakthrough on the market.
Drop and fire testing of spent fuel and HLW transport casks at 'BAM test site technical safety'
(2011)
BAM, as a competent German government institute for the mechanical and thermal testing of radioactive material transport and storage containers, operates unique drop and fire test facilities for experimental investigations on the open air BAM Test Site Technical Safety. To be able to perform even drop tests with full scale spent fuel or HAW casks (i.e. the German CASTOR cask designs), BAM constructed in 2004 a large drop test facility capable to handle 200 ton test objects, and to drop them onto a steel plate covered unyielding target with a mass of nearly 2600 ton. Drop test campaigns of the 181 ton GNS CONSTOR V/TC, the 129 ton MHI MSF-69BG and a 1:2 scale model of the GNS CASTOR HAW28M (CASTOR HAW/TB2) have been performed since then. The experimental BAM drop testing activities can be supported also by drop testing of smaller packages (up to 2 ton) in an in-house test facility and by dynamic, guided impact testing of package components and material specimen inside a new drop test machine. In May 2008, a new modern fire test facility was put into operation. The facility provides two test stands fired with liquid propane. Testing in every case has to be completed by computational investigations, where BAM operates appropriate finite element modelling on appropriate computer codes, e.g. ABAQUS, LS-DYNA, ANSYS and other analytical tools.
Fire testing is an essential part of the hypothetical, cumulative mechanical and thermal accident test conditions that shall guarantee package safety in severe accidents. Not only for radioactive material transport packages but also for other containments of dangerous goods, international standards require specific thermal load specifications. Following the guideline Safety in technology and chemistry' BAM, as a scientific and technical German federal government institute, operates a 12 km² large open air test facility for experimental investigations of dangerous goods and their containments. On an area beside the well-known 200-ton drop test facility, BAM has put into operation a new fire test facility. This facility provides two fire test stands that utilise liquid propane as fuel from a central, earth-covered 60m³ LPG storage tank. From that storage the propane is pumped via pipelines to the test stands where the gas is released from nozzles, and ignited by ignition burners. The fire exposure test facility areas are 12×8 m. Fire test facility B (with gas release nozzles submerged in a water pool) is designed for fire testing of containers that may burst during the test. Fire test facility A (with ring burner systems) is designed for heavy test objects up to 200 tons, e.g. for full-scale spent fuel casks. This paper presents a detailed description of the facility, insight into first tests performed, and results of calorimeter fire tests, using containers of various sizes, to verify the absorbed heat fluxes, demonstrating that regulatory fire test conditions are met, and that the propane fire is equivalent to a kerosene or heating oil pool fire.
In Zeiten knapper Kassen wird überall nach Wegen gesucht Kosten einzusparen. Im Bauwesen geht es dabei um Kosteneinsparungen ohne Reduktion der Sicherheit und Dauerhaftigkeit des Bauwerks. Beim Bauen im Bestand können mit einer zerstörungsfreien Prüfung von Bauwerken die Weiternutzung oder die erforderlichen Umbauten optimiert werden und so Kosten eingespart werden.
A large number of pharmacologically active compounds have been detected in the aquatic environment during the last decade [1] and this gives rise to many concerns [2]. The substances have been disclosed by accident, clever search or elaborate mass spectrometry. Nowadays a broad spectrum of drug parent compounds can be screened for [3], yet the knowledge about the presence of isomers and transformation products (metabolites, conjugates, degradates) is still limited.
The failure of laminates usually is initiated by the failure of the plies with the maximum transverse stresses. The failure of those plies generally reduces the load carrying capability of the laminate, even though they carry only a small part of the external load. The analysis of failure under off-axis stresses accordingly is essential for the prediction of the strength of laminates. This is taken into account in the "mechanisms based failure criteria" e.g. by Puck. Most of these inter fiber failure criteria are not based on the micromechanics of the failure process but on prescribed stress interaction functions. The failure of plies under transverse loading obviously is governed by the bond strength between fiber and matrix fiber. The interfacial debonding was studied e.g. by Paris et al. and Corea et al.. The bond strength between fiber and matrix usually is measured by using micromechanical tests e.g. pull-out, push-out or fragmentation tests. Stress analyses as well as fracture mechanical analyses show that the interfacial failure over a large range is dominated by shear stresses (Kim and Mai, Pisanova et al, Marotzke and Qiao). The stress distribution arising in those experiments however differs from the stresses acting in a lamina under transverse loading. In transverse failure of a lamina, radial stresses as well as shear stresses are dominating the failure process of the interface. In addition longitudinal shear stresses are present. Experimental work concerning off-axis loading of single fibers was done e.g. by Tandon and Kim and by Ogihara and Koyanagi. They studied the influence of the fiber alignment by using a specimen in form of a cruciform with skew wings.
This paper demonstrates exemplarily how numerical and experimental approaches can be combined reasonably in mechanical assessment of package integrity according to the IAEA regulations. The paper also concentrates on the question about how static mechanical approaches can be applied, and what their problems are in relation to dynamic calculation approaches. Under defined impact tests, which represent accident transport conditions, the package has to withstand impact loading, e.g. resulting from a 9 m free drop onto an unyielding target in sequence with a 1 m puncture drop test. Owing to the local character of the interaction between the puncture bar and the cask body, it is possible to develop a dynamic numerical model for the 1 m puncture drop which allows an appropriate simulation of the interaction area. Results from existing experimental drop tests with prototype or small scale cask models can be used for verification and validation of applied analysis codes and models. The link between analysis and experimental drop testing is described exemplarily by considering a regulatory 1 m puncture bar drop test onto the cask body of a recently approved German high level waste transport package. For the 9 m drop test of the package, it is difficult to develop a dynamic numerical model of the package due to the complexity of the interaction between cask body, impact limiters and unyielding target. Dynamic calculations require an extensive verification with experimental results. The simulation of a 9 m drop of a package with impact limiters is thereby often more complex than the simulation of a 1 m puncture drop onto the cask body. A different approximation method can be applied for the consideration of dynamic effects on the impact loading of the package. In a first step, maximum impact force and rigid body deceleration of the cask body during the impact process can be calculated with simplified numerical tools. This rigid body deceleration can subsequently be applied on a verified static numerical model. Dynamic effects, which cannot be covered by the static numerical analysis, have therefore to be considered by using an additional dynamic factor. The paper describes this approach exemplarily for a 9 m horizontal drop of a typical spent fuel cask design.
The extremely low acoustic impedance of polypropylene ferroelectret combined with its piezoelectric properties makes this material suitable for construction of aircoupled ultrasonic transducers for non-destructive testing. For the fabrication of transducers with a stable quality, the reproducibility of their key parameters is of interest.
The reproducibility was evaluated by means of (i) impedance spectroscopy and (ii) pulse-echo measurements. (i) Impedance spectroscopy was applied to identify the resonance frequency, the coupling factor and the acoustic impedance of several nominally identical transducers. (ii) Pulse-echo measurements yielded the signal form of these transducers.
The variation of the signal amplitude measured with pulseecho technique was about 10 dB. A part of this variation Comes from the deposition of transducer electrodes and another part from local variations of ferroelectret properties. The variation of the signal amplitude was caused by the observed variation of the coupling factor, which was also about 10 dB. The variation of the acoustic impedance was only about 1 dB, thus having no effect on the variation of the signal amplitude.
These results indicate that the variability can be reduced by improving the control of electrode deposition and by optimizing the production technology affecting the reproducibility of material properties.
Charakterisierung der Wandler für Luftultraschallprüfung aus zellulärem Polypropylen-Ferroelektret
(2011)
In den letzten Jahren stieg die Anfrage für zerstörungsfreie Prüfung (ZIP) mit Luftultraschall deutlich. Die klassische ZfP mit Ultraschall nutzt Flüssigkeiten als Koppelmittel zwischen dem Wandler und dem Prüfkörper. Für die Prüfung von Gegenständen mit empfindlicher Oberfläche, die das Koppelmittel beschädigen oder verunreinigen kann, ist deswegen Luftultraschall besser geeignet. Eine mögliche Anwendung ist beispielsweise der Nachweis von Delaminationen in glas- und kohlefaserverstärkten Verbundwerkstoffen sowie Sandwichbauteilen, die in der Luftfahrt- und der Automobilindustrie eingesetzt werden.
Caffeine (1,3,7-trimethylxanthine) and coprostanol (5β-cholestan-3β-ol) were detected in samples of Berlin's surface water. Their concentrations correlated with the contamination status of the samples, suggesting their usefulness as markers of human activity. Remarkably, caffeine concentrations were always well above the limit of quantitation of 0.025 µg/L.
In order to screen surface water samples in larger series, the development of two novel methods was required: a monoclonal antibody-based immunoassay for caffeine and a dispersive liquid-liquid microextraction (DLLME) method, followed by liquid chromatography tandem mass spectrometry (LC-MS/MS) for coprostanol.
The caffeine immunoassay developed shows the best analytical limit of detection (LOD) obtained so far for caffeine (0.001 µg/L), allows high-throughput analysis, and does not require sample pre-treatment. The assay was also successfully employed to measure caffeine in beverages, shampoos, caffeine tab-lets, and human saliva.
Antibodies to coprostanol are not commercially available. A new strategy to generate anti-coprostanol antibodies was elaborated using an analogous com-pound as hapten – isolithocholic acid (ILA) – and immunizing a group of mice. A polyclonal anti-ILA serum was produced, which binds coprostanol but the low affinity did not permit setting up an immunoassay to measure environmental concentrations of the analyte (in the range of ng/L).
Specific anti-ILA immunoglobulin G were also found in the faeces of the immunized mice.
Coprostanol was quantified in the water samples using a newly developed LC-MS/MS method using atmospheric pressure chemical ionisation (APCI). Concentrations above 0.1 µg/L were determined after sample preconcentration using DLLME. This extraction method also proved to be successful for enrichment of coprostanol-related compounds such as cholesterol, cholestanol, cholestanone, ergosterol, and stigmasterol.
IGUS is the International Group of Experts on the Explosion Risks of Unstable Substances. IGUS was established in 1962 with the objective to harmonize test methods used by different countries to identify and quantify the explosive properties of unstable materials. Over the years, IGUS has continued to offer scientists, who are advisers to their governments, and others, a forum to exchange data and information. The Energetic and Oxidizing Substances (EOS) working group as a sub-group of IGUS is dealing with test methods, Classification and safety aspects relating to organic peroxides, self-reactive substances and other energetic substances, fertilizers, ammonium nitrate and oxidizers.
The EOS working group holds an annual meeting alternating between Europe, the United States and Japan. The 2011 meeting took place from the 27th to the 29th of April 2011 at the Madison Hotel in Washington, D. C. The meeting was hosted by the Organic Peroxide Producers Safety Division (OPPSD) of the Society of Plastics Industry, Inc. (SPI). This was the fourth EOS meeting held in the USA since 1994. Of particular importance is the fact that 39 colleagues from authorities, universities, research institutes and industries attended the meeting. The delegates came from USA, Canada, China, France, The Netherlands, Norway, Sweden, Italy, Japan, United Kingdom and Germany. This confirms the breadth and scope of this forum and the value the participants associate with being able to contact other colleagues from around the world enabling the effective exchange of scientific results and discussion on the wide-ranging Problems concerning energetic and oxidizing materials.
Under environmental conditions water exists in all three classical States of matter: solid, liquid and gas. The water molecule is non-linear and therefore polar. In comparison with other liquids water has anomalous features; about 63 exceptional properties are recorded. This article starts with reviewing properties of water, typical occurrences and definitions such as relative and absolute humidity and moisture content.
Water is present everywhere in nature and engineering; it may be helpful or harmful. The survey concerns both: atmospheric hygrometry and usual measuring methods of the moisture content of solids and liquids as well as water Sorption. The determination of the atmospheric humidity is among the more difficult problems in metrology. In contrast, humidity determination of materials is simple; however the definition of the dry state is difficult. Because water is bound at and in solids and liquids in many different ways it tums out that the humidity content of materials is difficult to define and to measure accurately. We provide a survey on the measuring methods, describe the most important ones and discuss advantages and accuracy.
In the search for extraterrestrial water special remote measuring methods have been developed analysing the spectrum of electromagnetic radiation either of natural sources or produced by a probe and reflected. Spacious deposits have been detected photographically. In situ investigations are made using conventional methods.
With regard to the problems of measurements, Standardisation of measuring methods and procedures is required. There exist many institutions, which are engaged in investigating the use of water and standardising measuring methods. In tabular form, we give a survey on existing Standards.
This paper studies the dielectric dispersion of high frequency radar wave in concrete in early-aged and hardened concrete specimens. Frequency-dependent spectra of phase velocity ν(ω) were measured to deduce the spectra of real part of dielectric permittivity ε'(ω). The dispersion was measured by three high nominal ground penetrating radar frequencies (1.5, 1.6 and 2.6 GHz), experimenting on two steel bars with concrete cover 50 and 100 mm. It was found that ν(ω) and ε'(ω) dispersed at lower frequency, but became stable at high frequency regions, which agrees with the classical GPR plateau. The same frequency components at different nominal antenna frequencies show a close range of ν(ω) and ε'(ω) in concrete of different ages. The results in this paper warrant further investigation of using GPR wave to study material properties.
Using ground penetrating radar and time-frequency analysis to characterize construction materials
(2011)
For decades, applications of nondestructive evaluation-civil engineering (NDE-CE) focus on object identifications (such as steel bars, tendon ducts and backwall reflections) in infrastructures. Because of the advantage of efficient visualization of internal structure, utilization of these methods can probably be extended to material characterization (MC) of aging and adversely exposed infrastructures. However, two factors yield a big gap between NDE and MC. First, for the ease of visualization, the primary focus of NDE-signal processing is object identification, which usually alters the originality of the signal. Second, there is lack of relationship and inverse models bridging the NDE-derived and conventional material properties compared to other disciplines of science, such as geophysics. These disadvantages make laboratory and field-scale NDE-MC still a far-reaching holy grail and is possibly the greatest hurdle to be regularly adopted in CE structures. This paper attempts to address this gap from object identification to MC using ground penetrating radar (GPR) as one of the most frequently used NDE-CE methods, and signal processing with joint timefrequency domain (JTFA) analysis. Three examples of material property characterization regarding the individual effects of steel bar corrosion in concrete, hydration and moisture content distribution of construction materials are given.
In order to reduce experimental effort, tribological tests are performed for coating selection, simulating the friction, wear and scuffing behaviour between the piston ring and cylinder liner, as well as lubricant evaluation. The creation of test standards in piston ring/cylinder liner simulation is discussed. PVD coatings, HVOF coatings and nitriding treatments have been applied to piston rings as alternative for chromium coatings. CrN/TiN coating seems very effective for increasing the wear and scuffing resistance. Biodegradable engine oils based on esters and polyglycols reduce friction and exceed the wear resistance of reference engine oils based on hydrocarbons for the new generation engines with high cylinder pressures.
Die industrielle Computertomographie (CT) ist ein gut bekanntes Verfahren zur zerstörungsfreien Prüfung von Werkstücken. In den letzten Jahren wird die CT aber zunehmend auch für dimensioneile Messungen von Werkstücken eingesetzt. Der wesentliche Vorteil der CT liegt in der Kompletterfassung mit hoher Messpunktdichte, die auch für andere Messverfahren unzugängliche, innere Geometrien einschließt. An kleinen Bauteilen können Strukturen bis herunter zu wenigen Mikrometern gemessen werden, wodurch sich das Verfahren gut für die Messung von Mikroteilen eignet. Nachteilig ist, dass viele Einflussgrößen das Messergebnis beeinflussen, was die Rückführung der Messergebnisse, die Bestimmung der Messunsicherheit und die Definition von Spezifikationen für CT-Anlagen erschwert.
Der Beitrag stellt nach einer Einführung in das Verfahren Anwendungsbeispiele der CT an Mikroteilen vor. Darüber hinaus geht der Beitrag auf Prüfkörper und -verfahren zur Einmessung und Überprüfung von CT-Anlagen ein und berichtet über aktuelle Normungsaktivitäten. Abschließend werden Möglichkeiten zur weiteren Steigerung der Auflösung aufgezeigt, um zukünftig möglicherweise auch Nanogeometrien messen zu können.
The Final Gravettian level (level 2) of the abri Pataud (Dordogne, France) yielded a large assemblage of body ornaments that consists essentially of 85 quite standardized rectangular beads. Some uncertainty remained about the raw material in which these small beads were made: mammoth ivory, reindeer antler or bone? Non-invasive methods were employed in order to determine the raw material. First chemical analyses using microbeam Proton Induced X-ray Emission analysis (microPIXE) did not enable us to conclude definitively. Therefore, synchrotron and laboratory X-ray microtomography (microCT) were applied on eight beads and allowed us to identify ivory for all of them except for one, which shows slightly different morphological features.
This study reports three new crystalline aluminum isopropoxide oxide fluorides with molar ratios of Al:F equal to 1:1 and 1:1.25. These are the first three representatives isolated without the incorporation of external donor molecules. Compound 1 Al4F4(µ4-O)(µ-O'Pr)5[H(O'Pr)2] contains a tetranuclear unit consisting of two different five fold coordinated AlFO4-units, with F exclusively in the terminal position. Compound 2, Al4F4(µ4-O)(µ-O'Pr)5[H(O'Pr)2]·Al5F5(µ5-O)(µ-O'Pr)8, contains both a tetranuclear unit (as in 1) and a pentanuclear Al-unit. Al-atoms in the latter are five- and six fold coordinated. Compound 3, Al16F20(µ4-O)4(µ-O'Pr)20·2('PrOH), exhibits a slightly higher fluorination degree and contains an oligomeric chain of four F-linked tetranuclear Al-units. In addition to X-ray structure analysis, compound 1 was characterized by different solid state MAS NMR techniques, including 27Al triple quantum MAS NMR and 1H, 1H→13C CP, 19F and 27Al MAS NMR. On the basis of the collected data, a reliable decomposition of 27Al single pulse MAS NMR spectra and an unambiguous assignment of the resonances to the respective structural AlFO4-units are given. The new crystalline aluminum isopropoxide oxide fluorides are direct evidence of the fluorolytic sol–gel mechanism previously discussed.
This study proposes a new guideline for designing biodegradable apatite ceramics. Boron-containing hydroxyapatite (BHAp) particles were prepared by a high-temperature solid-state reaction processing method and were characterized in terms of their chemical composition, apatite lattice defects and in vitro biodegradability. Solid-state nuclear magnetic resonance analysis showed that boron-incorporation into hydroxyapatite (HAp) derived by thermo-chemical reactions between borate and calcium phosphate phases led to disordered phases (BCaP) of a CaO–P2O5–B2O3–OH system covering the crystalline HAp core. X-ray diffraction analysis indicated that the BCaP phase must consist mainly of a crystalline oxyboroapatite (OBAp) phase. An in vitro biodegradability test showed that BHAp degraded quicker than HAp or ß-tricalcium phosphate. The biodegradability of BHAp particles can be controlled by boron incorporation into a HAp lattice leading to the formation of a disordered OBAp phase.
Eine stets optimale Nutzung von Anlagen, Rohstoffen und Energie in Verbindung mit einer guten Prozessführung sind die wichtigsten Voraussetzungen für globale Wettbewerbsvorteile der Chemisch Pharmazeutischen Industrie und für die Branchen Energieerzeugung, Petrochemie, Nahrungsmittel, Papier- und Zellstoff oder Wasserversorgung. Überlegene Verfahren erfordern die fortwährende Kontrolle der geforderten Produktqualität, ihre präventive Sicherstellung und eine ständige Verbesserung des Wissens über den Prozess. Sensoren helfen dabei, alle wichtigen Messgrößen an kritischen Stellen transparent zu machen.
Sie sind die 'Sinnesorgane der Prozessleittechnik' für automatisierte Verfahren. Allein aufgrund stetig wachsender Anforderungen an Sensoren ergibt sich für viele Messaufgaben die Notwendigkeit einer ständigen Verbesserung der Sensoren. Für völlig neue Aufgaben müssen jedoch neue Messprinzipien gefunden werden, weil heute noch keine Sensor-Technologie existiert oder die wachsenden Anforderungen nicht mehr allein durch Weiterentwicklung bestehender Technologien erfüllt werden können.
Ende 2009 wurden Anforderungen und Wege für die konsequente Weiterentwicklung und Verbesserung von Prozess-Sensoren aus Anwendersicht aufgeschrieben. Das Projekt wurde von NAMUR und GMA initiiert und gemeinsam mit Industrieanwendern und Geräteherstellern als Technologie-Roadmap 'Prozess-Sensoren 2015+' veröffentlicht.
Was ist aus den Wünschen seither geworden? Wie kann die Umsetzung dieser Entwicklungsziele von den Geräteherstellern wirtschaftlich und marktgängig erfolgen? Wie werden neuartige Forschungsziele mit der angemessenen Forschungsförderung am besten vorangebracht?
Within the framework of the G8 partnership, the German Ministry of Economics and Technology has been realizing a 300 EUR million project of the storage of decommissioned Russian nuclear submarines based on a German-Russian agreement. The main parts of the project are the construction of the long-term storage facility as well as a radioactive waste storage facility at Sayda Bay. Long-term interim storage facility for this particular case has a period of about 70 years. The Energiewerke Nord GmbH (EWN) under the technical controlling of BAM carried out the project management. Foremost in this presentation is the finalization of the long-term storage facility for nuclear submarine compartments and the planning and realization of the radioactive waste storage building with special emphases of the parts carried out by BAM. Because BAM staff cannot stay permanently on site, a random inspection of different topics was the bases for the activities of BAM. The key aspects of activities are the long-term storage of the nuclear compartments, maintenance building, the decommissioning of the compartments and the transportation of the very heavy weight compartments (1600 metric tons). Details relating of the progress of the construction work as well as information about technical recommendations will also be briefly illustrated. Within this scope, problems and difficulties during the construction of the storage facility as well as logistical challenges including transportation of the reactor compartments will also be discussed.
Aus wirtschaftlich-technischer Perspektive ergeben sich in den letzten zehn Jahren hinsichtlich der Werkstoffinnovation und -auswahl für geschweißte Rohrleitungen im Wesentlichen zwei Entwicklungsrichtungen:
Im Bereich der niedriglegierten Stähle werden immer höher festere Feinkombaustähle mit Streckgrenzen von inzwischen über 900 MPa verwendet. Wirtschaftliches Ziel ist hierbei eine möglichst hohe Kosteneinsparung durch Reduktion der Wanddicke.
Für korrosionsbeanspruchte Komponenten, unter anderem im Petrochemie- und Energieanlagenbau besteht das wirtschaftliche Ziel primär darin, eine höhere Kosteneinsparung durch neue Legierungskonzepte zu erzielen und zwar möglichst so, dass bei mindestens gleicher Festigkeit auf die Verwendung von teuren Elementen, wie beispielsweise Nickel, verzichtet werden kann. Beispiele hierfür sind insbesondere hochlegierte martensitische Cr-V-Stähle, supermartensitische Stähle, Lean-Duplexstähle, superaustenitische Stähle und austenitische Cr-Mn-Stähle.
Für einige der neu eingeführten Grundwerkstoffe sind die Zusatzwerkstoffe noch in der Entwicklung. In jedem Fall stellen diese Werkstoffinnovationen besondere Ansprüche hinsichtlich einer Rissvermeidung während der schweißtechnischen Verarbeitung, um von vornherein riss- bzw. fehlerfreie Rohrleitungen herzustellen, die eine hohe Sicherheit gegen ein Versagen während der Inbetriebnahme und im Verlauf der vorgesehenen Lebensdauer aufweisen. Fast alle dieser neu eingeführten Rohrleitungswerkstoffe weisen eine reduzierte Heiß- oder Kaltrissresistenz vor allem während des Schweißens mit modernen Hochleistungsprozessen, bspw. Laserhybridschweißen, auf. Dabei besteht nach wie vor Forschungsbedarf hinsichtlich der jeweiligen Entstehungsmechanismen. Da es in den letzten zehn Jahren immer häufiger zu Produktionsausfällen und Schadensfällen mit teilweise katastrophalen Konsequenzen gekommen ist, werden die Ursachen und die Vermeidung fertigungsbedingter Heiß- und Kaltrisse im Folgenden zusammengefasst.
The formation of magnesium fluoride sols and xerogels according to the fluorolytic sol–gel synthesis based on the reaction of Mg(OMe)2 with non-aqueous HF has been thoroughly investigated by X-ray scattering (WAXS/XRD), TEM, SAXS, DLS and 19F MAS NMR spectroscopy. Mechanistic insights were gained by following the reaction progress and formation of intermediate phases of the fluorination of magnesium alkoxides. For F:Mg ratios of 0.3 and 0.4 the formation of two crystalline phases was observed containing the recently obtained compound [Mg6F2(OCH3)10(CH3OH)14] hexanuclear dicubane units. The stoichiometric reaction yields magnesium fluoride nanoparticles with crystallite sizes below 5 nm, which show broad reflections in the X-ray diffraction pattern. Metal fluoride sols prepared by this way undergo tremendous changes over the first several weeks after synthesis. Immediately after the fluorination, particles of about 120 nm—probably agglomerates—are formed, which break apart in the course of about one month of ageing and low-viscous, transparent sols with particles of about 12 nm are obtained. At the same time structural re-organisation processes within the magnesium fluoride particles are observed by an increase of the (110) reflection in WAXS.
The present contribution highlights recent trends in investigating hydrogen diffusion and cracking in steel welds. For such studies, supermartensitic stainless steels (SMSS) have exemplarily been selected. These materials have been used for offshore and marine constructions for about two decades now. They present a versatility of improved properties such as high strength to thickness ratio, good weldability and good corrosion resistance. However, as shown by respective failure cases, SMSS welds might become prone to hydrogen assisted cracking and the degradation phenomena are more easily to investigate due to the nearly homogeneous martensitic microstructure than in other materials. Generally, it has to be distinguished between cracking that occurs during or shortly after fabrication welding, or during subsequent operation of SMSS components. In order to achieve crack avoidance during fabrication and service, conclusive test sequences have to be applied, ranging from field tests at real components and full scale tests investigating the materials behavior under real service conditions to basic and small scale tests, such as tensile and corrosion tests, oriented more towards a materials ranking. Considerable testing of SMSS welds has been carried out and the present paper particularly summarizes spotlights on 1:1 scale component testing of welded tubulars, slow strain rate testing and basic tests oriented to elucidate the hydrogen behavior and degradation in SMSS weld microstructures. Also, permeation tests, hydrogen dependent degradation of mechanical properties and thermal desorption spectroscopy are adressed. As a specific item, first results of lately conducted investigations for tracking hydrogen movement in such weld microstructures by using high energy synchrotron radiation are elucidated.
Schadensfälle in den letzten zehn Jahren mit teilweise katastrophalen Folgen belegen, dass der Vermeidung von Rissen beim Schweißen von Rohrleitungen besondere Aufmerksamkeit zu schenken ist. In der Analyse solcher Schäden ist zu unterscheiden, ob die Risse bereits während oder kurz nach der schweißtechnischen Fertigung der Rohrkomponenten oder während des anschließenden Betriebes entstanden sind. Im vorliegenden Beitrag wird sich vor allem auf die Vermeidung einer Heiß- und Kaltrissbildung beim Schweißen von Rohrleitungen konzentriert und es werden weitere Forschungsperspektiven abgeleitet.
Die hier vorgestellten Untersuchungen dienen der Erweiterung des Anwendungsbereiches für reaktive Brandschutzsysteme auf Stahlbauteilen im nationalen Zulassungsverfahren.
Für die Wirksamkeit reaktiver Brandschutzsysteme ist die Haftfähigkeit der reaktiven Brandschutzbeschichtung auf dem Untergrund (Stahl) von entscheidender Bedeutung. Die Haftfähigkeit der Beschichtung ist neben der Oberflächenbeschaffenheit und den Eigenschaften des reaktiven Systems selbst im Wesentlichen von der Form des Bauteils und den sich im Brandfall einstellenden erformungen (Krümmungen und Dehnungen) abhängig.
The human factors approach relies on understanding the properties of human capability and limitations under various conditions and the application of that knowledge in designing and developing safe systems. Following the principles of the MTO (Man Technology Organisation) approach, emphasis should be given to the way people interact with technical as well as organisational systems.
A model describing human factor influences in relation to the performance shaping factors and their effect on manual ultrasonic inspection performance had been built and a part of it empirically tested. The experimental task involved repeated inspection of 18 defects according to the standard procedure under no, middle and high time pressure. Stress coping strategies, the mental workload of the task, stress reaction and organisational factors have been measured. The results have shown that time pressure, mental workload and experience influence the quality of the inspection performance. Organisational factors and their influence on the inspection results were rated as important by the operators. However, further research is necessary into the effects of stress.
Particles produced by previous laser shots may have significant influence on the analytical signal in laser-induced breakdown spectroscopy (LIBS) and laser ablation inductively coupled plasma (LA-ICP) spectrometry if they remain close to the position of laser sampling. The effects of these particles on the laser-induced breakdown event are demonstrated in several ways. LIBS-experiments were conducted in an ablation cell at atmospheric conditions in argon or air applying a dual-pulse arrangement with orthogonal pre-pulse, i.e., plasma breakdown in a gas generated by a focussed laser beam parallel and close to the sample surface followed by a delayed crossing laser pulse in orthogonal direction which actually ablates material from the sample and produces the LIBS plasma. The optical emission of the LIBS plasma as well as the absorption of the pre-pulse laser was measured. In the presence of particles in the focus of the pre-pulse laser, the plasma breakdown is affected and more energy of the pre-pulse laser is absorbed than without particles. As a result, the analyte line emission from the LIBS plasma of the second laser is enhanced. It is assumed that the enhancement is not only due to an increase of mass ablated by the second laser but also to better atomization and excitation conditions favored by a reduced gas density in the pre-pulse plasma. Higher laser pulse frequencies increase the probability of particle-laser interaction and, therefore, reduce the shot-to-shot line intensity variation as compared to lower particle loadings in the cell. Additional experiments using an aerosol chamber were performed to further quantify the laser absorption by the plasma in dependence on time both with and without the presence of particles. The overall implication of laser-particle interactions for LIBS and LA-ICP-MS/OES are discussed.
Es ist mittlerweile eine zunehmend bekannte Tatsache, dass „nichtrostende“ Stähle trotz ihres Namens rosten können. Werden die spezifischen Besonderheiten und Anforderungen, die sich beim Einsatz nichtrostender Stähle ergeben, aus Unkenntnis oder Nachlässigkeit nicht beachtet, kann dies zu unerwarteten Korrosionserscheinungen und auch zum funktionalen Versagen von Konstruktionen führen. Im Folgenden wird dargestellt, dass nichtrostende Stähle nur dann korrosionsbeständig bleiben, wenn auch Reinigung und Pflege der Oberflächen mehr Beachtung finden. Bereits in der Planungsphase, spätestens aber bei der Ausführung muss klar sein, wie mit den Oberflächen urngegangen werden soll, um ihre positiven Eigenschaften zu erhalten. Nicht zuletzt müssen auch die Betreiber und Nutzer wissen, dass nichtrostende Stähle in vielen Bereichen erheblichen Pflege- und Erhaltungsbedarf haben.
Micro gears are applied in an increasing quantity in many applications. Therefore, precise measurements are of growing importance to ensure their quality. This contribution describes the measurement of gears of a micro planetary gear set with a tactile probe, a tactile-optical probe, an optical sensor, and computed tomography (CT). For the tactile measurements, a high precision piezoresistive microprobe was used. A so-called fiber probe was applied for tactile-optical measurements. This probe applies image processing to determine the position of the tactile probing element. For all tactile and tactile-optical measurements, single point probing was used. The optical measurements were carried out with an imaging sensor based on focus variation. Due to limited accessibility, on some gears not all regions could be measured by the optical sensor and the tactile-optical probe. In contrast to this, with CT the whole part could be measured with high point density. We used a micro-CT system and carried out measurements with Synchrotron-CT. All the sensors used deliver measurement data in Cartesian coordinates. It is a challenge to transfer these data into coordinates in which gear parameters are defined. For this, special attention must be paid to the determination of the gear axis and to the orientation of the teeth. The applied procedures are detailed for different micro gears. The comparison between data of different measurements was carried out successfully. The deviations between the CT data and the tactile or tactile-optical data lie in the range of only a few micrometers.
Die Nutzung und Weiterverarbeitung von Sekundärstoffen kann in der Baustoffherstellung einen Beitrag zum nachhaltigen Bauen leisten. Im Rahmen des Teilprojekts B wurde die Bewertung dieser Potenziale anhand von Beispielen ausgebaut und verifiziert. Die Basis dieser Bewertungsgrundlage ist die Erfüllung der grundlegenden technischen Anforderungen (ökobilanzielle Indikatoren, vergleichende ökobilanzielle Betrachtung). Im Teilprojekt E geht es um die Freisetzung umweltrelevanter Stoffe aus zementgebundenen Baustoffen. Überprüft werden sollte die Übereinstimmung zwischen Laborergebnissen, Modellierungen und realen Grundwasserkonzentrationen. Es wurden Schlitzwände errichtet, die in den Grundwasserleiter einbinden und umweltrelevante Parameter bestimmt. Grundsätzlich hat sich selbst bei Großbaustellen nur eine geringe Beeinflussung der Grundwasserqualität durch Beton ergeben.