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Eingeladener Vortrag
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Die ISO-Normen für Druckgasflaschen aus Aluminiumlegierungen erfordern in der Regel eine Wärmebehandlung nach dem Umformungsprozess. Eine solche Wärmebehandlung ist ein kostspieliger Teil bei der Herstellung. Wegen des zunehmenden internationalen Handelsaufkommens müssen Marktüberwachungsbehörden über einfache und zuverlässige Testverfahren zur Überprüfung der ordnungsgemäß durchgeführten Wärmebehandlung an Druckgasflaschen verfügen. In diesem Beitrag wird beispielhaft die unterschiedliche Leistungsfähigkeit der wärmebehandelten und der nicht-wärmebehandelten Gasflaschen gezeigt und verschiedene Verfahren auf ihre Eignung als einfach durchzuführende Stichprobenkontrolle untersucht.
This paper describes experiences and results of experiments with several metallic dusts within the nanometer range. The nano dusts (aluminium, iron, zinc, titanium and copper) were tested in a modified experimental setup for the test apparatus 20 L-sphere (also known as 20-L Siwek Chamber), that enables the test samples to be kept under inert atmospheric conditions nearly until ignition. This setup was already introduced in earlier papers by the authors. It was designed to allow the determination of safety characteristics of nano powders under most critical circumstances (e.g. minimisation of the influence of oxidation before the test itself). Furthermore the influence of passivation on explosion behaviour is investigated and additional tests with deposited dust were carried out to describe the burning behaviour of all dusts. For a better characterisation all samples were tested with a simultaneous thermal analysis (STA). To minimise the influence of oxidation all samples were handled at inert conditions until shortly before ignition or start of the test respectively.
Checking the performance of energy dispersive X-ray spectrometers as well as validation of the results obtained with energy dispersive X-ray spectrometry (EDX) at a scanning electron microscope (SEM) involve the use of (certified) reference and dedicated test materials. This paper gives an overview on the test materials mostly employed by SEM/EDX users and accredited laboratories as well as on those recommended in international standards. The new BAM reference material EDS-CRM, which is currently in the process of certification, is specifically designed for the characterization of EDS systems at a SEM through calibration of the spectrometer efficiency in analytical laboratories in a simple manner. The certification of the spectra by means of a reference EDS is described. The focus is on the traceability of EDS efficiency which is ensured by measurements of the absolute detection efficiency of silicon drift detectors (SDD) and Si(Li) detectors at the laboratory of the PTB using the electron storage ring BESSY II as a primary X-ray source standard. A new test material in development at BAM for testing the performance of an EDS in the energy range below 1 keV is also briefly presented.
Cyanides are among the most important inorganic pollutants to be tested and monitored in environmental compartments. They can be distinguished and determined as free cyanide, weak acid dissociable cyanide or as total cyanide. However, in any case obtained, measurement results are operationally defined referring to the applied analytical method. In 2011, the International Standard ISO 11262 has been published which specifies a normative analytical method for the determination of total cyanide in soil. The objective of the project described in this paper was to provide the first soil reference material (CRM) certified for its mass fraction of total cyanide on the basis of this standard. A total of 12 German laboratories with proven experience in the determination of cyanides in environmental samples participated in the certification study. Measurement results were evaluated in full compliance with the requirements of ISO Guide 35. Taking into account the results of the inter-laboratory comparison as well as the outcome of the homogeneity and stability studies, a certified mass fraction of total cyanide of 21.1 mg/kg and an expanded uncertainty (k=2) of 1.3 mg/kg were assigned to the material. The reference material has been issued as CRM BAM-U114.
We investigate a single-pixel camera (SPC) that relies on non-mechanical scanning with a terahertz (THz) spatial light modulator (SLM) and Compressed Sensing (CS) for image generation. The camera is based on a 350 GHz multiplier source and a Golay cell detector. The SLM consists of a Germanium disc, which is illuminated by a halogen lamp. The light of the lamp is transmitted through a thin-film transistor (TFT) liquid crystal display (LCD). This enables the generation of light patterns on the Germanium disc, which in turn produce reflecting patterns for THz radiation. Using up to 1000 different patterns the pseudo-inverse reconstruction algorithm and the CS algorithm CoSaMP are evaluated with respect to image quality. It is shown that CS allows a reduction of the necessary measurements by a factor of three without compromising the image quality.
This paper shows how Angle-Resolved Scattering can reveal wear on engineered surfaces. The samples studied, three discs made of steel 100Cr6H used in gear wheels in the automotive industry, were assessed after they had undergone ball-on-disc tests. Scattering maps recorded for spatial frequencies from 0.1 µm-1 to 2.7 µm-1 show a contrast inversion around 0.36 µm-1 revealing the wear trace. Besides measurements of rms roughness, where mean values are 20 nm and 24 nm depending on the locations considered, stationarity and isotropy, we demonstrate the ability of the technique to reveal localized wear on this type of surface in a rapid, robust and convenient way. We show that the tool trace is influenced by the load magnitude rather than by the number of oscillation cycles and highlight the key role played by surface roughness in how the sample responds to wear tests.
Abfallgebinde, die im Endlager Konrad eingelagert werden sollen, müssen die Anforderungen und Kriterien erfüllen, die in den Endlagerungsbedingungen (SE-IB-29/08-Rev-1 [1]) und in der Produktkontrolle (SE-IB-30/08-Rev-1) festgelegt sind. Die Qualifizierung der Abfallbehälter erfolgt auf dieser Grundlage in Form von Bauartprüfungen, die von der Bundesanstalt für Materialforschung und -prüfung (BAM) im Auftrag des Bundesamtes für Strahlenschutz (BfS) durchgeführt werden. Darüber hinaus sind die im Hinblick auf Behälterbauartprüfungen relevanten Nebenbestimmungen aus dem Planfeststellungsbeschluss für das Endlager Konrad zu berücksichtigen. Zur besseren Anwendbarkeit werden diese Nebenbestimmungen in die Endlagerungsbedingungen und die Produktkontrolle eingearbeitet. Begleitend ist als Hilfestellung für die Abfallablieferer und Behälterhersteller ein Leitfaden geplant, der praktikable Nachweisstrategien aufzeigt und, soweit erforderlich, Hintergrundinformationen zu den Spezifikationen der Regelwerke liefert. Die BAM ist vom BfS beauftragt, hierfür Vorschläge zu entwickeln und Empfehlungen abzugeben.
Time reversal techniques are used in ocean acoustics, medical imaging, seismology, and non-destructive evaluation to backpropagate recorded signals to the source of origin. We demonstrate experimentally a technique which improves the temporal focus achieved at the source location by utilizing deconvolution. One experiment consists of propagating a signal from a transducer within a concrete block to a single receiver on the surface, and then applying time reversal or deconvolution to focus the energy back at the source location. Another two experiments are run to study the robust nature of deconvolution by investigating the effect of changing the stabilization constant used in the deconvolution and the impact multiple sources have upon deconvolutions focusing abilities. The results show that we are able to generate an improved temporal focus at the source transducer using deconvolution while maintaining the robust nature of time reversal. Additionally, deconvolutions costs are negligible due to it being a preprocessing step to the recorded data. The technique can be applied for detailed investigation of the source mechanisms (e.g. cracks) but also for monitoring purposes.
Given the frequent incidences of Non-Accident Releases (NARs) of hazardous materials from tank cars, there in an increasing interest in transporting hazardous materials in total containment conditions (i.e., no pressure relief devices). However, the ability of tank cars to meet thermal protection requirements provided in the Code of Federal Regulations under conditions of total containment has not been established. Also, the modeling tool commonly used by industry to evaluate thermal protection, AFFTAC, has not been validated under these conditions. The intent of this effort was to evaluate through a series of third-scale fire tests, the ability of tank cars to meet the thermal protection requirements under total containment conditions, and also, to validate AFFTAC for such conditions.
This paper describes the test design and planning effort associated with this research, including the design and evaluation of a fire test setup to simulate a credible, fully engulfing, pool fire that is consistent and repeatable, and the design and hydro-static testing of a third-scale tank specimen. The fire design includes controls on the spatial distribution and temperature variation of the flame temperature, the heat flux, and the radiative balance, to best reflect large liquid hydrocarbon pool fire conditions that may be experienced during derailment scenarios.
Technical background
(2015)
The major components of sector field instruments can be listed as follows and will be described in more detail in the following chapter. (Specific details for the different types of instruments will be given in the corresponding instrumental sections in Chapters 11-17.) The general principle of all mass spectrometers follows ionisation after sample introduction, Separation of the ions according to their mlz ratio and final detection at the detection unit. The transport and Separation of ions follow the principles of ion optics.
Hydrophilic interaction chromatography (HILIC) coupled with inductively coupled plasma mass spectrometry (ICP-MS) were optimised for the direct determination of gadolinium-based contrast agents in tap water. In comparison to our previous work, a new developed zwitterionic HILIC column (ZIC-cHILIC) was used for speciation of Gd-containing contrast agents. The limit of quantification (LOQ) for the five contrast agents Gd-BOPTA, Gd-DPTA-BMA, Gd-BT-DO3A, Gd-DOTA and Gd-DTPA are in the range of 512 ng Gd per litre. Additionally, a new internal standard, Pr-DOTA, was investigated to correct intensity drifts, minor and major changes in the sample volumes and possible matrix effects. With the speciation method described, tap water samples from the area of Berlin were analysed and for the first time, three Gd species, Gd-BT-DO3A, Gd-DOTA and Gd-BOPTA, were found in tap water samples at concentrations of about 10–20 ng Gd per litre. These are the same Gd species which have been previously detected predominantly in surface waters of the Berlin area.
This report focuses on the characterization of CD4 expression level in terms of equivalent number of reference fluorophores (ERF). Twelve different flow cytometer platforms across sixteen laboratories were utilized in this study. As a first step the participants were asked to calibrate the fluorescein isothiocyanate (FITC) channel of each flow cytometer using commercially available calibration standard consisting of five populations of microspheres. Each population had an assigned value of equivalent fluorescein fluorophores (EFF denotes a special case of the generic term ERF with FITC as the reference fluorophore). The EFF values were assigned at the National Institute of Standards and Technology (NIST). A surface-labelled lyophilized cell preparation was provided by the National Institute of Biological Standards and Control (NIBSC), using human peripheral blood mononuclear cells (PBMC) pre-labeled with a FITC conjugated anti-CD4 monoclonal antibody. Three PBMC sample vials, provided to each participant, were used for the CD4 expression analysis. The PBMC are purported to have a fixed number of surface CD4 receptors. On the basis of the microsphere calibration, the EFF value of the PBMC samples was measured to characterize the population average CD4 expression level of the PBMC preparations. Both the results of data analysis performed by each participant and the results of centralized analysis of all participants' raw data are reported. Centralized analysis gave a mean EFF value of 22,300 and an uncertainty of 750, corresponding to 3.3% (level of confidence 68%) of the mean EFF value. The next step will entail the measurement of the ERF values of the lyophilized PBMC stained with labels for other fluorescence channels. The ultimate goal is to show that lyophilized PBMC is a suitable biological reference cell material for multicolor flow cytometry and that it can be used to present multicolor flow cytometry measurements in terms of ABC (antibodies bound per cell) units.
Besonders beim Bauen im Bestand und der Bauwerkserhaltung werden zur Bestimmung des Tragvermögens von historischen, oft unter Denkmalschutz stehenden, natursteinernen Bauteilen Materialkennwerte benötigt. Die üblichen Verfahren mittels Probeentnahme am Objekt und Bestimmung der Kennwerte im Labor bedeuten bei Denkmälern einen massiven Eingriff und sollten vermieden werden. Vermehrt wird daher der Einsatz von zerstörungsfreien Untersuchungsmethoden erforscht und angewendet. Eine dieser Methoden stellt die Ultraschallprüfung dar.
Changes in fuel composition and the introduction of alternative fuels often create problems of degradation in materials. The objective of this research is to study the interaction of the sealing materials FKM, EPDM, CR, CSM, N8R, IIR, VMQ, FVMQ and PA and biofuels such as non-aged and 2 year aged biodiesel (FAME), E1 0 (fuel with 10% ethanol, E85 (fuel with 85% ethanol} and non-aged and 1 year aged 810 (heating oil with 10% biodiesel) in comparison with premium grade fuel without ethanol. Exposure tests were performed with test specimens at 20 °C, 40 oc and 70 oc for 84 days to document the changes in mass, volume and tensile properties. The sealing materials FKM, FVMQ and PA were evaluated as resistant in E10, and FVMQ, VMQ and PA as resistant in E85 at 20 oc and 40 oc. S welling resulted from the high absorption by the elastemers CR, CSM, EPDM, IIR and N8R in comparison to their dissolution in non-aged biodiesei at 40 °C. FKM was still resistant in aged biodiesei at 40 oc but only to a limited degree at 70 °C. The sealing materials CR, CSM, EPDM, IIR and N8R were damaged to a high extent in non-aged and aged 810. Of all the sealing materials, FKM and FVMQ showed high compatibility with these biofuels up to 70 °C.
The aim of this work was to study the interaction between high density polyethylene (HDPE) grades as material for dangeraus goods packagings and biofuels such as E10 (fuel with 10% ethanol), E85 (fuel with 85% ethanol), biodiesei and 810 (heating oil with 10% biodiesel). Jerricans made of two polyethylene grades were filled with these fuels and exposed to temperatures of 20 oc and 40 oc for more than one year. Tensile properlies (tensile strength, breaking elongation and elasticity modulus) and Melt Flow Rate (MFR) were determined, and Fourier Transform Infrared Spectroscopy (FTIR) was used to evaluate changes in the chemical structure.
Measurements of the MFR and tensile properlies of the polyethylene grades after exposure to E1 0, E85 and 810 showed only a slightly damaging influence. A n increase in the peak of 1585 cm·1 for the (C=C) stretching vibrations was visible in the FTIR spectra after immersion tests with E85. A n increase in the MFR with the immersion time of the grades in biodiesei was measured - in parlicular, after one year of exposure. The elasticity modulus of the polyethylene grades was reduced with the immersion time too. The FTIR spectra showed a broadening of the C=O peak of 1740 cm·1 and the appearance of the hydroxyl group at 3500 cm·1.
The tribological profile of alumina (99.7%) mated against rotating disks made in binder-less niobium carbide (NbC) and cobalt-bonded NbC were determined under unidirectional sliding tests (0.1 m/s to 8.0 m/s; 22 °C and 400 °C) as well as in oscillation tests (f = 20 Hz, Δx = 0.2 mm, 2/50/98% rel. humidity, n = 105/106 cycles) under unlubricated (dry) conditions. In addition, the microstructure and mechanical properties of binderless NbC and NbC bonded with 8% cobalt were determined as well. The reason for testing hot-pressed NbC was to avoid side effects generated by sintering additives and/or second phases. The tribological data obtained were benchmarked with different ceramics, cermets and thermally sprayed coatings. NbC and cobalt-bonded NbC exhibited low wear rates under dry sliding associated with high load carrying capacity. The tribological profile established revealed a strong position of NbC bearing materials under tribological considerations and for closed tribo-systems against traditional references, such as WC, Cr3C2 and (Ti,Mo)(C,N).