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Eingeladener Vortrag
- nein (1024)
Within the National Metrology Institutes (NMIs) and designated laboratories, an interlaboratory comparison, CCQM-P107, was conducted to verify the degree of international comparability concerning the results of purity analysis. The mass fractions of Ag, Bi, Cd, Cr, Ni, Tl at the lower mg/kg-level in a high purity zinc material were determined, but the real measurand in metrological sense was the sum of the six mass fractions. Homogeneity was investigated by glow discharge mass spectrometry, reference values were obtained using isotope dilution mass spectrometry. Six NMIs participated, contributing eight independent data sets. The agreement amongst the results of the participants, their median and the agreement with the reference values were usually excellent and in almost all cases below the target uncertainty of 30% relative. In this manner, the accuracy of results and the comparability between the participants was demonstrated to be established.
Forefields of receding glaciers are unique and sensitive environments representing natural soil chronosequences, where sulfate availability is assumed to be a limiting factor. Bacterial mineralization of organosulfur is an important sulfate-providing process in soils. We analyzed the diversity of sulfonate-desulfurizing (desulfonating) bacteria in the Damma glacier forefield on the basis of the key gene asfA by terminal restriction fragment length polymorphism and clone libraries. The community structure and sequence diversity of desulfonating bacteria differed significantly between forefield soils deglaciated in the 1990s and the 1950s. Soil age had a strong effect on the desulfonating rhizosphere communities of Agrostis rupestris, but only a slight impact on the ones from Leucanthemopsis alpina. AsfA affiliated to Polaromonas sp. was predominantly found in the more recent ice-free soils and the corresponding rhizospheres of A. rupestris, while a group of unidentified sequences was found to be dominating the matured soils and the corresponding rhizospheres of A. rupestris. The desulfonating bacterial diversity was not affected by varying levels of sulfate concentrations. The level of asfA diversity in recently deglaciated soils suggests that desulfonating bacteria are a critical factor in sulfur cycling, with defined groups dominating at different stages of soil formation.
Bisphenol A polycarbonate/acrylonitrile–butadiene–styrene (PC/ABS) with and without bisphenol A bis(diphenyl phosphate) (BDP) and 5 wt.% zinc borate (Znb) were investigated. The pyrolysis was studied by thermogravimetry (TG), TG-FTIR and NMR, the fire behaviour with a cone calorimeter applying different heat fluxes, LOI and UL 94. Fire residues were examined with NMR. BDP affects the decomposition of PC/ABS and acts as a flame retardant in the gas and condensed phases. The addition of Znb results in an additional hydrolysis of PC. The fire behaviour is similar to PC/ABS, aside from a slightly increased LOI and a reduced peak heat release rate, both caused by borates improving the barrier properties of the char. In PC/ABS + BDP + Znb, the addition of Znb yields a borate network and amorphous phosphates. Znb also reacts with BDP to form alpha-zinc phosphate and borophosphates that suppress the original flame retardancy mechanisms of BDP. The inorganic–organic residue formed provides more effective flame retardancy, in particular at low irradiation in the cone calorimeter, and a clear synergy in LOI, whereas for more developed fires BDP + Znb become less effective than BDP in PC/ABS with respect to the total heat evolved.
The determination of amino groups on surfaces capable of binding biomolecules is important for the understanding and optimization of technologically relevant coupling processes. In this study, three different types of amino-functionalized model surfaces, amino thiolate on Au, amino siloxane on Si, and polyethylene (PE) foils and films reacted with 1,2-diaminoethane (DAE) were derivatized with 3,5-bis(trifluoromethyl)phenyl isothiocyanate. Subsequently, these samples were analyzed by chemical derivatization X-ray photoelectron spectroscopy (CD-XPS) and near-edge X-ray absorption fine structure spectroscopy (NEXAFS). The determination of amino groups by this analytical approach allows gaining insight into the availability of groups on surfaces that can actually serve as attachment sites for biomolecules in technical applications. In the case of the amino thiolate on Au, almost 90% of the expected amino groups were detected by CD-XPS. Investigation of the amino siloxane films revealed lower yields for the derivatization reaction in the order of 30%. The lowered reaction yields are thought to be due to interactions between the amino siloxane`s amino and silanol groups or the underlying substrate, making them inaccessible to the derivatization agent. The aminated PE samples are characterized by a complex surface chemistry and structure, and reaction yields of the derivatization reaction cannot be unequivocally derived. However, 1-3% of the total carbon atoms in the surface layer were found to be bound to amino groups accessible to the derivatization agent. It can be concluded that, depending on the detailed character of the investigated amino-terminated surface, the amount of amino groups accessible to CD-XPS can be substantially lower than the total amount of amino groups present at the surface.
Effect and measurement of the machine compliance in the macro range of instrumented indentation test
(2010)
The contribution concerns the strong effect of the machine compliance in the upper macro range of the instrumented indentation test on hard materials. To achieve a minimum uncertainty in determination of the machine compliance the measurement and analysis needed for the determination are studied in detail. Based on the assumption that the hardness and/or the indentation modulus are force independent, four methods on the determination of the machine compliance are described. Experimental results of a commercial testing machine up to 2500 N and of a standard machine up to 200 N are analyzed. The results show that the uncertainty of the compliance is usually higher than requested for a precisely enough determination of hardness and further materials parameters. Especially for the calibration of reference materials with high hardness and/or Youngs modulus, the machine compliance should be limited in ISO 14577 part 3, 2003 [1].
Fenoxycarb ist ein insektizider Wirkstoff,
der wegen seiner hormonähnlichen Wirkung in sehr
geringen Konzentrationen in Holzschutzmitteln eingesetzt
werden kann. Das hat zur Folge, dass aus Extrakten von
behandeltem Holz relativ geringe Fenoxycarb-Mengen vor
dem Hintergrund ebenfalls extrahierter Holzinhaltsstoffe
zu bestimmen sind. In Vergleichsanalysen verschiedener
Laboratorien wurde gezeigt, dass Fenoxycarb durch Methanol
mit hoher Ausbeute aus Holz extrahierbar ist und
in den Extrakten durch Hochdruckflüssigchromatographie
in Kopplung mit UV-Detektion bestimmt werden kann.
Fenoxycarb-Konzentrationen im unteren Bereich der
erforderlichen Einbringmengen können mit dem erprobten
Verfahren nur nach zusätzlicher Probenaufarbeitung
bestimmt werden. Bedingt durch schwer auswertbare
Chromatogramme sind die Abweichungen der Ergebnisse
zwischen verschiedenen Laboratorien relativ hoch.
Femtosecond (fs) laser pulse ablation (pulse duration of 150 fs, wavelength of 775 nm, repetition rate of 1 kHz) of single-crystalline TeO2 surfaces was performed in air using the direct focusing technique. The lateral and vertical dimensions of laser ablated craters as well as the laser damage thresholds were evaluated for different pulse numbers applied to the same spot. The joint observation using optical microscopy, atomic force microscopy and scanning electron microscopy revealed the surface morphology of the ablated craters and also showed that the ablation threshold depends significantly on the number of laser pulses applied to the same spot due to incubation effects. The incubation effects change the absorption processes involved in fs-laser ablation of the transparent material from multiphoton absorption to a single-photon absorption. These results are discussed on the basis of recent models of the interaction of fs-laser pulses with dielectrics.
Moisture ingress is one of major damaging factors for masonry buildings. As the complex resistivity (CR) is sensitive to textural properties as well as to the pore fluid chemistry of wet porous media, its non-destructive application can provide helpful information for conservators. In a comprehensive laboratory study it has been shown that CR might even be able to distinguish between salt content and saturation degree in only one measurement. The combined use of electrical and electromagnetic measurement techniques in two field-scale flooding experiments has shown some unexpected differences. Possible reasons are discussed and it is shown that bringing together the information of both methods leads to a clearer picture.
Simulation of Mechanical Behaviour in a Single-Crystal Nickel-Basis Superalloy at High Temperature
(2010)
In a research project fatigue tests on two identical wing sections that are used as representative substitute components were performed to estimate lifetime enhancement of light-weight aircraft such as general aviation gliders. Single step fatigue tests at limit load on one component were compared with spectrum loading on the other. A characteristic damage behaviour was observed. Local buckling due to high shear loading of the sandwich core of the wing shell causes the main damage. Even though an intentionally high load level was chosen no increase of micro-cracking could be detected. Additionally no delamination effects in laminates or bondings were observed except the skin-core delamination which causes the buckling effect in the wing shell due to fatigue loading. Finally the concept of using representative substructures and accompanying specimen tests is an effective approach for in-service loading investigations and could also be applied to research on wind turbine blades.
The peer evaluation of single accreditation bodies in order to sign an Arrangement for Recognition of the international accreditation organizations International Accreditation Forum, Inc. (IAF) and International Laboratory Accreditation Cooperation (ILAC), whether performed by Regional Accreditation Groups or directly by IAF and/or ILAC, is standard practice. The fundamental requirements for such evaluations are well specified in documents. However, the careful evaluation of all their Arrangement members poses an enormous logistic task for IAF and ILAC, and the signatories can be evaluated more thoroughly within their Regional Groups. Hence, IAF and ILAC typically evaluate only the Regional Accreditation Groups and accept all signatories of a Regional Accreditation Group once successfully evaluated by their respective Regional Group. However, the requirements for the evaluation of a Regional Group are extensive, and the evaluation procedure is highly complicated and must be conducted very carefully in order to assure that the results of accreditation can be trusted. This article describes the evaluation procedure used by IAF and/or ILAC for Regional Groups wishing to sign the IAF/ILAC Arrangement. We wish to inform and to aid these Regional Groups setting out for evaluation, and also to build confidence in the IAF/ILAC Arrangements.
Der Beitrag der BAM zur Sicherheitstechnik am Beispiel der Schadensanalyse von Eisenbahnkomponenten
(2010)
Non-destructive tests (NDT) are an essential tool used in special inspections to gather detailed information about the condition of a bridge. The inspection of bridge decks is a critical task, and, currently, can be successfully carried out using a wide range of NDT techniques. Nevertheless, some of these techniques are excessively expensive and time consuming. One of these techniques, the ground penetrating radar (GPR), has been used for some decades in the non-destructive inspection and diagnosis of concrete bridges. GPR is useful to find general information about the true position of reinforcement and tendon ducts, and check the quality of the construction and materials. A significant number of reinforced and prestressed concrete bridges are deteriorating at a rapid rate and need to be repaired and strengthened. During these rehabilitation processes, designers are often faced with a lack of original design plans and unawareness of the real position of reinforcement and tendon ducts. In this paper, three case studies of the use of GPR techniques for the inspection of concrete bridges are presented and analysed. The main aim of this research is to show the strong need and usefulness of these techniques, which can provide non-visible information about structural geometry and integrity required for strengthening and rehabilitation purposes.
By addition of LiF-containing sintering additives to commercial BaTiO3 powder, more than 98% of the theoretical density was reached at a sintering temperature of 900 °C both on powder compacts and laminates. Dielectric measurements were performed on ceramic samples in the temperature and frequency ranges from -20 °C to 125 °C and from 103 to 106 Hz, respectively. High relative permittivity (εr ~ 3160) and low dielectric loss (tan δ ~ 0.014) were measured for tapes of the favoured material. The breakdown strength for tapes with a thickness of about 80 µm is 30 kV/mm. The microprobe analysis showed, that no interfacial reaction between the dielectric layer and the Ag-electrode had occurred.
The newly developed barium titanate ceramics completely densifying at 900 °C turned out to be promising for integration of buried capacitors in LTCC multilayers.