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Zur Alterung von Smalten - Materialuntersuchungen bei der Restaurierung eines Gründerzeit-Mosaiks
(2001)
Das Mosaik "Muse der Kunst" war in Berlin-Mitte mehrere Jahrzehnte hinter einer Vermauerung verborgen, bevor es nun wiederentdeckt und restauriert wurde. Die Smalten zeigten zum Teil Risse, Verkrustungen und Farbveränderungen in Folge von Alterungsprozessen der historischen Materialien. Einzelne Deckgläser von Goldsmalten waren abgesprengt.
Zur genaueren Kenntnis des Einflusses der Ermüdungsbelastung auf das Versagen von Beton wurde das Ermüdungsverhalten von gekerbten Betonbalken in kraft- und verformungsgeregelten Dreipunktbiegezugversuchen untersucht. Für die verformungsgeregelten Versuche wurde eine neuentwickelte Versuchstechnik angewendet, mit der auch unter hochzyklischer Beanspruchung mit Lastspielzahlen von bis zu einer Million Zyklen sowohl der ansteigende als auch der abfallende Ast in einem Kraft-Verformungsdiagramm aufgezeichnet werden kann.
Glass-ceramics containing Ca2KNa(PO4)2 as the main crystalline phase have a solubility which is 8 times higher than that of alpha-tricalcium phosphate ceramics. When using these compositions in drug delivery systems, especially in bone, it is necessary to create a material with a high open porosity. A Ca2KNa(PO4)2-based glass-ceramic was prepared from a borosilicate glass melt. The processed material includes minor amounts of boron which are low enough for medical application. Tissue response was studied using an animal model. Particles were implanted in rabbit femurs. Bone and soft tissue development occurred at the particle interfaces. In general, most particles were enclosed in the network of trabecular bone. The advantages of using a biomaterial with high porosity (pore size of 1-3 micron), together with rapid biodegradation, bioactivity and biocompatibility, despite traces of boron, were shown. 4 refs.
In vivo test of a high porous rapidly resorbable dicalcium potassium sodium phosphate glass-ceramics
(2002)
Fabrication of carbon/silica hybrid materials using cationic polymerization and the sol-gel process
(2002)
Results are reported from a pilot study under the Consultative Committee for Amount of Substance (CCQM) to compare measurements of and resolve any relevant measurement issues in, the amount of thermal SiO2 oxide on (100) and (111) orientation Si wafer substrates in the thickness range 1.5 - 8 nm. As a result of the invitation to participate in this activity, 45 sets of measurements have been made in different laboratories using 10 analytical methods: medium-energy ion scattering spectrometry (MEIS), nuclear reaction analysis (NRA), RBS, elastic backscattering spectrometry (EBS), XPS, SIMS, ellipsometry, grazing-incidence x-ray reflectrometry (GIXRR), neutron reflectometry and transmission electron microscopy (TEM). The measurements are made on separate sets of 10 carefully prepared samples, all of which have been characterised by a combination of ellipsometry and XPS using carefully established reference conditions and reference parameters.
The results have been assessed against the National Physical Laboratory (NPL) data and all show excellent linearity. The remaining data sets correlate with the NPL data with average root-mean-square scatters of 0.15 nm, half being better than 0.1 nm and a few at or better than 0.05 nm. Each set of data allows a relative scaling constant and a zero thickness offset to be determined. Each method has an inherent zero thickness offset between 0 nm and 1 nm and it is these offsets, measured here for the first time, that have caused many problems in the past. There are three basic classes of offset: water and carbonadeous contamination equivalent to ~1 nm as seen by ellipsometry; adsorbed oxygen mainly from water at an equivalent thickness of 0.5 nm as seen by MEIS, NRA, RBS and possibly GIXRR; and no offset as seen by XPS using the Si 2p peaks. Each technique has a different uncertainty for the scaling constant and consistent results have been achieved. X-Ray photoelectron spectroscopy has large uncertainties for the scaling constant but a high precision and, critically, if used correctly, has zero offset. Thus, a combination of XPS and the other methods allows the XPS scaling constant to be determined with low uncertainty, traceable via the other methods. XPS laboratories returning results early were invited to test a new reference procedure. All showed very significant improvements. The reference attenuation lengths thus need scaling by 0.986 ± 0.009 (at an expansion factor of 2) deduced from the data for the other methods. Several other methods have small offsets and, to the extent that these can be shown to be constant or measurable, then these methods will also show low uncertainty. Recommendations are provided for parameters for XPS, MEIS, RBS and NRA to improve their accuracy.
Ein effektives Wassermanagement ist ein wichtiger Aspekt in der Entwicklung von Brennstoffzellen hinsichtlich Langzeitstabilität und Optimierung der Leistungsfähigkeit. Eine zentrale Rolle spielt dabei die Gasdiffusionslage, die für die gleichmäßige Verteilung der Reaktionsgase auf die elektrochemisch aktive Schicht (Katalysator) sorgen soll. In diesem Beitrag werden gemeinsame Forschungsaktivitäten des Helmholtz-Zentrums Berlin für Materialien und Energie (Entwicklung bildgebender Verfahren) sowie des Zentrums für Sonnenenergie- und Wasserstoff-Forschung (ZSW, Entwicklung von Brennstoffzellen) vorgestellt. Im Rahmen dieser Kooperation werden die Entstehung, die Verteilung und der Transport von flüssigem Wasser, kurz das Wassermanagement, unter Betriebsbedingungen untersucht. Mittels Synchrotronradiografie und -tomografie werden kleinste Wassercluster in der Gasdiffusionslage detektiert. Die gewonnenen Erkenntnisse dienen der Modifikation und einer gezielten Auswahl der eingesetzten Materialien.
The German Federal Institute for Materials Research and Testing (BAM) has established a testing guideline to assess the suitability of geosynthetic or geocomposite drain (GCD) elements for final landfill cover systems. In an earlier paper the uniform procedure according to the BAM guideline for determining long-term water flow capacity was described, and the structural stability of drain cores under creep was investigated. The extrapolation of creep curves is permissible only when it can be shown, over the extrapolated period (at least 100 years), that oxidative aging does not invoke any relevant changes in the polyolefin material. This can be shown by measuring antioxidant depletion and mechanical degradation of the drain cores and filter/protection geotextiles in oven aging and water immersion tests. In this paper the results of such aging studies on three different GCD products are reported. Degradation of the tensile strength of HALS-stabilized polypropylene needle-punched nonwoven geotextiles (PP NWGTs) starts right from the beginning of the oven aging. This has to be taken into account for lifetime predictions based on residual tensile strength. The rate of oxidative degradation of NWGTs decreases significantly with increasing mass per area. Therefore the expected service life sets a limit on acceptable geotextile grammage. Antioxidant depletion in the drain cores, which are made of relatively thick PP strands or HDPE ribs, is about an order of magnitude slower than in filter and protection NWGTs, which are made of thin fibers. Service life values in excess of 100 years may be obtained for the products when the geotextiles and drain cores are properly stabilized and designed.
The present work shows results on elemental distribution analyses in Cu(In,Ga)Se2 thin films for solar cells performed by use of wavelength-dispersive and energy-dispersive X-ray spectrometry (EDX) in a scanning electron microscope, EDX in a transmission electron microscope, X-ray photoelectron, angle-dependent soft X-ray emission, secondary ion-mass (SIMS), time-of-flight SIMS, sputtered neutral mass, glow-discharge optical emission and glow-discharge mass, Auger electron, and Rutherford backscattering spectrometry, by use of scanning Auger electron microscopy, Raman depth profiling, and Raman mapping, as well as by use of elastic recoil detection analysis, grazing-incidence X-ray and electron backscatter diffraction, and grazing-incidence X-ray fluorescence analysis. The Cu(In,Ga)Se2 thin films used for the present comparison were produced during the same identical deposition run and exhibit thicknesses of about 2 µm. The analysis techniques were compared with respect to their spatial and depth resolutions, measuring speeds, availabilities, and detection limits.
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.
During the mineralisation of metal carbonates MCO3 (M = Ca, Sr, Ba, Mn, Cd, Pb) liquid-like amorphous intermediates emerge. These intermediates that form via a liquid/liquid phase separation behave like a classical emulsion and are stabilized electrostatically. The occurrence of these intermediates is attributed to the formation of highly hydrated networks whose stability is mainly based on weak interactions and the variability of the metal-containing pre-critical clusters. Their existence and compositional freedom are evidenced by electrospray ionization mass spectrometry (ESI-MS). Liquid intermediates in non-classical crystallisation pathways seem to be more common than assumed.
Germination induces the glucosylation of the Fusarium mycotoxin deoxynivalenol in various grains
(2012)
In food, the mycotoxin deoxynivalenol (DON) often occurs in conjunction with its 3-β-D-glucopyranoside (D3G). The transformation of DON to D3G through glucosylation is catalysed by plant enzymes, however, the exact circumstances are not well understood. In order to investigate the role of enzymatic glucosylation in germinating grains, DON treated kernels were steeped and germinated under laboratory conditions. Furthermore, the effect of malting on the DON content of the contaminated barley was investigated. In all cases, DON and its derivatives were quantified by HPLC-MS/MS before, during and after the experiments. Amongst the six tested cereals; wheat, rye, barley, spelt, and millet transformed DON to D3G during germination whilst the oats were inactive. For wheat, barley, and spelt the initial DON content was reduced by 50%, with the loss being almost entirely accounted for by D3G formation. As D3G might be cleaved during digestion, the elevated D3G concentration may obscure the toxicologically relevant DON content in processed food and beer. The germination process has a major influence on the 'masking' of DON, leading to high quantities of D3G that may be missed in common mycotoxin analyses.
Das Wissen über die Materialeigenschaften und die Versagensmechanismen bei Lehmbaustoffen ist begrenzt und lückenhaft. Im Rahmen des EU-Projekts NIKER (www.niker.eu) wurden deshalb die mechanischen Eigenschaften von Bauteilen aus Lehm unter statischer Druck- und Schubbeanspruchung bestimmt. Ziel der Untersuchungen war es, grundlegende Daten zum Verformungs- und Versagensverhalten von Lehmbauteilen zu erhalten und dieses mit einem numerischen Modell zu beschreiben. Die Versuchsergebnisse belegten das spröde Verhalten von Lehmsteinmauerwerk bei uniaxialer Druckbelastung und zeigten, dass das Versagen von Lehmsteinmauerwerk infolge Schubbelastung nach Erstrissbildung in Mörtelfugen und Lehmsteinen durch Gleiten der Lehmsteine entlang der Mörtelfugen erfolgt. Die numerische Makromodellierung erbrachte zwar befriedigende Resultate hinsichtlich des Spannungs-Dehnungs-Verhaltens, jedoch konnte bei der simulierten Rissbildung keine Übereinstimmung mit den in den Versuchen beobachteten Rissbildern erzielt werden. Bei Lehmsteinmauerwerk ist also eine wesentlich aufwendigere Mikromodellierung notwendig, um das Versagensverhalten korrekt beschreiben zu können.--------------------------------------------------------------------------------------------------------------
Knowledge of the material properties and failure mechanisms of earthen materials is limited and scattered. Within the framework of the NIKER project (www.niker.eu) funded by EC, the mechanical properties of earthen material elements were therefore determined under static compression and shear loads. The aim was to obtain fundamental data on deformation behaviour and failure mechanisms of earthen material structural elements and to describe them by means of a numerical model. The test results confirmed the brittle behaviour of earth block masonry under monoaxial compressive load and showed that the failure of earth block masonry under shear load occurs by sliding of the earth blocks along the mortar joints after initial cracking in mortar joints and earth block. Numerical macro modelling showed satisfying results with regard to stress-strain behaviour, but the simulated crack pattern was not consistent with experimental observations. In the case of earth block masonry, it is thus necessary to use micro modelling approaches in order to correctly predict the failure process at local level.
Der Beitrag gibt einen Überblick über die Eigenschaften industriell hergestellter Bauprodukte aus Lehm für den Mauerwerksbau. Die Qualität der industriellen Fertigung dieser Produktgruppe hat inzwischen einen Stand erreicht, der vergleichbar mit dem anderer Bauprodukte ist. Lehm-Putzmörtel gibt es als Universalputze für ein- oder mehrlagige Anwendung oder in Form von Unter-, Ober- oder Feinputzen. Lehmsteine werden in verschiedenen Größen und mit Lochung angeboten. Die mechanischen Eigenschaften verschiedener Lehmsteinsorten sind geprägt durch Druckfestigkeiten bis 11 N/mm2, mit üblichen Werten bei 2 bis 5 N/mm2. Ein kritischer Punkt ist die Abhängigkeit der Festigkeitseigenschaften der Lehmsteine von der Materialfeuchte. Die vorliegenden Untersuchungen haben jedoch gezeigt, dass in einem Luftfeuchtebereich von 40 bis 70 % RLF die Druckfestigkeit von Lehmsteinen verhältnismäßig konstant ist. Mauerwerk, errichtet mit Lehmsteinen und Lehm-Mauermörtel, zeigt ähnliche Druckfestigkeiten und E-Module wie Mauerwerk, das mit Porenbetonsteinen errichtet wurde. Infolge einer geringeren Haftscherfestigkeit zwischen Lehmmörtel und Lehmstein ist die Schubfestigkeit von Lehmsteinmauerwerk vergleichsweise niedrig.-------------------------------------------------------------------------------------------------------------------------------------
Properties of industrially produced earthen building products for masonry and behaviour of earth block masonry. The contribution gives an overview of the properties of industrially produced earthen building products for masonry. In the meantime the quality of the industrial production of this group of building materials reached a level similar to that of other products for construction. Earth plasters exist as plasters for universal, one or multi layer applications or as lower, upper or finish plasters. Earth blocks are provided in different sizes and with different perforations. The mechanical properties of different earth block types are signified by compressive strength of up to 11 N/mm2 but are typically in a range between 2 and 5 N/mm2. A critical point is the correlation of the strength of earthen materials with their moisture content. Results from earth blocks showed that in a relative humidity window between 40 and 70 % rh the compressive strength of earth blocks is fairly constant. Masonry made from earth block and earth mortar exhibited compressive strength and elastic modules similar to masonry made with aerated autoclaved concrete blocks. The shear strength of earth block masonry, however, is fairly low, due to the weak bond between earth block and earth mortar.
The analysis of biomolecules requires highly sensitive and selective detection methods capable of tolerating a complex, biological matrix. First applications of biomolecule detection by ICP-MS relied on the use of heteroelements as a label for quantification. However, the combination of immunoassays and ICP-MS facilitates multiparametric analyses through elemental tagging, and provides a powerful alternative to common bioanalytical methods. This approach extends the detection of biomarkers in clinical diagnosis, and has the potential to provide a deeper understanding of the investigated biological system. The results might lead to the detection of diseases at an early stage, or guide treatment plans. Immunoassays are well accepted and established for diagnostic purposes, albeit ICP-MS is scarcely applied for the detection of immune-based assays. However, the screening of biomarkers demands high throughput and multiplex/multiparametric techniques, considering the variety of analytes to be queried. Finally, quantitative information on the expression level of biomarkers is highly desirable to identify abnormalities in a given organism. Thus, it is the aim of this review to introduce the fundamentals, and to discuss the enormous strength of ICP-MS for the detection of different immunoassays on the basis of selected applications, with a special focus on LA-ICP-MS.
We have developed lanthanide labeling strategies for antibodies to adapt conventional biochemical workflows like Western blot immunoassays for detection by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) analysis with a special interest to apply the multi-element capabilities of ICP-MS for the design of multiplexed immunoassays. In this paper the lanthanide labeling of antibodies with MeCAT was investigated and the reaction conditions were optimized for application in a Western blot immunoassay analyzed by LA-ICP-MS. Furthermore, the MeCAT labeling strategy was compared with two other commercially available labeling reagents, MAXPAR and SCN-DOTA. As a proof-of-principle experiment chemically induced alterations of cytochrome P450 protein expression were investigated and the suitability of the differentially labeled antibodies for Western blot immunoassays of a complex liver microsomal protein fraction was tested. Limits of detection (LODs) in the lower fmol range were reached in the Western blot application using MeCAT and MAXPAR as element labeling reagents, whereas even sub-fmol LODs can be achieved in a dot blot experiment for the pure antibodies.
Synchrotron X-ray radiography and tomography investigations of a custom-made polymer electrolyte membrane fuel cell optimised for visualisation purposes are presented. The 3D water distribution and transport pathways in the porous carbon fibre gas diffusion layers (GDLs) were investigated. The authors found that water is not only moving from the GDL into the channel, but can also take the opposite way, that is, from the channel into free pore space of the GDL. Such movement of water into the opposite direction has been subject of speculations but has so far not yet been reported and might bring new insights into the general water transport behaviour, which might give new aspects to the general description of water transport processes and influence modelling assumptions to describe the process taking place in the GDL.