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Eingeladener Vortrag
- nein (902)
Chemical derivatization XPS is used for the quantitative determination of amines at conventional organic surfaces, and it is also applied to plasma-processed aminated surfaces. When using TFBA and PFB as derivatization reagents for tagging primary amino groups, unexpected fluorine species were observed in the second case. The existence of reaction pathways other than those expected for amine derivatization with PFB or TFBA has to be assumed. This phenomenon is tentatively interpreted as the result of C—F bond cleavage during derivatization reactions of TFBA and PFB at plasma-polymerized allylamine and other plasma-processed aminated surfaces. As a consequence, quantification procedures based on derivatization by PFB or TFBA will underestimate amine surface concentrations.
A set of ten calibration materials based on acrylonitrile-butadiene-styrene terpolymer (ABS) containing the elements Br, Pb, Cd, Cr, and Hg was produced in order to control polymer samples in regard to the restriction on the use of certain hazardous substances (RoHS) directive. The materials were produced with respect to the special demands of X-ray fluorescence analysis (XRF) and inductively coupled plasma mass spectrometry in combination with laser ablation (LA-ICP-MS).
The mass fractions of all elements were 0-1500 mg/kg and the materials were produced as granulates and solid discs with a diameter of 40 mm and thicknesses of 1, 2, and 6 mm. It could be shown that the signals measured by XRF strongly depend on the thickness of polymeric samples.
Macroscopic homogeneity was assessed with XRF measuring a total of 180 samples. The microscopic homogeneities were determined for a material with average elemental mass fractions with the aid of synchrotron radiation (SR) µ-XRF and LA-ICP-MS. Sufficient macroscopic and microscopic homogeneities for all elements could be achieved. It was observed that organic additives show a better homogeneity than oxides.
XRF and LA-ICP-MS were successfully calibrated with the new materials. Limits of detection were in the range of 0.4-22 mg/kg for XRF and 2.3-26.8 mg/kg for LA-ICP-MS. The materials are considered as candidate reference materials (RM) by the Federal Institute of Materials Research and Testing (BAM, Germany).
New applications of low-temperature co-fired ceramics (LTCC), such as pressure sensors or integrated functional layers, require materials that possess higher coefficients of thermal expansion (CTE). To fabricate LTCC with elevated CTE, two methods of material design are examined: firstly, glass ceramic composites (GCC), which consist of >50 vol% glass in the starting powder, and, secondly, glass-bonded ceramics (GBC), where glass is added as a sintering aid only. The CTE of GBC is mainly determined by the crystalline component. For GCC, the CTE can be well predicted, if CTE and elastic data of each phase in the microstructure are known. A nonlinear characteristic of the CTE versus phase composition was found with increasing Ecrystals/Eglass ratio and absolute CTE difference between the components. The glass composition and glass amount can be used to compensate the fixed properties of a crystalline material in a desired way. However, because the CTE and permittivity of a glass cannot be chosen independently, an optimum glass composition has to be found. For a given LTCC, it is possible to control the devitrification by shifting the glass composition. In this way, the resulting CTE values can be predicted more exactly and tailoring becomes possible. Different LTCC materials, based on the crystalline compounds Ba(La,Nd)2Ti4O12, ZrO2 (Y-TZP), SiO2 (quartz), and specially developed glasses, possessing an elevated CTE of around 10 × 10-6 K-1 while showing permittivity εr between 6 and 63, are introduced.
Monitoring the vulcanization of elastomers: Comparison of curemeter and ultrasonic online control
(2009)
The vulcanization of elastomeric materials has a high impact on the properties of the final product. Therefore, it is important to monitor and control this crosslinking process. A common technique to attain the necessary curing time is the use of a curemeter in accordance with ISO 6502 in order to determine the time for full cure of a sample with a standardized geometry. Based on this result and a lot of practical experience, the required curing time for a given product geometry is estimated. Within the scope of this work, a new analysis technique will be compared with the standard procedure. The ultrasonic online control employs ultrasound waves to measure the changes in material properties caused by vulcanization. For this study, a natural rubber compound with a conventional curing system was investigated by both techniques. It was found that the results of the ultrasonic technique show good agreement with the results of the curemeter.
Quantitative and Qualitative Comparison of Particulate Emissions from Office Machines (ABSTRACT)
(2009)
BETOSCAN - An instrumented mobile robot system for the diagnosis of reinforced concrete floors
(2009)
Grundlegende Anforderungen des Brand- und Explosionsschutzes im weitesten Sinn und entsprechende sicherheitstechnische Standards werden in europäischen Richtlinien und Normen beschrieben. Der Beitrag skizziert beispielhaft aktuelle Entwicklungen und in einigen Fällen deren Auswirkungen auf das entspechende nationale Regelwerk.
Hydrolytic degradation and functional stability of a segmented shape memory poly(ester urethane)
(2009)
In order to understand the effects of water and hydrolytic ageing on semi-crystalline poly(ester urethane) and its shape memory functionality, water immersion experiments at elevated temperature have been performed on a model substance and various parameters were monitored: change of the melting/crystallisation temperatures, substantial increase in crystallinity, temperature dependence of the water diffusion coefficient and solubility, hydrogen-bonding index and phase mixing by peak deconvolution of the FT-IR carbonyl region and day-to-day tensile and thermo-mechanical cyclic tensile tests. A rising fraction of freezable water agglomerates in the polymer was found for specimens cooled from the immersion temperature. The degradation process could be divided into three phases: an induction phase, a phase of continuous degradation and a phase of accelerated degradation. Shape recovery remains fairly constant during phase one and decreases slowly during phase two. The increase in crystallinity in phase two is accompanied by an increase in shape fixing ability.
The dispersed iron oxide nanoparticles of ferrofluids in aqueous solution are difficult to characterize due to their protective polymer coatings. We report on the bimodal size distribution of superparamagnetic iron oxide nanoparticles found in the MRI contrast agent Resovist, which is a representative example of commercial nanoparticle-based pharmaceutical formulations. The radii of the majority of the nanoparticles (>99%) range from 4 to 13 nm (less than 1% of the particles display radii up to 21 nm). The maxima of the size distributions are at 5.0 and 9.9 nm. The analysis was performed with in situ characterization of Resovist via online coupling of asymmetrical flow field-flow fractionation (A4F) with small-angle X-ray scattering (SAXS) using a standard copper X-ray tube as a radiation source. The outlet of the A4F was directly coupled to a flow capillary on the SAXS instrument. SAXS curves of nanoparticle fractions were recorded at 1-min time intervals. We recommend using the A4F-SAXS coupling as a routine method for analysis of dispersed nanoparticles with sizes in the range of 1-100 nm. It allows a fast and quantitative comparison of different batches without the need for sample preparation.
The traffic infrastructure in the vicinity of large airports is often very well developed, and, therefore, supports the establishment of significant industrial development. Regional or overall worldwide air traffic accessibility is an important aspect of site choice for many companies. Since air traffic has constantly increased in recent years, this has lead to the presumption that the risk of aircraft crashes in areas near airports is also greater than before. However, the risk of accidents in the neighborhood of an airport can be minimized by implementing some limitations.
Wear mechanisms, as adhesion, abrasion, fatigue and tribochemical wear, are complex in their physical and chemical nature. A theoretical description and prediction of wear are in most cases still far from reality. It is, therefore, important to use test rigs before a practical application of a given material combination under tribological loading.
On the other hand, model equations can be helpful for wear description, if a single wear mechanism is dominant.
Under oscillating and continuous sliding contact conditions, equations for wear calculation are presented to describe running-in and stationary wear behaviour of metals and ceramics. By using shear energy density, real area of contact, flash temperature, activation energy and numerical simulations with the method of movable cellular automata (MCA), wear data were calculated and compared to experimental laboratory results.
Forefields of receding glaciers are unique and sensitive environments representing natural chronosequences. In such habitats, microbial nitrogen fixation is of particular interest since the low concentration of bioavailable nitrogen is one of the key limitations for growth of plants and soil microorganisms. Asymbiotic nitrogen fixation in the Damma glacier (Swiss Central Alps) forefield soils was assessed using the acetylene reduction assay. Free-living diazotrophic diversity and population structure were resolved by assembling four NifH sequence libraries for bulk and rhizosphere soils at two soil age classes (8- and 70-year ice-free forefield). A total of 318 NifH sequences were analyzed and grouped into 45 unique phylotypes. Phylogenetic analyses revealed a higher diversity as well as a broader distribution of NifH sequences among phylogenetic clusters than formerly observed in other environments. This illustrates the importance of free-living diazotrophs and their potential contribution to the global nitrogen input in this nutrient-poor environment. NifH diversity in bulk soils was higher than in rhizosphere soils. Moreover, the four libraries displayed low similarity values. This indicated that both soil age and the presence of pioneer plants influence diversification and population structure of free-living diazotrophs.
Phosphorus (P) is an essential element for all living organisms and cannot be replaced. Municipal sewage sludge is a carrier of phosphorus, but also contains organic pollutants and heavy metals. A two-step thermal treatment is suggested, including mono-incineration of sewage sludge and subsequent thermochemical treatment of the ashes. Organic pollutants are completely destroyed by mono-incineration. The resulting sewage sludge ashes contain P, but also heavy metals. P in the ashes exhibits low bioavailability, a disadvantage in farming. Therefore, in a second thermochemical step, P is transferred into mineral phases available for plants, and heavy metals are removed as well. The thermochemical treatment was investigated in a laboratory-scale rotary furnace by treating seven different sewage sludge ashes under systematic variation of operational parameters. Heavy metal removal and the increase of the P-bioavailability were the focus of the investigation. The present experimental study shows that these objectives have been achieved with the proposed process. The P-bioavailability was significantly increased due to the formation of new mineral phases such as chlorapatite, farringtonite and stanfieldite during thermochemical treatment.
The objective of this work was to test the compliance of commercially available batteries with the German Battery Ordinance, a project of the German government that was initiated by the Federal Environment Agency. Different types of commercially available dry cells were analysed for their cadmium, lead and mercury contents. The dry cells underwent mechanical pre-treatment, separation of the different components and microwave-assisted digestion before determination of the heavy metals. Mercury is sometimes added to prevent the generation of gaseous hydrogen from the electrochemical process. Lead could be present since it is sometimes used as an alloying element of zinc. Cadmium has no technical importance and is an undesirable impurity. None of the batteries contained higher heavy metal mass fractions than the permissible limits.
JATROPHA - The seed of energy CO2-neutral fuels and lubricants based on sustainable non-food oils
(2009)
Sulfate attack constitutes a major risk of chemical aggression for concrete and other building materials. Mainly structures exposed to sewage waters and sulfate rich soils are affected. The measurement of sulfate ingress is important for damage assessment previous to repair works and for quality assurance of the effectiveness of protecting coatings or during concrete removal.
Laser induced breakdown spectroscopy is introduced for the quantitative measurement of sulfur contents in building materials, providing detailed depth profiles and imaging element distributions with 1 mm spatial resolution. Detailed statistical evaluation is possible due to the spatial resolution and the fast measurement of the method. Practical applications of the method for damage assessment are demonstrated for three different sewage plants.
Methode und Prüfkörper zum Nachweis von Gussdefekten in Aluminiumbauteilen mit Computertomographie
(2009)
Accelerated weathering test for plastics and coatings that are exposed to acidic precipitation
(2009)
Due to the occurrence of acidic precipitation, and due to the fact that polymers and stabilizers may be sensititve to acids, it is important to have a laboratory test that combines weathering exposure with acidic exposure. The loss of stabilization caused by an acid damage of stabilizing system gets evident only over the weathering progress. For solid samples, for wich mostly the surface properties are relevant, the "Acid Dew and Fog Test" (ADF test) was established. For woven or tufted materials, the "Acid Rain Test" (AR test) was developed. The proposed weathering tests aim at plastics as well as at coatings.
High-power piezo-electric motors with power densities of 1.4 kW/kg display a potential for substituting hydraulic actuators. For this application, two novel tribometers of the same type have been designed using commercially available components for sliding motion at 40 kHz with amplitudes between 2.5 µm and 5 µm. The tribometers are equipped with means to measure amplitude, frequency, power required to keep the samples in motion and load applied. The effective motion between the two contacting bodies is monitored in each of the tribometers. These data are used to evaluate the coefficient of friction. The wear rate was determined after the tests. The set-ups were tested using well-known 100Cr6H (AISI 52100) samples before investigating novel, non-commercial substrates such as AlFeCrTi-alloys and tungsten carbide-based coatings as well as Magnéli-type coatings (Tin-2Cr2O2n-1 and TinO2n-1). This paper presents the principle of the ultra-high frequency tribometers and first tribological quantities of materials and coatings tested up to and above 1011 cycles. Very low wear rates in the range 10-8 mm³/Nm down to 10-10 mm³/Nm were determined under dry oscillation in air.