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Numerous membrane importers rely on accessory water-soluble proteins to capture their substrates. These substrate-binding Proteins (SBP) have a strong affinity for their ligands; yet, Substrate release onto the low-affinity membrane transporter must occur for uptake to proceed. It is generally accepted that release is facilitated by the association of SBP and transporter, upon which the SBP adopts a conformation similar to the unliganded state, whose affinity is sufficiently reduced. Despite the appeal of this mechanism, however, direct supporting evidence is lacking. Here, we use experimental and theoretical methods to demonstrate that an allosteric mechanism of enhanced substrate release is indeed plausible.
First, we report the atomic-resolution structure of APO TeaA, the SBP of the Na!-coupled ectoine TRAP transporter TeaBC from Halomonas elongata DSM2581T, and compare it with the substrate-bound structure previously reported. Conformational freeenergy landscape calculations based upon molecular Dynamics simulations are then used to dissect the mechanism that couples ectoine binding to structural change in TeaA. These insights allow us to design a triple mutation that biases TeaA toward apo-like conformations without directly perturbing the binding cleft, thus mimicking the influence of the membrane transporter. Calorimetric measurements demonstrate that the ectoine affinity of the conformationally biased triple mutant is 100-fold weaker than that of the wild type. By contrast, a control mutant predicted to be conformationally unbiased displays wild-type affinity. This work thus demonstrates that substrate release from SBPs onto their Membrane transporters can be facilitated by the latter through a mechanism of allosteric modulation of the former.
The introduction of carbon nanotubes (CNTs) modifies bulk polymer properties, depending on intrinsic quality, dispersion, alignment, interfacial chemistry and mechanical properties of the nanofiller. These effects can be exploited to enhance the matrices of conventional microscale fibre-reinforced polymer composites, by using primary reinforcing fibres grafted with CNTs. This paper presents a methodology that combines atomic force microscopy, polarised Raman spectroscopy, and nanoindentation techniques, to study the distribution, alignment and orientation of CNTs in the vicinity of epoxy-embedded micrometre-scale silica fibres, as well as, the resulting local mechanical properties of the matrix. Raman maps of key features in the CNT spectra clearly show the CNT distribution and orientation, including a parted morphology associated with long grafted CNTs. The hardness and indentation modulus of the epoxy matrix were improved locally by 28% and 24%, respectively, due to the reinforcing effects of CNTs. Moreover, a slower stress relaxation was observed in the epoxy region containing CNTs, which may be due to restricted molecular mobility of the matrix. The proposed methodology is likely to be relevant to further studies of nanocomposites and hierarchical composites.
The isotopic composition of boron is a well established tool in various areas of Science and industries. Boron isotope compositions are typically reported as 6"B values which indicate the isotopic difference of a sample relative to the internationally accepted isotope reference material NIST SRM 951. A significant drawback of all of the available boron isotope reference materials is that non covers a natural boron isotope composition apart from NIST SRM 951.
The variation of isotope abundance ratios is increasingly used to unravell natural and technical questions. In the past the investigation and interpretation of such variations was the field of a limited number of experts. With new upcoming techniques and research topics in the last decades, such as provenance and authenticity of food, the number of published isotope data strongly increased. The development of inductively coupled plasma mass spectrometers (ICPMS) from an instrument for simple quantitative analysis to highly sophisticated isotope abundance ratio machines influenced this process significantly. While in former times only experts in mass spectrometry were able to produce reproducible isotope data, nowadays many laboratories, never been in touch with mass spectrometry before, produce isotope data with an ICPMS. Especially for such user isotope reference materials (IRM) are indispensible to enable a reliable method validation. The fast development and the broad availability of ICPMS also lead to an expansion of the classical research areas and new elements are under investigation. Here all users require IRM to correct for mass fractionation or mass discrimination or at least to enable isotope data related to a common accepted basis. Despite this growing interest suitable IRM are still lacking for a number of isotope systems such as magnesium.
Highly energetic silicon tetraazide 1 is synthesized safely in high yield and high purity. The compound is prepared as a solution in benzene which allows it to be handled safely. Stable Lewis base adducts of Si(N3)4 (e.g. 2) are also prepared by treatment of either Si(N3)4 or the disodium salt of hexaazidosilicate (3) with Lewis bases (2,2-bipyridine or 1,10-phenanthroline). Unlike Si(N3)4 the Lewis base adduct 2 is thermally stable and does not decompose below 265 °C. The decomposition is very energetic (ΔHd = -2.4 kJg-1) which means 2 and related Lewis base adducts could replace environmentally harmful Pb(N3)4 used as primary explosive.
The wear behaviour of thin steel wires has been analyzed under oscillating sliding conditions in crossed cylinders contact geometry. The focus of this analysis was the influence of the crossing angle between the wires on the wear. The wires used had 0.45 mm in diameter and the material was cold-drawn eutectoid carbon steel (0.8% C) with a tensile strength higher than 2800 MPa. Two different types of tests were carried out, the first one representing the influence of the crossing angle for a constant load and the second one representing the influence of the crossing angle with constant contact pressure. In the first type of tests it was seen that as the contact angle decreases the contact pressure decreases too and hence less energy specific wear resistance is observed. As a consequence less wear is produced, thus increasing the life of the wires. In the second type of tests it was seen that with constant contact pressure but different crossing angles, nearly the same energy specific wear resistance was observed. This points at an identical wear behaviour in both type of tests but with a running-in and a steady state period as two different wear periods. The tests showed that the running in period may play an important role in the overall wear particle generation and hence the wear occurring in the steady state period is rather mild.
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.
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.
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.
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.
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.
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.
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.
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.