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Eingeladener Vortrag
- nein (250)
The 1,3-diphenyl-1H-pyrazolo[3,4-b]-quinoline chromophore is a versatile building block for the construction of brightly fluorescent molecular sensors. Facile synthetic procedures allow integration of the chromophore into fluorophore-spacer-receptor systems as well as fluoroionophores operating via intramolecular charge transfer. Whereas the former photoinduced electron-transfer probes show strong analyte-induced fluorescence enhancement, the latter exhibit bright ratiometric dual emission. Employing prototype macrocyclic receptors, the favorable signaling features for metal ion recognition are demonstrated.
The preparation and structural investigation of 17O-enriched xNa2O(100-x)P2O5 glasses (46.5<=x<=62.8) by nuclear magnetic resonance (NMR) is described. Enriched phosphoric acid was prepared by hydrolysis of PCl5 with 17O-enriched water and neutralized with sodium carbonate. The sodium metaphosphate was then melted at 800 °C for 15 h and quenched. Polyphosphate and ultraphosphate glass compositions were prepared by remelting the metaphosphate with sodium carbonate and phosphorus pentoxide, respectively. 31P magic angle sample spinning (MAS) NMR was used to determine the Na2O/P2O5 content in the glasses. 17O NMR spectra (quadrupole echo for non-rotating samples and multiple-quantum excitation for rotating samples (MQMAS)) show two oxygen sites in the samples with large quadrupolar coupling constants (4.7 and 7.7 MHz), in accordance with the high phosphorus electronegativity. According to the correlation of 17O quadrupolar constants with bond ionicity, these two components are attributed to bridging POP and non-bridging PO...Na oxygens. The average POP bond angle is estimated with the quadrupolar asymmetry derived from the fit of the static echo spectra. The MQMAS spectrum shows a distribution of non-bridging oxygen chemical shifts, attributed to a variation of bond length and angle.
A novel fluorescent host-guest material, molecular sieves of AlPO4-5-type doped with 2,2'-bipyridyl-3,3'-diol, was prepared and spectroscopically characterized. The composite crystals show a pronounced optical anisotropy, indicating a high degree of alignment of the guest molecules within the zeolitic pore system. A mean tilting angle of 22 was found for the orientation of the individual dye molecules in the straight channels. The corrected fluorescence emission spectra were determined, and time-resolved fluorescence studies revealed that the dye molecules are preferentially found in three different types of microenvironment. By invoking pH-dependent studies of the dye in aqueous solution, we could trace these spectroscopic features back to two main influences, coadsorbed water within AlPO4-5 pores and guest-host interactions with a few relatively weak Brnsted acid (defect) sites of the inorganic host network.
In collaboration with the United States Department of Agriculture and a number of major milling companies, the "Insect-Detect" immunoassay for analyzing insect contamination in grains has been compared with three more traditional methods, X-ray analysis, cracking and flotation, and the insect fragment test (IFT). Testing was carried out in blind fashion using clean wheat samples that were spiked with differing numbers of grain kernels infested with late instar larvae of the granary weevil (Sitophilus granarius (L.)). Three different laboratories analyzed the samples for each of the four methods. The collaborative trials showed that the insect immunoassay clearly provided the most accurate measurement of actual insect infestation, followed by X-ray analysis. While both cracking and flotation and IFT procedures provided a general measure of contamination, they showed much greater variability.
Nowadays, micro-x-ray fluorescence analysis has become an established tool for the non-destructive investigation of art objects. However, as these types of sample often forms complex and inhomogeneous layer systems, the quantitative evaluation of the measurements is far from a standard routine. In this paper a fingerprint model is described, which we developed to discriminate between different iron-gall inks of historical manuscripts or compositions. Fundamental parameter methods are used to take self-attenuation, interference from the paper background and diffusion of the ink into the paper into account. The capability of the method to contribute to the solution of archaeometric problems is exemplified by the investigation of an ancient composition. Finally, the restrictions of the model and possible improvements are discussed. Copyright © 2004 John Wiley & Sons, Ltd.
A constitutive model for the mechanical behavior at high temperatures of superalloys with a high volume fraction of the ? ? phase is derived from an analysis of the main deformation mechanisms. The model assumes periodically distributed cubic ? ? particles and an homogeneous slip distribution perpendicular to the slip planes inside the matrix channels and the particles. It accounts for octahedral and cubic slip in the ? channels, recovery by climb of loops around the precipitates until complete annihilation, shear of both matrix and precipitates by complete matrix dislocations and partial slip reversal during unloading. The back-stresses of the constitutive law are identified with the long-range internal stresses in the microstructure which are explicitly calculated by Fourier series for a simplified distribution of the plastic strains in the microstructure. In particular the three types of channels are distinguished. The internal variables of the model are the plastic strains produced by each mechanism, the number of mobile loops in the ? channels and the scalar dislocation density in the ?/? ? interfaces for each slip system.
A reference material for calibration and testing of instruments with nanometric lateral resolution
(2002)
A reference material for calibration and testing of instruments with nanometric lateral resolution
(2002)
A consortium has recently been initiated to study the macroscopic and microscopic properties of basaltic and andesitic rocks as analogue materials for Mars. The goal of this project is the integration of diverse spectroscopic approaches to
evaluate the composition and texture of Mars materials using both in situ and remote sensing techniques. Initial emphasis is placed on assessment of the mineral composition for low albedo areas (basalt vs andesite vs weathering) of the Martian surface through spectral analysis of a suite of samples that have been exceptionally well characterized in the laboratory. The initial results indicate that the visible/NIR reflectance spectra, mid-IR reflectance and emission spectra, and Mössbauer spectra contain consistent diagnostic features associated with the measured modal mineralogy and provide baseline data for the first group of well characterized basalts. The consortium study involves integrating multiple remote sensing techniques for recent and upcoming missions to Mars in order to compare the results obtained by these instruments and thereby strengthen interpretive results.
A consortium has recently been initiated to study the macroscopic and microscopic properties of basaltic and andesitic rocks as analogue materials for Mars. The goal of this project is the integration of diverse spectroscopic approaches to
evaluate the composition and texture of Mars materials using both in situ and remote sensing techniques. Initial emphasis is placed on assessment of the mineral composition for low albedo areas (basalt vs andesite vs weathering) of the Martian surface through spectral analysis of a suite of samples that have been exceptionally well characterized in the laboratory. The initial results indicate that the visible/NIR reflectance spectra, mid-IR reflectance and emission spectra, and Mössbauer spectra contain consistent diagnostic features associated with the measured modal mineralogy and provide baseline data for the first group of well characterized basalts. The consortium study involves integrating multiple remote sensing techniques for recent and upcoming missions to Mars in order to compare the results obtained by these instruments and thereby strengthen interpretive results.
Ability of Non-Destructive Testing to Contribute to Humanitarium Mine Detection and Clearance
(2002)
A comparative analysis of selected standards and guidelines on Acoustic Emission testing published by international and national organisations yields an assessment of the current status of standardisation. Areas where existing documents do not yet exist or appear unsatifactory for some reason are identified and formulated as perspectives for further work. In the future, structural integrity assessment with Acoustic Emission methods is expected to gain in importance.
The dismutation of CHClF2 to CHF3 and CHCl3 was used to probe the effect of γ-Al2O3 fluorination on fluorine-against-chlorine (Cl/F) exchange reactions. X-ray photoelectron spectroscopy (XPS), X-ray excited Auger electron spectroscopy (XAES) and X-ray absorption near edge structure (XANES) spectroscopy were employed to probe the modifications at the surface of γ-Al2O3 accompanying the initial stages of fluorination. The results suggest that fluorine uptake by γ-Al2O3 starts initially at the surface of the oxide particles, with the formation of a fluorine species that is characterised by a single bond and a high effective charge q. Catalytic Cl/F-exchange is only observed after accumulation of higher fluorine concentrations, for which insertion of fluorine into the sub-surface region of the oxide crystallites has commenced. Quantitative XPS shows that the fluorination level must exceed approximately 10 atom% of the anions to achieve catalytic activity. The spectroscopic evidence suggests that the formation of aluminium oxofluorides is sufficient to provide catalytic activity. The presence of an AlF3 phase is not a condition for the observation of catalytic activity, even though defect-rich AlF3 is ultimately the endpoint of the fluorination process and is itself a Cl/F exchange catalyst.
A series of Cp(C5H5)ZrCl2 and Cp2ZrCl2 pre-catalysts (Cp = C5HMe4, C4Me4P, C5Me5, C5H4tBu, C5H3-1,3-tBu2, C5H2-1,2,4-tBu3) together with (C5H5)2ZrCl2 was used for the directed oligomerization of propene and 1-hexene in comparative experiments. Oligomer characterization was carried out by 1H NMR, SEC (GPC), MALDI-TOF MS, cryoscopy and Raman spectroscopy. From 1H NMR the nature and relative ratio of the double-bond end group is determined together with n if every oligomer molecule contains such a double-bond end group. Normally vinylidene double bonds (from -hydrogen elimination) are found. From 1H NMR and MALDI-TOF MS also vinyl end groups (from -methyl elimination) are observed in the case of oligopropenes with (C4Me4P)- (C5H5)ZrCl2 and with the symmetrical methyl containing Cp2ZrCl2 pre-catalysts. The vinylidene/vinyl ratio depends on the ligand and increases from C5HMe4 (65/35) over C4Me4P (61/39) to C5Me5 (9/91). A comparison of n from 1H NMR and SEC together with MALDI-TOF MS shows that the phospholyl-zirconocenes and (C5HMe4)2ZrCl2 also exhibit chain transfer to aluminium, thereby giving saturated oligomers.
The application of impulse radar for structural investigation of concrete elements has been increased during the last years related to technical developments, i. e. of high frequency antennas. In this paper, case studies will be presented related to the location of reinforcing bars, tendon ducts and repaired concrete areas in concrete bridges, anchors and dowels in concrete highways and delaminations of layered structures as they are used for non-ballasted railway tracks. It is shown that impulse radar can be applied in case of regular inspection and for searching the cause of damages but also for quality assessment in civil engineering.
Prestressing steels can be exposed in prestressed concrete structures in construction stage (ungrouted duct) to environmental conditions causing formation and growth of hydrogen induced cracks with brittle fracture of the steel. The risk of this hydrogen induced stress corrosion cracking can be minimized by appropriate treatment, but there is a requirement for construction to approve only prestressing steel having no enhanced susceptibility to stress corrosion cracking. The paper describes the historical development of the different test methods proposed in the past and gives an overview on the general requirements for a suitable test method to assess the hydrogen-induced stress corrosion susceptibility of prestressing steels.
Since 1982, based on investigations on construction sites and transfer of the results into laboratory tests, a test method is available enabling realistic estimation of suitable application possibilities of prestressing steels. This so called DIBt-test is approved to distinguish between prestressing steels susceptible to hydrogen induced stress corrosion cracking and those suitable and therefore approvable steels at practical environmental conditions. Furthermore the test enables estimation of corrosion risk for newly developed prestressing steels with higher strength.
Translated Abstract
Beurteilung der Prüfverfahren zur Untersuchung der Spannungsrisskorrosionsempfindlichkeit von Spannstählen
Spannstähle können in Spannbetonbauwerken im Bauzustand (unverpresstes Hüllrohr) Umgebungsbedingungen ausgesetzt sein, die zur Bildung und Ausbreitung wasserstoffinduzierter Risse mit Sprödbruch des Stahles führen können. Das Risiko dieser wasserstoffinduzierten Spannungsrisskorrosion kann einerseits durch eine sachgemäße Verarbeitung der Spannstähle minimiert werden, andererseits besteht die Notwendigkeit nur solche Spannstähle für die Baupraxis zuzulassen, die unter baupraktischen Bedingungen keine erhöhte Empfindlichkeit für Spannungsrisskorrosion besitzen. Die vorliegende Arbeit beschreibt die historische Entwicklung der verschiedenen vorgeschlagenen Prüfverfahren und gibt einen Überblick über die allgemeinen Anforderungen an ein geeignetes Verfahren zur Beurteilung der wasserstoffinduzierten Spannungsrisskorrosionsempfindlichkeit von Spannstählen.
Seit 1982 steht, begründet durch Untersuchungen auf Baustellen und Umsetzung der Ergebnisse in Laborversuchen, ein Prüfverfahren zur Verfügung, das eine wesentlich realistischere Einschätzung der Einsatzmöglichkeiten von Spannstählen zulässt. Dieser sog. DIBt-Test hat sich bewährt, um unter praktischen Umgebungsbedingungen gegen H-induzierte Spannungsrisskorrosion empfindliche Spannstähle von geeigneten und damit zulassungswürdigen Stählen zu unterscheiden. Des weiteren erlaubt die Prüfung ebenfalls eine Abschätzung des Korrosionsrisikos für neuentwickelte, höherfeste Spannstähle.
BAM Reference Procedures
(2002)
The European biocides directive (98/8/EG) demand the control of emissions into the envi-ronment like soil, water and air. In this study a method for measuring the input of biocides into the indoor air from materials should be developed. The emission of two products containing biocides (plastic foil, wool carpet) and six different types of biocide containing formulations applied on wood or ceramic tiles were investigated in 20 or 23 l glass emission chambers. Each chamber test was performed over a period of 100 up to 200 days. SVOC show totally different emission curves in chamber tests compared to volatile organic com-pounds (VOC). They reach their maximum value after some days or weeks. Thus a period of 3 months is sometimes necessary for exact measurements. Area specific emission rates (SERa in µg/m²h) for permethrin (0.006), propiconazole (0.2), dichlofluanid (1.5), tolylfluanid (1.2), octylisothiazolinone (2.5) and for iodpropinylbutyl-carbamat (1.7) were determined.
The adhesion of poly(methyl methacrylate) (PMMA) and polystyrene (PS) films, whose surface has been previously structured by dynamic plowing lithography (DPL), has been measured by means of forcedisplacement curves. The different adhesion of modified and unmodified PS leads to the assumption that polymer chains are broken during DPL. After measuring the energy dissipated by the tip during DPL, in order to check that the transferred energy is sufficient to break covalent bonds, the polymer chain scission caused by the lithographic process has been definitely confirmed by size exclusion chromatography measurements of the lithographed films.
Bridge-Management-Systems
(2002)
This Report describes the certification of the reference material antimony implanted in Si/SiO2 intended to be used for calibration of surface and near surface analytical methods. It describes the preparation, homogeneity measurements and the analytical work performed for the certification of both Areal density of antimony Atoms (retained dose) and the isotope amount Ratio as well as giving considerations on the stability of the material.
The Bundesanstalt für Materialforschung und -prüfung (Federal Institute for Materials Research and Testing) (BAM) is establishing a system of primary reference materials to meet the demands for metrological traceability and to act as national standards in the field of elemental analysis. For all elements of the periodic table - except those that are gases or radioactive - two different kinds of reference materials are being certified. One is for analyte calibration (Type A) and one for problems concerning matrix matching (Type B). These substances are of very high purity and of defined stoichiometry. As far as possible, pure elements and metals rather than pure compounds are used. The certification of both types of material requires most elements of the periodic table to be certified at very low levels using trace element analysis methods. The application of these methods is described and examples of the certification of copper and iron are given.
FAU membranes of type NaX and MFI membranes of type silicalite-1 which contain adsorbed azobenzene (AZB), have photoswitchable permeation properties due to the transcis photoisomerization of AZB. The change of gas permeation through these hostguest composite membranes depends on the irradiation wavelength, the quality of the membranes and the amount of adsorbed AZB. The permeances of the gases in the trans-form of the zeolite-encapsulated AZB were higher than those in the cis-form. The separation factors of equimolar mixtures of N2/CO2 and CH4/CO2 fed through the FAUAZB membrane were higher at trans-switching than at cis-switching. The changes of the permeances of single gases and of the separation factors of equimolar gas mixtures by photoinduced transcis switching were found to be reversible over numerous switching cycles. The experimental results are in agreement with predictions made by Monte Carlo simulations for passing of permeant gases through these hostguest systems with the zeolite-hosted AZB in the trans- and in the cis-configuration.
Alkyl polyglycosides today represent the most important sugar surfactant. Nonionic sugar surfactants produced via different synthetic routes are mixtures of alkyl homologues, oligomers, anomers and isomers. Alkyl homologues and oligomers of alkyl mono- and diglucosides were separated by reversed-phase high-performance liquid chromatography (HPLC) with methanolwater as the mobile phase using a gradient elution. The gradient was optimized in respect to a simultaneous separation of alkyl glycosides according to their alkyl chain length and alkyl polyoxyethylene glucosides with regard to their length of the polyoxyethylene spacer. The separation of alkyl glycosides into ?- and ?-anomers was carried out by normal-phase HPLC with isooctaneethyl acetate (60:40, v/v)2-propanol in the gradient mode. Light scattering detection was used. Matrix-assisted laser desorption ionization time-of-flight mass spectra of alkyl glucosides and dodecyl glucosides with oxyethylene spacer groups are presented.
Characterization of bond performance of textiles in cement matrices using fiber optic sensors
(2002)
In this study an attempt is made to investigate the influence of surface treatments such as oxidation and sizing on a high-strength carbon fibre in respect of interfacial adhesion in composite materials with a cyanate matrix. For analysing the fibre/resin interfacial adhesion the single-fibre pull-out technique has been used. The interfacial shear strengths obtained by this technique have been compared with results of interlaminar shear strength measurements corresponding to woven composite plates. In order to clarify the nature of this interfacial adhesion, both morphological (by atomic force microscopy, AFM) and chemical characterisation (by Fourier transform infrared, FTIR), have also been carried out.