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- Concrete (6)
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- Non-destructive testing (5)
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Eingeladener Vortrag
- nein (250)
The 57Fe-Moessbauer spectrum of (dmpipzH2)2[FeIII(H2O)2Cl4][FeIII Cl4]Cl2 (1) consists of two doublets caused by a strongly distorted octahedral and a non-distorted tetrahedral component. Both (dmpipzH2)[FeIIIBr4]2 (2) and (trienH2)[FeIIIBr4]Br (3) show only one doublet indicating a more strongly distorted iron(III) species for 2 and a less-distorted one in the case of 3. For all compounds investigated, the ESR spectra reveal the existence of ground states with predominant antiferromagnetic coupling. The Néel temperatures amount to <4.2 K for 1, 4 K for 3 and 48 K for 2. In the case of 2, both the Moessbauer and the ESR spectra reveal the formation of exchange-coupled {FeBr4} units which has been attributed to a significant cation influence. The fine structure of residual paramagnetic [FeBr4]- subunits remaining in the crystalline matrix could be directly determined. Temperature dependent AC and DC susceptibility measurements of 2 and 3 confirmed the results.
Raman spectroscopic and 35Cl-NMR scans of Hydro-Xan®, a preparation containing the biocatalytically effective Tetrachlorinedecaoxide anion (TCDO), are described. The spectroscopic analyses showed that HydroXan® does not contain chlorite initially used in the preparation anymore. Furthermore, a structure of four equal chlorate-like ClO3-groups was indicated for TCDO by the scans. Such a structure is supported by the long-term stability of HydroXan® found at tests over 267 days.
Non-destructive evaluation of advanced materials by synchrotron radiation refraction topography
(2002)
Results of the inter-laboratory comparison "Determination of nanometric step heights with AFM"
(2002)
The interaction of nanosecond laser pulses in the ultraviolet wavelength range and femtosecond laser pulses in the near-infrared region with the direct semiconductor SiC and the composite compound SiC-TiC-TiB2 was investigated in respect to resulting physicochemical processes. Surface analytical techniques, such as XPS, µ-Raman, and EDX were used to identify the chemical changes between untreated and laser-treated areas. Single-pulse irradiation led to material
modifications in the condensed state in most instances. Multi-pulse results differed depending on the pulse duration. In the nanosecond case, melting of the surface and redeposited material (debris) were observed. With femtosecond pulses instead, only negligible melting and few debris could be detected. Additionally, periodic structures (ripples) appeared, with parallel orientation and in most cases two different periodicities for a particular material. Laser ablation of all the studied compound materials exhibited preferential ablation of the lighter component elements. Crystal structure changes of the irradiated surface were observed as a consequence of laser-induced melting and resolidification. An oxidation process interfered with all this processes so that unstoichiometric oxides were formed.
Part 3 of the ISO 14577 ¡°Instrumented indentation test for hardness and materials parameters¡° (IIT) concerns the calibration of reference blocks. Besides the widely spread activities for supplying reference blocks in the nano and micro range it is needed to be taken into account the macro range too. The paper reports on test results on ceramic materials which are tailored for reference blocks. The specimens made of Si3N4, SiC, or Al2O3 ceramics are highly homogenous and exhibit an increased quality with a roughness Ra ¡Ü 0.005 ¦Ìm. They are successfully used for reference blocks of the traditional Vickers and Knoop hardness. In comparison, the capability of hardened steel which is used for traditional hardness techniques is studied.
Instrumented indentation test for hardness and materials parameter from millinewtons to kilonewtons
(2002)
The ISO/DIS 14577 Metallic materials - Instrumented indentation test for hardness and
materials parameters Part 1-3 (IIT) concerns test forces up to 30 kN. The paper reports on
IIT at test forces ranging from 0.002 N to 1000 N on non magnetizable steel X8 CrMnN 18-
18 (1.386) with well polished surface using Vickers indenter and four hardness machines of
different design (Nano Indenter XP, Fischerscope H 100, Zwick Z005 with Universal
hardness head and a laboratory four-column set up materials testing machine) according to
the standard. Using mostly identical test parameters the results of the different machines are
almost in good agreement. Estimated small differences are caused by the different
uncertainties of the used machines and by different methods of mathematical analysis of the
detected raw data.
In 13C cross-polarisation magic angle spinning (CPMAS) spectra of soil samples, the paramagnetic soil constituents partially discriminate against the signal intensity of the 13C atoms. The aim of the present study was to check to what extent this signal depression depends on the paramagnetic ion content and if it is selective for a certain kind of carbon species. The spectra of a variety of particle size fractions of five quite different soils were recorded. A procedure was developed to compare quantitatively the relative carbon content of the different spectra. It was found that iron ions differ in their efficiency to discriminate against the carbon signals. Nevertheless a strong linear correlation between the detectability of carbon and 3(wt.%Fe) was observed for both the total signal and the signal of the different carbon species as well. This underlines that iron ions mainly influence the depression of the 13C signal in soil spectra. Furthermore we found, that for CFe ratios of 1.5 to 20 non-selective signal losses dominate. Despite a high percentage of non-detectable carbon (up to 90%), the 13C CPMAS spectra of our soil samples correctly reflect the relative composition of soil organic matter.
Long-term experiences with cathodic corrosion protection of steel reinforced concrete structures
(2002)
On the Applicability of Plasma Assisted Chemical Micropatterning to Different Polymeric Biomaterials
(2002)
A plasma process sequence has been developed to prepare chemical micropatterns on polymeric biomaterial surfaces. These patterns induce a guided localized cell layover at microscopic dimension. Two subsequent plasma steps are applied. In the first functionalization step a microwave ammonia plasma introduces amino groups to obtain areas for very good cell adhesion; the second passivation step combines pattern generation and creation of cell repelling areas. This downstream microwave hydrogen plasma process removes functional groups and changes the linkages of polymer chains at the outermost surfaces. Similar results have been obtained on different polymers including polystyrene (PS), polyhydroxyethylmethacrylate (PHEMA), polyetheretherketone (PEEK), polyethyleneterephthalate (PET) and polyethylenenaphthalate (PEN). Such a rather universal chemical structuring process could widen the availability of biomaterials with specific surface preparations.
Optical filters and fabrics are important parts of laser safety equipment such as goggles and curtains. A choice of these materials with varying absorption spectra is investigated with respect to their resistance to Ti:sapphire femtosecond laser radiation (800 nm wavelength, 1 kHz repetition rate). Pulse durations down to 30 fs and multiple-pulse irradiation conditions are employed to evaluate technically relevant damage thresholds. The ablation threshold fluences of the absorbing filters are comparable to those observed for transparent materials with 30-fs-pulses. These investigations together with scanning electron microscopy of the surface morphology after laser treatment provide insight into the interaction mechanism of the short pulses with the materials.
The removal and accelerated corrosion monitoring of metal coating systems is of general interest in materials science
and engineering technology. The femtosecond and nanosecond laser ablation and delamination at 800 nm and 532 nm,
respectively, of anodic oxide layers on aluminium alloys in electrolyte contact were investigated. Laser-induced
modifications of the oxide layer resulted in an ionic contact between electrolyte and metal, which produced a current
transient and thus allowed the in-situ electrochemical monitoring of the modification. Oxide coatings with different
optical properties, almost transparent and opaque, were examined. The transparent anodic oxides showed contrasting
ablation mechanisms in the nanosecond and femtosecond pulse duration regime: nanosecond pulses caused spallation,
whereas femtosecond treatment led to ablation. Current signals measured in the transparent film were consistent with
light absorption below the metal-oxide interface and with film spallation. Irradiation of the opaque coating yielded ionic
current transients within the so-called shock-affected-zone of the oxide layer. This investigation provided insight into the
role of the penetration depth of light and the heat-affected zone, the extent of the shock-affected zone, and the defect
formation in the coating and at the solid-solid interface between metal and oxide.
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.
The effectiveness of pressure relief devices on cylinders and tanks from a German point of view
(2002)
Fire accidents during road and rail transport are not occurring very often. In particular fire accidents with total fire engulfment of tanks seem to be rather rare. Up to now authorities in Europe officially are of the opinion that in densely populated regions like Europe in the space of time between the beginning of a fire and the rupture of a tank measures could be taken like cooling of the heated tank surface and evacuation of the area probably affected by an explosion. Therefore, no requirements with regard to fire protection measures concerning transport tanks for land mode like the application of safety relief devices have to be met. Due to some catastrophic accidents being discussed in public even European authorities are considering the pros and cons of fire protection measures.
Nevertheless in sparsely populated regions and during transport at sea fire accidents have been looked at since ever as seriously dangerous events. Therefore, multi modal tanks for the transport of dangerous goods have to be fitted with safety relief devices. The delivery capacity of these devices has to be such that, in the event of total fire engulfment, the pressure inside the tank does not exceed certain limits.
With regard to accident records and results of fire tests it has to be stated that portable tanks may rupture violently, even if the tanks are fitted with pressure-relief devices adequately designed for the heat flux of full fire engulfment.
Therefore, the lecture will be dealing with the results of fire testing of tanks and conclusions to be drawn and considerations on:
the advantages of different fire protection measures for transport tanks,
the pros and cons of safety relief devices for cylinders and transport tanks,
improvement of regulations and recommendations.
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 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.
Rapid and accurate non-destructive evaluation (NDE) techniques are needed to assess the in-place condition of concrete structures. However the time and effort required to perform NDE tests using conventional surface-mounted contact sensors hinder rapid evaluation of full-scale structures. The authors are cooperating in research to develop rapid and robust methods that collect mechanical wave signals from concrete structures and to characterize defects in concrete
using that signal data. The suitability of surface waves and laser-based, non-contact wave detection techniques for this purpose are examined here. After a brief introduction to non-contact sensing, an experimental set-up is described and results from experimental tests are presented. Mechanical surface waves in a concrete slab specimen are generated with several different conventional sources. The ability of a laser vibrometer to detect wave propagation from concrete that does not have any reflective treatment (normal concrete surface) is demonstrated, allowing the generation of ultrasonic images. Test results from a concrete specimen containing a subsurface defect are then presented. The obtained ultrasonic images illustrate some limitations of using surface waves to detect subsurface defects in concrete, although approaches to improve the results are proposed.
Various dibutyltin derivatives were polycondensed with aliphatic ,-dicarboxylic acids having chain lengths from 4 (succinic acid) to 22 carbon atoms. White crystalline products were obtained from all experiments, and the structure of the products was independent of the synthetic method. Viscosity measurements revealed low molecular weights (n 1 500 Da) in all cases. Vapor pressure osmometry (VPO) measurements and matrix-assisted laser desorption time-of-flight (MALDI-TOF) mass spectrometry proved that cyclic dimers and trimer were formed from dicarboxylic acids having 6 to 16 carbons, but mainly the monomeric cycle from docosane dioic acid. Heating to 250°C did not change the structure. Therefore, the results indicate that the macrocycles are the result of a thermodynamically controlled ring-closing polycondensation. This means that linear high-molecular weight poly(dibutyltin dicarboxylate)s cannot exist above room temperature.
BAM Reference Procedures
(2002)
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.
The isoelectric point is a material property for the characterization of acid-base behavior of the powder surface. The IEP of two alumina powders (AKP-30, Grade A) with different particle size characteristics in aqueous suspension has been determined by colloid vibration current (CVI) and particle charge detection (PCD) methods in moderately concentrated suspensions in order to qualify these methods for a future standardization. The solid loading of the suspensions were 1 and 5 vol%. The comparison of the IEP determined by PCD and CVI was in good agreement. However, the solid loading dependence of IEP and a large IEP hysteresis (at 1 vol%) were observed, which do not allow a proper determination of the IEP. The recording of the potential curve and therfore the determination of the IEP with CVI was difficult for the suspension of Grade A powder due to formation of agglomerates at pH values near the pHIEP.
Characterization of bond performance of textiles in cement matrices using fiber optic sensors
(2002)
Laboratory model test for monitoring the new main railway station of Berlin - The Lehrter Bahnhof
(2002)
Today's civil engineering NDT needs are for quantitative, fast to apply and easy to interpret methods. They are required on site both for evaluation of existing structures/infrastructure and for quality control in new construction. With this purpose, BAM has carried out in-situ feasibility studies, using radar, impact-echo and ultrasonic-echo methods. Two examples are given of their combined application on different railway slab–track constructions, using high frequency radar, scanning impact-echo and ultrasonic array methods. The aim was to evaluate limitations and advantages, comparability and complementarity of these methods. The on-site measurements demonstrated the possibility to investigate, with good accuracy via NDT, the bonding conditions between sleepers and slab, to locate voids and measure layer thickness. The acoustic and electromagnetic methods used, were found to be complementary.
Investigation of interphases between thermoplastic and thermosetting polymers - an AFM approach
(2002)
The gelcasting process was used for manufacturing porous ceramic bodies from nano sized powders. 3 different powders with specific surface areas between 12 and 30 m²/g were used. Solid content of the corresponding slurries was dependent on the milling procedure and the use of a suitable dispersant. For bimodal GradeA powder solid content was as high as 58 vol%. For sintering temperatures between 1250 and 1600°C the porosity varied between 45 and 20%, whereas the pore radii varied between 50 and 91nm. The grain size of crystallites in the sintered microstructures was about 1um. The reflection ratio for visible light increased in comparison to a reference sample made from conventional powder from 0.8 to 0.95 in the wavelenght range around 400nm.
Fire Tests with LPG Vessels
(2002)
The results and execution of many full scale fire engulfment tests on 3.6 and 4.85 m³ LPG tanks, protected with thin sublimation and intumescent coatings, mineral wool with steel jackets, vermiculite coatings and water spray systems, are presented.
Additional furnace tests with coated steel plates have been carried out to optimize the necessary coating thickness.
Similarly, an overview of the test conditions for the recognition based on technical rules and BAM requirements for fire protection systems of LPG tanks will be shown and explained.
When the internal pressure reaches the vessel bursting pressure a violent tank rupture, fragmenting of the shell and spontaneous release of the content are the consequences. In case of LPG this event is called "boiling liquid expanding vapour explosion (BLEVE)" with expanding fireball as an additional severe consequence.
For this reason the sufficient fire protection of LPG vessels is an important item.
The tests demonstrated sufficient vessel safety during 90 minutes of a full fire engulfment.
It will also be shown that the examinations and results are transferable to bigger tanks.
The transferability of the test results is illustrated by diagrams which show the dependence of the coating thickness against the shell thickness of the tank.
All tested tanks were equipped with pressure relief valves (PRVs) and partially filled with propane.
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.
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.
Various dibutyltin derivatives were polycondensed with aliphatic ,-dicarboxylic acids having chain lengths from 4 (succinic acid) to 22 carbon atoms. White crystalline products were obtained from all experiments, and the structure of the products was independent of the synthetic method. Viscosity measurements revealed low molecular weights (n 1 500 Da) in all cases. Vapor pressure osmometry (VPO) measurements and matrix-assisted laser desorption time-of-flight (MALDI-TOF) mass spectrometry proved that cyclic dimers and trimer were formed from dicarboxylic acids having 6 to 16 carbons, but mainly the monomeric cycle from docosane dioic acid. Heating to 250°C did not change the structure. Therefore, the results indicate that the macrocycles are the result of a thermodynamically controlled ring-closing polycondensation. This means that linear high-molecular weight poly(dibutyltin dicarboxylate)s cannot exist above room temperature.
This paper presents investigations on the tribological behaviour of PTFE composites against steel at cryogenic temperatures. The results showed that the friction coefficient decreases with temperature down to 77 K, but did not follow a linear evolution further down to extreme low temperatures. It can be stated that the cryogenic environment has a significant influence on the tribological performance of the polymer composites. The effect of low temperatures was more clearly detected at low sliding speed, where friction heat is reduced. A change in wear mechanism from adhesive to abrasive was observed in this case. SEM and AFM analyses showed that the PTFE matrix composites investigated under these experimental conditions have transferred material onto the disc down to very low temperatures. Chemical analyses indicate the presence of iron fluorides.