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In the course of tomorrow's hydrogen-based energy transition, the construction of the corresponding infrastructure will play a central role. The majority of materials used to date are typically welded for component fabrication. In that context, steels are widely applied and can be prone to hydrogen embrittlement. For the evaluation of any hydrogen effect on, for example, the mechanical properties of a welded metallic material, the hydrogen content must be precisely determined. According to ISO 3690, carrier gas hot extraction (CGHE) can be used. In addition to the pure quantification of hydrogen, thermal desorption analysis (TDA) with varied heating rates can be used to determine and evaluate the bonding state at microstructural defects in the material. For both techniques, experimental and measurement influences have to be considered, which have a great effect on the result. For CGHE, for example, ISO 3690 suggests different sample geometries as well as minimum extraction times. The present study summarizes results and experiences of numerous investigations with different sample temperatures and geometries (ISO 3690 type B and cylindrical TDA samples) regarding: the influence of the sample surface (polished/welded), measurement accuracies depending on the sample volume. In particular, a deviating extraction temperature to the set temperature, can significantly falsify the measurement results. Based on the results, methods are shown to quickly reach the desired extraction temperature without having to physically interfere with the measurement equipment. This serves to substantially improve the reliability of hydrogen measurement through increased signal stability and accelerated hydrogen desorption. In general, an independent temperature measurement with dummy samples for the selected heating procedure is advisable to exclude possible unwanted temperature influences already before the measurement. In addition (and way more important), the methods described can be transferred directly to industrial applications.
Crystallization is a complex phenomenon with farreaching implications for the production and formulation of active pharmaceutical ingredients. Understanding this process is critical for achieving control over key physicochemical properties that can affect, for example, the bioavailability and stability of a drug. In this study, we were able to reveal intricate and diverse dynamics of the formation of metastable intermediates of paracetamol crystallization varying with the choice of solvent. We demonstrate the efficacy of our novel approach utilizing an objective function-based non-negative matrix factorization technique for the analysis of time-resolved Raman
spectroscopy data, in conjunction with time-lapse photography.
Furthermore, we emphasize the crucial importance of integrating Raman spectroscopy with supplementary experimental instrumentation for the mathematical analysis of the obtained spectra.
Vibration measurements have many causes and many technical and natural sources. Problems can sometimes be solved by short-term measurements, but in many cases, a long-term measurement is necessary. In long-term measurements of days, weeks, months and even years, it is easy to collect a huge quantity of raw data, but at the end, the post-processing of these data can be exhausting (for example one-year vibration data of a wind energy tower). A software has been developed which con-sists of measuring and evaluation routines where the measuring routines can operate different meas-uring systems and different measuring cards. The main advantage of this software is the fact that the interesting evaluations can be integrated in the measuring process so that the characteristics of the vibration can be extracted without storing all the raw data. Only important time segments are stored, for example train passages. The overall concept of the software and the main evaluation routines will be described in some details. Examples of our measurement experience will illustrate the capabilities of the software. 1) Surveying construction work in nearby sensitive buildings (for example an old wind tunnel), including a stable alarm system and meaningful vibration limits. 2) Prediction of train-induced vibration for a planned building to prevent annoyance and to improve the building design. 3) Modal analysis and long term measurements of several single- or multi-span, concrete or steel bridges 4) Modal and wave analysis of coupled floors in a historical building (“Neues Palais” at Potsdam). 5) Soil properties of various measurement sites (different routines to evaluate the dispersion). Moreover, from many projects, amplitudes, frequencies, and attenuation laws have been collected and analysed for the different sources such as vibratory or impact pile driving and ground compaction, demolition work with different machines, blasting in quarries and in tunnel works, bomb and mine clearing.
Vibration measurements have many causes and many technical and natural sources. Problems can sometimes be solved by short-term measurements, but in many cases, a long-term measurement is necessary. In long-term measurements of days, weeks, months and even years, it is easy to collect a huge quantity of raw data, but at the end, the post-processing of these data can be exhausting (for example one-year vibration data of a wind energy tower). A software has been developed which con-sists of measuring and evaluation routines where the measuring routines can operate different meas-uring systems and different measuring cards. The main advantage of this software is the fact that the interesting evaluations can be integrated in the measuring process so that the characteristics of the vibration can be extracted without storing all the raw data. Only important time segments are stored, for example train passages. The overall concept of the software and the main evaluation routines will be described in some details. Examples of our measurement experience will illustrate the capabilities of the software. 1) Surveying construction work in nearby sensitive buildings (for example an old wind tunnel), including a stable alarm system and meaningful vibration limits. 2) Prediction of train-induced vibration for a planned building to prevent annoyance and to improve the building design. 3) Modal analysis and long term measurements of several single- or multi-span, concrete or steel bridges 4) Modal and wave analysis of coupled floors in a historical building (“Neues Palais” at Potsdam). 5) Soil properties of various measurement sites (different routines to evaluate the dispersion). Moreover, from many projects, amplitudes, frequencies, and attenuation laws have been collected and analysed for the different sources such as vibratory or impact pile driving and ground compaction, demolition work with different machines, blasting in quarries and in tunnel works, bomb and mine clearing.
Increasing requirements on the infrastructure caused by more and heavier traffic coincide with both the aging and the progressive degradation of bridge constructions. These exemplary issues lead to a non-negligible need for reassessments of existing bridges. Compared to the new building design, safety reserves can be used in the evaluation of such existing structures, since uncertainties that may arise during the design, construction and previous Service time are better known or no longer present. Uncertainties can be evaiuated more precisely by measurements. In the meantime, the application of advanced NDT-methods on concrete structures have become so capable, that crucial structure Parameters like certain material properties or geometrical dimensions can be quantified without significant destructive interventions. The measured data can be explicitly incorporated into the probabilistic computation models used for the bridge reassessment in form of random variables. Therewith, a previously insufficient model can be refined to achieve a higher level of approximation. This contribution emphasises two fundamental steps of the measured data based probabilistic reassessment: The sensitivity analyses to identify the cruciai Parameters and the needed accuracy of the related information as well as the comparison with expected uncertainties of non-destructively measured Parameters.
Increasing requirements on the infrastructure caused by more and heavier traffic coincide with both the aging and the progressive degradation of bridge constructions. These exemplary issues lead to a non-negligible need for reassessments of existing bridges. Compared to the new building design, safety reserves can be used in the evaluation of such existing structures, since uncertainties that may arise during the design, construction and previous Service time are better known or no longer present. Uncertainties can be evaiuated more precisely by measurements. In the meantime, the application of advanced NDT-methods on concrete structures have become so capable, that crucial structure Parameters like certain material properties or geometrical dimensions can be quantified without significant destructive interventions. The measured data can be explicitly incorporated into the probabilistic computation models used for the bridge reassessment in form of random variables. Therewith, a previously insufficient model can be refined to achieve a higher level of approximation. This contribution emphasises two fundamental steps of the measured data based probabilistic reassessment: The sensitivity analyses to identify the cruciai Parameters and the needed accuracy of the related information as well as the comparison with expected uncertainties of non-destructively measured Parameters.
BAM is the German Federal Institute for Materials Research and Testing and the competent authority for mechanical and thermal safety assessment of transport packages for spent fuel and high level waste. In context with safety assessment of RAM packages BAM performed numerous drop tests in the last decades. The tests were mostly accompanied by extensive and various measurement techniques especially by instrumented measurements with strain gages and accelerometers.
The procedure of drop testing and the resulting measurement analysis are the main methods to evaluate the safety against mechanical test conditions. Measurement techniques are dedicated to answer questions in regard to the structural integrity of a RAM package, the mechanical behaviour of the prototype as well as of its content under impact conditions.
Test results like deceleration-time functions constitute a main basis for the validation of assumptions in the safety analysis and for the evaluation of numerical calculations. In this context the adequate selection of accelerometers and measurement systems for the performance of drop tests is important. Therefore it is not only necessary to find suitable positions for the accelerometers at the test specimens, but also to consider technical boundary conditions as e.g. temperature. Accelerometers are widely used for the measuring of motion i.e. velocity or the displacement of the rigid cask body, vibration and shock events.
Acceleration measurements as well as their analysis are often very complex and extensive also because they are in turn embedded in complex drop test experiments having to consider difficult boundary conditions as for example very low specimen temperatures, large drop heights and sophisticated drop orientations of the specimen. In every case special instruments and adequate technical equipment is required to accelerations under these and transient shock conditions which are characterized in our case by impact times in the range of a few milliseconds up to perhaps 100 Milliseconds naturally depending on container design and drop test conditions as drop height and target.
The paper gives an overview of drop tests under kinematic aspects performed with RAM packages. Furthermore, experimental advancements of accelerometer instrumentation within drop testing, e.g. the characteristics and possibilities of accelerometers, behavior of accelerometers and various influence factors are shown.
The reassessment of bridges is becoming increasingly important. The basic requirement for analyses of structural safety is reliable knowledge about individual structures. This paper introduces the new approach to evaluate the quality of measured data gained from non-destructive testing (NDT) to provide reliable, objective, and relevant information about existing bridges. The purpose is to relate this validated knowledge to probabilistic analyses. Bridging the gap between NDT and numerical reassessments indicates reduced numerical uncertainties and residual service time extensions. This paper deals with an application of this approach using measurement data collected by ultrasonic technique at a prestressed concrete bridge.
The reassessment of bridges is becoming increasingly important. The basic requirement for analyses of structural safety is reliable knowledge about individual structures. This paper introduces the new approach to evaluate the quality of measured data gained from non-destructive testing (NDT) to provide reliable, objective, and relevant information about existing bridges. The purpose is to relate this validated knowledge to probabilistic analyses. Bridging the gap between NDT and numerical reassessments indicates reduced numerical uncertainties and residual service time extensions. This paper deals with an application of this approach using measurement data collected by ultrasonic technique at a prestressed concrete bridge.
BAM is the German Federal Institute for Materials Research and Testing and the competent authority for mechanical and thermal safety assessment of transport packages for spent fuel and high level waste. In context with safety assessment of RAM packages BAM performed numerous drop tests in the last decades. The tests were mostly accompanied by extensive and various measurement techniques especially by instrumented measurements with strain gages and accelerometers.
The procedure of drop testing and the resulting measurement analysis are the main methods to evaluate the safety against mechanical test conditions. Measurement techniques are dedicated to answer questions in regard to the structural integrity of a RAM package, the mechanical behavior of the prototype as well as of its content under impact conditions.
Test results like deceleration-time functions constitute a main basis for the validation of assumptions in the safety analysis and for the evaluation of numerical calculations. In this context the adequate selection of accelerometers and measurement systems for the performance of drop tests is important. Therefore it is not only necessary to find suitable positions for the accelerometers at the test specimens, but also to consider technical boundary conditions as e.g. temperature.
BAM is the German Federal Institute for Materials Research and Testing and the competent authority for mechanical and thermal safety assessment of transport packages for spent fuel and high level waste. In context with safety assessment of RAM packages BAM performed numerous drop tests in the last decades. The tests were mostly accompanied by extensive and various measurement techniques especially by instrumented measurements with strain gages and accelerometers.
The procedure of drop testing and the resulting measurement analysis are the main methods to evaluate the safety against mechanical test conditions. Measurement techniques are dedicated to answer questions in regard to the structural integrity of a RAM package, the mechanical behavior of the prototype as well as of its content under impact conditions.
Test results like deceleration-time functions constitute a main basis for the validation of assumptions in the safety analysis and for the evaluation of numerical calculations. In this context the adequate selection of accelerometers and measurement systems for the performance of drop tests is important. Therefore it is not only necessary to find suitable positions for the accelerometers at the test specimens, but also to consider technical boundary conditions as e.g. temperature.
Hydrogen determination in weld seams is standardized in ISO 3690. In accordance to this standard, a defined time for hydrogen collection has to be anticipated for different extraction temperatures. In other words, the temperature is the most important value that has to be monitored in addition to the aimed hydrogen determination.
The specimen geometry has influence on the real sample temperature during CGHE vs. the adjusted furnace temperature. This presentation gives a short summary on possible influences on the "correct" hydrogen determination temperature during carrier gas hot extraction (CGHE) using infrared radiation driven furnace. The main findings are: (1) specimen surface is important in terms of polished or oxidized condition, (2) specimen geometry is important for fast heating, (3) PID-values of control software are a considerable influence to accelerate the heating process depite thick specimens and (4) independent sample temperature determination before CGHE is strongly recommended.
A laser-induced breakdown spectroscopy (LIBS) system was combined with a bead-on-plate Tungsten Inert Gas (TIG) welding process for the in situ measurement of chemical compositions in austenitic stainless steels during welding.Monitoring the weld pool's chemical composition allows governing the weld pool solidification behavior, and thus enables the reduction of susceptibility to weld defects. Conventional inspection methods for weld seams (e.g. ultrasonic inspection) cannot be performed during the welding process. The analysis system also allows in situ study of the correlation between the occurrence ofweld defects and changes in the chemical composition in theweld pool or in the two-phase regionwhere solid and liquid phase coexist. First experiments showed that both the shielding Ar gas and the welding arc plasma have a significant effect on the selected Cr II, Ni II and MnII characteristicemissions, namely an artificial increase of intensity values via unspecific emission in the spectra.
In situ investigations showed that this artificial intensity increase reached a maximum in presence of weld plume. Moreover, an explicit decay has been observedwith the termination of thewelding plumedue to infrared radiation during sample cooling. Furthermore, LIBS can be used after welding to map element distribution. For austenitic stainless steels,Mnaccumulations on both sides of theweld could be detected between the heat affected zone (HAZ) and the base material.
The press conference on the results of the European Project FP7 constitutes a dissemination event dedicated to the production and characterization of "Shape-engineered TiO2 nanoparticles for metrology of functional properties: setting design rules from material synthesis to nanostructured devices" with the main large-scale applications in the three reference sectors: energy, health and environment.
Structural health monitoring contributes to early damage detection in the built infrastructure. During the last two decades, the sensor networks transferred from wired to wireless sensor networks.
Several methods exist to measure moisture in building materials. Most of the introduced commercial humidity measurement methods as provide information about the local or near surface moisture. A feasibility study is presented to demonstrate, how the Received Signal Strength Indicator (RSSI) of a BlueTooth® Low Energy (BLE) signal, transmitted from the BLE-module embedded in building materials with changing moisture content. The BLE-module communicates with a mobile Smart Device as tablet or mobile phone. The RSSI indicates to what extend the received signal strength is changed due to moisture, while the transmitted signal strength remains constant.
Welded plate girders are used in heavy steel construction, industrial buildings and bride construction. Residual stresses are present in all plate structures. They are mainly caused by welding. In addition, they influence the load bearing capacity of these welded components. However, Eurocode (EC) does not provide any specific residual stress patterns for consideration of residual stress impact on load capacity. Hence, the decision for a particular problem has to be made by the designer. Many codes, including EC 3, permit the use of non-linear finite element analysis (FEA) for the design of structures. This contribution gives an overview on recent research topics: modeling, experimental measuring and evaluation of residual stresses as well as welding simulation tools and simplified methodologies for assessment of weld residual stresses.
Welded I-girders are used in many applications in steel construction, especially a tailored mixture of different plate thicknesses is difficult to manufacture by rolling. Residual stresses are mainly caused by
welding and it is in most cases impractical to anneal the structures. Eurocode 3 (EC 3) does not provide any
specific residual stress pattern. Hence,
the decision for a particular problem has to be taken by the designer. Stability failures are often decisive in the design of steel beam and column members. Many standards, including EC 3, permit the use of non-linear FEA for the design of structures. Load influencing imperfections are mainly geometric deviations from the
ideal shape and residual stresses(both due to assembly or weld manufacturing). Currently the residual stresses are considered by simplified “robust” procedures fixed in common standards(such as EC 3. Models mostly based on specimens from mild steel. Information about high-strength steels is less
available for realistic assessment of residual stresses in full-scale I-girders. Hence, the scope of this work is the measurement of residual welding stresses on component-like I-girders S355 and S690 by sectioning method and global structural welding simulation.
Laboratory experiments on press hardened steels in different delivered states exposed to hydrogen
(2015)
The legal and economical demands in the automotive industry lead to increasing efforts reducing the CO2 emissions. A way to achieve that goal is to reduce the total weight of the car and therefore the fuel consumption. With the application of high strength steels in car body manufacturing it is possible to decrease the sheet thickness of the used materials and therefore the weight of the automobile. Components made of high strength steels can be produced by cold forming as well as by hot forming. In high strength steel the hydrogen content plays a crucial role for the component behavior. It is known that the hydrogen diffusivity and solubility are based on several factors, for example increasing dislocation density by cold working processes, vacancies, chemical composition and grain boundaries. The understanding and the control of the interaction between hydrogen and the high strength press hardened steels is an important factor for the application of the materials. The scope of this work is the determination of hydrogen diffusion and permeability kinetics in press hardened steel samples. An electrochemical hydrogen permeation method was applied on boron-manganese steel grades with different rolling reduction in initial ferrite/pearlite matrix as well as for the as-quenched martensite microstructure. The diffusible hydrogen contents of the specimens were measured using the carrier gas hot extraction technique (CGHE).
Carrier gas hot extraction (CGHE) technique was used for measurement of hydrogen in press-hardened (and as delivered) condition of 22MnB5 steel primarily coated with a thin layer of Al–Si. The CGHE technique was applied using different temperature programs: isothermal heating, temperature step, and linear heating in solid state. The effusing hydrogen was measured using thermal conductivity device (TCD) and high resolution mass spectroscopy (MS). Single isothermal heating at 400 and 900 °C allowed determining absolute value of effusing hydrogen. The linear heating, also known as thermal desorption analysis (TDA), revealed temperature dependent hydrogen effusion peaks. The deconvolution of the TDA spectra by peak fitting allowed the calculation of hydrogen desorption energies for each peak. The results showed good agreement between hydrogen concentrations measured with MS and TCD. In addition, the as-received ferrite-perlite microstructure showed only hydrogen effusion above 400 °C. The subsequent press hardening process leads to hydrogen uptake in the microstructure. In general, the press-hardened 22MnB5 revealed a hydrogen concentration of 0.4 to 0.5 ppm. The biggest concentration was released at isothermal holding at 400 °C indicating reversibly trapped hydrogen. TDA results with different heating rates confirmed mostly diffusible and reversible trapped hydrogen due to calculated activation energies in the range from 4 to 20 kJ mol-1; it was ascertained that nearly 90 % of the hydrogen left the specimens below 400 °C. Melt extraction (ME) was performed to measure the total hydrogen amount (including the diffusible and trapped hydrogen) and showed that above 900 °C up to 1 ppm hydrogen is trapped.