Analytische Chemie
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Paper des Monats
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A systematic study has been carried out to investigate the neutron transmission signal as a function of sample temperature. In particular, the experimentally determined wavelength-dependent neutron attenuation spectra for a martensitic steel at temperatures ranging from 21 to 700°C are compared with simulated data. A theoretical description that includes the Debye–Waller factor in order to describe the temperature influence on the neutron cross sections was implemented in the nxsPlotter software and used for the simulations. The analysis of the attenuation coefficients at varying temperatures shows that the missing contributions due to elastic and inelastic scattering can be clearly distinguished: while the elastically scattered intensities decrease with higher temperatures, the inelastically scattered intensities increase, and the two can be separated from each other by analysing unique sharp features in the form of Bragg edges. This study presents the first systematic approach to quantify this effect and can serve as a basis , for example, to correct measurements taken during in situ heat treatments, in many cases being a prerequisite for obtaining quantifiable results.
During their life span, concrete structures interact with many kinds of external mechanical loads. Most of these loads are considered in advance and result in reversible deformations. Nevertheless, some of the loads cause irreversible, sometimes unnoticed changes below the macroscopic scale depending on the type and dimension of the impact. As the functionality of concrete structures is often relevant to safety and society, their condition must be known and, therefore, assessed on a regular basis. Out of the spectrum of non-destructive monitoring methods, Coda Wave Interferometry using embedded ultrasonic sensors is one particularly sensitive technique to evaluate changes to heterogeneous media. However, there are various influences on Coda waves in concrete, and the interpretation of their superimposed effect is ambiguous. In this study, we quantify the relations of uniaxial compression and uniaxial tension on Coda waves propagating in normal concrete. We found that both the signal correlation of ultrasonic signals as well as their velocity variation directly reflect the stress change in concrete structures in a laboratory environment. For the linear elastic range up to 30% of the strength, we calculated a velocity variation of −0.97‰/MPa for compression and 0.33%/MPa for tension using linear regression. In addition, these parameters revealed even weak irreversible changes after removal of the load. Furthermore, we show the time-dependent effects of shrinkage and creep on Coda waves by providing the development of the signal parameters over time during half a year together with creep recovery. Our observations showed that time-dependent material changes must be taken into account for any comparison of ultrasonic signals that are far apart in time. The study’s results demonstrate how Coda Wave Interferometry is capable of monitoring stress changes and detecting even small-size microstructural changes. By indicating the stated relations and their separation from further impacts, e.g., temperature and moisture, we anticipate our study to contribute to the qualification of Coda Wave Interferometry for its application as an early-warning system for concrete structures.
What is meant by ‘Micro Non-Destructive Testing and Evaluation’? This was the central subject of debate in this Special Issue.
At present, sub-millimeter-size components or even assemblies are pervading the industrial and scientific world. Classic examples are electronic devices and watches (as well as parts thereof), but recent examples encompass additively manufactured lattice structures, stents, or other microparts. Moreover, most assemblies contain micro-components. Testing such components or their miniaturized parts would fit well within the topic of micro non-destructive testing and evaluation.
In all cases, performance and integrity testing, quality control, and dimensional tolerances need to be measured at the sub-millimeter level (ideally with a spatial resolution of about a micron); most of the time, such features and components are embedded in much larger assemblies, which also need to be taken into account. The solution to this dilemma (i.e. measuring large parts with high resolution) depends on the part and on the problem under consideration.
Another possible definition of micro non-destructive testing and evaluation can relate to the characterization of micro-features (e.g., the microstructure) in much larger specimens, such as damage in concrete cores or porosity in additively manufactured components. A further aspect is the use of microscopic probes to evaluate macroscopic properties. This is the case, for instance but not at all exclusively, in the use of diffraction techniques to determine macroscopic stress.
The splits between testing and characterization at the micro-level (or of micro parts) from one side and handling of macroscopic assemblies on the other represent a great challenge for many fields of materials characterization. On top of that, including the use of microscopic methods to test integrity would add a further level of complexity.
Imaging, mechanical testing, non-destructive testing, measurement of properties, structural health monitoring, and dimensional metrology all need to be re-defined if we want to cope with the multi-faceted topic of micro non-destructive testing and evaluation.
The challenge has already been accepted by the scientific and engineering communities for a while but is still far from being universally tackled. This Special Issue yields an interesting answer to the questions posed above. It presents the progress made and the different aspects of the challenge as well as at indicates the paths for the future of NDT&E.
Since 1997, the Committee for Health-related Evaluation of Building Products (AgBB) has been developing the basis for building regulations for protection against indoor health risks that may arise when building products are used. In 2009, the AgBB decided to include relevant VVOCs in the assessment procedure. The ISO 16000-6 (2021) states that the use of the thermal desorption gas chromatography technique is appropriate for VVOCs, if adaptations are considered. However, a suitable method for the trustworthy quantification of VVOC emissions from building products and in the indoor air is still missing.
This webinar will present the results of a research project on the development of a procedure for VVOC analysis:
• identification of the gaps towards standardization
• investigations on gas standards and the suitability of chromatography columns
• investigations on sorbent combinations and water management
• validation of the method and screening of VVOC emissions from building products.
The BAMline at the synchrotron X-ray source BESSY II (Berlin, Germany) is supporting researchers in a wide range of research areas since more than 20 years. These fields include biology, cultural heritage, medicine, and also materials science. As a non-destructive characterization method, synchrotron X-ray imaging, especially tomography with hard X-Rays, plays an important role in structural 3D characterization. A recent upgrade of key equipment at the BAMline expands the imaging capabilities towards shorter acquisition times. Therefore, in-situ and operando experiments can now be routinely conducted. Also, different energy resolutions can be set up to optimize flux and energy resolution as desired. This requires an adaptation of the used reconstruction methods in order to perform necessary analyses also during the experiment. In this presentation the equipment, data handling pipeline as well as various examples from material science are presented.
The BAMline at the 3rd generation synchrotron X-ray source BESSY II has been supporting researchers in a wide range of research areas for over 20 years. In addition to materials science, these fields also include biology, cultural heritage, and medicine. Being a non-destructive characterization method, synchrotron X-ray imaging, in particular tomography (SXCT), plays a particularly important role in structural characterization. A recent upgrade of key BAMline equipment expands the imaging capabilities: The upgraded dual multilayer monochromator offers flexibility by providing different energy spectra to optimize flux and energy resolution as desired. Different spectra (8 – 60 keV with ΔE/E 0.01%, 1.5%, 4% and pink beam) can be selected. The upgraded detector (in white beam configuration, equipped with an sCMOS camera) allows the higher flux to be exploited with reduced readout times. Shorter tomographic acquisition times in the range of seconds are now possible. Hence, in-situ and operando examinations are routinely available. An integrated slip ring allows continuous rotation of the sample stage for ease of wiring. The pink beam option allows tomographic observation of processes occurring in the time domain of a few seconds with a resolution down to ~ 1 µm. Different scan methods, optimized for quality and speed are available and discussed. Examples of energy related materials from fuel cell and battery research are shown.
An optional end station allows refraction enhanced imaging (synchrotron X-Ray refraction radiography (SXRR) and tomography (SXRCT)). That includes an analyzer Si-crystal in Bragg alignment between sample and detector. This technique obtains sensitivity to smaller structures (cracks, pores) down to a few wavelengths, while obtaining field of view sizes in the range of several mm. Besides medicine (e.g., teeth explants), several applications are found in material science, like studies on diesel particulate filters, ceramics, additively manufactured (AM) alloys and metal matrix composites (MMC). The in-situ capabilities include mechanical load (tension and compression) and heating up to 1100°C. A case study, the microstructural evolution during heat treatment of an AM AlSi10Mg, will be shown.
Thirteen laboratories participated in an international interlaboratory comparison for the determination of 87Sr/86Sr isotope ratios in four cement reference materials (RM) using the conventional method for 87Sr/86Sr isotope ratios analyses. Sample dissolution and Sr isolation via ion exchange chromatography were required since the cement samples were distributed as powders. Analytical preparation included the use of various digestion methods including mixed mineral acids, microwave/acid, bomb/acid digestion or borate fusion, followed by Sr separation using ion exchange chromatography. In this study, we evaluated whether any statistically significant differences were attributable to instrumental differences (i.e., MC-ICP-MS and MC-TIMS), or to laboratory-specific techniques (different sample preparation techniques, Sr isolation and the procedures for correcting the data outputs). To evaluate these effects, consensus values for cement RMs and associated standard uncertainties were estimated by fitting a linear, Gaussian mixed effects model using the R function “lmer” defined in package “lme4”. No statistically significant effects (SSE) attributable to instrumental differences regardless of whether the materials are considered together or separately were evident. There were SSE attributable to differences between laboratories for three cement RMs when the individual cements were considered separately. Since consideration or disregard for such differences does not induce significant changes in the estimate of the consensus values for the 87Sr/86Sr isotope ratios in cement RMs, these effects can safely be neglected when calculating the best estimates for the true values of 87Sr/86Sr isotope ratios in these RMs.
Responsible treatment of the environment and resources is a key element of sustainability. The building and construction industry is one of the largest consumers of natural resources. Consequently, there is a particular need for regulations and technologies that help to create closed material cycles. From the technological point of view, such efforts are complicated by the growing material diversity and the amount of composites contained in present and future construction and demolition waste (CDW). Nowadays, simple but proven techniques like manual sorting are mainly used. However, this practice not only poses health risks and dangers to the staff performing the work, but also relies on merely obvious, visually striking differences. Automated, sensor-based sorting of these building materials could complement or replace this practice to improve processing speed, recycling rates, sorting quality, and prevailing health conditions. The preliminary results for the identification of a wide variety of building materials with LIBS are presented.
Isotope reference materials
(2022)
The variation of isotope ratios is increasingly used to unravel 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 or food authenticity studies, the number of published isotope data strongly increased. Instrumental developments such as the enhancement of inductively coupled plasma mass spectrometers (ICP-MS) from an instrument for simple quantitative analysis to highly sophisticated isotope ratio machines influenced this process significantly. While in former times only experts in mass spectrometry were able to produce reliable isotope data, nowadays many laboratories, never been in touch with mass spectrometry before, produce isotope data with an ICP-MS. Isotope reference materials (iCRM) are indispensable to enable a reliable method validation or in rare cases even SI-traceability. The fast development and the broad availability of ICP-MS also lead to an expansion of the classical research areas and new elements are under investigation. Irrespective of the investigated element or the knowledge of the user all isotope ratio applications require reference materials either for correction of instrumental isotope fractionation, for method validation or to provide a common accepted basis as needed for delta measurements. This presentation will outline the basic principles and illustrate the urgent need for new iCRMs. Consequently, the production and certification of iCRMs will be discussed and illustrated by examples of already completed certification projects. Finally, plans for future iCRMs to be produced at BAM will be presented.
Concrete structures often show severe damage during their lifetime. One such damage is pitting corrosion of the steel reinforcement caused by chloride ingress into the porous concrete structure. Laser-induced breakdown spectroscopy (LIBS) is a promising method in civil engineering, which is used for detection of chlorine in concrete structures in addition to conventional methods of wet chemistry. To assess LIBS as a trustful analytical technique, its accuracy and robustness is carefully tested. The presentation will outline the results of the interlaboratory comparison of chlorine quantification in cement paste samples, which was carried out by 12 laboratories in 10 countries. Two sets of samples with chloride content ranging from 0.06-1.95 wt.% in the training set and 0.23-1.51 wt.% in the test sample set (“unknowns”), with additional variations in the type of cement and chlorine source (salt type) were sent to the laboratories. The overall result demonstrates that LIBS is suitable for the quantification of the investigated sample compositions: average relative bias was mostly below 15 %. Considering that the laboratories did not receive instructions on how to perform the analysis or how to process the data, the results can be evaluated as a true status quo of the LIBS technique for this type of analysis.
Modeling is an important tool for understanding a physical phenomenon. It helps to interpret results of experiments and optimize experimental parameters for obtaining a desirable result. Modeling laser induced plasma is beneficial for many scientific and industrial fields, e.g., analytical chemistry, pulsed laser deposition, plasma enhanced chemical vapor deposition, laser welding, additive manufacturing etc. In this presentation, a personal experience in development of a physical model of laser induced plasma will be given in a chronological sequence starting from early 2000th and until now.
Over the time, the model evolved from its simple analytical form that described plasma emission spectra to its current numerical form that describes plasma dynamics, chemistry, and interaction with a substrate surface. Several examples will be given for the application of the model to practical problems such as spectroscopic chemical analysis, plasma enhanced chemical vapor deposition, and surface modification by laser ablation.
Current trends in materials and life sciences are flanked by the need to push detection limits to single molecules or single cells, enable the characterization of increasingly complex matrices or sophisticated nanostructures, speed up the time of analysis, reduce instrument complexity and costs, and improve the reliability of data. This requires suitable analytical tools such as spectroscopic, separation and imaging techniques, mass spectrometry, and hyphenated techniques as well as sensors and their adaptation to application-specific challenges in the environmental, food, consumer product, health sector, nanotechnology, and bioanalysis. Increasing concerns about health threatening known or emerging pollutants in drinking water, consumer products, and food and about the safety of nanomaterials led to a new awareness of the importance of analytical sciences. Another important driver in this direction is the increasing demand by legislation, particularly in view of the 17 sustainable development goals by the United Nations addressing clean energy, industry, and innovation, sustainable cities, clean water, and responsible consumption and production. In this respect, also the development of analytical methods that enable the characterization of material flows in production processes and support recycling concepts of precious raw materials becomes more and more relevant. In the future, this will provide the basis for greener production in the chemical industry utilizing recycled or sustainable starting materials.
This makes analytical chemistry an essential player in terms of the circular economy helping to increase the sustainability of production processes. In the life sciences sector, products based on proteins, such as therapeutic and diagnostic antibodies, increase in importance. These increasingly biotechnologically produced functional biomolecules pose a high level of complexity of matrix and structural features that can be met only by highly advanced methods for separation, characterization, and detection. In addition, metrological traceability and target definition are still significant challenges for the future, particularly in the life sciences.
However, innovative reference materials as required for the health and food sector and the characterization of advanced materials can only be developed when suitable analytical protocols are available. The so-called reproducibility crisis in sciences underlines the importance of improved measures of quality control for all kinds of measurements and material characterization. This calls for thorough method validation concepts, suitable reference materials, and regular interlaboratory comparisons of measurements as well as better training of scientists in analytical sciences.
The important contribution of analytical sciences to these developments is highlighted by a broad collection of research papers, trend articles, and critical reviews from these different application fields. Special emphasis is dedicated to often-overlooked quality assurance and reference materials.
Current trends in materials and life sciences are flanked by the need to push detection limits to single molecules or single cells, enable the characterization of increasingly complex matrices or sophisticated nanostructures, speed up the time of analysis, reduce instrument complexity and costs, and improve the reliability of data. This requires suitable analytical tools such as spectroscopic, separation and imaging techniques, mass spectrometry, and hyphenated techniques as well as sensors and their adaptation to application-specific challenges in the environmental, food, consumer product, health sector, nanotechnology, and bioanalysis. Increasing concerns about health threatening known or emerging pollutants in drinking water, consumer products, and food and about the safety of nanomaterials led to a new awareness of the importance of analytical sciences. Another important driver in this direction is the increasing demand by legislation, particularly in view of the 17 sustainable development goals by the United Nations addressing clean energy, industry, and innovation, sustainable cities, clean water, and responsible consumption and production. In this respect, also the development of analytical methods that enable the characterization of material flows in production processes and support recycling concepts of precious raw materials becomes more and more relevant. In the future, this will provide the basis for greener production in the chemical industry utilizing recycled or sustainable starting materials.
This makes analytical chemistry an essential player in terms of the circular economy helping to increase the sustainability of production processes. In the life sciences sector, products based on proteins, such as therapeutic and diagnostic antibodies, increase in importance. These increasingly biotechnologically produced functional biomolecules pose a high level of complexity of matrix and structural features that can be met only by highly advanced methods for separation, characterization, and detection. In addition, metrological traceability and target definition are still significant challenges for the future, particularly in the life sciences.
However, innovative reference materials as required for the health and food sector and the characterization of advanced materials can only be developed when suitable analytical protocols are available. The so-called reproducibility crisis in sciences underlines the importance of improved measures of quality control for all kinds of measurements and material characterization. This calls for thorough method validation concepts, suitable reference materials, and regular interlaboratory comparisons of measurements as well as better training of scientists in analytical sciences.
The important contribution of analytical sciences to these developments is highlighted by a broad collection of research papers, trend articles, and critical reviews from these different application fields. Special emphasis is dedicated to often-overlooked quality assurance and reference materials.
Wastewater contains harmful chemicals and heavy metals that are known to cause various environmental and health problems. Therefore, the water quality control using sensitive, simple, fast, accurate, and portable tools is of great importance. This study aimed to evaluate the pollution parameters of wastewaters collected at different treatment stages from a wastewater treatment plant (WWTP) that treats domestic and industrial wastewaters by using an electronic nose (E-nose) and a voltammetric electronic tongue (E-tongue) combined with chemometric techniques. Water and wastewater pollution parameters determination were performed using inductively coupled plasma optical emission spectrometry for the determination of cations, and anions by using ion chromatography. Chemometric techniques, such as Principal Component Analysis (PCA), Discriminant Function Analysis (DFA), Support Vector Machines (SVMs), and Hierarchical Cluster Analysis (HCA), were used to process the E-nose and E-tongue datasets to describe the similarities between the samples. In addition, Partial Least Squares Regression (PLSR) model was constructed using electronic sensing data to simultaneously predict the concentration values of physicochemical parameters. The obtained correlation coefficient, for training and testing sets, is higher than 0.91 for the prediction of the concentration of all physicochemical parameters, except for iron (Fe) which remains 0.84. These results suggest that simple, portable, and inexpensive tools such as electronic nose and tongue are suitable for wastewater analysis.
The acquisition and appropriate processing of relevant information about the considered system remains a major challenge in assessment of existing structures. Both the values and the validity of computed results such as failure probabilities essentially depend on the quantity and quality of the incorporated knowledge. One source of information are onsite measurements of structural or material characteristics to be modeled as basic variables in reliability assessment. The explicit use of (quantitative) measurement results in assessment requires the quantification of the quality of the measured information, i.e., the uncertainty associated with the information acquisition and processing. This uncertainty can be referred to as measurement uncertainty. Another crucial aspect is to ensure the comparability of the measurement results.This contribution attempts to outline the necessity and the advantages of measurement uncertainty calculations in modeling of measurement data-based random variables to be included in reliability assessment. It is shown, how measured data representing time-invariant characteristics, in this case non-destructively measured inner geometrical dimensions, can be transferred into measurement results that are both comparable and quality-evaluated. The calculations are based on the rules provided in the guide to the expression of uncertainty in measurement (GUM). The GUM-framework is internationally accepted in metrology and can serve as starting point for the appropriate processing of measured data to be used in assessment. In conclusion, the effects of incorporating the non-destructively measured data into reliability analysis are presented using a prestressed concrete bridge as case-study.
The composition of thin films of polymer blends in vertical direction is still under discussion. For explaining the thickness dependence of some properties like the thermal glass transition temperature, a three-layer model has been introduced consisting of an adsorbed layer with a reduced segmental mobility at the substrate, a bulk-like layer in the middle of the film and an outermost surface layer with a higher molecular mobility. X-ray photoelectron spectroscopy (ER-XPS) measurements with a varying excitation energy from 400 eV to 1486.6 eV and, herewith, an information depth from 1.5 nm to 10 nm were performed at PVME/PS films with compositions of 25/75 wt% and 50/50 wt% and thicknesses between 15 nm and 190 nm. As expected, it was found that the PVME concentration decreases with increasing information depth. Secondly, a complex correlation between the PVME concentration at the surface and the film thickness was found. The PVME concentration increases with decreasing film thickness until a maximum at 30 nm. For thinner films, the PVME concentration decreases. These data agree with previous investigations obtained with specific heat spectroscopy.
We thank BESSY II (HZB) for the allocation of beamtime at the HE-SGM beamline and for technical support. DFG (Project number 124846229) is acknowledged for financial support.
Designing the shape and size of catalyst particles, and their interfacial charge, at the nanometer scale can radically change their performance. We demonstrate this with ceria nanoparticles. In aqueous media, nanoceria is a functional mimic of haloperoxidases, a group of enzymes that oxidize organic substrates, or of peroxidases that can degrade reactive oxygen species (ROS) such as H2O2 by oxidizing an organic substrate. We show that the chemical activity of CeO2−x nanoparticles in haloperoxidase- and peroxidaselike reactions scales with their active surface area, their surface charge, given by the ζ-potential, and their surface defects (via the Ce3+/Ce4+ ratio). Haloperoxidase-like reactions are controlled through the ζ-potential as they involve the adsorption of charged halide anions to the CeO2 surface, whereas peroxidase-like reactions without charged substrates are controlled through the specific surface area SBET. Mesoporous CeO2−x particles, with large surface areas, were prepared via template-free hydrothermal reactions and characterized by small-angle X-ray scattering. Surface area, ζ-potential and the Ce3+/Ce4+ ratio are controlled in a simple and predictable manner by the synthesis time of the hydrothermal reaction as demonstrated by X-ray photoelectron spectroscopy, sorption and ζ-potential measurements. The surface area increased with synthesis time, whilst the Ce3+/Ce4+ ratio scales inversely with decreasing ζ-potential. In this way the catalytic activity of mesoporous CeO2−x particles could be tailored selectively for haloperoxidase- and peroxidase-like reactions. The ease of tuning the surface properties of mesoporous CeO2x particles by varying the synthesis time makes the synthesis a powerful general tool for the preparation of nanocatalysts according to individual needs.
Das europäische Projekt MefHySto befasst sich mit dem Bedarf an großmaßstäblichen Energiespeichern, die für eine Umstellung der Energieversorgung auf erneuerbare Energien erforderlich sind. Eine solche Speicherung ist entscheidend, um Energie zu Spitzenzeiten zu liefern, wenn die erneuerbaren Energiequellen schwanken. Eine mögliche Lösung für die Energiespeicherung ist der großtechnische Einsatz von Wasserstoff. Die messtechnische Rückführbarkeit in der Energieinfrastruktur für die Wasserstoffspeicherung ist dann von entscheidender Bedeutung und eine bessere Kenntnis der chemischen und physikalischen Eigenschaften von Wasserstoff sowie rückführbare Messungen und validierte Techniken unverzichtbar.
The COVID-19 pandemic posed new and manifold challenges to organizations and their operations worldwide. Conformity assessment bodies (CABs), such as testing or medical laboratories, certification, and inspection bodies, were also affected by the associated disruptions. Their role in this crisis is highly relevant, as CABs are essential pillars of the quality infrastructure: their activities ensure that products and services meet requirements as defined in standards and regulations, thereby contributing to their safety and reliability. The question arises of how CABs and their operations were affected by the pandemic and how they responded. To this end, we present the results of an international survey of 986 CABs of all types in Germany, the UK, Italy, and New Zealand. Overall, CABs reported, on average, a reduction in demand for their services during the pandemic, facing restrictions in all countries. In addition, the pandemic had an overall negative impact on the CABs’ investment and innovation activities. However, investments in digital infrastructure were increased as a countermeasure, with CABs reporting a higher need for digitalization. The paper highlights and discusses results from in-depth analyses relevant to policymakers and industry alike.
Introduction of a monitoring system for Bingham fluids in additive manufacturing with concrete
(2022)
Freeform additive manufacturing of concrete structures is a rising technology in civil engineering with several fascinating advantages. Nonetheless, to ensure reliability and structural integrity, standards and quality control are required in the future to bring this technology into the market. As the concrete is manufactured continuously, continuous quality control of the printing process is also required, i.e. comprehensive process monitoring. At BAM, a test rig will be installed, enabling the printing of concrete structures with a maximum size of 2 m x 1 m x 1 m (l x w x h). Here, process monitoring is the focus of the test rig. In this study, we show the results of the first pump tests, including the measurement of several parameters such as temperature and pressure along the supply system, i.e. from the concrete pump to the printer head.
Introduction of a monitoring system for Bingham fluids in additive manufacturing with concrete
(2022)
Freeform additive manufacturing of concrete structures is a rising technology in civil engineering with several fascinating advantages. Nonetheless, to ensure reliability and structural integrity, standards and quality control are required in the future to bring this technology into the market. As the concrete is manufactured continuously, continuous quality control of the printing process is also required, i.e. comprehensive process monitoring. At BAM, a test rig will be installed, enabling the printing of concrete structures with a maximum size of 2 m x 1 m x 1 m (l x w x h). Here, process monitoring is the focus of the test rig. In this study, we show the results of the first pump tests, including the measurement of several parameters such as temperature and pressure along the supply system, i.e. from the concrete pump to the printer head.
„Made in Germany“ steht für Vertrauen in Qualität und Sicherheit, das auch in der digitalen und grünen Transformation gelten soll. In einer zunehmend digitalisierten Welt muss auch die Qualitätssicherung von Produkten, Prozessen und Dienstleistungen neu gedacht werden. Ziel der Initiative QI-Digital ist es, die bewährte Qualitätsinfrastruktur (QI) noch besser zu machen. Für eine moderne und effiziente Qualitätssicherung. Die zentralen Akteure der deutschen QI haben sich in QI-Digital zusammengeschlossen, um konkrete Lösungen für innovative Anwendungsfälle zu entwickeln. Dabei ist ein ganzheitlicher und praxisbezogener Ansatz wichtig, in dem ein weiter Kreis interessierter Stakeholder aktiv eingebunden wird.
Im Kurzvortrag wird die Initiative, inkl. ihrer Akteure, Ziele, Projekte und Beteiligungsmöglichkeiten vorgestellt.
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in the Netherlands. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends.
The study on Dutch CABs is part of a global project that covers various other countries (see www.qi-fokus.de).
The geometric phase in the beat signal from coherent interference of two frequency-offset light beams is measured using a novel distributed optical fiber sensing setup. In a fiber optic medium, with changing beam intensities, to the best of our knowledge, ours is the first measurement of the mentioned geometric phase. Experimental results of applying a 100-Hz sinusoidal stimulus to a polarization scrambler and a piezoelectric transducer inline to an optical fiber are presented. The results may enable novel distributed fiber sensing techniques.
pH presents one of the most important analytes in the life and material sciences, indicating, e.g., diseases and corrosion processes. This includes the optical monitoring of pH in living cells for studying cellular internalization pathways, such as phagocytosis, endocytosis, and receptor mediated internalization with the aid of molecular and nanoscale fluorescent sensors. Nanoparticle (NP)-based sensors, that are labelled or stained with a multitude of sensor dyes, have several advantages as compared to conventional molecular probes like enhanced brightness, i.e., amplified signals, ease of designing ratiometric systems by combining analyte-sensitive and inert reference dyes, and increased photostability. Moreover, this can enable the use of hydrophobic dyes in aqueous environments. Versatile templates and carriers for the fabrication of nanosensors by staining and/or labelling with different fluorophores and sensor molecules are surface-functionalized particles like silica (SiO2) and polystyrene (PS) particles. Here we present a platform of blue-red-green fluorescent pH nanosensors for the measurement of acidic, neutral, and basic pH utilizing both types of matrices and two spectrally distinguishable sensor dyes with an integrated reference dye and demonstrate its applicability for cellular studies.
Mechanically stable structures with interconnected hierarchical porosity combine the benefits of both small
and large pores, such as high surface area, pore volume, and good mass transport capabilities. Hence, lightweight micro-/meso-/macroporous monoliths are prepared from ordered mesoporous silica COK-12 by means of spark plasma sintering (SPS, S-sintering) and compared to conventionally (C-) sintered monoliths. A multi-scale model is developed to fit the small angle X-ray scattering data and obtain information on the hexagonal lattice parameters, pore sizes from the macro to the micro range, as well as the dimensions of the silica population. For both sintering techniques, the overall mesoporosity, hexagonal pore ordering, and amorphous character are preserved. The monoliths' porosity (77–49%), mesopore size (6.2–5.2 nm), pore volume (0.50–0.22 g cm-3
), and specific surface area (451–180 m2 g-1) decrease with increasing processing temperature and pressure. While the difference in porosity is enhanced, the
structural parameters between the C-and S-sintered monoliths are largely converging at 900 C, except for the mesopore size and lattice parameter, whose dimensions are more extensively preserved in the
S-sintered monoliths, however, coming along with larger deviations from the theoretical lattice. Their higher mechanical properties (biaxial strength up to 49 MPa, 724 MPa HV 9.807 N) at comparable porosities and ability to withstand ultrasonic treatment and dead-end filtration up to 7 bar allow S-sintered monoliths to reach a high permeance (2634 L m-2 h-1 bar-1), permeability (1.25 x 10^-14 m2), and ability to reduce the chemical oxygen demand by 90% during filtration of a surfactant-stabilized oil in water emulsion, while indicating reasonable resistance towards fouling.
In coastal systems, organisms are exposed to amultitude of stressors whose interactions and effects are poorly studied. Pharmaceutical drugs and Climate Change consequences, such as lowered pH, are examples of stressors affecting marine organisms, as bivalves. Although a vast literature is available for the effects of these stressors when acting individually, very limited information exists on the impacts that the combination of both can have on marine bivalves. For this reason, this study aimed to evaluate the impacts of a simulated ocean acidification scenario (control pH, 8.0; lowered pH, pH 7.6) on the effects of the antiepileptic carbamazepine (CBZ, 1 μg/L) and the antihistamine cetirizine (CTZ, 0.6 μg/L), when acting individually and combined (CBZ + CTZ), on the edible clam Ruditapes philippinarum. After 28 days of exposure, drug concentrations, bioconcentration factors and biochemical parameters related to the clams' metabolic capacity and oxidative stress were evaluated. The results showed that R. philippinarum clams responded differently to pharmaceutical drugs depending on the pH tested, influencing both bioconcentration and biological responses. In general, drug combined treatments showed fewer impacts than drugs acting alone, and acidification seemed to activate at a higher extension the elimination processes that were not activated under control pH. Also, lowered pH per se exerted negative impacts (e.g., cellular damage) on R. philippinarum and the combination with pharmaceutical drugs did not enhance the toxicity.
Avoiding the formation of defects such as keyhole pores is a major challenge for the production of metal parts by Laser Powder Bed Fusion (LPBF). The use of in-situ monitoring by thermographic cameras is a promising approach to detect defects, however the data is hard to analyze by conventional algorithms. Therefore, we investigate the use of Machine Learning (ML) in this study, as it is a suitable tool to model complex processes with many influencing factors. A ML model for defect prediction is created based on features extracted from process thermograms. The porosity information calculated from an x-ray Micro Computed Tomography (µCT) scan is used as reference. Physical characteristics of the keyhole pore formation are incorporated into the model to increase the prediction accuracy. Based on the prediction result, the quality of the input data is inferred and future demands on in-situ monitoring of LPBF processes are derived.
Ein Umlaufkühler ist im Betrieb explodiert. Splitter des zerborstenen Gehäuses aus Kunststoff wurden mit dem Kühlwasser in die Umgebung geschleudert, am Betriebsort entstand Personenschaden. Bei Funktionsprüfungen am beschädigten Gerät traten unerwartet - aber reproduzierbar - Knalleffekte bei Berührung der Außenoberfläche der Kupfer-Kühlschlange auf. Ein möglicher Mechanismus konnte im Labor durch Synthese von Kupferazid auf Kupferproben und Auslösung vergleichbarer Knalleffekte nachgestellt werden. Damit ist die Plausibilität des beschriebenen Schadensereignisses mit diesem oder einem ähnlich reagierenden Stoff belegt. Ein eindeutiger Nachweis darüber, dass bei dem aufgetretenen Schadensfall dieselbe chemische Reaktion stattgefunden hat, war nicht möglich, da die Belag-Überreste aus dem explodierten Kühlgerät für eine Analyse nicht mehr in ausreichender Menge verfügbar gewesen sind.
In Coastal Systems, pollutants as pharmaceutical drugs exert changes from the molecular to the organism level in marine bivalves. Besides pollutants, Coastal Systems are prone to changes in environmental Parameters, as the alteration of salinity values because of Climate Change. Together, these Stressors (pharmaceutical drugs and salinity changes) can exert different threats than each Stressor acting individually; for example, salinity can change the physical-chemical properties of the drugs and/or the sensitivity of the organisms to them. However, limited Information is available on this subject, with variable results, and for this reason, this study aimed to evaluate the impacts of salinity changes (15,25 and 35) on the effects of the antiepileptic carbamazepine (CBZ, 1 (ig/L) and the antihistamine cetirizine (CTZ, 0.6 pg/L), when acting individually and combined (CBZ + CTZ), in the edible clam Ruditapes philippinarum. After 28 days ofexposure, drugs concentrations, bioconcentration factors and biochemical parameters, related to clam's metabolic caparity and oxidative stress were evaluated. The results showed that dams under low salinity suffered more changes in metabolic, antioxidant and biotransformation activities, in comparison with the remaining salinities under study. However, limited impacts were observed when comparing drug effects at low salinity. Indeed, it seemed that CTZ and CBZ + CTZ, under high salinity (salinity 35) were the worst exposure conditions for the dams, since they caused higher leveis of cellular damage. It Stands out that salinity changes altered the impact of pharmaceutical drugs on marine bivalves.
In a joint project of partners from industry and research, the automated recycling of construction and demolition waste (CDW) is investigated and tested by combing laser-induced breakdown spectroscopy (LIBS) and near-infrared (NIR) spectroscopy. Joint processing of information (data fusion) is expected to significantly improve the sorting quality of various materials like concrete, main masonry building materials, organic components, etc., and may enable the detection and separation of impurities such as SO3-cotaining building materials (gypsum, aerated concrete, etc.). The project focuses primarily on the Berlin site to analyze the entire value chain, minimize economic/technological barriers and obstacles at the cluster level, and sustainably increase recovery and recycling rates. First measurements with LIBS and NIR spectroscopy show promising results in distinguishing various material types and indicate the potential for a successful combination. In addition, X-ray fluorescence (XRF) spectroscopy is being performed to obtain more information about the quantitative elemental composition of the different building materials. Future work will apply the developed sorting methodology in a fully automated measurement setup with CDW on a conveyor belt.
This sequence of X-Ray images shows how one of the most common Italian moka pots actually work! The sequence starts with a completely prepared moka pot (water in the bottom part, coffee in the middle and hot plate on). During the process the water starts to boil and the steam pressure pushes the hot water through the coffee into the bassin at the top of the pot.
This video sequence and additional explanations can also be found on Wikipedia.
X-Ray computed tomography (XCT) scan of 11 individual metallic powder particles, made of (Mn,Fe)2(P,Si) alloy. The data set consists of 4 single XCT scans which have been stitched together [3] after reconstruction. The powder material is an (Mn,Fe)2(P,Si) alloy with an average density of 6.4 g/cm³. The particle size range is about 100 - 150 µm with equivalent pore diameters up to 75 µm. The powder and the metallic alloy are described in detail in [1, 2].
By means of laser thermography, surface defects, in particular surface breaking cracks, can be detected with high sensitivity. Basically, this requires a focused heat source (high-power laser), a thermographic camera and a relative movement between laser and test object, as well as a suitable evaluation algorithm to distinguish between surface defects and defect-free areas. In this paper we report on a method in which the relative motion is realised by a robot to fully inspect large and non-planar test objects such as rail sections, turbine blades, gears, etc. We show the influence of the excitation laser, which can be varied in terms of spot geometry, wavelength, and scan scheme, and we demonstrate our evaluation algorithms with the aim of automatically detecting surface defects.
In a joint project of partners from industry and research, the automated recycling of construction and demolition waste (CDW) is investigated and tested by combing laser-induced breakdown spectroscopy (LIBS) and near-infrared (NIR) spectroscopy. Joint processing of information (data fusion) is expected to significantly improve the sorting quality of various materials like concrete, main masonry building materials, organic components, etc., and may enable the detection and separation of impurities such as SO3-cotaining building materials (gypsum, aerated concrete, etc.). The project focuses primarily on the Berlin site to analyze the entire value chain, minimize economic/technological barriers and obstacles at the cluster level, and sustainably increase recovery and recycling rates. First measurements with LIBS and NIR spectroscopy show promising results in distinguishing various material types and indicate the potential for a successful combination. In addition, X-ray fluorescence (XRF) spectroscopy is being performed to obtain more information about the quantitative elemental composition of the different building materials. Future work will apply the developed sorting methodology in a fully automated measurement setup with CDW on a conveyor belt.
Evaluation of marker materials and spectroscopic methods for tracer-based sorting of plastic wastes
(2022)
Plastics are a ubiquitous material with good mechanical, chemical and thermal properties, and are used in all industrial sectors. Large quantities, widespread use, and insufficient management of plastic wastes lead to low recycling rates. The key challenge in recycling plastic waste is achieving a higher degree of homogeneity between the different polymer material streams. Modern waste sorting plants use automated sensor-based sorting systems capable to sort out commodity plastics, while many engineering plastics, such as polyoxymethylene (POM), will end up in mixed waste streams and are therefore not recycled. A novel approach to increasing recycling rates is tracer-based sorting (TBS), which uses a traceable plastic additive or marker that enables or enhances polymer type identification based on the tracer’s unique fingerprint (e.g., fluorescence). With future TBS applications in mind, we have summarized the literature and assessed TBS techniques and spectroscopic detection methods. Furthermore, a comprehensive list of potential tracer substances suitable for thermoplastics was derived from the literature. We also derived a set of criteria to select the most promising tracer candidates (3 out of 80) based on their material properties, toxicity profiles, and detectability that could be applied to enable the circularity of, for example, POM or other thermoplastics.
Nebivolol (NEB), a β-blocker frequently used to treat cardiovascular diseases, has been widely detected in aquatic environments, and can be degraded under exposure to UV radiation, leading to the formation of certain transformation products (UV-TPs). Thus, the toxic effects of NEB and its UV-TPs on aquatic organisms are of great importance for aquatic ecosystems. In the present study, the degradation pathway of NEB under UV radiation was investigated. Subsequently, zebrafish embryos/larvae were used to assess the median lethal concentration (LC50) of NEB, and to clarify the sub-lethal effects of NEB and its UV-TPs for the first time. It was found that UV radiation could reduce the toxic effects of NEB on the early development of zebrafish. Transcriptomic analysis identified the top 20 enriched Kyoto Encyclopedia of Genes and Genomes (KEGG) pathways in zebrafish larvae exposed to NEB, most of which were associated with the antioxidant, nervous, and immune systems. The number of differentially expressed genes (DEGs) in the pathways were reduced after UV radiation. Furthermore, the analysis of protein biomarkers, including CAT and GST (antioxidant response), AChE and ACh (neurotoxicity), CRP and LYS (immune response), revealed that NEB exposure reduced the activity of these biomarkers, whereas UV radiation could alleviate the effects. The present study provides initial insights into the mechanisms underlying toxic effects of NEB and the detoxification effects of UV radiation on the early development of zebrafish. It highlights the necessity of considering the toxicity of UV-TPs when evaluating the toxicity of emerging pollutants in aquatic systems.
Inflammatory bowel diseases (IBD) comprise mainly ulcerative colitis (UC) and Crohn´s disease (CD). Both forms present with a chronic inflammation of the (gastro) intestinal tract, which induces excessive changes in the composition of the associated extracellular matrix (ECM). In UC, the inflammation is limited to the colon, whereas it can occur throughout the entire gastrointestinal tract in CD. Tools for early diagnosis of IBD are still very limited and highly invasive and measures for standardized evaluation of structural changes are scarce. To investigate an efficient non-invasive way of diagnosing intestinal inflammation and early changes of the ECM, very small superparamagnetic iron oxide nanoparticles (VSOPs) in magnetic resonance imaging (MRI) were applied in two mouse models of experimental colitis: the dextran sulfate sodium (DSS)-induced colitis and the transfer model of colitis. For further validation of ECM changes and inflammation, tissue sections were analyzed by immunohistochemistry. For in depth ex-vivo investigation of VSOPs localization within the tissue, Europium-doped VSOPs served to visualize the contrast agent by imaging mass cytometry (IMC). VSOPs accumulation in the inflamed colon wall of DSS-induced colitis mice was visualized in T2* weighted MRI scans. Components of the ECM, especially the hyaluronic acid content, were found to influence VSOPs binding. Using IMC, colocalization of VSOPs with macrophages and endothelial cells in colon tissue was shown. In contrast to the DSS model, colonic inflammation could not be visualized with VSOP-enhanced MRI in transfer colitis. VSOPs present a potential contrast agent for contrast-enhanced MRI to detect intestinal inflammation in mice at an early stage and in a less invasive manner depending on hyaluronic acid content.
In this work, molecular imprinting was combined with direct fluorescence detection of the pesticide Glyphosate (GPS). Firstly, the solubility of highly polar GPS in organic solvents was improved by using lipophilic tetrabutylammonium (TBA+) and tetrahexylammonium (THA+) counterions. Secondly, to achieve fluorescence detection, a fluorescent crosslinker containing urea-binding motifs was used as a probe for GPS-TBA and GPS-THA salts in chloroform, generating stable complexes through hydrogen bond formation. The GPS/fluorescent dye complexes were imprinted into 2–3 nm fluorescent molecularly imprinted polymer (MIP) shells on the surface of sub-micron silica particles using chloroform as porogen. Thus, the MIP binding behavior could be easily evaluated by fluorescence titrations in suspension to monitor the spectral changes upon addition of the GPS analytes. While MIPs prepared with GPS-TBA and GPS-THA both displayed satisfactory imprinting following titration with the corresponding analytes in chloroform, GPS-THA MIPs displayed better selectivity against competing molecules. Moreover, the THA+ counterion was found to be a more powerful phase transfer agent than TBA+ in a biphasic assay, enabling the direct fluorescence detection and quantification of GPS in water. A limit of detection of 1.45 μM and a linear range of 5–55 μM were obtained, which match well with WHO guidelines for the acceptable daily intake of GPS in water (5.32 μM).
Ultrasonic measurement technology has become indispensable in NDT-CE. Air-coupled ultrasonic (ACU) measurement techniques promise to reduce measurement time. However, the signal quality suffers from large specific impedance mismatch at the transducer-air and air-specimen interface. Additionally, large pressure amplitudes are necessary for the penetration depth required in NDT-CE applications. To address the specific requirements of ultrasonic testing in NDT-CE, a robust ACU transducer was developed, that generates ultrasound by quickly switching a pressurized air flow. The simple design of the fluidic transducer makes the device maintenance free and resilient against harsh environmental conditions. Since the signal is generated by aeroacoustics, there is no specific impedance mismatch between the transducer and the surrounding air. The ultrasonic signal exhibits frequencies in the 30-60 kHz range and is therefore well suited to penetrate heterogenous materials such as concrete. This contribution gives an introduction in the working principle and signal characteristics of the fluidic transducer. Its applicability to measurements in concrete is verified. A detailed outlook is given to discuss the future potential of fluidic ultrasonic actuators.
Materials are key for our modern communities; current life seems nearly impossible without concrete, plastic and metal. In particular metals play important roles in all areas of our daily life - from building materials to high tech products.
However, due to the increasing consumption of metals and corresponding waste production, an elevated release of metals from buildings and consumer goods into the environment takes place. Furthermore, metals in direct contact with the environment undergo corrosion processes which leads also to a release of metals into the (aquatic) environment. Besides this immediate metal release, the lifespan of products/buildings are substantially reduced – hence unnecessary economic costs arise. Thus, research in this regard is needed within the force field of metal/material environment.
However, to evaluate the environmental impact of materials as well as developing “safe” materials, new analytical methods are highly needed. One promising powerful tool in this regard is single cell-ICP-ToF-MS for multi-elemental analysis on a single cell/organism level.
Within this presentation the concept, strength as well as challenge of single cell-ICP-MS are briefly introduced. Afterwards, two application examples are presented: (i) assessing the environmental impact of metals and (ii) the impact of the environment on metal-based materials and the derivation of potential environmental-friendly material protection strategies. These applications highlight the strength of new analytical approaches to explore the durability and safety of newly developed materials. Thus, analytical chemistry is one corner stone to transformation of modern society into circular economy (CEco).
(i) Diatoms are located at the bottom of the food chain. Thus, toxicological relevant metals taken up by diatoms can possibly accumulate within the food web and cause harmful effects. Diatoms are a common test system in ecotoxicology. To investigate potential metal uptake and harmful effects on a single cell level, we developed an on-line single cell-ICP-ToF-MS approach for multi-elemental diatom analysis. Our approach is a new potential tool in ecotoxicological testing for metal-based materials.
(ii) Next to classical corrosion processes, microorganisms are responsible for so called microbially influenced corrosion (MIC). MIC is a highly unpredictable process relying on the interaction pathways between cells and the metal surface. To shed light on MIC processes and derivate potential metal protection strategies, we applied single cell-ICP-ToF-MS for MIC research on a single bacteria/archaea level. It turned out that microorganism are taking up particular metals from alloys - thus, single bacteria-ICP-ToF-MS will enable the development of environmental friendly corrosion protection strategies.
Several countries, which use or used nuclear power, started to destruct nuclear power plants. Thus, large amounts of radioactive waste have to be stored safely during the next decades. Large underground caverns will
be used a nuclear waste disposal. Once the cavern is full, a sealing construction is required. The sealing should avoid the contact to any fluids or substances of the storage barrels and reduce hazardous radiation.
Ultrasonic measurement technology has become indispensable in NDT-CE. Air-coupled ultrasonic (ACU) measurement techniques promise to reduce measurement time. However, the signal quality suffers from large specific impedance mismatch at the transducer-air and air-specimen interface. Additionally, large pressure amplitudes are necessary for the penetration depth required in NDT-CE applications.
To address the specific requirements of ultrasonic testing in NDT-CE, a robust ACU transducer was developed, that generates ultrasound by quickly switching a pressurized air flow. The simple design of the fluidic transducer makes the device maintenance free and resilient against harsh environmental conditions. Since the signal is generated by aeroacoustics, there is no specific impedance mismatch between the transducer and the surrounding air. The ultrasonic signal exhibits frequencies in the 30-60 kHz range and is therefore well suited to penetrate heterogenous materials such as concrete. This contribution gives an introduction in the working principle and signal characteristics of the fluidic transducer. A detailed outlook is given to discuss the future potential of fluidic ultrasonic actuators.
Interdigital transducers (IDTs) are a well-known tool for excitation of surface acoustic waves. The use of IDTs is versatile, but they are most commonly employed as actuators for excitation of ultrasonic guided waves (UGWs). However, they are still a relatively new technology, which leaves many possibilities for future research, especially in the scope of newly emerging structural health monitoring (SHM) systems. IDTs offer low weight, design flexibility and beam directivity, which make them ideal candidates for employment in such systems.
Due to the IDTs’ and waves’ complexity, problems often cannot be described analytically, therefore they require numerical solutions and experimental validations. In this contribution, a novel, simple use of IDTs, in the scope of SHM is described. Firstly, numerical findings acquired with finite element method are presented. To validate those results, experiments in a plate-like waveguide are carried out. A good agreement between them is found. The results show the potential of the IDTs in yet another prospective application, which could be attractive for adoption in the future.
In non-destructive testing and structural health monitoring, ultrasonic guided waves (UGWs) are of great interest for finding and characterizing structural flaws. The interaction of the waves with the flaws can often not be described analytically due to waves’ complexity. This makes numerical simulations and experiments indispensable. However, mentioned field of research is still relatively young and most of the methods focus on flaw localization, using time of flight of the reflected signal. This leaves many possibilities for further research, especially when it comes to separate analysis of different propagating modes.
It is well-known that ultrasonic wave modes convert when interacting with flaws. When a fundamental mode (A0 or S0) encounters a notch, it interacts and converts to another fundamental mode. In this contribution, this effect is used to analyze the depth of a notch. Firstly, numerical simulations are presented, which show notch depth proportionality to amplitude ratio of fundamental modes. To validate these results, experiments were carried out on a metal plate with a shallow notch which was gradually deepened. UGWs were excited using a polymer-based interdigital transducer (IDT) and detected with a 3D laser Doppler vibrometer. The IDT is employed to ensure excitation of a single mode and thus to reduce the complexity of the analysis. Good agreement between numerical and experimental results has been found. The results show the potential of UGWs not only for defect reconstruction and localization, but also its precise sizing.