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Climate change and related energy policies, exacerbated by unforeseen geopolitical developments, pose new challenges for gas analytics, such as the use of hydrogen, hydrogen-containing alternative gaseous fuels (NH3, etc.), the use of alternative methane-based energy gases (LNG, LPG, etc.) or decarbonisation via CCSU. In all topics, the quality, i.e. the actual chemical composition of the gases, naturally plays a decisive role. BAM is meeting this strategic importance with the further development of hydrogen analytics and is continuing to develop the methods used in order to support the German economy and research landscape with traceability, reference materials and analytical procedures as quickly as possible.
Mass spectrometry plays an important role for trace analysis in hydrogen matrix. The presentation shows first experimental results from the application of PTR-TOF-MS (Proton Transfer Reaction Time-of-Flight Mass Spectrometry).
Mycotoxins (toxins formed by fungi) in food and have caused problems for mankind since the beginning of time. The group of ergot alkaloids plays a special role in human history. Several tens of thousands of deaths during the middle ages caused by to ergotism (the disease caused by continuous intake of ergot alkaloid contaminated food) underscore the importance of reliable analytical methods to ensure food safety.
More than 50 compounds belong to the group of ergot alkaloids. The 12 most found structures – the major ergot alkaloids – are typically measured, when it comes to ergot alkaloid quantification. High performance liquid chromatography (HPLC) with a fluorescence detector (FLD) is typically used to quantify the ergot alkaloid content. The main disadvantage of this method are the high costs for calibration standards (12 different calibration substances are required). But also the time and effort required for the analysis of 12 peaks and overlapping signals that occur in complex food samples such as bread. As all ergot alkaloids share the ergoline structure and just differ in the substituents attached to this backbone, measurement of all ergot alkaloids in one sum parameter presents a time and cost saving alternative. The most important step for the development of such a sum parameter method is the reaction used to transfer all ergot alkaloids to one uniform structure. In the talk two promising reactions, the acidic esterification to lysergic acid methyl ester and hydrazinolysis to lysergic acid hydrazide, are examined for possible use in a routine analysis method. In addition to yield and reaction rate, factor such as the handling of the reaction and the possibility of parallelization play a role. Next to the current status of the ongoing research project, in this talk, current approaches to ergot alkaloid quantitation will be discussed.
The aim of this work is to achieve reliable nondestructive evaluation (NDE) of adhesively bonded aerospace components by developing novel multidimensional data fusion techniques, which would combine the information obtained by ultrasonic and X-ray NDE methods. Separately, both NDE techniques have their advantages and limitations. The integration of data obtained from pulse echo immersion ultrasound testing and radiography holds immense potential to help improve the reliability of non-destructive evaluation. In this study, distinctive features obtained from single techniques, traditional ultrasonic pulse echo testing, and radiography, as well as fused images, were investigated and the suitability of these distinctive features and fusion techniques for improving the probability of defect detection was evaluated. For this purpose, aluminum single lap joints with brass inclusions were analyzed using ultrasound pulse echo and radiography techniques. The distinctive features were extracted from the data obtained, and images of features obtained by both techniques were fused together. Different combinations of features and fusion algorithms were investigated, considering the desire to automate data evaluation in the future.
Validation of novel ultrasonic phased array borehole probe by using simulation and measurement
(2022)
Low-frequency ultrasonic testing is a well-established non-destructive testing (NDT) method in civil engineering for material characterization and the localization of cracks, reinforcing bars and delamination. A novel ultrasonic borehole probe is developed for in situ quality assurance of sealing structures in radioactive waste repositories using existing research boreholes. The aim is to examine the sealing structures made of salt concrete for any possible cracks and delamination and to localize built-in components. A prototype has been developed using 12 individual horizontal dry point contact (DPC) shear wave transducers separated by equidistant transmitter/receiver arrays. The probe is equipped with a commercially available portable ultrasonic flaw detector used in the NDT civil engineering industry. To increase the sound pressure generated, the number of transducers in the novel probe is increased to 32 transducers. In addition, the timed excitation of each transducer directs a focused beam of sound to a specific angle and distance based on the previously calculated delay time. This narrows the sensitivity of test volume and improves the signal-to-noise ratio of the received signals. In this paper, the newly designed phased array borehole probe is validated by beam computation in the CIVA software and experimental investigations on a half-cylindrical test specimen to investigate the directional characteristics. In combination with geophysical reconstruction methods, it is expected that an optimised radiation pattern of the probe will improve the signal quality and thus increase the reliability of the imaging results. This is an important consideration for the construction of safe sealing structures for the safe disposal of radioactive or toxic waste.
Mycotoxins (toxic compounds formed by fungi) in food and feed have caused problems for mankind since the beginning of time. The group of ergot alkaloids plays a special role in human history. Several tens of thousands of deaths during the middle ages caused by to ergotism (the disease caused by continuous intake of ergot alkaloid contaminated food) underscore the importance of reliable analytical methods to ensure food safety.
More than 50 compounds belong to the group of ergot alkaloids. The 12 most found structures – the major ergot alkaloids – are typically measured, when it comes to ergot alkaloid quantification. High performance liquid chromatography (HPLC) with a fluorescence detector (FLD) is typically used to quantify the ergot alkaloid content. The main disadvantage of this method are the high costs for calibration standards (12 different calibration substances are required). But also, the time and effort required for the analysis of 12 peaks and overlapping signals that occur in complex food samples such as bread. As all ergot alkaloids share the ergoline structure and just differ in the substituents attached to this backbone, measurement of all ergot alkaloids in one sum parameter presents a time and cost saving alternative. The most important step for the development of such a sum parameter method is the reaction used to transfer all ergot alkaloids to one uniform structure. Two promising reactions, the acidic esterification to lysergic acid methyl ester and hydrazinolysis to lysergic acid hydrazide, were examined for possible use in a routine analysis method. In addition to yield and reaction rate, factors such as handling of the reaction and the possibility of parallel sample workup play a role.
Investigation of degradation of the aluminum current collector in lithium-ion batteries by GD-OES
(2022)
Lithium-ion batteries (LIBs) are one technology to overcome the challenges of climate and energy crisis. They are widely used in electric vehicles, consumer electronics, or as storage for renewable energy sources. However, despite innovations in batteries' components like cathode and anode materials, separators, and electrolytes, the aging mechanism related to metallic aluminum current collector degradation causes a significant drop in their performance and prevents the durable use of LIBs. Glow-discharge optical emission spectroscopy (GD-OES) is a powerful method for depth-profiling of batteries' electrode materials. This work investigates aging-induced aluminum deposition on commercial lithium cobalt oxide (LCO) batteries' cathodes. The results illustrate the depth-resolved elemental distribution from the cathode surface to the current collector. An accumulation of aluminum is found on the cathode surface by GD-OES, consistent with results from energy-dispersive X-ray spectroscopy (EDX) combined with focused ion beam (FIB) cutting. In comparison to FIB-EDX, GD-OES allows a fast and manageable depth-profiling. Results from different positions on an aged cathode indicate an inhomogeneous aluminum film growth on the surface. The conclusions from these experiments can lead to a better understanding of the degradation of the aluminum current collector, thus leading to higher lifetimes of LIBs.
In industrialised countries more than 80% of the time is spent indoors. Products, such as building materials and furniture, emit volatile organic compounds (VOCs), which are therefore ubiquitous in indoor air. VOC in combination may, under certain environmental and occupational conditions, result in reported sensory irritation and health complaints. Emission concentrations can become further elevated in new or refurbished buildings where the rate of air exchange with fresh ambient air may be limited due to improved energy saving aspects. A healthy indoor environment can be achieved by controlling the sources and by eliminating or limiting the release of harmful substances into the air. One way is to use (building) materials proved to be low emitting. Meanwhile, a worldwide network of professional commercial and non-commercial laboratories performing emission tests for the evaluation of products for interior use has been established. Therefore, comparability of test results must be ensured. A laboratory’s proficiency can be proven by internal and external validation measures that both include the application of suitable emission reference materials (ERM). For the emission test chamber procedure according to EN 16516, no artificial ERM is commercially available. The EU-funded EMPIR project MetrIAQ aims to fill this gap by developing new and improved ERMs. The goal is to obtain a material with a reproducible and temporally constant compound release (less than 10% variability over 14 days). Different approaches, such as the impregnation of porous materials, are being tested. The generation as well as results of the most promising materials will be presented.
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Croatia. 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.
This study is part of a global project that covers various other countries (see www.qi-fokus.de).
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in the United Kingdom. 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.
This study is part of a global project that covers various other countries (see www.qi-fokus.de).
A recent upgrade of key equipment of the BAMline widens its imaging capabilities: shorter scan acquisition times are now possible, in situ and operando studies can now be routinely performed, and different energy spectra can easily be set up. In fact, the upgraded double-multilayer monochromator brings full flexibility by yielding different energy spectra to optimize flux and energy resolution as desired.
Deciphering microbiological influenced corrosion processes on steel with single cell-ICP-ToF-MS
(2022)
Microbiologically influenced corrosion (MIC) is a highly unpredictable process dictated by the environment, microorganisms, and the respective electron source. Interaction pathways between cells and the metal surface remain unclear. The development of this novel single cell-inductively coupled plasma-time of flight-mass spectrometry analytical method and a MIC-specific staining procedure facilitate the investigation of steel-MIC interactions. With this it is possible to analyze the multi-elemental fingerprint of individual cells. The detection method revealed elemental selectivity for the corrosive methanogenic archaeal strain Methanobacterium-affiliated IM1. The interface between material and environmental analysis thus receives special attention, e.g., when considering MIC on solid steel. Hence, the possible uptake of individual elements from different steel samples is investigated. Results showed the cells responded at a single-cell level to the different types of supplemented elements and displayed the abilities to interact with chromium, vanadium, titanium, cobalt, and molybdenum from solid metal surfaces. The information obtained will be used in the future to elucidate underlying mechanisms and develop possible material protection concepts, thus combining modern methods of analytical sciences with materials research.
References.
Geführte Ultraschallwellen sind für die Materialcharakterisierung hervorragend geeignet, da ihr Ausbreitungsverhalten abhängig von den Materialeigenschaften des untersuchten Werkstoffs ist.
Um aus dem messtechnisch ermittelten Ausbreitungsverhalten geführter Ultraschallwellen Rückschlüsse auf die Materialparameter zu ziehen, werden in der aktuellen Forschung verschiedene inverse Methoden diskutiert. Dispersionsabbildungen im Frequenz-Wellenzahl-Bereich repräsentieren das Ausbreitungsverhalten geführter Ultraschallwellen. Maschinelles Lernen und insbesondere Convolutional-Neural-Networks (CNNs) sind eine Möglichkeit der automatisierten inversen Bestimmung der Materialparameter aus den Dispersionsabbildungen.
In diesem Beitrag wird anhand synthetischer Daten gezeigt, wie das Ausbreitungsverhalten von geführten Ultraschallwellen unter Verwendung von CNNs und Dispersionsabbildungen genutzt werden kann, um die elastischen Konstanten einer isotropen plattenförmigen Struktur zu bestimmen. Anhand dieses Beispiels wird das generelle Vorgehen zur Anwendung maschineller neuronaler Lernverfahren aufgezeigt. Hierfür werden die verwendeten Daten analysiert, das Preprocessing erläutert und eine einfache CNN-Architektur gewählt. Im Rahmen der Auswertung wird insbesondere Wert auf die Erklärbarkeit und Zuverlässigkeit des verwendeten CNNs gelegt und so Grenzen und Möglichkeiten aufgezeigt.
In non-destructive testing and structural health monitoring with ultrasonic waves, the quantification of damage in components is one of the main tasks. In many shell-like structures, such as plates, pipes, or laminate components, ultrasonic waves propagate as guided waves. Although guided waves enable the testing of large areas, their multimodal and dispersive properties make it challenging to analyze signals. So, there is a need for more advanced algorithms to handle these properties, especially when reconstructing damage position and geometry.
The reconstruction can be formulated as an inverse problem where the measured signals are fitted with a simulative forward model. Due to the small wavelength of ultrasonic waves, classic forward models based on, e.g., the Finite Element Method are computationally intensive. In contrast, the authors use the semi-analytical Scaled Boundary Finite Element Method (SBFEM) to reduce the computational effort. The SBFEM approximates arbitrary long, undamaged parts of the structure with only a few degrees of freedom.
This contribution summarizes a general inverse procedure based on algorithmic differentiation in combination with the SBFEM. Results are presented for damaged 2D cross-sectional models of waveguides. These results include an analysis of the robustness of the proposed algorithms against noise.
This paper considers an indirect measurement approach to reconstruct a defect in a two-dimensional waveguide model for a non-destructive ultrasonic inspection via derivative-based optimization. The propagation of the mechanical waves is simulated by the scaled boundary finite element method that builds on a semi-analytical approach. The simulated data are then fitted to given data associated with the reflected waves from a defect which is to be reconstructed. For this purpose, we apply an iteratively regularized Gauss-Newton method in combination with algorithmic differentiation to provide the required derivative information accurately and efficiently. We present numerical results for three kinds of defects, namely, a crack, delamination, and corrosion. The objective function and the properties of the reconstruction method are investigated. The examples show that the parameterization of the defect can be reconstructed efficiently as well as robustly in the presence of noise.
In the interest of exploring their potential in the field of single particle analysis, a Microdroplet Generator (MDG) was coupled to an ICP-ToF-MS.
Isotopic Dilution Analysis was also incorporated for the size determination of three different Platinum Nanoparticles samples (50, 63 and 70 nm). The performance of the technique was validated by comparison to traditional size characterization techniques (sp-ICP-ToF-MS, TEM), while the robustness of the technique was proven by incorporating NaCl in the samples’ matrix, up to 100 mg/L.
LIBS is a complementary method to XRF and can detect all elements without the need for vacuum conditions. Automated systems are already commercially available capable of scanning surfaces with a resolution of up to 0.1 mm within a few minutes. In addition to possible applications in R&D, LIBS is also used for practical applications in building materials laboratories and even on-site.
In view of ageing infrastructure facilities, a reliable assessment of the condition of concrete structures is of increasing interest. For concrete structures, the ingress of potential harmful ions is affecting the serviceability and eventually structural performance. Pitting corrosion induced by penetrating chlorides is the dominant deterioration mechanism. Condition assessment based on frequently performed chloride profiling can be useful to identify the extent and evolution of chloride ingress. This could prove to be more economical than extensive repairs, especially for important infrastructure facilities.
Currently the most common procedure for determining the chloride content is wet chemical analysis with standard resolution of 10 mm. The heterogeneity is not considered. LIBS is an economical alternative for determining the chloride content at depth intervals of 1 mm or less. It provides 2D distributions of multiple elements and can locate spots with higher concentrations. The results are directly correlated to the mass of binder and can also be performed on-site with a mobile LIBS-System.
The application of a LIBS-system is presented. Calibration is required for quantitative analysis. Concrete cores were drilled, sliced and analyzed to determine the 2D-distribution of harmful elements. By comparing the chloride ingress and the carbonation, the interaction of both processes can be visualized in a measurement that takes less than 10 minutes for a 50 mm x 100 mm drill core.
A leaflet on the use of LIBS for the chloride ingress assessment has been completed.
In many scientific fields, isotopic analysis can offer valuable information, e.g., for tracing the origin of food products, environmental contaminants, forensic and archaeological samples (provenance determination), for age determination of minerals (geochronological dating) or for elucidating chemical processes. Up to date, typically bulk analysis is aimed at measuring the isotopic composition of the entire elemental content of the sample. However, the analyte element is usually present under the form of different elemental species. Thus, separating species of interest from one another and from matrix components prior to isotope ratio measurements can provide species-specific isotopic information, which could be used for tracing the origin of environmental pollutants and elucidation of (environmental) speciation. Using on-line hyphenations of separation techniques with multicollector-ICP-MS (MC-ICP-MS) can save time and effort and enables the analysis of different species during a single measurement.
In this work, we developed an on-line hyphenation of CE with multicollector-ICP-MS (CE/MC-ICP-MS) for isotopic analysis of sulfur species. With this method, the isotopic composition of sulfur in sulfate originating from river water could be analyzed without sample preparation. The results were compared with data from off-line analysis of the same samples to ensure accuracy. The precision of the results of the on-line measurements was high enough to distinguish the rivers from one another by the isotopic signature of the river water sulfate. Next to environmental applications, a current field is species-specific isotopic analysis of biomolecules, as sulfur is the only covalently bound constituent of proteins which can be analyzed by MC-ICP-MS. Data analysis of transient signals in terms of isotope ratio determination is further issue - we developed a small free accessible App allowing for fast data analysis taking relevant aspects (e.g., mass bias correction, peak picking, …) into account.