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Paper des Monats
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The site of Schöningen (Germany), dated to ca. 300,000 years ago, yielded the earliest large-scale record of humanly-made wooden tools. These include wooden spears and shorter double-pointed sticks, discovered in association with herbivores that were hunted and butchered along a lakeshore. Wooden tools have not been systematically analysed to the same standard as other Palaeolithic technologies, such as lithic or bone tools. Our multianalytical study includes micro-CT scanning, 3-dimensional microscopy, and Fourier transform infrared spectroscopy, supporting a systematic technological and taphonomic analysis, thus setting a new standard for wooden tool analysis. In illustrating the biography of one of Schöningen’s double-pointed sticks, we demonstrate new human behaviours for this time period, including sophisticated woodworking techniques. The hominins selected a spruce branch which they then debarked and shaped into an aerodynamic and ergonomic tool. They likely seasoned the wood to avoid cracking and warping. After a long period of use, it was probably lost while hunting, and was then rapidly buried in mud. Taphonomic alterations include damage from trampling, fungal attack, root damage and compression. Through our detailed analysis we show that Middle Pleistocene humans had a rich awareness of raw material properties, and possessed sophisticated woodworking skills. Alongside new detailed morphometrics of the object, an ethnographic review supports a primary function as a throwing stick for hunting, indicating potential hunting strategies and social contexts including for communal hunts involving children. The Schöningen throwing sticks may have been used to strategically disadvantage larger ungulates, potentially from distances of up to 30 metres. They also demonstrate that the hominins were technologically capable of capturing smaller fast prey and avian fauna, a behaviour evidenced at contemporaneous Middle Pleistocene archaeological sites.
VOC-emissions and their odours from building products and furnishings present indoors should not have an impact on personal well-being or health. Odours can be measured by applying the standard ISO 16000-28. Indoor air determination of odour emissions from building products using test chambers. One of the described procedures is the assessment of perceived intensity using a comparative scale by a group of panellists. In this paper, the perceived intensity sampling procedure and its evaluation method are investigated and shown to need improvement. New technical developments in the methodology used to increase the reproducibility of measurement results are discussed. Since odour tests are used for labelling, they have a major influence on the assessment of construction products, similar to the procedure of the German Committee for Health Evaluation of Building Products (AgBB). In the original ISO standard, the evaluation is typically performed using a sampling container separated from the emission chamber. For a better sample presentation, an adapter was developed to connect the emission test chamber to the evaluation funnel and thus enable an odour assessment which is comparable to a direct measurement. The investigations show that losses of odourous substances can be greatly reduced, which is very desirable when seeking to obtain reliable results in odour measurement. Another experimental series was carried out to reduce the measurement effort in the evaluation of perceived intensity. Application of the developed greater than or less than/equal to. query could be helpful here. The results show that the query mostly leads to the same result as the evaluation of the perceived intensity using the method according to the standard but is much easier to perform. Overall, the results can contribute to improving the acceptance of the evaluation of perceived intensity using ISO 16000-28 and to determining odours from building materials increasingly more precisely.
In this article, we present two Coptic papyri, P 11934 and P 11935 from the Berlin collection excavated in Ashmunein (ancient Hermopolis) by Otto Rubensohn in 1906. We employ a multi-disciplinary approach that takes into account both their materiality – writing support as well as ink – and their content, as has become ‘best practice’. 1 Material aspects of written documents have traditionally been the purview of papyrologists. Recently developed methods of scientific analysis generate sets of archaeometric data with the potential to improve understanding of the materiality of ancient document production, as well as to yield new evidence for genuine papyrological research questions. To achieve this, a large corpus of comparative data needs to be built. Our contribution offers a first step in this direction. We aim at presenting the papyri, which were selected because of the ink corrosion during conservation work at the Berlin collection, in a format that is exhaustive both for material and textual aspects. The inks from both papyri were analysed using a combination of techniques, contributing to our better understanding of the development of ink technology in Late Antiquity.
For a significant increase in the strength of high-strength fine-grained structural steels with a nominal yield strength ≥690 MPa, the addition of microalloying elements such as Nb and Ti is required. The standard specifications for the chemical composition of these steels (e.g., in EN 10025-6) often only give the manufacturer limit contents to achieve the defined properties. The effect of the alloying elements in the heat affected zone (HAZ) is sometimes completely contrary.
This makes it difficult to adequately predict the batch dependency regarding weldability and the load-bearing behaviour of the welded joint. Three different micro-alloyed steels of the grade S690QL were produced on a laboratory scale, focusing on different Nb and Ti contents. To investigate the tempering effect, these were gas metal arc welded in three layers. In addition to metallographic investigations of individual HAZ areas, thermodynamic phase calculations were carried out using Thermo-Calc, following variations in the chemical composition. This provides an understanding of phase transformation, precipitation growth, and dissolution during welding as a function of temperature and cooling conditions. The results show
a divergent metallurgical behaviour in the HAZ of the three different micro-alloyed steels. Thereby, the Ti micro-alloyed grade showed a strong softening of the HAZ in contrast to the Nb micro-alloyed grade. This can be attributed to a contrary precipitation behaviour during welding.
An interlaboratory comparison (ILC)was organised to characterise 87Sr/86Sr isotope ratios in geological and industrial reference materials by applying the so-called conventional method for determining 87Sr/86Sr isotope ratios. Four cements (VDZ 100a,VDZ 200a, VDZ 300a, IAG OPC-1), one limestone (IAG CGL ML-3) and one slate (IAG OU-6) reference materials were selected, covering a wide range of naturally occurring Sr isotopic signatures. Thirteen laboratories received aliquots of these six reference materials together with a detailed technical protocol. The consensus values for the six reference materials and their associated measurement uncertainties were obtained by applying a Gaussian, linear mixed effects model fitted to all the measurement results. By combining the consensus values and their uncertainties with an uncertainty contribution for potential heterogeneity, reference values ranging from 0.708134 mol mol-1 to 0.729778 mol mol-1 were obtained with relative expanded uncertainties of ≤ 0.007 %. This study represents an ILC on conventional 87Sr/86Sr isotope ratios, within which metrological principles were considered and the compatibility of measurement results obtained by MC-ICP-MS and by MC-TIMS is demonstrated. The materials characterised in this study can be used as reference materials for validation and quality control purposes and to estimate measurement uncertainties in conventional 87Sr/86Sr isotope ratio measurement.
Outer membrane lipopolysaccharides (LPS) play a crucial role in determining attachment behavior and pathogenicity of bacteria. The aim of this study was to develop a simple procedure for anchoring bacterial lipopolysaccharides to polystyrene (PS) microparticles as a model system for in situ attachment studies. By using a swellcapture methodology, commercially available LPS of Pseudomonas aeruginosa (strain ATCC 27316 serotype 10.22) was anchored onto PS microparticles in a proof-of-concept study. A detailed chemical and morphological characterization has proven the success of LPS incorporation. It was shown that the coverage and structure of the LPS film was concentration dependent. The procedure can easily be adapted to LPS of other bacterial strains to generate a synthetic model toolkit for attachment studies.
Growth factors are a class of proteins that play a role in the proliferation (the increase in the number of cells resulting from cell division) and differentiation (when a cell undergoes changes in gene expression becoming a more specific type of cell) of cells. They can have both positive (accelerating the normal healing process) and negative effects (causing cancer) on disease progression and have potential applications in gene therapy and wound healing. However, their short half-life, low stability, and susceptibility to degradation by enzymes at body temperature make them easily degradable in vivo. To improve their effectiveness and stability, growth factors require carriers for delivery that protect them from heat, pH changes, and proteolysis. These carriers should also be able to deliver the growth factors to their intended destination. This review focuses on the current scientific literature concerning the physicochemical properties (such as biocompatibility, high affinity for binding growth factors, improved bioactivity and stability of the growth factors, protection from heat, pH changes or appropriate electric charge for growth factor attachment via electrostatic interactions) of macroions, growth factors, and macroion-growth factor assemblies, as well as their potential uses in medicine (e.g., diabetic wound healing, tissue regeneration, and cancer therapy).
Specific attention is given to three types of growth factors: vascular endothelial growth factors, human fibroblast growth factors, and neurotrophins, as well as selected biocompatible synthetic macroions (obtained through standard polymerization techniques) and polysaccharides (natural macroions composed of repeating monomeric units of monosaccharides). Understanding the mechanisms by which growth factors bind to potential carriers could lead to more effective delivery methods for these proteins, which are of significant interest in the diagnosis and treatment of neurodegenerative and civilization diseases, as well as in the healing of chronic wounds.
This article reports temperature-dependent elastic properties (Young’s modulus, shear modulus) of three alloys measured by the dynamic resonance method. The alloys Ti-6Al-4V, Inconel IN718, and AISI 316 L were each investigated in a variant produced by an additive manufacturing processing route and by a conventional manufacturing processing route. The datasets include information on processing routes and parameters, heat treatments, grain size, specimen dimensions, and weight, as well as Young’s and shear modulus along with their measurement uncertainty. The process routes and methods are described in detail. The datasets were generated in an accredited testing lab, audited as BAM reference data, and are hosted in the open data repository Zenodo. Possible data usages include the verification of the correctness of the test setup via Young’s modulus comparison in low-cycle fatigue (LCF) or thermo-mechanical fatigue (TMF) testing campaigns, the design auf VHCF specimens and the use as input data for simulation purposes.
The reduction in train-induced ground vibrations by different railway lines and by mitigation measures in the propagation path was analysed in a unified approach by two-dimensional finite element calculations. In general, there was no reduction at low frequencies, and the reduction be-came stronger with increasing frequencies. A maximum reduction of 0.1 at high frequencies was established with an open trench. Reductions between 0.7 and 0.2 have been found for the other sit-uations, filled trenches, walls, plates, and blocks, as well as for railway lines on dams, in cuts and in a tunnel. Bridges can produce amplifications due to their resonance frequencies, but also strong reductions due to massive bridge piers. The influence of some parameters has been analysed, such as the bridge span, the inclination of the dam and the cut, the stiffness of the soil, and the tunnel structure. The dynamic track stiffnesses of a surface, bridge, and tunnel track have been calculated using the 3D finite-element boundary-element method for comparison with corresponding meas-urements.
BPA is a chemical commonly used in the production of polymer-based materials that can have detrimental effects on the thyroid gland and impact human reproductive health. Various expensive methods, such as liquid and gas chromatography, have been suggested for detecting BPA.
The fluorescence polarization immunoassay (FPIA) is an inexpensive and efficient homogeneous mix-and-read method that allows for high-throughput screening. FPIA offers high specificity and sensitivity and can be carried out in a single phase within a timeframe of 20–30 min. In this study, new tracer molecules were designed that linked the fluorescein fluorophore with and without a spacer to the bisphenol A moiety. To assess the influence of the C6 spacer on the sensitivity of an assay based on the respective antibody, hapten–protein conjugates were synthesized and assessed for performance in an ELISA setup, and this resulted in a highly sensitive assay with a detection limit of 0.05 µg/L. The lowest limit of detection was reached by employing the spacer derivate in the FPIA and was 1.0 µg/L, working range from 2 to 155 µg/L. The validation of the methods was conducted using actual samples compared to LC–MS/MS, which served as the reference method. The FPIA and ELISA both demonstrated satisfactory concordance.
Mistle: bringing spectral library predictions to metaproteomics with an efficient search index
(2023)
Motivation: Deep learning has moved to the forefront of tandem mass spectrometry-driven proteomics and authentic prediction for peptide fragmentation is more feasible than ever. Still, at this point spectral prediction is mainly used to validate database search results or for confined search spaces. Fully predicted spectral libraries have not yet been efficiently adapted to large search space problems that often occur in metaproteomics or proteogenomics.
Results: In this study, we showcase a workflow that uses Prosit for spectral library predictions on two common metaproteomes and implement an indexing and search algorithm, Mistle, to efficiently identify experimental mass spectra within the library. Hence, the workflow emulates a classic protein sequence database search with protein digestion but builds a searchable index from spectral predictions as an in-between step.
We compare Mistle to popular search engines, both on a spectral and database search level, and provide evidence that this approach is more accurate than a database search using MSFragger. Mistle outperforms other spectral library search engines in terms of run time and proves to be extremely memory efficient with a 4- to 22-fold decrease in RAM usage. This makes Mistle universally applicable to large search spaces, e.g. covering comprehensive sequence databases of diverse microbiomes.
Availability and implementation: Mistle is freely available on GitHub at https://github.com/BAMeScience/Mistle.
The application of compact NMR instruments to hot flowing samples or exothermically reacting mixtures is limited by the temperature sensitivity of permanent magnets. Typically, such temperature effects directly influence the achievable magnetic field homogeneity and hence measurement quality. The internal-temperature control loop of the magnet and instruments is not designed for such temperature compensation. Passive insulation is restricted by the small dimensions within the magnet borehole. Here, we present a design approach for active heat shielding with the aim of variable temperature control of NMR samples for benchtop NMR instruments using a compressed airstream which is variable in flow and temperature. Based on the system identification and surface temperature measurements through thermography, a model predictive control was set up to minimise any disturbance effect on the permanent magnet from the probe or sample temperature. This methodology will facilitate the application of variable-temperature shielding and, therefore, extend the application of compact NMR instruments to flowing sample temperatures that differ from the magnet temperature.
Capillary active interior insulation materials are an important approach to minimize energy losses of historical buildings. A key factor for their performance is a high liquid conductivity, which enables redistribution of liquid moisture within the material. We set up an experiment to investigate the development of moisture profiles within two different interior insulation materials, calcium-silicate (CaSi) and expanded perlite (EP), under constant boundary conditions. The moisture profiles were determined by two different methods: simple destructive sample slicing with subsequent thermogravimetric drying as well as non-destructive NMR measurements with high spatial resolution. The moisture profiles obtained from both methods show good agreement, when compared at the low spatial resolution of sample slicing, which demonstrates the reliability of this method. Moreover, the measured T2-relaxation-time distributions across the sample depth were measured, which may give further insight into the saturation degree of the different pore sizes. In order to explain differences in the moisture profiles between CaSi and EP, we determined their pore-size distribution with different methods: conversion of the NMR T2 relaxationtime distribution at full saturation, mercury intrusion porosimetry and indirect determination from pressure plate measurements. CaSi shows a unimodal distribution at small pore diameters, while in EP, a bi-modal or wider distribution was found. We assume that the smaller pore diameters of CaSi lead to a higher capillary conductivity, which causes a more distributed moisture profile in comparison with that of EP.
Transition metal phosphates (TMPs) have attracted interest as materials for (electro-) catalysis, and electrochemistry due to their low-cost, stability, and tunability. In this work, an automated synthesis platform was used for the preparation of transition metal phosphate crystals to efficiently explore the multidimensional parameter space, determining the phase selection, crystal sizes, shapes. By using X-ray diffraction and spectroscopy-based methods and electron microscopy imaging, a complete characterization of the phase stability fields, phase transitions, and crystal morphology/sizes was achieved. In an automated three-reactant synthesis, the individual effect of each reactant species NH4+, M2+, and PO43- on the formation of transition metal phosphate phases: M-struvite NH4MPO4·6H2O, M-phosphate octahydrate M3(PO4)2·8H2O with M = Ni, Co and an amorphous phase, was investigated. The NH4+ concentration dictates the phase composition, morphology, and particle size in the Ni-system (crystalline Ni-struvite versus amorphous Ni-PO4 phase), whereas in the Co-system all reactant species - NH4+, Co2+, and PO43- - influence the reaction outcome equivalently (Co-struvite vs. Co-phosphate octahydrate). The coordination environment for all crystalline compounds and of the amorphous Ni-PO4 phase was resolved by X-ray absorption spectroscopy, revealing matching characteristics to its crystalline analogue, Ni3(PO4)2·8H2O. The automated synthesis turned out to be significantly advantageous for the exploration of phase diagrams due to its simple modularity, facile traceability, and enhanced reproducibility compared to a typical manual synthesis.
Adipokinetic hormone (AKH) is a neuropeptide produced in the insect corpora cardiaca that plays an essential role in mobilising carbohydrates and lipids from the fat body to the haemolymph. AKH acts by binding to a rhodopsin-like G protein-coupled receptor (GPCR), the adipokinetic hormone receptor (AKHR). In this study, we tackle AKH ligand and receptor gene evolution as well as the evolutionary origins of AKH gene paralogues from the order Blattodea (termites and cockroaches). Phylogenetic analyses of AKH precursor sequences point to an ancient AKH gene duplication event in the common ancestor of Blaberoidea, yielding a new group of putative decapeptides. In total, 16 different AKH peptides from 90 species were obtained. Two octapeptides and seven putatively novel decapeptides are predicted for the first time. AKH receptor sequences from 18 species, spanning solitary cockroaches and subsocial wood roaches as well as lower and higher termites, were subsequently acquired using classical molecular methods and in silico approaches employing transcriptomic data. Aligned AKHR open reading frames revealed 7 highly conserved transmembrane regions, a typical arrangement for GPCRs.
Phylogenetic analyses based on AKHR sequences support accepted relationships among termite, subsocial (Cryptocercus spp.) and solitary cockroach lineages to a large extent, while putative post-translational modification sites do not greatly differ between solitary and subsocial roaches and social termites. Our study provides important information not only for AKH and AKHR functional research but also for further analyses interested in their development as potential candidates for biorational pest control agents against invasive termites and cockroaches.
Regardless of the experimental care practiced in acquiring X-ray computed tomography (XCT) data, artifacts might still exist, such as noise and blur. This is typical for fast XCT data acquisitions (e.g., in-situ investigations), or low-dose XCT. Such artifacts can complicate subsequent analysis of the data. Digital filters can moderately cure extensive artifacts. The selection of filter type, intensity, and order of application is not always straight forward. To tackle these problems, a complete sequential multilevel, multi-scale framework: BAM SynthCOND, employing newly designed deep convolutional neural networks (DCNNs), was formulated. Although data conditioning with neural networks is not uncommon, the main complication is that completely artifact-free XCT data for training do not exist. Thus, training data were acquired from an in-house developed library (BAM SynthMAT) capable of generating synthetic XCT material microstructures. Some novel DCNN architectures were introduced (2D/3D ACEnet_Denoise, 2D/3D ACEnet_Deblur) along with the concept of Assertive Contrast Enhancement (ACE) training, which boosts the performance of neural networks trained with continuous loss functions. The proposed methodology accomplished very good generalization from low resemblance synthetic training data. Indeed, denoising, sharpening (deblurring), and even ring artifact removal performance were achieved on experimental post-CT scans of challenging multiphase Al-Si Metal Matrix Composite (MMC) microstructures. The conditioning efficiencies were: 92% for combined denoising/sharpening, 99% for standalone denoising, and 95% for standalone sharpening. The results proved to be independent of the artifact intensity. We believe that the novel concepts and methodology developed in this work can be directly applied on the CT projections prior to reconstruction, or easily be extended to other imaging techniques such as: Microscopy, Neutron Tomography, Ultrasonics, etc.
For a comprehensive safety assessment of stationary lithium-ion-battery applications, it is necessary to better understand the consequences of thermal runaway (TR). In this study, experimental tests comprising twelve TR experiments including four single-cell tests, two cell stack tests and six second-life module tests (2.65 kW h and 6.85 kW h) with an NMC-cathode under similar initial conditions were conducted. The temperature (direct at cells/modules and in near field), mass loss, cell/module voltage, and qualitative vent gas composition (Fourier transform infrared (FTIR) and diode laser spectroscopy (DLS) for HF) were measured. The results of the tests showed that the battery TR is accompanied by severe and in some cases violent chemical reactions. In most cases, TR was not accompanied by pregassing of the modules. Jet flames up to a length of 5 m and fragment throwing to distances to more than 30 m were detected. The TR of the tested modules was accompanied by significant mass loss of up to 82%. The maximum HF concentration measured was 76 ppm, whereby the measured HF concentrations in the module tests were not necessarily higher than that in the cell stack tests.
Subsequently, an explosion of the released vent gas occurred in one of the tests, resulting in the intensification of the negative consequences. According to the evaluation of the gas measurements with regard to toxicity base on the “Acute Exposure Guideline Levels” (AEGL), there is some concern with regards to CO, which may be equally as important to consider as the release of HF.
Climate change is becoming one of the greatest challenges facing our society, particularly due to the continued use of fossil fuels. The steadily increasing demand for energy and the continuously growing world population will further intensify these challenges. The development of renewable energies is therefore of central importance. The 2020 EU Energy Roadmap aims to increase the share of renewable energies (gross energy consumption) to 55% by 2050.
Hydrogen (H2) has the highest potential to become the primary renewable energy source. It is envisioned that by 2050 up to 24% of the total energy demand of Europe is to be ensured by H2. However, a decisive disadvantage of the climate friendly alternatives is the massive containment demand, which needs to be highly secure, cost efficient and easily extractable.
Underground geological formations (UGF) represent a seemingly optimal alternative to meet the rapidly increasing storage demand. In this context, many studies are currently underway to determine the feasibility and risks of UGF. However, little or no consideration is being given to microbiology. Therefore, in this Research Topic we will focus on achieving a greater understanding of the impact microorganisms exert on UGF, with a particular emphasis on interdisciplinary studies.
As many subsurface microbial communities can use H2 as an electron donor, production of seemingly undesirable metabolic byproducts, such as hydrogen sulfide, methane, and acids, are also to be expected. However, the rate of the H2 conversion by the microorganisms, how their metabolic activities impact the UGF on a short-term and long-term scale, the extent of damages microorganisms exert on the infrastructure, or potential use of microorganisms to enhance UGF are just a few questions that require urgent research to assess the role of microorganisms in this new anthropogenic use of the subsurface environment. These and many questions can be addressed in this article collection. In particular, understanding microbial community changes and activity rates will help assess operational and environmental risks, develop mitigation strategies and provide new insights on life under extreme conditions (i.e., pressure, salinity).
In this Research Topic, the editorial team particularly welcomes Original Research, Hypothesis and Theory, Method, and Review manuscripts that deal with the latest advances in microbiology in formations that are planned or currently prepared for hydrogen storage, from both fundamental and practical points of view. The ultimate objective is to promote a deeper understanding into the sustainability of UGF and generate interdisciplinary research involving microbiologists, reservoir engineers, geologists, chemists, physicists.
The topics of interest include, but are not limited to:
• Microbial diversity in different underground hydrogen storage sites or formations currently being considered for hydrogen storage
• Mechanism and impact of microbial growth under high H2 pressure
• Potential role of microorganisms in the short-term and long-term storage of hydrogen
• Potential influences of microorganisms on the hydrogen storage infrastructure systems, e.g., microbiologically influenced corrosion, biofilm growth
• Hydrogen-solid-microorganism interactions, including the influence of microbial growth on UGF geological parameters
• Mechanism and modelling of microbial impact on hydrogen storage
UGF relevant for this Research Topic include porous media, salt caverns, deep aquifers, hard rock caverns and depleted oil/gas reservoirs.
Since its isolation, graphene has received growing attention from academia and industry due to its unique properties. However, the “what is my material” barrier hinders further commercialization. X-ray photoelectron spectroscopy (XPS) is considered as a method of choice for the determination of the elemental and chemical composition. In this work the influence of the morphology of graphene particles on the XPS results is studied and investigated as a function of X-ray energy, using conventional XPS with Al K𝜶 radiation and hard X-ray photoemission spectroscopy (HAXPES) using Cr K𝜶 radiation. Thereby, the information depth is varied between 10 and 30 nm. For this purpose, two commercial powders containing graphene nanoplatelets with lateral dimensions of either ≈100 nm or in the micrometer range are compared. These larger ones exist as stack of graphene layers which is inspected with scanning electron microscopy. Both kinds of particles are then functionalized with either oxygen or fluorine. The size of the graphene particles is found to influence the degree of functionalization. Only the combination of XPS and HAXPES allows to detect the functionalization at the outermost surface of the particles or even of the stacks and to provide new insights into the functionalization process.
In this study, five laboratories, namely, BRML (Romania), TUBITAK UME (Turkey), IMBIH (Bosnia and Herzegovina), BAM (Germany), and DTI (Denmark), developed and validated analytical procedures by ICP-MS, ICP-OES, MWP-AES, WD-XRF, and ID-MS for the determination of inorganic
impurities in solid and liquid biofuels, established the budget of uncertainties, and developed the method for determining the amount of ash in the measurement range 0–1.2% with absolute repeatability less than 0.1% and absolute reproducibility of 0.2% (according to EN ISO 18122). In order to create homogeneous certified reference materials, improved methodologies for the measurement and characterization of solid and liquid biofuels were developed. Thus, information regarding the precision, accuracy, and bias of the method, and identifying the factors that intervened in the measurement of uncertainty were experimentally determined, supplementing the information from the existing standards in the field.
Excessive discharge of quaternary ammoniumdisinfectants such as benzalkonium chloride (BAC) into aquatic systems can trigger several physiological responses in environmental microorganisms. In this study, we isolated a less-susceptible strain of Aeromonas hydrophila to BAC, designated as INISA09, froma wastewater treatment plant in Costa Rica. We characterized its phenotypic response upon exposure to three dierent concentrations of BAC and characterizedmechanisms related to its resistance using genomic and proteomic approaches. The genome of the strain, mapped against 52 dierent sequenced A. hydrophila strains, consists of approximately 4.6Mb with 4,273 genes. We found a massive genome rearrangement and thousands of missense mutations compared to the reference strain A. hydrophila ATCC 7966.
We identified 15,762 missense mutations mainly associated with transport, antimicrobial resistance, and outer membrane proteins.
In addition, a quantitative proteomic analysis revealed a significant upregulation of several efflux pumps and the downregulation of porins when the strain was exposed to three BAC concentrations.Other genes related tomembrane fatty acid metabolism and redox metabolic reactions also showed an altered expression.
Our findings indicate that the response of A. hydrophila INISA09 to BAC primarily occurs at the envelop level, which is the primary target of BAC. Our study elucidates the mechanisms of antimicrobial susceptibility in aquatic environments against a widely used disinfectant and will help better understand howbacteria can adapt to biocide pollution. To our knowledge, this is the first study addressing the resistance to BAC in an environmental A. hydrophila isolate. We propose that this bacterial species could also serve as a new model to study antimicrobial pollution in aquatic environments.
Safety characteristics are used to keep processes, including flammable gases, vapors, and combustible dusts, safe. In the standards for the determination of safety characteristics of gases and vapors, the induction spark is commonly used. However, classic transformers are hard to obtain, and replacement with new electronic transformers is not explicitly allowed in the standards. This article presents the investigation of five gases that are normally used to calibrate devices for the determination of safety characteristics, the maximum experimental safe gap (MESG), with an electronic transformer, and the values are compared to the ones that are obtained with the standard transformer. Additionally, calorimetric measurements on the net energy of both ignition sources were performed as well as open-circuit voltage measurements. It is concluded that the classic type of transformer can be replaced by the new type obtaining the same results for the MESG and introducing the same amount of energy into the system.
This article refers to the research article entitled “Creep-Fatigue of P92 in Service-Like Tests with Combined Stress- and Strain-Controlled Dwell Times” [1]. It presents experimental mechanical data from complex service-like creep-fatigue experiments performed isothermally at 620 °C and a low strain amplitude of 0.2 % on tempered martensite-ferritic grade P92 steel. The data sets in text file format provide cyclic deformation (min. and max. stresses) and the total (hysteresis) data of all recorded fatigue cycles for three different creep-fatigue experiments: 1) a standard relaxation fatigue (RF) test with symmetrical dwell times of three minutes introduced at minimum and maximum strain, 2) a fully strain-controlled service-like relaxation (SLR) test combining these three-minute peak strain dwells with a 30-minute dwell in between at zero strain, and 3) a partly stress-controlled service-like creep (SLC) test combining the three-minute peak strain dwells with 30-minute dwells at constant stress. Such service-like (SL) tests with additional long-term stress- and strain-controlled dwell times are non-standard, rare, and expensive, making these data very valuable. They may be used to approximate cyclic softening in the technically relevant range, for the design of complex SL experiments, or for detailed analyses of stress-strain hystereses (e.g., for stress or strain partitioning methods, for the determination of hysteresis energies (work), inelastic strain components, etc.). In addition, the latter analyses may supply important input for advanced parametric lifetime modeling of components under creep-fatigue loading or model calibration parameters.
Advanced experimental and numerical approaches are being developed to
capture the localization of plasticity at the nanometer scale as a function of the multiscale and heterogeneous microstructure present in metallic materials.
These innovative approaches promise new avenues to understand microstructural effects on mechanical properties, accelerate alloy design, and enable more accurate mechanical property prediction. This article provides an overview of emerging approaches with a focus on the localization of plasticity by crystallographic slip. New insights into the mechanisms and mechanics of strain localization are addressed. The consequences of the localization of plasticity by deformation slip for mechanical properties of metallic materials are also detailed.
Copolymer thin films with two types of functional groups have excellent performance as sensors, for example. The formation and deposition of allyl alcohol‐acrylic acid copolymer films by pulsed high frequency plasma is a complex process. As usual, the chemical composition of the top surface of the films was investigated by XPS and FTIR measurements. Furthermore, contact angle measurements with water were used to characterise the hydrophilicity and wettability of the polymer films.
After plasma deposition, a significant decrease in functional groups (OH and COOH) was observed compared to the classically copolymerised equivalent.
The remaining functional groups, i.e. the majority of these groups, were sufficient for application as sensor layers. Segmental mobility and conductivity, important for sensor applications, were analysed by broadband dielectric spectroscopy.
Ring-opening polymerizations of l-lactide are studied in bulk at 140 or 160 °C with zinc n-hexanoate, zinc 4-chlorothiophenolate, and zinc pentafluoro thiophenolate (ZnSPF) as catalysts. The reactivity increases in the given order.
With all three catalysts a high fraction of cycles is obtained only at polymerization (annealing) times around 7 d. With ZnSPF weight average molecular weights (Mw) up to 178 000, a Tm around 199 °C and a 𝚫Hm around 99 J g−1 were achieved. The samples annealed for 4 or 7 d also display a saw tooth pattern of the mass peak distribution in the matrix-assisted laser desorption/ionization time of flight spectra indicating transesterification reactions across the surface of extended ring crystals. This process optimizes the thermodynamical properties of the crystalline cyclic polylactides and is responsible for the high Tm and 𝚫Hm values.
The huge atomic heterogeneity of high-entropy materials along with a possibility to unravel the behavior of individual components at the atomic scale suggests a great promise in designing new compositionally complex systems with the desired multi-functionality. Herein, we apply multi-edge X-ray absorption spectroscopy (extended X-ray absorption fine structure (EXAFS), X-ray absorption near edge structure (XANES), and X-ray magnetic circular dichroism (XMCD)) to probe the structural, electronic, and magnetic properties of all individual constituents in the single-phase face-centered cubic (fcc)-structured nanocrystalline thin film of Cr20Mn26Fe18Co19Ni17 (at.%) high-entropy alloy on the local scale. The local crystallographic ordering and component-dependent lattice displacements were explored within the reverse Monte Carlo approach applied to EXAFS spectra collected at the K absorption edges of several constituents at room temperature. A homogeneous short-range fcc atomic environment around the absorbers of each type with very similar statistically averaged interatomic distances (2.54–2.55 Å) to their nearest-neighbors and enlarged structural relaxations of Cr atoms were revealed. XANES and XMCD spectra collected at the L2,3 absorption edges of all principal components at low temperature from the oxidized and in situ cleaned surfaces were used to probe the oxidation states, the changes in the electronic structure, and magnetic behavior of all constituents at the surface and in the sub-surface volume of the film. The spin and orbital magnetic moments of Fe, Co, and Ni components were quantitatively evaluated. The presence of magnetic phase transitions and the co-existence of different magnetic phases were uncovered by conventional magnetometry in a broad temperature range.
Mesoporous glasses are a promising class of bioresorbable biomaterials characterized by high surface area and extended porosity in the range of 2 to 50 nm. These peculiar properties make them ideal materials for the controlled release of therapeutic ions and molecules. Whilst mesoporous silicate-based glasses (MSG) have been widely investigated, much less work has been done on mesoporous phosphate-based glasses (MPG). In the present study, MPG in the P2O5–CaO–Na2O system, undoped and doped with 1, 3, and 5 mol% of Cu ions were synthesized via a combination of the sol–gel method and supramolecular templating. The non-ionic triblock copolymer Pluronic P123 was used as a templating agent. The porous structure was studied via a combination of Scanning Electron Microscopy (SEM), Small-Angle X-ray Scattering (SAXS), and N2 adsorption–desorption analysis at 77 K. The structure of the phosphate network was investigated via solid state 31P Magic Angle Spinning Nuclear Magnetic Resonance (31P MAS-NMR) and Fourier Transform Infrared (FTIR) spectroscopy. Degradation studies, performed in water via Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES), showed that phosphates, Ca2+, Na+ and Cu ions are released in a controlled manner over a 7 days period. The controlled release of Cu, proportional to the copper loading, imbues antibacterial properties to MPG. A significant statistical reduction of Staphylococcus aureus (S. aureus) and Escherichia coli (E. coli) bacterial viability was observed over a 3 days period. E. coli appeared to be more resistant than S. aureus to the antibacterial effect of copper. This study shows that copper doped MPG have great potential as bioresorbable materials for controlled delivery of antibacterial ions.
In this work, we report on our progress for investigating a new experimental approach for thermographic detection of internal defects by performing 2D photothermal super resolution reconstruction. We use modern high-power laser projector technology to repeatedly excite the sample surface photothermally with varying spatially structured 2D pixel patterns. In the subsequent (blind) numerical reconstruction, multiple measurements are combined by exploiting the joint-sparse nature of the defects within the specimen using nonlinear convex optimization methods. As a result, a 2D-sparse defect/inhomogeneity map can be obtained. Using such spatially structured heating combined with compressed sensing and computational imaging methods allows to significantly reduce the experimental complexity and to study larger test surfaces as compared to the one-dimensional approach reported earlier.
Crystalline porous materials are recognized as promising proton conductors for the proton exchange membrane (PEM) in fuel cell technology owing to their tunable framework structure. However, it is still a challenging bulk synthesis for real-world applications of these materials. Herein, we report the mechanochemical gram-scale synthesis of two isostructural metal hydrogen-bonded organic frameworks (MHOFs) of Co(II) and Ni(II) based on 1-hydroxyethylidenediphosphonic acid (HEDPH4) with 2,2′-bipyridine (2,2′-bipy): Co(HEDPH3)2(2,2′-bipy)·H2O (1) and Ni(HEDPH3)2(2,2′-bipy)·H2O (2). In situ monitoring of the mechanochemical synthesis using different synchrotron-based techniques revealed a one-step mechanism – the starting materials are directly converted to the product. With the existence of extensive hydrogen bonds with amphiprotic uncoordinated phosphonate hydroxyl and oxygen atoms, both frameworks exhibited proton conduction in the range of 10–4 S cm–1 at room temperature under humid conditions. This study demonstrates the potential of green mechanosynthesis for bulk material preparation of framework-based solid-state proton conductors.
Mechanically flexible single crystals of molecular materials offer potential for a multitude of new directions in advanced materials design. Before the full potential of such materials can be exploited, insight into their mechanisms of action must be better understood. Such insight can be only obtained through synergistic use of advanced experimentation and simulation. We herein report the first detailed mechanistic study of elasto-plastic flexibility in a molecular solid. An atomistic origin for this mechanical behaviour is proposed through a combination of atomic force microscopy, μ-focus synchrotron X-ray diffraction, Raman spectroscopy, ab initio simulation, and computed elastic tensors. Our findings suggest that elastic and plastic bending are intimately linked and result from extensions of the same molecular deformations. The proposed mechanism bridges the gap between contested mechanisms, suggesting its applicability as a general mechanism for elastic and plastic bending in organic molecular crystals.
Motivation: Inferring taxonomy in mass spectrometry-based shotgun proteomics is a complex task. In multi-species or viral samples of unknown taxonomic origin, the presence of proteins and corresponding taxa must be inferred from a list of identified peptides, which is often complicated by protein homology: many proteins do not only share peptides within a taxon but also between taxa. However, the correct taxonomic inference is crucial when identifying different viral strains with high-sequence homology—considering, e.g., the different epidemiological characteristics of the various strains of severe acute respiratory syndrome-related coronavirus-2. Additionally, many viruses mutate frequently, further complicating the correct identification of viral proteomic samples.
Results: We present PepGM, a probabilistic graphical model for the taxonomic assignment of virus proteomic samples with strain-level resolution and associated confidence scores. PepGM combines the results of a standard proteomic database search algorithm with belief propagation to calculate the marginal distributions, and thus confidence scores, for potential taxonomic assignments. We demonstrate the performance of PepGM using several publicly available virus proteomic datasets, showing its strain-level resolution performance. In two out of eight cases, the taxonomic assignments were only correct on the species level, which PepGM clearly indicates by lower confidence scores.
Availability and implementation: PepGM is written in Python and embedded into a Snakemake workflow. It is available at https://github.com/BAMeScience/PepGM.
In this article the progress of the research on cement hydration mechanisms is critically reviewed, starting with the work of Le Chatelier and Michaelis during the late 19th century. Proposed mechanisms are discussed in the light of experimental data to highlight the role of new or improved analytical techniques. The focus of this article lies on the dormant period and the silicate reaction.
Today many of the mechanisms proposed throughout time cannot withstand experimental evidence and need to be rejected, including the classical protective hydrate layer theory. However, it seems likely that hydrated surface species are involved in the mechanism. Theories that aim to explain the rate changes solely based on the nucleation and growth of portlandite can also not withstand experimental evidence. Nevertheless, the retardation of portlandite crystal growth through silicate ions is a relevant factor. Especially since it might present a mechanism for the nucleation of calcium silicate hydrate (C-S-H), backing up theories that propose C-S-H and portlandite to grow from the same nuclei.
Finally, an overview over facts, that are currently considered to be valid and hence need to be regarded in future mechanisms is given.
A combination of TLC-bioautography, MALDI-TOF-MS and LC–MS/MS methods was used to identify flavonoids with anti-α-amylase activity in extracts of Lathyrus pratensis L. (herb), L. polyphillus L. (fruits), Thermopsis lanceolata R. Br. (herb) and S. japonica L. (buds). After the TLC-autobiography assay, substances with anti-amylase activity were identified by MALDI-TOF-MS followed by confirmation of the result by LC–MS/MS. Results of the study revealed that the flavonoids apigenin, luteolin, formononetin, genistein and kaempferol display marked anti-α-amylase activity. Formononetin showed the largest activity. Compared with LC–MS/MS, MALDI-TOF-MS is a quick and convenient method; results can be obtained within minutes; and only minor sample amounts are required which allows us to analyse mixtures of substances without preliminary separation. However, the inability to distinguish between isomers is the main limitation of the method.
The osseointegration in/around additively manufactured (AM) lattice structures of a new titanium alloy, Ti–19Nb–14Zr, was evaluated. Different lattices with increasingly high sidewalls gradually closing them were manufactured and implanted in sheep. After removal, the bone–interface implant (BII) and bone–implant contact (BIC) were studied from 3D X-ray computed tomography images. Measured BII of less than 10 µm and BIC of 95% are evidence of excellent osseointegration.
Since AMnaturally leads to a high-roughness surface finish, the wettability of the implant is increased.
The new alloy possesses an increased affinity to the bone. The lattice provides crevices in which the biological tissue can jump in and cling. The combination of these factors is pushing ossification beyond its natural limits. Therefore, the quality and speed of the ossification and osseointegration in/around these Ti–19Nb–14Zr laterally closed lattice implants open the possibility of bone spline key of prostheses. This enables the stabilization of the implant into the bone while keeping the possibility of punctual hooks allowing the implant to be removed more easily if required. Thus, this new titanium alloy and such laterally closed lattice structures are appropriate candidates to be implemented in a new generation of implants.
For dangerous goods packagings, drop testing onto an essential unyielding target can be used to assess the mechanical resistance to impact loads. Adopted regulations like ADR/RID require that the impact surface provided shall be integral with a mass at least 50 times than that of the heaviest package to be tested. The problem is that many manufacturers do not possess impact targets that satisfy the required 50 times mass ratio for regulative drop tests during series production. The objective of this work is to verify existing and define improved criteria for impact target structures based on systematic investigations. Previous evidence highlights the relevance of other parameters in addition to the mass ratio. Therefore, in this research, a variation of drop test parameters was carried out experimentally. Furthermore, numerical vibration analysis was applied to investigate the deformability of the impact surface. The results conclude that the mass ratio of 1:50 cannot be defined as a decisive criterion. In order to determine the influence of further drop test parameters, the research findings were used to validate a parametric model which assesses impact target deflection. An approximation quality of over 90 % was achieved. As a result, new evaluation criteria are proposed. Firstly, a method for identifying critical impact target designs is provided. Secondly, a new comprehensive formula compares the approximated maximum deflection of a real impact target to the respective theoretical threshold derived from a worst-case assumption. In practice, this leads to great advantages in the evaluation of already installed impact targets for dangerous goods packagings.
Comparative study of the co-assembly behaviour of 3-chloro-4-hydroxy-phenylazo dyes with DTAB
(2023)
The co-assembly of three one-fold negatively charged 3-chloro-4-hydroxy-phenylazo dyes (Yellow, Blue and Red) with the cationic surfactant dodecyltrimethylammoniumbromide (DTAB) was studied to probe dye–DTAB binding stoichiometry and assembly morphology. For each dye, phase separation was observed above a given dye : DTAB ratio with the ratio depending on the dye. While Yellow and DTAB showed liquid/liquid phase separation above Yellow : DTAB = 1 : 1.67, crystalline dye–DTAB complexes were observed for Blue–DTAB and Red–DTAB above Blue : DTAB = 1 : 2.56 and Red : DTAB = 1 : 2.94 respecively. In homogeneous solution, UV/vis spectroscopic investigations suggest stochiometries of Yellow : DTAB = 1 : 2, Blue : DTAB = 1 : 3 and Red : DTAB = 1 : 4. It was concluded, that Yellow exhibits the highest dye : DTAB binding stoichiometry in both, dye–surfactant complexes in the 2-phase region and in solution, whereas the lowest dye : DTAB binding stoichiometry was observed for Red–DTAB in both cases. The observed stoichiometries are inversely correlated to the impact dye addition has on the morphology of DTAB micelles. Generally, addition of dye to DTAB micelles leads to a reduction in spontaneous curvature of these micelles and to the formation of triaxial ellipsoidal or cylindrical micelles from oblate ellipsoidal DTAB micelles. At a DTAB concentration of 30 mM and a dye concentration of 5 mM, this effect was most pronounced for Red and least pronounced for Yellow, whilst Blue showed an intermediate effect.
The prediction of the properties of the materials used in the operation of components is of enormous importance, in order to accelerate the development process of new components. To evaluate new materials in terms of their performance (in a component), the development of new innovative methods is necessary. These methods can also be summarized under the term lab-to-field or materials – upscaling, meaning materials being characterised in a laboratory and their properties being upscaled to the component performance by means of e.g. simulation. i-TRIBOMAT is a EU funded project (H2020, GA Nr. 814494) aiming at building an Open Innovation Test Bed for tribological material characterization and offering corresponding services from tribological characterization of new materials to simulation models for predicting the performance of industrial components. By bundling the infrastructure, know-how for characterization and building a digital platform, i-TRIBOMAT becomes the world’s largest open innovation test bed for tribological material characterization.
A technique for calculating the main solidification parameters for a two-dimensional columnar crystal growth during complete penetration laser beam welding of thin steel sheets was developed. Given that the weld pool interface is described by Lamé curves (superellipses) within the horizontal plane of growth, general analytical solutions were derived for the geometry of the crystal axis and the corresponding growth rate and cross-sectional area of the crystal. A dimensionless analysis was performed to provide insights on the dependence of the solidification parameters on the shape and dimensions of the rear part of the weld pool boundary. The derived solutions were applied for the case of complete penetration laser beam keyhole welding of 2 mm thick 316L austenitic chromium-nickel steel sheets. It was shown that the reconstruction of the weld pool boundary with Lamé curves provides higher accuracy and flexibility compared to results obtained with elliptical functions. The validity of the proposed technique and the derived analytical solutions was backed up by a comparison of the obtained solutions to known analytical solutions and experimentally determined shapes and sizes of the crystals on the top surface of the sheet. The dimensions of the calculated crystal axis correlated well with the experimentally obtained results.
This paper reports the results of an international interlaboratory study sponsored by the Versailles Project on Advanced Materials and Standards (VAMAS) and led by the National Institute of Standards and Technology (NIST) on the measurement of water vapor sorption isotherms at 25 °C on a pelletized nanoporous carbon (BAM-P109, a certified reference material). Thirteen laboratories participated in the study and contributed nine pure water vapor isotherms and four relative humidity isotherms, using nitrogen as the carrier gas. From these data, reference isotherms, along with the 95% uncertainty interval (Uk=2), were determined and are reported in a tabular format.
The flow properties of powdery or granular filling substances for dangerous goods packagings are safety-relevant parameters. To specify the flow behavior, the angle of repose is measured in the recognized test centers for dangerous goods packagings in Germany. Previous investigations performed on non-hazardous substances revealed that some of the methods currently used have disadvantages in application. Additionally, for occupational health and safety reasons, it was generally viewed critically to carry out measurements of the angle of repose for dangerous goods at all. Instead, the dimensionless Hausner ratio to describe the flow behavior was proposed.
In this work, the investigations were extended to real hazardous substances to concretize the assessment. Five exemplary hazardous substances were tested for their angle of repose using the methods commonly applied in the test centers. The Hausner ratio was also determined. In addition, the influence of a different climatic preconditioning on the angle of repose measurement was examined using three selected non-hazardous bulk materials.
The results show that the measurement of the angle of repose is not fundamentally excluded for dangerous goods. However, for reasons of applicability, repeatability and occupational health and safety, only the ISO method can be applied for dangerous filling substances. This method provides conservative results regarding a safety-related evaluation of flow properties for the transport of dangerous goods.
In principle, both the ISO method and the determination of the Hausner ratio can be used for dangerous goods. It is also essential especially with finely powdered filling goods, to carry out controlled preconditioning.
Composition and Explosibility of Gas Emissions from Lithium-Ion Batteries Undergoing Thermal Runaway
(2023)
Lithium-based batteries have the potential to undergo thermal runaway (TR), during which mixtures of gases are released. The purpose of this study was to assess the explosibility of the gaseous emission from LIBs of an NMC-based cathode during thermal runaway. In the current project, a series of pouch lithium-based battery cells was exposed to abuse conditions (thermal) to study the total amount of gases released and the composition of the gas mixture. First, the battery cells were placed in a closed vessel, and the pressure and temperature rise inside the vessel were measured. In a second step, the composition of gases was analysed using a Fourier transform Infrared (FTIR) spectrometer.
We found that the amount of released gases was up to 102 ± 4 L, with a clear dependence on the battery capacity. This study showed that the concentration of gaseous emissions such as carbon monoxide (CO), methane (CH4), ethylene (C2H4), ethane (C2H6), and hydrogen cyanide (HCN) increased with higher cell capacity. Of the five studied flammable gases, the maximum concentrations of carbon monoxide (16.85 vol%), methane (7.6 vol%), and ethylene (7.86 vol%) were identified to be within their explosible range. Applying Le Chatelier’s law, a calculated lower explosion limit (LEL) of 7% in volume fraction was obtained for the gas mixture. The upper explosion limit (UEL) of the gas mixture was also found to be 31% in volume. A filter comprising pyrobubbles was used for the removal of the studied gas components released during the thermal abuse. The investigation revealed that the pyrobubbles filter was highly effect in the removal of HCN (up to 94% removal) and CO2 (up to 100% removal). Herein, we report the dependency of the method of thermal runaway trigger on the measured maximum temperature.
Asymmetrical Flow Field-Flow Fractionation (AF4), as a cleaning technique, was combined on-line with the multielemental analytical capabilities of an Inductively Coupled Plasma-Time of Flight-Mass Spectrometer (ICP-ToF-MS). In that manner, the heavy ionic matrix effect of untreated cells' samples can be significantly reduced. As a proof of concept, commercial baker's yeast cells were analysed.
Elemental composition and thickness determination of thin films by electron probe microanalysis
(2023)
Electron probe microanalysis (EPMA) applies to solid samples of homogenous (bulk) chemical composition and can usually not be applied to structures which are inhomogeneous in the micrometer range such as thin film systems down to a few nm. However, in combination with the established thin film software Stratagem, the thickness as well as the elemental composition of thin films on a substrate can be determined. This has been recently successfully demonstrated for Fe-Ni on Si and Si-Ge on Al2O3 thin film systems. For both systems five samples of different elemental composition and a reference were produced and characterised by inductively coupled plasma mass spectrometry (ICP-MS), Rutherford backscattering (RBS), and transmission electron microscopy (TEM) as reference values. Last year, a new and open-source thin film evaluation programme called BadgerFilm has been released. It can also be used to determine thin film composition and thickness from intensity ratios of the unknown sample and standards (k-ratios). In this contribution, we reevaluated the data acquired for the Fe-Ni and Si-Ge systems using the BadgerFilm software package and compared the obtained elemental compositions and thickness values with the results of the Stratagem software and the reference methods. The conclusion is that the BadgerFilm software shows good agreement with the elemental composition and thickness calculated by Stratagem (mostly <2% for both composition and thickness) and with the reference values for two representative thin film systems (<1%–2% for composition and <10%–20% for thickness).
We investigated the performance of nitrogen microwave inductively coupled atmospheric-pressure plasma mass spectrometry (MICAP-MS) under matrix effects and its applicability to trace element analysis in steels. Influences of different gas flows and ion optics on the matrix tolerance are studied, indicating that nebulizer gas flow has the most significant impact. Optimization of ion optics improves matrix tolerance for light elements due to the reduction of the inelastic collisional scattering effect. With optimized operating conditions, MICAP-MS achieves an internal standard intensity recovery of over 90% at an Fe concentration of 500 mg L−1. Even at an Fe concentration of 1 g L−1, the recovery remains above 80%. Three certified reference materials – non-alloy, low-alloy and high-alloy steel – were analyzed using MICAP-MS. The determined mass concentrations of the trace and minor components show metrological compatibility to the reference values. No significant differences are observed between the results obtained with aqueous and matrix-matched calibration, demonstrating the strong matrix tolerance of MICAP-MS, and its promising applicability to steel analysis.
Half of global material consumption involves mineral material. The circularity is still low so that the enhanced use of secondary building material is required to close loops. Three different secondary building materials are discussed based on exemplary research results: construction and demolition waste (C&D waste), soil-like material, and incineration bottom ash (IBA). Focus was placed on the environmental compatibility of the materials examined mainly by standardized leaching tests. C&D waste was investigated after a wet treatment using a jigging machine, and soil-like material and IBA were characterized with respect to their material composition. Their environmental compatibilities in particular were studied using standard leaching tests (batch tests and column tests).
It was concluded that soil-like material can mostly be utilized even when the precautionary limit values set are exceeded by a factor of less than two. For C&D waste, the fine fraction below 2 mm and the content of brick material is problematic. IBA fulfills quality level “HMVA-2” following German regulations. Improved levels of utilization might be achievable with better treatment technologies.
Cardiac troponin I (cTnI) is a crucial biomarker for diagnosing cardiac vascular diseases, including acute myocardial infarction (AMI). This study presents a proof-of-concept chemiluminescence-based immunosensor for rapid and accurate measurement of cTnI, with the potential for online monitoring. The immunosensor incorporates a flow cell design and a sensitive complementary metal-oxide-semiconductor (CMOS) camera for optical readout. A microfluidic setup was established to enable selective and quasi-online determination of cTnI within ten minutes. The sensor was tested with recombinant cTnI in phosphate buffer, demonstrating measurements in the concentration range of 2–25 µg/L, with a limit of detection (LoD) of 0.6 µg/L (23 pmol/L) achieved using the optimized system. The immunosensor exhibited high selectivity, as no cross-reactivity was observed with other recombinant proteins such as cTnT and cTnC at a concentration of 16 µg/L. Measurements with diluted blood plasma and serum yielded an LoD of 60 µg/L (2.4 nmol/L) and 70 µg/L (2.9 nmol/L), respectively. This biosensor offers a promising approach for the rapid and sensitive detection of cTnI, contributing to the diagnosis and management of acute myocardial infarction and other cardiac vascular diseases.
In Leichtbauanwendungen sind Materialien mit geringen Dichten und hohen Festigkeiten gefragt. Insbesondere Faser-Kunststoff-Verbunde (FKV) erfüllen diese Anforderungen und werden zunehmend für Strukturbauteile eingesetzt. Die Oberflächen moderner Rotorblätter von Windkraftanlagen werden aus FKV gefertigt. Das Versagen dieser Materialien hat massiven Einfluss auf die Einsatzfähigkeit der gesamten Windkraftanlage. Daher ist die Kenntnis des Versagensverhaltens dieser Komponenten unter statischer und zyklischer Belastung von großem Interesse, um die Betriebsbeanspruchung abzuschätzen. Im Idealfall wird die Schadensentwicklung unter Betriebslast mit zerstörungsfreien in-situ-Prüfverfahren ermittelt. Hier berichten wir über die Beobachtung der Rissentwicklung in Carbon-Faserverstärkten Kunststoffen (CFK) unter kontinuierlicher Zugbelastung durch in-situ Synchrotron-Röntgenrefraktionsradiographie. Eine selbst entwickelte elektromechanische Zugprüfmaschine mit einem Kraftbereich bis zu 15 kN wurde in den Strahlengang an der BAMline (BESSY II) integriert. Da in herkömmlichen (Absorptions-) Radiographien Defekte wie Zwischenfaserbrüche oder Faser-Matrix-Enthaftung keinen ausreichenden Kontrast verursachen, wird zur Kontrastanhebung die Röntgenrefraktion benutzt. Hier wird das sogenannte Diffraction Enhanced Imaging (DEI) angewandt, um Primär- und gebrochene Strahlung mit Hilfe eines Analysatorkristalls zu trennen. Diese Technik ermöglicht schnelle Messungen mit einem Gesichtsfeld von einigen Quadratmillimetern (hier: 14 mm × 7.2 mm) und ist ideal für in-situ Untersuchungen. Die Bildgebung und der Zugversuch erfolgen mit einer Bildfrequenz von 0.7 / s und einer Dehnrate von 0.00055 / s . Bei 0°/90° Fasergelegen treten die ersten Zwischenfaserrisse bei 380 MPa (Dehnung 0.8 %) auf. Vor dem Versagen bei ca. 760 MPa (Dehnung 2.0 %) beobachten wir die Ausbildung eines nahezu äquidistanten Rissmusters (Risse in ca. 1 mm Abstand), das sich im geschädigten Zustand über die gesamte Probe erstreckt.
Die Brechung von Röntgenstrahlen (Röntgenrefraktion) an Grenzflächen zwischen Materialien unterschiedlicher Dichte ist analog zur Ablenk-ung von sichtbarem Licht an z.B. Glasoberflächen. Es gibt jedoch zwei wesentliche Unterschiede:
a) konvexe Grenzflächen verursachen Divergenz (d.h. der Brechungsindex n ist kleiner als 1), und
b) die Ablenkungswinkel sind sehr klein, und reichen von einigen Bogensekunden bis zu einigen Bogenminuten (d.h. n ist nahe bei 1);
Wie auch bei sichtbarem Licht ist die Ablenkungsrichtung der Röntgenstrahlen abhängig von der Orientierung der durchstrahlten Grenzfläche. Aufgrund dieser Eigenschaften eignen sich Röntgenrefraktionsmethoden hervorragend für:
a) die Erkennung und Quantifizierung von Defekten wie Poren und Mikrorissen und
b) die Bewertung von Porosität und Partikeleigenschaften wie Orientierung, Größe und räumliche Verteilung.
Wir zeigen die Anwendung der Röntgenrefraktionsradiographie (2,5D Technik) und der -tomographie (3D Technik) für die Untersuchung verschiedener Probleme in der Werkstoffwissenschaft und -technologie:
a) Sintern von SiC-Grünkörpern
b) Porositätsanalyse in Dieselpartikelfiltersilikaten
c) Faser-Matrix-Haftung in Metall- und Polymermatrixverbundwerkstoffen
d) Mikrorissbildung in Glaskeramik.
Wir zeigen, dass der Einsatz von Röntgenrefraktionsmethoden quantitative Ergebnisse liefert, die direkt als Parameter in Werkstoffmodellen verwendet werden können.
For the first time, µ-X-ray fluorescence (µ-XRF) mapping combined with fluorine K-edge µ-X-ray absorption near-edge structure (µ-XANES) spectroscopy was applied to depict per- and polyfluoroalkyl substances (PFAS) contamination and inorganic fluoride in samples concentrations down to 100 µg/kg fluoride. To demonstrate the matrix tolerance of the method, several PFAS contaminated soil and sludge samples as well as selected consumer product samples (textiles, food contact paper and permanent baking sheet) were investigated. µ-XRF mapping allows for a unique element-specific visualisation at the sample surface and enables localisation of fluorine containing compounds to a depth of 1 µm. Manually selected fluorine rich spots were subsequently analysed via fluorine K-edge µ-XANES spectroscopy. To support spectral interpretation with respect to inorganic and organic chemical distribution and compound class determination, linear combination (LC) fitting was applied to all recorded µ-XANES spectra. Complementarily, solvent extracts of all samples were target-analysed via LC-MS/MS spectrometry. The detected PFAS sum values range from 20 to 1136 µg/kg dry weight (dw). All environmentally exposed samples revealed higher concentration of PFAS with a chain length >C8 (e.g. 580 µg/kg dw PFOS for Soil1), whereas the consumer product samples showed a more uniform distribution with regard to chain lengths from C4 to C8. Independent from quantified PFAS amounts via target analysis, µ-XRF mapping combined with µ-XANES spectroscopy was successfully applied to detect both point-specific concentration maxima and evenly distributed surface coatings of fluorinated organic contaminants in the corresponding samples.