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Paper des Monats
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The entire process involving the determination of Cl by molecular emission detection in Laser-Induced Breakdown Spectroscopy (LIBS) is thoroughly studied in this paper. This critical evaluation considers how spectra are normalized, how interferences from other molecular species signals are removed, and how signal integration is applied. Moreover, a data treatment protocol is proposed to achieve reliable and accurate Cl determination from the CaCl molecular spectral signal, not requiring the use of more complex numerical approaches. Calcium chloride dihydrate (CaCl2⋅2H2O) and high purity anhydrite samples (CaSO4) are used to optimize the acquisition conditions and data treatment of CaCl emission signal. Using the developed protocol, calibration curves for Cl, covering the concentration range from 0 μg/g to 60,000 μg/g of Cl, are successfully achieved. Finally, the suitability of the proposed methodology for Cl determination is successfully applied in industrial gypsum waste samples, where the results obtained by LIBS are validated using high-resolution molecular absorption spectroscopy (HR-CS-MAS) and potentiometric titration.
A series of NaYF4:Yb3+/Tm3+@NaYF4:Yb3+/Er3+ nanoparticles doped with Tm3+ and Er3+ were successfully prepared by the solvothermal method. Under 980 nm laser excitation, intense upconversion emission peaks of Tm3+ and Er3+ were observed for all samples. By doping Tm3+ and Er3+ with core–shell partitioning, not only a significant increase in fluorescence intensity could be achieved, but also simultaneous temperature measurements on multiple thermocouple energy levels could be realised. In addition, the temperature sensing performance of different thermocouple energy levels was also investigated, and it was found that the 3 F3 → 3 H6 and 1 G4 → 3 F4 thermocouple energy level pairs of Tm3+ were the best, with maximum absolute sensitivity and maximum relative sensitivity of up to 0.0250 K−1 and 2.155% K−1 respectively, higher than the sensitivity of other thermocouple energy levels. It has a temperature resolution of less than 0.0139 K, which is lower than that of most materials available today. By using this material as a probe to build a fiber optic temperature sensor platform, it was found to have reliable temperature measurement performance.
Additive manufacturing by laser metal deposition (LMD) requires continuous online monitoring to ensure quality of printed parts. Optical emission spectroscopy (OES) is proposed for the online detection of printing defects by monitoring minute variations in the temperature of a printed spot during laser scan. A two-lens optical system is attached to a moving laser head and focused on a molten pool created on a substrate during LMD. The light emitted by the pool is collected by an ultraviolet–visible (UV–vis) spectrometer and processed.
Two metrics are used to monitor variations in the surface temperature: the spectrally integrated emission intensity and correlation coefficient. The variations in the temperature are introduced by artificial defects, shallow grooves, and holes of various widths and diameters carved on a substrate surface. The metrics show sufficient sensitivity for revealing the surface defects, except for the smallest
holes with an under-millimeter diameter. Additionally, numeric simulations are carried out for the detection of emission in the UV–vis and near-infrared (NIR) spectral ranges at various surface temperatures. It is concluded that both the metrics perform better in the NIR range. In general, this work demonstrates that spectrally resolved OES suits well for monitoring surface defects during 3D metal
printing.
Whereas the characterization of nanomaterials using different analytical techniques is often highly automated and standardized, the sample preparation that precedes it causes a bottleneck in nanomaterial analysis as it is performed manually. Usually, this pretreatment depends on the skills and experience of the analysts. Furthermore, adequate reporting of the sample preparation is often missing. In this overview, some solutions for techniques widely used in nano-analytics to overcome this problem are discussed. Two examples of sample preparation optimization by au-tomation are presented, which demonstrate that this approach is leading to increased analytical confidence. Our first example is motivated by the need to exclude human bias and focuses on the development of automation in sample introduction. To this end, a robotic system has been de-veloped, which can prepare stable and homogeneous nanomaterial suspensions amenable to a variety of well-established analytical methods, such as dynamic light scattering (DLS), small-angle X-ray scattering (SAXS), field-flow fractionation (FFF) or single-particle inductively coupled mass spectrometry (sp-ICP-MS). Our second example addresses biological samples, such as cells exposed to nanomaterials, which are still challenging for reliable analysis. An air–liquid interface has been developed for the exposure of biological samples to nanomaterial-containing aerosols. The system exposes transmission electron microscopy (TEM) grids under reproducible conditions, whilst also allowing characterization of aerosol composition with mass spectrometry. Such an approach enables correlative measurements combining biological with physicochemical analysis. These case studies demonstrate that standardization and automation of sample preparation setups, combined with appropriate measurement processes and data reduction are crucial steps towards more reliable and reproducible data.
Colours, nano and surface
(2022)
The basic ideas of colours and pigments are presented. The correlation between nanomaterials and colours are explained. Different methods are presented for investigating nanoparticles and their surface. At the end a case study is presented explaining the importance of coating for the properties of nanoparticles.
Damage detection of reinforced concrete (RC) structures is becoming a more attractive domain due to the safety issues arising in the last few decades. The damage in concrete can be caused by excessive exploitation of the structure or environmental effects. The cracks in concrete can be detected by different nondestructive testing methods. However, the available methods used for this purpose have numerous limitations. The technologies available in the market nowadays have difficulties detecting slowly progressive, locally limited damage. In addition, some of These methods cannot be applied, especially in hard-to-reach areas in the superstructures. In order to avoid these deficiencies, an embedded ultrasonic methodology can be used to detect cracks in RC structures. In this study, the methodology of crack detection supported with the advanced Signal processing algorithm was proposed and verified on RC structures of various types, and cracks occurring between embedded sensors can be detected. Moreover, different pairs of ultrasonic sensors located in the considered structures are used for the analysis of the sensitivity of distance between them. It is shown that the ultrasonic sensors placed in the range of 1.5–2 m can detect cracks, even when the other methods failed to detect changes in the structure. The obtained results confirmed that diffuse ultrasonic sensor methodology is able to monitor real structures more effectively than traditional techniques.
A facile and efficient methodology is described for the solvothermal synthesis of size-tunable, stable, and uniform NiCu core–shell nanoparticles (NPs) for application in catalysis. The diameter of the NPs is tuned in a range from 6 nm to 30 nm and to adjust the Ni:Cu ratio from 30:1 to 1:1. Furthermore, the influence of different reaction parameters on the final NPs is studied. The NPs are structurally characterized by a method combination of transmission electron microscopy, anomalous small-angle X-ray scattering, X-ray absorption fine structure, and X-ray photoelectron spectroscopy. Using these analytical methods, it is possible to elucidate a core–shell–shell structure of all particles and their chemical composition. In all cases, a depletion from the core to the shell is observed, with the core consisting of NiCu alloy, surrounded by an inner Ni-rich shell and an outer NiO shell. The SiO2-supported NiCu core–shell NPs show pronounced selectivity of >99% for CO in the catalytic reduction of CO2 to CO using hydrogen as reactant (reverse water–gas shift reaction) independent of size and Ni:Cu ratio.
Here, we describe an optimized fast and simple extraction method for the determination of per- and polyfluorinated alkyl substances (PFASs) in soils utilizing high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR–CS–GFMAS). To omit the bias of the solid phase extraction (SPE) step commonly used during the analysis of extractable organically bound fluorine (EOF) we optimized a fast and simple SPE-free extraction method. The developed extraction method consists of a liquid-solid extraction using acidified methanol without any additional SPE. Four extraction steps were representative to determine a high proportion of the EOF (>80% of eight extractions). Comparison of the optimized method with and without an additional SPE clean-up step revealed a drastic underestimation of EOF concentrations using SPE. Differences of up to 94% were observed which were not explainable by coextracted inorganic fluoride. Therefore, not only a more accurate but also a more economic as well as ecologic method (bypassing of unnecessary SPE) was developed. The procedural limit of quantification (LOQ) of the developed method was 10.30 μg/kg which was sufficient for quantifying EOF concentrations in all tested samples. For future PFAS monitoring and potential regulative decisions the herein presented optimized extraction method can offer a valuable contribution.
The influence of solvent polarity and surface ligand rigidification on the SWIR emission profile of gold nanoclusters with an anistropic surface was investigated. A strong enhancement of the SWIR emission band at 1200 nm was observed when measuring in different local environments: in solution, in polymer composites, and in solids. SWIR in vivo imaging of mice assisted by deep learning after intravenous administration of these gold nanoclusters provides high definition pseudo-3D views of vascular blood vessels.
Integration of fiber reinforcement in high-performance cementitious materials has become widely applied in many fields of construction. One of the most investigated advantages of steel Fiber reinforced concrete (SFRC) is the deceleration of crack growth and hence its improved sustainability.
Additional benefits are associated with its structural properties, as fibers can significantly increase the ductility and the tensile strength of concrete. In some applications it is even possible to entirely replace the conventional reinforcement, leading to significant logistical and environmental benefits.
Fiber reinforcement can, however, have critical disadvantages and even hinder the Performance of concrete, since it can induce an anisotropic material behavior of the mixture if the fibers are not appropriately oriented. For a safe use of SFRC in the future, reliable non-destructive testing (NDT) methods need to be identified to assess the fibers’ orientation in hardened concrete. In this study,
ultrasonic material testing, electrical impedance testing, and X-ray computed tomography have been investigated for this purpose using specially produced samples with biased or random Fiber orientations. We demonstrate the capabilities of each of these NDT techniques for fiber orientation measurements and draw conclusions based on these results about the most promising areas for future research and development.
n situ monitoring of mechanochemical reactions between dicyandiamide (DCD) and CuX2 salts (X = Cl−, NO3−), for the preparation of compounds of agrochemical interest, showed the appearance of a number of phases. It is demonstrated that milling conditions, such as the amount of water added in wet grinding and/or the milling frequency, may affect the course of the mechanochemical reactions, and drive the reaction towards the formation of different products. It has been possible to discover by in situ monitored experiments two novel crystalline forms, namely the neutral complexes [Cu(DCD)2(OH2)2(NO3)2] (2) and [Cu(DCD)2(OH2)Cl2]·H2O (4), in addition to the previously known molecular salt [Cu(DCD)2(OH2)2][NO3]2·2H2O (1, DIVWAG) and neutral complex [Cu(DCD)2(OH2)Cl2] (3, AQCYCU), for which no synthesis conditions were available. Compounds 2 and 4 were fully characterized via a combination of solid-state techniques, including X-ray diffraction, Raman spectroscopy and TGA.
A brief introduction will be given on modeling chemical reactions in laser induced plasmas using stoichiometric and non-stoichiometric approaches. Several applications will be considered, which can benefit from such modeling. Those include plasma enhanced chemical vapor deposition (PECVD), surface modification and surface coating, and molecular analysis by LIBS. Each application will be illustrated by simulations of relevant chemical systems. For PECVD, chemical systems are BCl3/H2/Ar, BF3/H2/Ar, BCl3/BF3, Mo/BF3/H2; for surface modification/coating it is Ti/air; for molecular LIBS they are CaCO3/Ar, Ca(OH)2/Ar, and CaCl2/Ar. Advantages and shortcomings of equilibrium chemical hydrodynamic models of laser induced plasmas will be discussed.
Imaging Keratan Sulfate in Ocular Tissue Sections by Immunofluorescence Microscopy and LA-ICP-MS
(2022)
Carbohydrate-specific antibodies can serve as valuable tools to monitor alterations in the extracellular matrix resulting from pathologies. Here, the keratan sulfate-specific monoclonal antibody MZ15 was characterized in more detail by immunofluorescence microscopy as well as laser ablation ICP-MS using tissue cryosections and paraffin-embedded samples. Pretreatment with keratanase II prevented staining of samples and therefore demonstrated efficient enzymatic keratan sulfate degradation. Random fluorescent labeling and site-directed introduction of a metal cage into MZ15 were successful and allowed for a highly sensitive detection of the keratan sulfate landscape in the corneal stroma from rats and human tissue.
X-ray photoelectron spectroscopy (XPS) was performed on the meniscus of a droplet of ionic liquid 1-propyl-3-methyl-imidazolium bis(trifluoromethylsulfonyl) imide [PMIM]+[NTf2]− (Solarpur®) in ultrahigh vacuum. High-resolution spectra of F 1s, O 1s, N 1s, C 1s, and S 2p are presented along with a survey spectrum and the valence band structure. The spectra presented here were generated using monochromatic Al Kα radiation (1486.6 eV).
Tire wear (TW) constitutes a significant source of microplastic in terrestrial ecosystems. It is known that particles emitted by roads can have an effect up to 100 m into adjacent areas. Here, we apply for the first-time thermal extraction desorption gas chromatography-mass spectrometry (TED-GC/MS) to determine TW in soil samples by detection of thermal decomposition products of styrene-butadiene rubber (SBR), without additional enrichment. Additionally, zinc contents were determined as an elemental marker for TW. Mixed soil samples were taken along three transects along a German motorway in 0.3, 2.0, and 5.0 m distance from the road. Sampling depths were 0–2, 2–5, 5–10, and 10–20 cm. Four fine fractions, 1 000–500, 500–100, 100–50, and <50 μm, were analyzed.
TW contents based on SBR ranged from 155 to 15 898 mg kg−1. TW contents based on zinc were between 413 and 44 812 mg kg−1. Comparison of individual values of SBR and zinc reveals SBR as a more specific marker. Results confirm that most TW ends up in the topsoil within a 2 m distance.
The sampling strategy resulted in representative data for a larger area. Standard deviations of quadruple TED-GC/MS determination of SBR were <10% for all grain size fractions. TED-GC/MS is a suitable analytical tool for determining TW in soil samples without the use of toxic chemicals, enrichment, or special sample preparation.
Alternative to conventional transmission-based radiography and computed tomography, X-ray refraction techniques are being increasingly used to detect damage in light materials. In fact, their range of application has been recently extended even to metals. The big advantage of X-ray refraction techniques is that they are able to detect nanometric defects, whose size would lie below the resolution of even state-of-the-art synchrotron-based X-ray computed tomography (SXCT). The superiority of synchrotron X-ray refraction radiography and tomography (SXRR and SXRCT) has been shown in the case of light materials, in particular composites. X-ray refraction techniques also yield a quantitifaction of the amount of damage (the so-called relative internal specific surface) and can well be compared with damage models. At the same time, it is impossible for SXRR and SXRCT to image single defects. We show that the combination of refraction- and transmission-based imaging techniques yields an impressive amount of additional information about the type and amount of defects in microstructured materials such as additively manufactured metals or metal matrix composites. We also show that the use of data fusion techniques allows the classification of defects in statistically significant representative volume elements.
Alternative to conventional transmission-based radiography and computed tomography, X-ray refraction techniques are being increasingly used to detect damage in light materials. In fact, their range of application has been recently extended even to metals. The big advantage of X-ray refraction techniques is that they are able to detect nanometric defects, whose size would lie below the resolution of even state-of-the-art synchrotron-based X-ray computed tomography (SXCT). The superiority of synchrotron X-ray refraction radiography and tomography (SXRR and SXRCT) has been shown in the case of light materials, in particular composites. X-ray refraction techniques also yield a quantitifaction of the amount of damage (the so-called relative internal specific surface) and can well be compared with damage models. At the same time, it is impossible for SXRR and SXRCT to image single defects. We show that the combination of refraction- and transmission-based imaging techniques yields an impressive amount of additional information about the type and amount of defects in microstructured materials such as additively manufactured metals or metal matrix composites. We also show that the use of data fusion techniques allows the classification of defects in statistically significant representative volume elements.
We report dielectric and calorimetric studies on metathesis and addition-type polytricyclononenes, both based on the same monomer bearing three pendant OSiMe3 groups. For the addition-type polymer, dielectric spectroscopy reveals a β*-process related to the microporosity, whereas for its metathesis counterpart, the segmental dynamics manifests as an α-process related to a glass transition. Besides active dielectric processes, a significant conductivity contribution is detected for both samples which for the microporous additiontype polymer is three orders of magnitude greater than for the metathesis polymer. The broadband dielectric spectroscopy is complemented by detailed calorimetric investigations, comprising DSC, FSC, and TMDSC. The calorimetric methods detected the glass transition for the metathesis polymer in agreement with the observed dielectric α-process. Furthermore, the already reported gas transport properties for both polymers are compared, setting them in correlation with the observed molecular mobility and conductivity behavior. The discussed results reflect significant differences in molecular mobility of the two polymers affecting the appearance of microporosity which strongly determines the gas transport properties.
Laser induced dielectric breakdown (LIDB) on a surface of solid Mo in H2/BF3 atmosphere at 30-760 Torr and in a gaseous mixture MoF6/H2/BF3 + at 760 Torr pressure is tested for synthesis and deposition of superhard molybdenum borides that are needed in many areas of industry and technology. The emission spectra of the plasma and the dynamics of the gas discharge near the substrate are investigated. A comparative analysis of the gas mixture before and after exposure to LIDB plasma is carried out using IR spectroscopy. The conditions for the formation of molybdenum borides are determined. A thermodynamic analysis of the MoF6/H2/BF3 and Mo/H2/BF3 systems is carried out to determine the temperature range for the formation of molybdenum borides and establish the main chemical reactions responsible for their formation. Deposits containing MoB and MoB2 phases are obtained. For the mixture MoF6/H2/BF3, the deposit exhibits an amorphous layered structure, which contains 19.15 wt% F, 30.45% O, and 0.8% Si. For the Mo/H2/BF3 system at the pressures 30 and 160 Torr, nanopowder of molybdenum boride is produced with a characteristic grain size of 100 nm. At pressures above 160 Torr, Mo nanopowder with a grain size <30 nm is obtained.
While the problem of the identification of mechanisms of hydrogen assisted damage has and is being thoroughly studied, the quantitative analysis of such damage still lacks suitable tools. In fact, while, for instance, electron microscopy yields excellent characterization, the quantitative analysis of damage requires at the same time large field-of-views and high spatial resolution. Synchrotron X-ray refraction techniques do possess both features. In this work, we show how synchrotron X-ray refraction computed tomography (SXRCT) can quantify damage induced by hydrogen embrittlement in a lean duplex steel, yielding results that overperform even those achievable by synchrotron X-ray absorption computed tomography. As already reported in literature, but this time using a non-destructive technique, we show that the hydrogen charge does not penetrate to the center of tensile specimens. By the comparison between virgin and hydrogen-charged specimens, we deduce that cracks in the specimen bulk are due to the rolling process rather than hydrogen-assisted. We show that (micro)cracks propagate from the surface of tensile specimens to the interior with increasing applied strain, and we deduce that a significant crack propagation can only be observed short before rupture.
Surface modification of titanium by laser ablation is investigated theoretically and experimentally. The modification consists in texturing the surface and redeposition of chemically transformed material from the ablation plasma. The redeposition is driven by the hydrodynamic flow in the plasma. Such surface modification improves the biocompatibility of titanium implants.
This course will provide an introduction to plasma diagnostic techniques. The major focus of the course will be on the discussions of the practical procedures as well as the underlying physical principles for the measurements of plasma fundamental characteristics (e.g., temperatures and electron number density). Particular emphasis will be placed on laser induced plasma–atomic emission spectrometry, but other analytical plasmas will also be used as examples when appropriate. Selected examples on how one can manipulate the operating conditions of the plasma source, based on the results of plasma diagnostic measurements, to improve its performance used for spectrochemical analysis will also be covered. Topics to be covered include thermal equilibrium, line profiles, temperatures, electron densities, excitation processes, temporal and spatial resolution.
With the increasing production of renewable energy and concomitant depletion of fossil resources, the demand for efficient water splitting electrocatalysts continues to grow. Iridium (Ir) and iridium oxides (IrOₓ) are currently the most promising candidates for an efficient oxygen evolution reaction (OER) in acidic medium, which remains the bottleneck in water electrolysis. Yet, the extremely high costs for Ir hamper a widespread production of hydrogen (H₂) on an industrial scale. Herein, the authors report a concept for the synthesis of electrode coatings with template-controlled mesoporosity surface-modified with highly active Ir species. The improved utilization of noble metal species relies on the synthesis of soft-templated metal oxide supports and a subsequent shape-conformal deposition of Ir species via atomic layer deposition (ALD) at two different reaction temperatures. The study reveals that a minimum Ir content in the mesoporous titania-based support is mandatory to provide a sufficient electrical bulk conductivity. After ALD, a significantly enhanced OER activity results in dependency of the ALD cycle number and temperature. The most active developed electrocatalyst film achieves an outstanding mass-specific activity of 2622 mA mg(Ir)⁻¹ at 1.60 V(RHE) in a rotating-disc electrode (RDE) setup at 25 °C using 0.5 m H₂SO₄ as a supporting electrolyte.
The roughness as a property of core–shell (CS) microparticles plays a key role in their functionality. Quantitative evaluation of the roughness of CS microparticles is, however, a challenging task with approaches using electron microscopy images being scarce and showing pronounced differences in terms of methodology and results. This work presents a generalized method for the reliable roughness determination of nonplanar specimens such as CS particles from electron microscopic images, the method being robust and reproducible with a high accuracy. It involves a self-written software package (Python) that analyzes the recorded images, extracts corresponding data, and calculates the roughness based on the deviation of the identified contour. Images of single particles are taken by a dual mode scanning electron microscopy (SEM) setup which permits imaging of the same field-of-view of the sample with high resolution and surface sensitive in SE InLens mode as well as in transmission mode (TSEM). Herein, a new type of polystyrene core–iron oxide shell–silica shell particles is developed to serve as a set of lower micrometer-sized study objects with different surface roughness; the analysis of their images by the semiautomatic workflow is demonstrating that the particles’ profile roughness can be quantitatively obtained.
The drug salinomycin (SAL) is a polyether antibiotic and used in veterinary Medicine as coccidiostat and growth promoter. Recently, SAL was suggested as a potential anticancer drug.
However, transformation products (TPs) resulting from metabolic and environmental degradation of SAL are incompletely known and structural information is missing. In this study, we therefore systematically investigated the formation and identification of SAL derived TPs using electrochemistry (EC) in an electrochemical reactor and rat and human liver microsome incubation (RLM and HLM) as TP generating methods. Liquid chromatography (LC) coupled to high-resolution mass spectrometry (HRMS) was applied to determine accurate masses in a suspected target analysis to identify TPs and to deduce occurring modification reactions of derived TPs. A total of 14 new, structurally different TPs were found (two EC-TPs, five RLM-TPs, and 11 HLM-TPs). The main modification reactions are decarbonylation for EC-TPs and oxidation (hydroxylation) for RLM/HLM-TPs. Of particular interest are potassium-based TPs identified after liver microsome incubation because these might have been overlooked or declared as oxidated sodium adducts in previous, non-HRMS-based studies due to the small mass difference between K and O + Na of 21 mDa. The MS fragmentation pattern of TPs was used to predict the position of identified modifications in the SAL molecule. The obtained knowledge regarding transformation reactions and novel TPs of SAL will contribute to elucidate SAL-metabolites with regards to structural prediction.
The integral collection of information such as strains, cracks, or temperatures by ultrasound offers the best prerequisites to monitor structures during their lifetime. In this paper, a novel approach is proposed which uses the collected information in the coda of ultrasonic signals to infer the condition of a structure. This approach is derived from component tests on a reinforced concrete beam subjected to four-point bending in the lab at Ruhr University Bochum. In addition to ultrasonic measurements, strain of the reinforcement is measured with fiber optic sensors. Approached by the methods of moment-curvature relations, the steel strains serve as a reference for velocity changes of the coda waves. In particular, a correlation between the relative velocity change and the average steel strain in the reinforcement is derived that covers 90% of the total bearing capacity. The purely empirical model yields a linear function with a high level of accuracy (R 2 =0.99, R2=0.99, RMSE≈90μ
RMSE≈90μ strain).
The 87Sr/86Sr isotope ratio can, in principle, be used for provenancing of cement. However, while commercial cements consist of multiple components, no detailed investigation into their individual 87Sr/86Sr isotope ratios or their influence on the integral 87Sr/86Sr isotope ratio of the resulting cement was conducted previously. Therefore, the present study aimed at determining and comparing the conventional 87Sr/86Sr isotope ratios of a diverse set of Portland cements and their corresponding Portland clinkers, the major component of these cements. Two approaches to remove the additives from the cements, i.e. to measure the conventional 87Sr/86Sr isotopic fingerprint of the clinker only, were tested, namely, treatment with a potassium hydroxide/sucrose solution and sieving on a 11-µm sieve. Dissolution in concentrated hydrochloric acid/nitric acid and in diluted nitric acid was employed to determine the 87Sr/86Sr isotope ratios of the cements and the individual clinkers. The aim was to find the most appropriate sample preparation procedure for cement provenancing, and the selection was realised by comparing the 87Sr/86Sr isotope ratios of differently treated cements with those of the corresponding clinkers. None of the methods to separate the clinkers from the cements proved to be satisfactory. However, it was found that the 87Sr/86Sr isotope ratios of clinker and cement generally corresponded, meaning that the latter can be used as a proxy for the clinker 87Sr/86Sr isotope ratio. Finally, the concentrated hydrochloric acid/nitric acid dissolution method was found to be the most suitable sample preparation method for the cements; it is thus recommended for 87Sr/86Sr isotope analyses for cement provenancing.
Storage is still limiting the implementation of hydrogen as an energy carrier to integrate the intermittent operation of renewable energy sources. Among different solutions to the currently used compressed or liquified hydrogen systems, physical adsorption at cryogenic temperature in porous materials is an attractive alternative due to its fast and reversible operation and the resulting reduction in storage pressure. The feasibility of cryoadsorption for hydrogen storage depends mainly on the performance of the used materials for the specific application, where metal-organic frameworks or MOFs are remarkable candidates. In this work, gravimetric and volumetric hydrogen uptakes at 77 K and up to 100 bar of commercially available MOFs were measured since these materials are made from relatively cheap and accessible building blocks. These materials also show relatively high porous properties and are currently near to large-scale production. The measuring device was calibrated at different room temperatures to calculate an average correction factor and standard deviation so that the correction deviation is included in the measurement error for better comparability with different measurements. The influence of measurement conditions was also studied, concluding that the available adsorbing area of material and the occupied volume of the sample are the most critical factors for a reproducible measurement, apart from the samples’ preparation before measurement. Finally, the actual volumetric storage density of the used powders was calculated by directly measuring their volume in the analysis cell, comparing that value with the maximum volumetric uptake considering the measured density of crystals. From this selection of commercial MOFs, the materials HKUST-1, PCN-250(Fe), MOF-177, and MOF-5 show true potential to fulfill a volumetric requirement of 40 g·L−1 on a material basis for hydrogen storage systems without further packing of the powders.
The benefits of including fibers in ultra-high performance concrete (UHPC) are attributed to their good bond with the matrix and, hence, an optimal utilization of their properties. At the same time, though, fiber reinforcement may contribute to anisotropy in the composite material and induce weak areas. The influence of the fibers’ orientation on the material properties is a matter of current scientific discourse and it is known to play a vital role in structural design. In the case studies presented herein, mechanical laboratory tests using pulsating load regimes on UHPC with a strength of more than 200 MPa were simulated by use of finite element models. The orientations of the fibers were measured for each test sample prior to failure using an X-ray computed tomography (CT) scanner, and these orientations are explicitly implemented into the model. The paper discusses the methodology of merging data retrieved by CT image processing and state-of-the-art FE simulation techniques Moreover, the CT scanning was carried out throughout the testing procedure, which further enables the comparison of the mechanical tests and the FE models in terms of damage propagation and failure patterns. The results indicate that the overall fiber configuration and behavior of the samples can be realistically modelled and validated by the proposed CT-FE coupling, which can enhance the structural analysis and design process of elements produced with steel fiber reinforced and UHPC materials.
Data-driven analysis for damage assessment has a large potential in structural health monitoring (SHM) systems, where sensors are permanently attached to the structure, enabling continuous and frequent measurements. In this contribution, we propose a machine learning (ML) approach for automated damage detection, based on an ML toolbox for industrial condition monitoring. The toolbox combines multiple complementary algorithms for feature extraction and selection and automatically chooses the best combination of methods for the dataset at hand. Here, this toolbox is applied to a guided wave-based SHM dataset for varying temperatures and damage locations, which is freely available on the Open Guided Waves platform. A classification rate of 96.2% is achieved, demonstrating reliable and automated damage detection. Moreover, the ability of the ML model to identify a damaged structure at untrained damage locations and temperatures is demonstrated.
Ultrasonic testing is a widely applied measurement method in materials research and medicine. Commonly, a transducer is coupled to the specimen directly or via a liquid coupling agent. While reducing acoustic transmission losses significantly, this procedure is time-consuming and cannot be used for sensitive specimens. Air-coupled ultrasound is a viable alternative in such cases, although suffering from very high acoustic transmission losses between transducer, air and specimen. The recently introduced fluidic transducer (FT) generates ultrasound by utilizing the instability of a supersonic air jet switched inside a fluidic amplifier. Since only air is used as the working medium and no vibrating surfaces are used for ultrasound generation, the transducer is able to efficiently generate large acoustic pressure amplitudes. The resulting acoustic field shares its directivity with the ejected high-velocity air jet. Thus, the acoustic energy needs to be redirected from the jet axis in order to make the fluidic transducer applicable to sensitive specimens. In this study, the effectivity of using sonic crystals (SCs) for this redirection is investigated using acoustic and flow measurements. SCs are air-permeable while being reflective to large acoustic frequency bands. It was shown that both a defect waveguide and a mirroring strategy successfully redirected the acoustic field from the air jet. Furthermore, the interaction of flow and SC showed strong acoustic quenching if the SC was placed too close to the FT outlet. Blockage of the jet entrainment due to the SC may result in slightly higher off-axis flow velocities locally, which should be considered in sensitive applications.
"The reassessment of bridges continues to take great importance both nationally and internationally. A major challenge is to find computation models reflecting the actual properties of the considered structures sufficiently accurate. Besides regular inspections, the conduction of advanced measurements is suitable to generate reliable information about a structure to be assessed. Prior to incorporating measurement results in reassessment, the relevance, the trueness, and the precision of the measured information needs to be stated. On the one hand, the use of information whose quality has not been assessed can lead to errors with serious consequences. On the other, the measurement of irrelevant information is inefficient. Although the use of measured data in assessment is currently mostly unregulated, their appreciation in reliability analyses is beneficial since the built environment can be assessed more realistically. Utilizing NDT in reassessment has the potential to extend remaining lifetimes of a structure, save resources, and improve infrastructural availabilities. The power of judgment regarding the decision on the reliability of an existing structure can be increased.
In this contribution, an approach is outlined to process non-destructively gathered measurement data in a comparableway in order to include themeasured information in probabilistic reliability assessments of existing structures. An essential part is the calculation of measurement uncertainties. The effect of incorporating evaluated NDT-results is demonstrated by means of a prestressed concrete bridge and GPR measurements conducted on this bridge as a case-study. The bridge is assessed regarding SLS Decompression using the NDT-results."
Corrosion of concrete reinforcement is one of the major damage mechanisms affecting both the load-bearing capacity and the serviceability of re-inforced concrete structures significantly. When externally discernible damages are observed during visual inspections on the structure, the extent of the damage inside the concrete is often already significant. Corrosion caused by carbonation often leads to severe discoloration of the surface or even large-area spalling of the concrete cover. In contrast, chloride-induced corrosion is usually difficult to observe visually but can cause much more serious damage in less time. The effect occurs locally and can lead to weakening of the cross-section of the reinforce-ment. This, in turn, can cause sudden structural collapses without prior notice.
In the meanwhile, various non-destructive and minimally invasive testing methods are available to evaluate the resistance to penetration of corrosion-pro-moting pollutants and to detect active corrosion. In this paper, a bridge crossing the river Regen is used as a case-study to demonstrate how the information ob-tained applying different testing methods can be combined and evaluated in the context of structural reassessments. Both the results of the permeability testing and the electrical resistance measurement are considered, as well as active corro-sion areas are localized using the half-cell potential mapping combined with the concrete cover measurement with the eddy current method and ground penetrat-ing radar. The results are evaluated using drill cores and in addition laser-induced breakdown spectroscopy was applied to obtain information about possible chlo-ride ion transport into the concrete.
Given the central role of fatty acids in cancer pathophysiology, the exploitation of fatty acid metabolism as a potential antineoplastic therapy has gained much attention. Several natural and synthetic compounds targeting fatty acid metabolism were hitherto identified, and their effectiveness against cancer cell proliferation and survival was determined. This review will discuss the most clinically viable inhibitors or drugs targeting various proteins or enzymes mapped on nine interconnected fatty acid metabolism-related processes. We will discuss the general significance of each of these processes and the effects of their inhibition on cancer cell progression. Moreover, their mechanisms of action, limitations, and future perspectives will be assessed.
Air-coupled ultrasonic (ACU) testing has proven to be a valuable method for increasing the speed in non-destructive ultrasonic testing and the investigation of sensitive specimens. A major obstacle to implementing ACU methods is the significant signal power loss at the air–specimen and transducer–air interfaces. The loss between transducer and air can be eliminated by using recently developed fluidic transducers. These transducers use pressurized air and a natural flow instability to generate high sound power signals. Due to this self-excited flow instability, the individual pulses are dissimilar in length, amplitude, and phase. These amplitude and angle modulated pulses offer the great opportunity to further increase the signal-to-noise ratio with pulse compression methods.
In practice, multi-input multi-output (MIMO) setups reduce the time required to scan the specimen surface, but demand high pulse discriminability. By applying envelope removal techniques to the individual pulses, the pulse discriminability is increased allowing only the remaining phase information to be targeted for analysis. Finally, semi-synthetic experiments are presented to verify the applicability of the envelope removal method and highlight the suitability of the fluidic transducer for MIMO setups.