Analytische Chemie
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Paper des Monats
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This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Latvia. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends.
The study on Latvian CABs is part of a global project that covers various other countries (see www.qi-fokus.de).
Interdigital transducers (IDTs) are a well-known tool for excitation of surface acoustic waves. The use of IDTs is versatile, but they are most commonly employed as actuators for excitation of ultrasonic guided waves (UGWs). However, they are still a relatively new technology, which leaves many possibilities for future research, especially in the scope of newly emerging structural health monitoring (SHM) systems. IDTs offer low weight, design flexibility and beam directivity, which make them ideal candidates for employment in such systems.
Due to the IDTs’ and waves’ complexity, problems often cannot be described analytically, therefore they require numerical solutions and experimental validations. In this contribution, a novel, simple use of IDTs, in the scope of SHM is described. Firstly, numerical findings acquired with finite element method are presented. To validate those results, experiments in a plate-like waveguide are carried out. A good agreement between them is found. The results show the potential of the IDTs in yet another prospective application, which could be attractive for adoption in the future.
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Germany. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends.
The study on German CABs is part of a global project that covers various other countries (see www.qi-fokus.de).
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Ireland. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends.
The study on Irish CABs is part of a global project that covers various other countries (see www.qi-fokus.de).
Rapid, cost-efficient, and eco-friendly methods are desired today for routine analysis of the Fusarium mycotoxin zearalenone (ZEN) in edible vegetable oils. Liquid chromatography with fluorescence detection (HPLC-FLD) is commonly used to reliably control the specified ZEN maximum levels, which requires efficient sample clean-up to avoid matrix interferences. Therefore, a highly selective extraction and clean-up method based on reversible covalent hydrazine chemistry (RCHC) using hydrazine-functionalized silica was developed. This efficient solid-phase extraction (SPE) involves reversible hydrazone formation of ZEN with the hydrazine moiety covalently bound to a solid phase. Optimal conditions were achieved with 1 mL SPE cartridges filled with 400 mg of hydrazine-functionalized silica. The developed RCHC-SPE method was validated in an interlaboratory comparison study (ILC) with twelve participants analyzing six edible vegetable oils with a focus on maize oils. The derived method parameters (ZEN recovery 83%, repeatability 7.0%, and reproducibility 18%) meet the performance criteria of Commission Regulation (EC) No 401/2006. The developed RCHC-SPE-based HPLC-FLD method allows the reliable quantification of ZEN in the range of 47–494 μg/kg for different types of edible vegetable oils, also for matrix-reach native oils. Due to the high efficiency, the significantly reduced matrix load helps to extend the lifetime of analytical equipment. Furthermore, the re-useability of the RCHC-SPE cartridges contributes to an eco-friendly approach and reduced analysis costs. To our knowledge, this is the first report on ZEN quantification in edible vegetable oils based on manual RCHC-SPE cartridges. Due to its high performance, the developed RCHC-SPE method is a promising alternative to the current European standard method EN 16924:2017 (HPLC-FLD part).
NaYF4:Yb3+/Tm3+@NaGdF4:Nd3+/Yb3+ upconversion nanoparticles (UCNPs) were prepared using a solvothermal method, and the effects of key factors such as the content of sensitiser Nd 3+ and Yb3+ on their luminescence properties were investigated. The nanoparticles are homogeneous in size and well dispersed. Under 808 nm excitation, it can produce strong upconversion fluorescence. At the same time, the nanoparticles have good temperature-sensing properties at the thermally coupled energy levels of 700 nm and 646 nm for Tm3+. Using its fluorescence intensity ratio (FIR), accurate temperature measurements can be performed, and it has been found that it exhibits different temperature sensing properties in low and high-temperature regions. The maximum relative sensitivity was found to be 0.88% K-1 and 1.89% K-1 for the lowtemperature region of 285 K-345 K and the high-temperature region of 345 K-495 K. The nanoparticles were applied to the internal temperature measurement of lithium batteries and the actual high-temperature environment, respectively, and were found to have good temperature measurementt performance.
Learned block iterative shrinkage thresholding algorithm for photothermal super resolution imaging
(2022)
Block-sparse regularization is already well known in active thermal imaging and is used for multiple-measurement-based inverse problems. The main bottleneck of this method is the choice of regularization parameters which differs for each experiment. We show the benefits of using a learned block iterative shrinkage thresholding algorithm (LBISTA) that is able to learn the choice of regularization parameters, without the need to manually select them. In addition, LBISTA enables the determination of a suitable weight matrix to solve the underlying inverse problem. Therefore, in this paper we present LBISTA and compare it with state-of-the-art block iterative shrinkage thresholding using synthetically generated and experimental test data from active thermography for defect reconstruction. Our results show that the use of the learned block-sparse optimization approach provides smaller normalized mean square errors for a small fixed number of iterations. Thus, this allows us to improve the convergence speed and only needs a few iterations to generate accurate defect reconstruction in photothermal super-resolution imaging.
A new “green” and mild synthesis of highly stable microcrystalline Cs2AgxNa1-xBiyIn1-yCl6 (CANBIC) perovskites under ambient conditions was developed that is scalable to the multi-gram production. Under UV illumination, the CANBIC perovskites emit intense broadband photoluminescence (PL) with a quantum yield (QY) of 92% observed for x = 0.35 and y = 0.01-0.02. The combination of strong UV absorbance and broadband visible emission, high PL QY, and long PL lifetimes of up to 1.4 μs, along with an outstanding stability makes these CANBICs a promising material class for many optical applications.
For test laboratories operating under accreditation schemes like ISO/IEC 17025 (ISO/IEC 17025), as the international reference for testing and calibration laboratories wanting to demonstrate their capacity to deliver reliable results, a periodical control of the critical instrumental parameters of an Energy-Dispersive X-ray Spectrometer (EDS) is required.
This periodical check of an EDS is specified with exact procedures and materials in the ISO 15632:2021 ”Microbeam Analysis – Selected instrumental performance parameters for the specification and checking of energy-dispersive X-ray spectrometers for use in electron probe microanalysis” (ISO 15632). The EDS check can be simplified to the acquisition of only one 10 kV spectrum from a dedicated test material, EDS-TM002, which is made available by BAM since 2009 (https://webshop.bam.de/webshop_en/). The optional BAM software “EDX spectrometer check” is destined to automatically evaluate this spectrum and determine the performance of the EDS in terms of energy resolution and calibration, as well as possible alteration of low-energy efficiency due to detector contamination. Nearly 200 laboratories have the EDS-TM and associated software package in use.
Practical examples based on various types of artifacts occurred in the EDS spectra and a long-term (>10 years) meticulous observation of the own spectrometers will be discussed. Different types of EDS spectrometers are considered, e.g. Si(Li) and SDD, of various window types (AP, the recent one Si3N4 or even windowless), and with different front contact layers (Au and Ni) (Hodoroaba and Procop, 2014). Evaluation of other parameters or effects such as the deadtime at different count rates or pileup effects is also explained with examples.
This study presents a practical procedure to give access to more information by tilting the sample holder and hence allowing images of a single particle to be recorded at different orientations under the same view angle. From the analysis of these images, extended information on surface roughness of the particle can be extracted. Thus, instead of obtaining 2D information from a single SEM image, three-dimensional (3D) information is obtained from 2D projections recorded at different particle orientations.
Lithium and boron are trace components of magmas, released during exsolution of a gas phase during volcanic activity. In this study, we determine the difusivity and isotopic fractionation of Li and B in hydrous silicate melts. Two glasses were synthesized with the same rhyolitic composition (4.2 wt% water), having diferent Li and B contents; these were studied in difusion-couple experiments that were performed using an internally heated pressure vessel, operated at 300 MPa in the temperature range 700–1250 °C for durations from 0 s to 24 h. From this we determined activation energies for Li and B difusion of 57±4 kJ/mol and 152±15 kJ/mol with pre-exponential factors of 1.53 × 10–7 m2/s and 3.80× 10–8 m2 /s, respectively. Lithium isotopic fractionation during difusion gave β values between 0.15 and 0.20, whereas B showed no clear isotopic fractionation. Our Li difusivities and isotopic fractionation results difer somewhat from earlier published values, but overall confrm that Li difusivity increases with water content. Our results on B difusion show that similarly to Li, B mobility increases in the presence of water. By applying the Eyring relation, we confrm that B difusivity is limited by viscous fow in silicate melts. Our results on Li and B difusion present a new tool for understanding degassing-related processes, ofering a potential geospeedometer to measure volcanic ascent rates.
Heterogeneous Oxysulfide@Fluoride Core/ Shell Nanocrystals for Upconversion-Based Nanothermometry
(2022)
Lanthanide (Ln3+)-doped upconversion nanoparticles (UCNPs) often suffer from weak luminescence, especially when their sizes are ultrasmall (less than 10 nm). Enhancing the upconversion luminescence (UCL) efficiency of ultrasmall UCNPs has remained a challenge that must be undertaken if any practical applications are to be envisaged. Herein, we present a Ln3+-doped oxysulfide@fluoride core/shell heterostructure which shows efficient UCL properties under 980nm excitation and good stability in solution. Through epitaxial heterogeneous growth, a ∼4 nm optically inert β-NaYF4 shell was coated onto ∼5 nm ultrasmall Gd2O2S:20%Yb,1%Tm. These Gd2O2S:20%Yb,1%Tm@NaYF4 core/shell UCNPs exhibit a more than 800-fold increase in UCL intensity compared to the unprotected core, a 180-fold increase in luminescence decay time of the 3H4 → 3H6 Tm3+ transition from 5 to 900 μs, and an upconversion quantum yield (UCQY) of 0.76% at an excitation power density of 155 W/cm2. Likewise, Gd2O2S:20%Yb,2%Er@NaYF4 core/shell UCNPs show a nearly 5000-fold
increase of their UCL intensity compared to the Gd2O2S:20%Yb,2%Er core and a maximum UCQY of 0.61%. In the Yb/Er core−shell UCNP system, the observed variation of luminescence intensity ratio seems to originate from a change in lattice strain as the temperature is elevated. For nanothermometry applications, the thermal sensitivities based on thermally coupled levels are estimated for both Yb/Tm and Yb/Er doped Gd2O2S@NaYF4 core/shell UCNPs.
The ability of industrial X-ray computed tomography (CT) to scan an object with several internal and external features at once causes increasing adoption in dimensional metrology. In order to evaluate the quality of a measurement value, the task-specific measurement uncertainty has to be determined. Currently, VDI/VDE 2630 part 2.1 gives a guideline to determine the uncertainty of CT measurements experimentally by conducting repeated measurements. This is costly and time-consuming. Thus, the aim is to determine the task-specific measurement uncertainty numerically by simulations (e. g. according to the guide to expression of uncertainty in measurement (GUM) Supplement 1). To achieve that, a digital twin is necessary. This contribution presents a simple first approach how a digital twin can be built. In order to evaluate this approach, a study comparing measurements and simulations of different real CT systems was carried out by determining the differences between the measurement results of the digital twin and of the measurement results of the real-world CT systems. The results have shown a moderate agreement between real and simulated data. To improve on this aspect, a standardized method to characterize CT systems and methods to implement CT parameters into the simulation with sufficient accuracy will be developed.
Im Rahmen des EU-Projekts „CONSENS – Integrated Control and Sensing“ wurde ein vollautomatisiertes, gemäß Atmosphère-Explosibles(ATEX)-Regeln zertifiziertes Analysatormodul auf Basis eines kommerziellen Benchtop-Kernspinresonanzspektrometers (Engl. nuclear magnetic resonance, NMR) entwickelt und im Umfeld einer modularen containerbasierten Produktionsanlage validiert. Auf Basis der gewonnenen Daten konnten sowohl eine iterative Optimierung der Prozessparameter erfolgen als auch Referenzdaten für die Kalibrierung eines Nahinfrarot-Spektrometers gewonnen werden.
The residual stresses and load transfer in multiphase metal alloys and their composites (with both random planar-oriented short fibers and particles) will be shown, as studied by neutron diffraction, by X-ray computed tomography, and by a model based on the reformulation of classic Maxwell’s homogenization method.
Contrary to common understanding and state-of-the-art models, we experimentally observe that randomly oriented phases possess non-hydrostatic residual stress. Moreover, we disclose that the unreinforced matrix alloy stays under hydrostatic compression even under external uniaxial compression.
The recently developed modeling approach allows calculating the residual stress in all phases of the composites. It rationalizes the presence of deviatoric stresses accounting for the interaction of random oriented phases with fibers having preferential orientation. It also allows the explanation of the unconventional in-situ behavior of the unreinforced alloy and the prediction of the micromechanical behavior of other similar alloys.
The availability of non-destructive methods is particularly important for composites, e.g., carbon or glass fiber-reinforced polymers because their properties strongly depend on the manufacturing process and in-service conditions. Composites are mostly used in thin-walled components which are perfectly suited for the characterisation with ultrasonic guided waves (UGWs).
In this contribution, we demonstrate sensitivities of UGW to different elastic constants of a composite material. Then we present a characterisation procedure which can be used to in-fer elastic properties. Our approach is based on an inverse procedure in which the numeri-cally calculated dispersion curves are fitted to the measured curves. The acquisition is done by applying a broadband piezoelectric transducer (PZT) to excite various UGW modes and a 3D laser Doppler vibrometer (3D LDV) to record them. Compared to the approaches based on laser excitation, the PZT provides a better signal-to-noise ratio because more energy is brought into the structure. Whereas the 3D LDV compared to a 1D LDV or a PZT allows cap-turing in-plane and out-of-plane components giving more dispersion information for a better characterisation. Since the inverse procedure requires many iterations before elastic prop-erties are retrieved, an efficient tool for the calculation of the dispersion curves is necessary. For this, the Scaled Boundary Finite Element Method is used. All in all, a good agreement be-tween theoretical and experimental curves is demonstrated.
The residual stresses and load transfer in multiphase metal alloys and their composites (with both random planar-oriented short fibers and particles) will be shown, as studied by neutron diffraction, by X-ray computed tomography, and by a model based on the reformulation of classic Maxwell’s homogenization method.
Contrary to common understanding and state-of-the-art models, we experimentally observe that randomly oriented phases possess non-hydrostatic residual stress. Moreover, we disclose that the unreinforced matrix alloy stays under hydrostatic compression even under external uniaxial compression.
The recently developed modeling approach allows calculating the residual stress in all phases of the composites. It rationalizes the presence of deviatoric stresses accounting for the interaction of random oriented phases with fibers having preferential orientation. It also allows the explanation of the unconventional in-situ behavior of the unreinforced alloy and the prediction of the micromechanical behavior of other similar alloys.
The application of temperature compensation strategies is crucial in structural health monitoring approaches based on guided waves. Actually, the varying temperature influences the performance of the inspection system inducing false alarms or missed detection, with a consequent reduction of reliability and impact on probability of detection (POD).
This paper quantitatively describes two different methods to compensate the temperature effect, namely the optimal baseline selection (OBS) and the baseline signal stretch (BSS) extending their application to the case of a distributed sensor networks (DSN). This latter introduces a number of possible data to explore compensation strategies which do not necessarily returns univocal results. Hence, a decision framework is needed, which takes into consideration multiple ultrasonic time traces with different arrival times and amplitude. In detail, the effect of temperature separation between baseline time-traces in OBS are investigated considering multiple couples of sensors employed in the DSN. A combined strategy that uses both OBS and a frequent value warning is introduced to find the more probable temperature with increasing reliability of the assessment. The same procedure is applied using the BSS algorithm. Finally, the use of both approaches is introduced, comparing the capability of the mixed algorithm to correctly sort temperature information from OBS and then apply the BSS combining the frequent value warning to have a unique correction all over the DSN.
Theoretical results are compared, using data from two several experiments, which use different frequency analysis with either predominantly A0 mode or S0 mode data or both. The focus is given on the fact that different paths are available in a sensor network and several possible combinations of results are available. Nonetheless, introducing a frequent value warning it is possible to increase the efficiency of the OBS and BSS approaches making use of fewer signal processing algorithms. These confirm that the performance of OBS quantitatively agrees with predictions. In addition, the possibility to combine BSS approached also demonstrates that the use of compensation strategies improves detectability and localization of damage even in a DSN. This result can be used to improve the SHM system reliability, with promising perspectives in increasing POD.