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Eingeladener Vortrag
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Metabolomics, the analysis of potentially all small molecules within a biological system, has become a valuable tool for biomarker identification and the elucidation of biological processes. While metabolites are often present in complex mixtures at extremely different concentrations, the dynamic range of available analytical methods to capture this variance is generally limited. Here, we show that gas chromatography coupled to atmospheric pressure chemical ionization mass spectrometry (GC-APCI-MS), a state of the art analytical technology applied in metabolomics analyses, shows an average linear range (LR) of 2.39 orders of magnitude for a set of 62 metabolites from a representative compound mixture. We further developed a computational tool to extend this dynamic range on average by more than 1 order of magnitude, demonstrated with a dilution series of the compound mixture, using robust and automatic reconstruction of intensity values exceeding the detection limit. The tool is freely available as an R package (CorrectOverloadedPeaks) from CRAN (https://cran.r-project.org/) and can be incorporated in a metabolomics data processing pipeline facilitating large screening assays.
Übersicht über die gefahrgutrechtlichen Anforderungen zur Bauartprüfung und dem Qualitätsmanagement für Verpackungen für nicht zulassungspflichtige Versandstücke.
In order to demonstrate the safety of both spent fuel and the storage system, a good understanding of the processes that might cause deterioration is required. The International Atomic Energy Agency (IAEA) continued the coordinated research on Spent Fuel Performance Assessment and Research (SPAR) into a fourth phase starting in 2015 to evaluate fuel and materials performance under wet and dry storage and to assess the impact of interim storage on associated spent fuel management activities (such as handling and transport). BAM’s understanding and experiences in the field of long-term storage of spent fuel and especially spent fuel characterization are presented to assist the preparation of the final project report.
Embrittlement of spent fuel claddings during long-term dry interim storage - Current approach at BAM
(2019)
The integrity of fuel rods and cladding tubes must be demonstrated throughout the dry interim storage of spent nuclear fuel in Germany. For at least a relevant number of casks, an extension of interim storage between 40 and 100 years is foreseeable. The drying procedure for the fuel rods in conjunction with the thermomechanical storage conditions may change the microstructure of the cladding tubes and lead to their possible embrittlement. The failure probability might increase under mechanical load by handling procedures (transport after storage) on potentially embrittled cladding tubes of fuel rods especially at low temperatures after long-term storage. Results of ring compression tests on unirradiated pre-hydrided as well as irradiated samples with radial hydrides are investigated by finite element analyses to be able to describe the failure process and to identify failure criteria.
The characterization of spent fuel and radioactive waste is essential in the evaluation of the ability of these materials to meet acceptance criteria. Prior to determining a method for spent fuel characterization, it is necessary to identify the type of data required to support safety and other analyses for the storage, transportation and final disposal of spent fuel. BAM’s understanding and capabilities in the field of spent fuel characterization are presented for the scope of a coordinated research project on the topic.
Additive Manufacturing (AM) in terms of laser powder-bed fusion (L-PBF) offers new prospects regarding the design of parts and enables therefore the production of lattice structures. These lattice structures shall be implemented in various industrial applications (e.g. gas turbines) for reasons of material savings or cooling
channels. However, internal defects, residual stress, and structural deviations from the nominal geometry are unavoidable.
In this work, the structural integrity of lattice structures manufactured by means of L-PBF was non-destructively investigated on a multiscale approach.
A workflow for quantitative 3D powder analysis in terms of particle size, particle shape, particle porosity, inter-particle distance and packing density was established.
Synchrotron computed tomography (CT) was used to correlate the packing
density with the particle size and particle shape. It was also observed that at least about 50% of the powder porosity was released during production of the struts.
Struts are the component of lattice structures and were investigated by means of laboratory CT. The focus was on the influence of the build angle on part porosity and surface quality. The surface topography analysis was advanced by the quantitative characterisation of re-entrant surface features. This characterisation was compared with conventional surface parameters showing their complementary
information, but also the need for AM specific surface parameters.
The mechanical behaviour of the lattice structure was investigated with in-situ CT under compression and successive digital volume correlation (DVC). The Deformation was found to be knot-dominated, and therefore the lattice folds unit cell layer wise.
The residual stress was determined experimentally for the first time in such lattice structures. Neutron diffraction was used for the non-destructive 3D stress investigation. The principal stress directions and values were determined in dependence of the number of measured directions. While a significant uni-axial stress state was found in the strut, a more hydrostatic stress state was found in the knot. In both cases, strut and knot, seven directions were at least needed to
find reliable principal stress directions.
Fatigue models that accurately resolve the complex three-dimensional failure mechanisms of concrete are numerically expensive. Especially the calibration of fatigue parameters to existing Wöhler lines requires solving for thousands or millions of cycles and a naive cycle-by-cycle integration is not feasible.
The proposed adaptive cycle jump methods provide a remedy to this challenge.
They greatly reduce the numerical effort of fatigue simulations and provide the basis for a development of those models.
This study was designed to examine and compare the operation of accreditation bodies in Europe. A management tool, the Process Maturity Benchmarking Tool (PMBT), was elaborated and validated by applying it to various accreditation bodies. By applying the tool, the values of indicators were determined, thus enabling a comparison of the accreditation bodies despite different operational processes and organizational forms.
The management tool PMBT is based on the analysis of selected processes with high relevance for the operation of accreditation bodies. The processes are derived from a process map designed for accreditation bodies in a universally applicable way. The indicators used to characterize the processes come from two sources: The first source relates to data already available from internal databases, reports, financial audits etc. The second source is derived from a self-evaluation of process maturity performed by the accreditation bodies. The criteria for evaluating process maturity were designed by applying the criteria of the EFQM excellence model 2013 of the European Foundation for Quality Management (EFQM) to the processes identified in the process map.
The project Comparison of the Operation of Accreditation Bodies in Europe comprised three stages. In the first stage, the processes of accreditation bodies were systematically analyzed. A process map was developed and processes of special relevance for the performance of accreditation bodies were identified and underpinned by indicators as described above. In the second stage, the processes of the German accreditation body DAkkS were assigned to the tool. This stage was used to check and modify the indicators when necessary. In the third stage, the transferability of the model was analyzed by extension to seven other accreditation bodies operating in Europe. The third stage of the project ended with a workshop attended by the eight accreditation bodies, which was used to present and discuss the results of the comparison and to identify best practices.
Packages for the transport of spent nuclear fuel shall meet the International Atomic Energy Agency regulations to ensure safety under different transport conditions. The physical state of spent fuel and the fuel rod cladding as well as the geometric configuration of fuel assemblies are important inputs for the evaluation of package capabilities under these conditions. Generally, the mechanical behavior of high burn-up spent fuel assemblies under transport conditions shall be analyzed with regard to the assumptions which are used in the containment and criticality safety analysis. Considering the complexity of the interactions between the fuel rods as well as between the fuel assemblies, basket, and cask containment, the exact mechanical analysis of such phenomena is nearly impossible. The gaps in Information concerning the material properties of cladding and pellet behavior, especially for the high burn-up fuel, make the analysis more complicated additionally. As a result, enveloping analytical approaches are usually used by BAM within the safety assessment of packages approved for transport of spent nuclear fuel.
To justify the safety margins of such approaches additional analyses are necessary. In this paper, numerical simulations of a spent fuel assembly Segment are presented. The segment modeled represents the part of a generalized BWR fuel assembly between two spacers.
Dynamic and quasi-static finite element calculations are performed to simulate the spent fuel behavior under regulatory defined accident conditions of transport. Beam elements are used for the modeling of the fuel rods representing the compound consisting of claddings and fuel pellets. The dynamic load applied is gathered from an experimental drop test with a spent fuel cask performed at BAM. A hot cell bending test performed at JRC Karlsruhe is the basis for obtaining the material behavior of the fuel rods. The material properties are determined by simulating the test setup of JRC and optimizing the results to fit the experimental load deflection curve. The simulations of the fuel assembly segment are used to get a better understanding about the loads on fuel rods under accident conditions of transport.
Packages for the transport of spent nuclear fuel shall meet the International Atomic Energy Agency regulations to ensure safety under different Transport conditions. The physical state of spent fuel and the fuel rod cladding as well as the geometric configuration of fuel assemblies are important inputs for the evaluation of package capabilities under these conditions. Generally, the mechanical behavior of high burn-up spent fuel assemblies under Transport conditions shall be analyzed with regard to the assumptions which are used in the containment and criticality safety analysis. In view of the complexity of the interactions between the fuel rods as well as between the fuel assemblies, basket, and cask containment, the exact mechanical analysis of such phenomena is nearly impossible. The gaps in information concerning the material properties of cladding and pellet behavior, especially for the high burn-up fuel, make the analysis more complicated additionally. As a result, enveloping analytical approaches are usually used by BAM within the safety assessment of packages approved for transport of spent nuclear fuel.
To justify the safety margins of such approaches additional analyses are necessary. In this paper, numerical simulations of a segment of a spent fuel assembly are presented. The segment modeled represents the part of a generalized BWR fuel assembly between two spacers. Explicit dynamic finite element calculations are performed to simulate the spent fuel behavior under regulatory defined accident conditions of transport. A beam element formulation is used for the modeling of the fuel rods representing the compound consisting of claddings and fuel pellets. The load applied is gathered from experimental drop tests with spent fuel casks performed at BAM. A hot cell bending test performed at JRC Karlsruhe is the basis for obtaining the material behavior of the fuel rods. The material properties are determined by
simulating the test setup of JRC and optimizing the results to fit the
experimental load deflection curve. The simulations of the fuel Assembly segment are used to get a better understanding about the loads on fuel rods under accident conditions of transport.
The high ionization potentials and low wavelength emission lines of halogens difficult the analysis of their organohalogen compounds by ICP-based methods [1]. Other techniques, such as combustion ion chromatography (CIC) or ion-selective electrodes have proven to be more reliable to determine these elements. However, these techniques are more time-consuming and/or have lower precision and accuracy.
High resolution continuum source graphite furnace molecular absorption spectrometry (HR CS GFMAS) allows the determination of solid and liquid samples by monitoring a molecule formed with the analyte and a molecule forming reagent. In the case of F, Cl and Br, several molecule forming agents have been studied for their determination. Among all of them, calcium can form a stable bond with the three elements and provides optimal analytical properties for trace analysis [2]. However, the spectral window of commercially available continuum source AAS instruments is not broad enough to cover the wavelength range necessary for a simultaneous determination. Thus, coupling it with a modular simultaneous echelle spectrograph (MOSES), which can register around 200 nm in a single measure, allows the simultaneous study of the three analytes [3].
This instrumentation is capable of register more than 200 nm of the spectra per measure keeping a high resolution. This spectral window is suitable for the monitorization of a variety of transitions of the three molecules. However, some of them are overlapped and the competitive mechanism of formation of the three molecules modify their sensitivity depending on the proportions in the sample.
In this study, a compromise in the conditions and modifiers were selected in order to maximize the sensitivity and signal to noise ratio for the three molecules. The determination was carried out by standard addition of CaF and Cl and Br were obtained from the PLS model.
References:
[1] X. Bu, T. Wang, G. Hall, J. Anal. At. Spectrom., 18, 1443–1451 (2003)
[2] M. Resano, E. García-Ruiz, M. Aramendía, M. A. Belarra, J. Anal. At. Spectrom., 34, 59–80 (2019)
[3] S. Geisler, M. Okruss, H. Becker-Ross, M. Dong Huang, N. Esser, S. Florek, Spectrochimica Acta PartB, 107, 11–16 (2015)
To increase the competitiveness of jacket substructures compared to monopiles a changeover from an individual towards a serial jacket production based on automated manufactured tubular joints com-bined with standardized pipes has to be achieved. Therefore, this paper addresses fatigue tests of automatical-ly welded tubular X-joints focusing on the location of the technical fatigue crack. For this X-joint, the detect-ed location of the technical crack is then compared to numerical investigations predicting the most fatigue prone notch considering the structural stress approach as well as the notch stress approach. Additionally, the fatigue prone hot spot according to both approaches is compared for a typical offshore jacket double-K-joint to emphasize the significance of the presented outcomes for the existing offshore structures. Besides, the welding process of the automated manufactured tubular X-joints is presented.
To increase the competitiveness of jacket substructures compared to monopiles a changeover from an individual towards a serial jacket production based on automated manufactured tubular joints com-bined with standardized pipes has to be achieved. Therefore, this paper addresses fatigue tests of automatical-ly welded tubular X-joints focusing on the location of the technical fatigue crack. For this X-joint, the detect-ed location of the technical crack is then compared to numerical investigations predicting the most fatigue prone notch considering the structural stress approach as well as the notch stress approach. Additionally, the fatigue prone hot spot according to both approaches is compared for a typical offshore jacket double-K-joint to emphasize the significance of the presented outcomes for the existing offshore structures. Besides, the welding process of the automated manufactured tubular X-joints is presented.
To increase the competitiveness of jacket substructures compared to monopiles a changeover from an individual towards a serial jacket production based on automated manufactured tubular joints combined with standardized pipes has to be achieved. Therefore, this paper addresses fatigue tests of automatically welded tubular X-joints focusing on the location of the technical fatigue crack. The detected location of the technical crack is compared to numerical investigations predicting the most fatigue prone notch considering the structural stress approach as well as the notch stress approach. Besides, the welding process of the automated manufactured tubular X-joints is presented.
To increase the competitiveness of jacket substructures compared to monopiles a changeover from an individual towards a serial jacket production based on automated manufactured tubular joints combined with standardized pipes has to be achieved. Therefore, this paper ad-dresses the welding process of automated manufactured tubular X-joints. Additionally, fatigue tests of the automatically welded tubular joints are presented focusing on the location of the technical fatigue crack. The detected location of the technical crack is compared to numerical investigations predicting the most fatigue prone notch considering the structural stress approach as well as the notch stress approach.
AI-reflectivity is a code based on artificial neural networks trained with simulated reflectivity data that quickly predicts film parameters from experimental X-ray reflectivity curves. This project has a common root with (ML-reflectivity)[https://github.com/schreiber-lab/ML-reflectivity] and evolved in parallel. Both are linked to the following publication:
Fast Fitting of Reflectivity Data of Growing Thin Films Using Neural Networks A. Greco, V. Starostin, C. Karapanagiotis, A. Hinderhofer, A. Gerlach, L. Pithan, S. Liehr, F. Schreiber, S. Kowarik (2019). J. Appl. Cryst.
For an online live demonstration using a pre-trained network have a look at github.
To increase the competitiveness of jacket substructures compared to monopiles a changeover from an individual towards a serial jacket production based on automated manufactured tubular joints combined with standardized pipes has to be achieved. Therefore, this paper addresses fatigue tests of automatically welded tubular X-joints focusing on the location of the technical fatigue crack. The detected location of the technical crack is compared to numerical investigations predicting the most fatigue prone notch considering the structural stress approach as well as the notch stress approach. Besides, the welding process of the automated manufactured tubular X-joints is presented.
To increase the competitiveness of jacket substructures compared to monopiles a changeover from an individual towards a serial jacket production based on automated manufactured tubular joints combined with standardized pipes has to be achieved. Therefore, this paper ad-dresses the welding process of automated manufactured tubular X-joints. Additionally, fatigue tests of the automatically welded tubular joints are presented focusing on the location of the technical fatigue crack. The detected location of the technical crack is compared to numerical investigations predicting the most fatigue prone notch con-sidering the structural stress approach as well as the notch stress ap-proach.
The analysis of the chemical composition of cement-based materials like concrete is a crucial task in civil engineering. Concrete is a multi-phase material made of cement, water, aggregates, additives and admixtures. During the damage assessment of concrete structures, the external ingress of harmful species like chlorine, alkalis or sulfates needs to be determined. In order to provide a fast and precise analysis of concrete the application of LIBS offers unique possibilities as the technique can detect all elements at air atmosphere.
To determine the condition of concrete, the information about the chemical composition, the ingress of harmful species as well as the evaluation of characteristic values like the used cement type or the type of aggregates are needed. This work presents the two-dimensional evaluation of concrete samples using LIBS and multivariate data analysis of atomic and molecular emission. For the evaluation of the main components different classification methods will be applied to identify the heterogeneity of the samples. With respect to their specific phase, different species will be quantified using multivariate regression (PLS) and important figures of merit will be presented. All results will be verified using Standard procedure of wet chemistry (XRF, potentiometric titration and ICP-OES).
Safety of long term containment and storage of radioactive waste is an essential issue, which is increasingly gaining international attention. Extending interim storage beyond initial license periods is one of the major challenges worldwide.
BAM has been involved in all kinds of radioactive waste container safety evaluation for storage and transportation including their long term performance from the very beginning. Today, all work related to the safe management of radioactive waste is linked by the activity field “Nuclear Waste Management” within the Focus Area “Energy” at BAM and in conjunction with a research strategy and agenda. Most recently, the working group “Long Term Safety of Container Systems and Components” was established to launch and perform research projects related to safety issues concerning the extended interim storage of radioactive waste.
For example, within our project LaMEP, we investigate ageing effects of metal and elastomer seals as well as polymeric neutron shielding materials, which are container components that fulfil major safety functions. The results of the experiments help to understand the long term behaviour of these components. Likewise, our project BRUZL started at BAM in 2018 with the aim of developing a fracture mechanics approach to understand and describe a potential brittle failure mechanism of fuel cladding during long-term interim storage. BAM also contributes to the GRS project “Development of methods and models and international exchange for safety evaluation in the frame of interim storage of radioactive waste”. Additionally, BAM is involved in several international research programmes dealing with extended interim storage, such as the European Joint Programme on Radioactive Waste Management (EURAD), the Extended Storage Collaboration Program (ESCP) and IAEA Coordinated Research Projects.
The present contribution provides a comprehensive overview of BAM research activities contributing to national and international gap analyses and to filling knowledge gaps regarding the safe long term management of radioactive waste.
The application of a LIBS system is presented. A diode-pumped low energy laser (3 mJ, 1.5 ns, 100 Hz) and a compact NIR spectrometer are used. A scanner allows the two-dimensional element mapping. For the quantitative analysis calibration of the system is carried out with reference samples in a concentration range of chlorine of 0.05 wt.% to 2.5 wt.%. To determine the 2D distribution of harmful elements (Cl, C), concrete cores were drilled, split and analyzed directly. By comparing the chloride ingress and the carbonation, the interaction of both processes can be visualized in one measurement that takes less than 10 minutes with a drill core of 50 mm x 100 mm. Results obtained were compared and verified with standard measurements.
Binder remnants in historical mortars represent a record of the connection between the raw materials that enter the kiln, the process parameters, and the end product of the calcination. Raman microspectroscopy combines high structural sensitivity with micrometre to sub-micrometre spatial resolution and compatibility with conventional thin-sectional samples in an almost unique fashion, making it an interesting complementary extension of the existing methodological arsenal for mortar analysis. Raman spectra are vibrational fingerprints of crystalline and amorphous compounds, and contain marker bands that are specific for minerals and their polymorphic forms. Relative intensities of bands that are related to the same crystalline species change according to crystal orientations, and band shifts can be caused by the incorporation of foreign ions into crystal lattices, as well as stoichiometric changes within solid solution series. Finally, variations in crystallinity affect band widths. These effects are demonstrated based on the analysis of three historical mortar samples: micrometric distribution maps of phases and polymorphs, crystal orientations, and compositional variations of solid solution series of unreacted clinker grains in the Portland cement mortars of two 19th century castings, and the crystallinities of thermal anhydrite clusters in a high-fired medieval gypsum mortar as a measure for the applied burning temperature were successfully acquired.
To increase the competitiveness of jacket substructures compared to monopiles a changeover from an individual towards a serial jacket production based on automated manufactured tubular joints combined with standardized pipes has to be achieved. Therefore, this paper addresses fatigue tests of automatically welded tubular X-joints focusing on the location of the technical fatigue crack. The detected location of the technical crack is compared to numerical investigations predicting the most fatigue prone notch considering the structural stress approach as well as the notch stress approach. Besides, the welding process of the automated manufactured tubular X-joints is presented.
The determination of mechanical properties of welded Steel structures such as strength or ductility is a subject of high interest for the majority of Companies in the area of metal Processing. The material Parameters can be obtained by performing the tensile test on the samples made from a part of a component. In some cases, it is highly expensive to produce the tensile specimens especially from the weld metal, which contains different type of microstructure such as weld seam or heat affected zone in an extremely small area. Therefore, a method is described in this paper to determine the material Parameters of high strength Steel structures and welded joints locally and without any additional effort to perform the tensile test. In this method, instrumented indentation technique (IIT), an indenter is pushed on the flat surface of a specimen in a certain period of time and simultaneously the applied force and the corresponding indentation path are measured. The data related to the force-indentation diagram is given as input to an artificial neural network (ANN) to obtain the material Parameters. The ANN can be trained by generating the large qualitative data sets with numerical Simulation of the IIT procedure. The Simulation must be run several times with the different material model parameter sets to generate the numerous
force-indentation diagrams as the inputs of ANN. Then, the trained ANN is validated by performing the IIT on the welded joints and comparing the obtained material Parameters from ANN with the tensile test.
Consequently, the mechanical properties of welded joints can be determined by performing the IIT and evaluating the resulting data by the ANN.
Predictive Methods for Determining the Thermal Decomposition Properties of Hazardous Substances
(2019)
Due to the fast development and availability of computers, predictive approaches are increasingly used in the evaluation process of hazardous substances complementary to experiments. Their use was recommended as alternative to experimental testing by the REACH regulation to complete the lack of knowledge on properties for existing substances that must be registered before 2018 (upon quantities). Among the proposed predictive approaches, Quantitative Structure Property Relationships (QSPR) are powerful methods to predict macroscopic properties from the only molecular structure of substances. In that context, the HAZPRED project (2015-2018, founded by the SAF€RA consortium) aims to develop theoretical models (e.g. QSPR) and small-scale tests to predict complex physico-chemical properties (e.g. thermal stability, explosivity) of hazardous substances to complete the lack of knowledge on these hazardous substances quickly or to understand their decomposition behaviour better. In particular, this contribution will present the work done in this project on the physical hazards of organic peroxides and self-reactive substances: gathering of existing experimental data, new experimental campaigns, review of existing models and proposition of new estimation methods.
The use of high niobium alloyed cast iron alloys is a relatively new approach in which the niobium addition intends to improve the properties of the material by the precipitation of hard niobium carbides during solidification. Steels can be replaced by ductile cast iron in some rolling applications, such as gears and cams, in order to reduce material costs. The aim of this work is to evaluate ductile iron alloyed with 1 weight percent (wt.%) niobium for the as cast specimens and with 1.8 wt.% and 2.4 wt.% niobium for the austempered specimens under lubricated slip-rolling tests using mixed/boundary conditions in an Amsler-type machine. Austempered ductile iron (ADI) alloyed with 1 wt.% chromium, or Carbidic ADI, was tested for comparison. For the as cast conditions, the niobium addition resulted in an increase of wear resistance owing to the low contact pressure of these tests. However, for the austempered specimens, the best performance was found for unalloyed ADI. The main factor acting in the initiation and propagation of cracks in ductile iron is the presence of the graphite nodules. The coarse carbides also contributed to the initiation of cracks and spalling of the material.
Experimental and numerical analyses of spent nuclear fuel behavior under transport conditions
(2019)
Packages for the transport of spent nuclear fuel shall meet the International Atomic Energy Agency regulations to ensure safety under different transport conditions. The physical state of the spent fuel and the fuel rod cladding as well as the geometric configuration of fuel assemblies are important inputs for the evaluation of the package capabilities under these conditions. The mechanical behavior of spent fuel assemblies shall be analyzed with regard to the assumptions which are used in the containment and criticality safety analysis. The package as a mechanical system is characterized by a complex set of interactions, e. g. between the fuel rods within the assembly as well as between the fuel assemblies, the basket, and the cask containment. This complexity makes it difficult to assume appropriate mechanical loads for the spent fuel inside the package. Another challenge is the assumption of material properties which represent the variation of the fuel rods regarding cladding material, burn-up and the operation history sufficiently. The objective of this paper is to give an overview about the current approaches and research for the evaluation of spent fuel behavior within the package design approval procedure. In this context, analytical, numerical and experimental results are discussed. The presented work is achieved within a collaboration of BAM with national and international partners.
In the last years, the Process Analytical Technology (PAT) research field has become of great importance due to its connection with the industrial world. This industry related research, along with the evolutionary progress that technology has seen lately, has allowed that key analytical techniques in an industrial environment have undergone a radical development. One of these techniques has been the near-infrared spectroscopy (NIRS). This technique, currently common in "online" industrial analysis, has seen a remarkable revolution, especially since the introduction of the microelectromechanical systems technology (MEMS) in the spectroscopy field. Nowadays it is possible to find compact spectrometers no bigger than a wristwatch in the market. Although there is an unavoidable question: can these compact spectrometers actually compete against the traditional spectrometers?
In this project different calibration parameters of two compact NIR spectrometers ("Spectral Engines Oy NIR-One Sensor NM2.0", with 1550 to 1950 nm range; and "NeoSpectra Si-ware", with 1300 to 2550 nm range) were evaluated, and the obtained results were compared with a reference spectrometer ("Bruker Optik GmbH Matrix-F", with 15000 to 4000 cm–1 range). In order to obtain the different calibration parameters, a sequence of quality performance tests were conducted. The results obtained after the different experiments carried out with both compact spectrometers prove that their performance is more than acceptable for routine analysis.
Afterward, model samples of different microplastics in soil at different known concentration were analyzed with all three spectrometers. Chemometric models capable to identify and classify microplastics in soil were established. For this analysis five of the most used plastics worldwide were used: polyethylene (PE), polyethylene terephthalate (PET), polypropylene (PP), polystyrene (PS), and polyvinyl chloride (PVC). After the Principal component analysis (PCA), it can be seen that only the NIR-One NM2.0 is capable to differentiate all types of microplastics in soil at concentrations of 1–2 %, while the NeoSpectra Si-ware is unable to identify the PET sample.
Engineering Modelling
(2019)
This chapter presents the most commonly used approach to analyse the
thermo-mechanical behaviour of concrete structures subjected to high temperatures as in the case of fire loading. Prescriptions of the Eurocode are detailed for the thermal as well as the mechanical analysis. Finally, recommendations from two national (Austrian and German) guidelines give some improvements for Underground infrastructure.
Advanced Modelling
(2019)
Halomonas elongata is a halophilic γ-proteobacterium that synthesizes and accumulates the compatible solute ectoine to cope with osmotic stress in saline environments. Ectoine possesses protecting properties and stabilizes proteins as well as whole cells against stresses like ionizing radiation and cytotoxins. These properties make ectoine a highly demanded ingredient in cosmetics and pharmaceuticals. To date H. elongata is the industrial Producer strain of ectoine, but several metabolic factors for optimum ectoine production remain to be explored.
In this work, we used up to date Metabolic engineering approaches following the ‘Push, Pull, Block – strategy’ to examine targets that contribute to ectoine synthesis. Firstly, the basics of glucose catabolism were inspected to PUSH and enhance carbon flow towards ectoine synthesis. Secondly, lysine biosynthesis was targeted to BLOCK a pathway that is competing for precursors with ectoine synthesis. Thirdly, the mechanosensitive (MS) channels of H. elongata have been examined as possible excretion routes for ectoine. An overexpression of the ectoine excretion channels potentially could PULL out product at the end of ectoine synthesis and increase overall ectoine flux. For the interrogation of central metabolic pathways, we established the new molecular tool CRISPR-mediated interference (CRISPRi) for targeted modulation of gene expression.
PUSH Glucose catabolism through the Entner-Doudoroff (ED) and Emden-Meyerhof-Parnas (EMP) pathway was targeted with CRISPRi and examined on gene expression level for ist response to changing salinity and different carbon sources. Changing salinity did not influence gene expression levels of glucose catabolism but the carbon source glucose triggered glycolysis through the (ED) pathway. When gene expression of the ED pathway was downregulated with CRISPRi, the growth rates remained constant. The observations indicate a metabolic overflow mechanism for glycolysis, in which fluxes are constantly high - even at lower salinity when no resources are demanded for ectoine synthesis. The further analysis of glucose to product conversion rates will advise optimum conditions for future industrial cultivation processes.
BLOCK Lysine biosynthesis was downregulated with CRISPRi, which led to a significant increase in ectoine production. Hence, the blockage of lysine biosynthesis would be a valuable strategy for the optimization of the industrial producer strain in future studies.
PULL MS channels and ectoine regulation are inevitably connected in osmoadaptation. Therefore, ectoine excretion, growth performance and gene expression levels of the MS channels were monitored in steady state conditions and in response to osmotic shock in the wildtype strain and in a MS channel deletion mutant. We observed that the MS channels were essential for the survival of osmotic shock but surprisingly their presence reduced cell growth under high salinity. The MS channels were only partially responsible for ectoine excretion.
Thus, alternative ectoine excretion channels must exist and remain to be explored.
Most knowledge about the structure, function, and evolution of early compound eyes is based on investigations in trilobites. However, these studies dealt mainly with the cuticular lenses and little was known about internal anatomy. Only recently some data on crystalline cones and retinula cells were reported for a Cambrian trilobite species. Here, we describe internal eye structures of two other trilobite genera. The Ordovician Asaphus sp. reveals preserved crystalline cones situated underneath the cuticular lenses. The same is true for the Devonian species Archegonus (Waribole) warsteinensis, which in addition shows the fine structure of the rhabdom in the retinula cells. These results suggest that an apposition eye with a crystalline cone is ancestral for Trilobita. The overall similarity of trilobite eyes to those of myriapods, crustaceans, and hexapods corroborates views of a phylogenetic position of trilobites in the stem lineage of Mandibulata.
Although concrete itself is not a combustible material, concrete mixtures with high density, such has high-performance concretes (HPCs), are susceptible to significant damage during fires due to explosive spalling. Past research has shown that the inclusion ofpolymer fibres in high density concrete can significantly mitigate this fire damage. The exact mechanisms causing this increased spalling resistance are not yet fully understood, but it is thought that the fibres facilitate moisture transport during fire exposure, which in turn contributes to relief of internal stresses in the spalling-susceptible region. In this study, X-ray Computed Tomography (CT) was applied to observe the interaction between polymer fibres and cracking during thermal exposure. For this purpose, two concrete samples containing different polymer fibre types were subjected to incremental application of a defined thermal exposure. CT images were acquired before and after each thermal exposure and powerful image processing tools were used to segment the various material components. This enabled a detailed analysis of crack formation and propagation as well as the visualization and quantification of polymer fibre characteristics within the concrete. The results demonstrated that the orientation of both fibres and cracks in polymerfibre reinforced concrete tend to be anisotropic. The results also indicated that crack geometry characteristics may be correlated with fibre orientation, with cracks tending to run parallel to fibre beds. Clear quantitative relationships were also observed between heating and increasing cracking levels, expressed in terms of both crack surface area and crack volume.
In this paper we report on the characterization by X-ray computed tomography of calcium phosphate (CaP) and polycaprolactone (PCL) coatings on Ti-6Al-4V alloy scaffolds used as a material for medical implants. The cylindrical scaffold has greater porosity of the inner part than the external part, thus, mimicking trabecular and cortical bone, respectively. The prismatic scaffolds have uniform porosity. Surface of the scaffolds was modified with calcium phosphate (CaP) and polycaprolactone (PCL) by dip-coating to improve biocompatibility and mechanical properties. Computed tomography performed with X-ray and synchrotron radiation revealed the defects of structure and morphology of CaP and PCL coatings showing small platelet-like and spider-web-like structures, respectively.
The risk analysis of road tunnels faces a growing complexity in fire scenarios, e.g. caused by new energy carriers. Essentially, such complex scenarios involve many interactions between the tunnel users, the fire source and the safety measures. One example is the alarm of tunnel users either initiated by the perception of smoke or by the fire alarm system. To consider these interactions for the quantification of consequences, e.g. fatalities, risk analysis requires a complex model. However, the complex model can compute in practice only few discrete scenarios due to its high computational cost, whereas risk analysis generally needs the consequences of a high number of random scenarios. Metamodels can solve this contradiction. They are able to approximate the consequences of many random scenarios with low computational cost based on the consequences of few discrete scenarios computed with the complex model. The efficiency of metamodels depends on the required number of these discrete scenarios. In this sense, this dissertation proposes an efficient metamodel within an innovative methodology for risk analysis of road tunnels to allow to consider an increased complexity of scenarios. This metamodel applies the following methods or models: the projection array-based design method specifies the experimental design for the discrete scenarios; the combination of the fire model FDS and the microscopic evacuation model FDS+Evac constitutes the complex model; and moving least squares produces the response surface model. The response surface model approximates the consequences of the random scenarios and therewith introduces an uncertainty, called metamodel uncertainty, which is quantified with the prediction interval method. Additionally, stochastic individual characteristics of tunnel users in discrete scenarios computed with FDS+Evac attribute evacuation uncertainties to the consequences. An original development in this dissertation, the ’direct approach’, directly transfers the evacuation uncertainties of the discrete scenarios to any random scenario. The evaluation of the metamodel in this dissertation shows following results. Firstly, the response surface model sufficiently represents the consequences of the complex model. Secondly, the metamodel uncertainty is also essential for this representation, but the prediction interval method reveals a drawback in the risk analysis. Potential approaches to deal with this drawback are discussed. Finally, the direct approach reproduces the evacuation uncertainty of the complex model which then clearly affects the consequences of random scenarios. Therefore, the consideration of the evacuation uncertainty plays an important role for the risk analysis. Furthermore, the projection array-based design method was adapted in this dissertation with two approaches, namely the combination of the experimental designs for FDS and FDS+Evac as well as their sequential refinement. Both approaches contribute to the efficiency of the metamodel. These results lead to following conclusions. Firstly, the metamodel efficiently integrates the consequences of discrete scenarios into risk analysis and thus allows to consider an increased complexity. Secondly, the metamodel is an advancement for risk analysis not only for road tunnelsbutalsomoregeneralinfiresafetyengineering. Forthesetworeasons,themetamodel might be interesting for other methodologies for risk analysis. In addition, the metamodel is generic and is therefore widely applicable on other issues beside from risk analysis, e.g. to assess the safety of structures related to time-consuming experiments depending on multiple variables.
The simulation of the structural response for impact scenarios strongly requires an accurate simulation of both the impact event as well as the subsequent wave propagation. The numerical modeling of the impact event is intrinsically ill-posed due to the instantaneous changes of velocities in the contact area, leading to unbounded accelerations for decreasing time steps which causes oscillations in the contact stresses. These oscillations then propagate into the bulk material. Using a rate dependent material model, like concrete, they might lead to significant errors and a wrong prediction of the structural response. A regularization is thus required to avoid oscillations in the contact stresses. Another issue is related to the numerical computation of the contact conditions. In impact simulations, the nonlinear contact computation needs to be evaluated in every time step. A segmentation technique of the contact area is accurate but time consuming and may result in a bottleneck for the simulation and implementation, especially for 3D problems. The modeling of the subsequent wave propagation requires small time steps, which is primarily due to accuracy reasons. Implicit schemes are thus not affordable. Explicit time integration schemes are efficient only for diagonal mass matrices, as in this case no solution of a linear system is required. In this work, a coupled finite element - Non-Uniform Rational B-Spline (FE-NURBS) approach is applied to impact problems. The coupled approach uses an intermediate NURBS layer to compute the contact forces between the contacting bodies discretized by FEs. The advantages of a smooth isogeometric contact formulation are used to compute the contact forces. A segmentation of the contact area is avoided and an efficient element-based integration is used. The impact event is regularized using a mesh dependent nonlinear penalty approach. The penalty function is a polynomial which ensures a smooth transition between the noncontact and the contact state during the impact. For finer meshes, the penalty regularization becomes stiffer while still avoiding artificial oscillations in the contact stresses. Efficient higher order space and time discretizations are used to model the wave propagation. Explicit time integration is combined with higher order spectral element spatial discretization.
The full-notch creep test (FNCT) is a common method to evaluate the environmental stress cracking (ESC) behavior of high-density polyethylene (PE-HD) container materials . The test procedure as specified in ISO 16770 provides a comparative measure of the resistance against ESC using the time to failure of specimens mechanically loaded in a well-defined liquid environment. Since the craze-crack damage mechanism underlying the ESC process is associated with brittle failure, the occurrence of globally brittle fracture surfaces is a prerequisite to consider an FNCT measurement as representative for ESC . Therefore, an optical evaluation of FNCT fracture surfaces concerning their brittleness is essential. Due to the experimental setup, an inevitable increase of the true mechanical stress and the associated appearance of small ductile parts on fracture surfaces is induced in any case. Hence, an FNCT experiment is considered as 'valid', if the corresponding fracture surface is predominantly brittle . Based on laser scanning microscopy (LSM) height data of FNCT fracture surfaces , a universal and easy-to-use phenomenological criterion was developed to assess the validity of distinct FNCT experiments. This criterion is supposed to facilitate a quick evaluation of FNCT results in practical routine testing.
During their lifetime, polymer components subjected to mechanical loads and environmental influences show a loss of their mechanical properties required for their specific applications. In this respect, the craze-crack damage mechanism slow crack growth (SCG) is relevant for PE-HD components used in high-performance applications such as pipes and containers for the storage and transport of dangerous goods. SCG is considered to be the major failure mechanism in polyolefins and it typically occurs suddenly and unexpectedly. Due to the fields of application, SCG is a safety relevant issue. To test for the resistance of PE-HD pipe and container materials against SCG, the full-notch creep test (FNCT) is widely applied in Europe. In this study, SCG phenomena in PE-HD are investigated in detail based on an improved FNCT, especially including the consideration of the influence of environmental liquids effecting the damage mechanism. Using an enhanced fracture surface and a crack propagation analysis with imaging techniques such as light microscopy (LM), laser scanning microscopy (LSM), X-ray computed tomography (CT-scan) and scanning electron microscopy (SEM), detailed data concerning SCG are obtained.
The combined application of FNCT and such imaging techniques is explicitly advantageous and recommended to gain important information on damage occurring to PE-HD induced by mechanical stress and the influence of environmental liquids, which is essential within the Fourth Industry Revolution.
The separation of two closely spaced defects in fields of Thermographic NDE is very challenging. The diffusive nature of thermal waves leads to a fundamental limitation in spatial resolution. Therefore, super resolution image reconstruction can be used. A new concerted ansatz based on spatially structured heating and joint sparsity of the signal ensemble allows for an improved reconstruction of closely spaced defects. This new technique has been studied using a 1D laser array with randomly chosen illumination pattern.
This paper presents the results after applying super resolution algorithms, such as the iterative joint sparsity (IJOSP) algorithm, to our processed measurement data. Different data processing techniques before applying the IJOSP algorithm as well as the influence of regularization parameters in the data processing techniques are discussed. Moreover, the degradation of super resolution reconstruction goodness by the choice of experimental parameters such as laser line width or number of measurements is shown.
The application of the super resolution results in a spatial resolution enhancement of approximately a factor of four which leads to a better separation of two closely spaced defects.
Alkali and alkaline earth chlorides are discussed as heat storage media and are characterized by their low price and high availability. Disadvantages are a high corrosion rate and formation of Cr6+ ions in the melt, as observed in various binary chlorine salt melts. In our work the system NaCl-KCl-MgCl2 is considered. The storage capacity in this salt system is between 2 and 3 MWh per 10 t salt, depending on composition, melting temperature and working temperature. At the same time the system offers a eutectic line, which allows a high variance of the composition and possibly different corrosion rates can be observed. Corrosion tests in melts were carried out and the corrosion layers investigated. The tests with chloride melts on 12% Cr steel show an inner corrosion zone of up to 40 µm depth after 96 hours. The corrosion mechanisms and potential solutions are discussed.
Fatigue safety verification of existing bridges that uses ‘‘re-calculation’’ based on codes, usually results in insufficient fatigue safety, triggering invasive interventions. Instead of “re-calculation”, Structural Health Monitoring (SHM) should be used for the assessment of the existing bridges. Monitoring systems provide data that can reduce uncertainties associated with the fatigue loading process and the structural resistance. The objective of this paper is to quantify the value of the SHM system implemented in a 60-years-old road viaduct to investigate its fatigue safety, through modeling of the fundamental decisions of performing monitoring in conjunction with its expected utility. The quantification of the conditional value of information is based on the decision tree analysis that considers the structural reliability, various decision scenarios as well as the cost-benefit assessments. This leads to a quantitative decision basis for the owner about how much time and money can be saved while the viaduct fulfills its function reliably and respects the safety requirements. The originality of this paper stands in the application of the value of information theory to an existing viaduct considering the fatigue failure of the system based on the monitoring data and the cost-benefit of monitoring method.
This file contains all the data used for the figures shown in the Dissertation of Ruben Gerrits with the title "An experimental study of fungal olivine weathering".
In this study, the weathering-affecting, rock-inhabiting fungus, Knufia petricola A95 and the Fe-bearing olivine (Fe0.2Mg1.8SiO4) were selected to investigate fungi-induced effects on mineral dissolution. The availability of a melanin-deficient mutant (ΔKppks) of K. petricola A95, that produced more extracellular polymeric substances (EPS) than the wild type (WT), enabled comparative studies of the role of melanin and EPS in weathering processes.
Compared with the original time-temperature superposition (TTS) principle, an extended non-linear time-temperature equivalent (TTE) principle is suggested in this work. Results shown us, all application of TTS and most of the TTE parameters, for example, the Orr-Sherby-Dorn, Manson-Succop, Larson-Müller, Manson-Haferd, Mendelson-Roberts-Manson parameters and the more general ‘single metamodel’ from Haque–Stewart are special cases of the new suggested principle. The merits of this new method are discussed.