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Eingeladener Vortrag
- nein (1102)
Separation and detection of antioxidants using a graphene based electrochemical sensor platform
(2019)
CVD-Graphene is ideally suited as an active element for electrical and electrochemical sensing platforms, since it provides for high sensitivity and low detection limit. Electrochemical sensors provide a simple way to measure analytes in fluids with high sensitivity without the need for complex instrumentation. Due to These aspects, graphene sensors are interesting for a wide range of applications in bio analytics. Antioxidants are natural or synthetic compounds, which inhibit oxidation processes and hence often find use as preservatives.
It has been suggested that the long-term consumption of diets rich in antioxidants is associated with a lower risk of developing diseases linked to oxidative stress. Gallic acid and ascorbic acid are representatives of antioxidants. We have developed a graphene-based sensor platform to separate and subsequently detect antioxidants. Graphene exhibits low detection limits for ascorbic acid and polyphenols. In this study, the sensing of gallic acid and ascorbic acid on bare CVD graphene in various solvents was investigated by Square Wave Voltammetry. Furthermore, the separation and detection of the bioanalytes by deploying different membranes were evaluated.
Background. Aflatoxin B1 (AFB1) is a toxic low-molecular-weight secondary fungal metabolite produced mainly by Aspergillus flavus and Aspergillus parasiticus not only at pre-harvest time but also at post-harvest stages including storage. AFB1 was classified as a Group I carcinogen by the World Health Organization for Research on Cancer in 1993. AFB1 is able to naturally contaminate medicinal plants and therefore causing serious health issues for humans consuming the related medicine. This study aimed to develop an efficient fluorescence polarization immunoassay (FPIA) and for the first time a rapid (5-10 min), low-cost, and simple membrane-based flow-through immunoassay (MBA) for determination of AFB1 in medical herbs based on a monoclonal antibody.
Methods. Two different techniques for AFB1detection in medical herbs (Herba Orígani vulgáris, Folia Urticae, Fructus Rubi idaei) were developed and compared, namely an easy-to-use semi-quantitative flow-through membrane-based enzyme immunoassay (MBA), and a homogeneous method which needs no separation or washing steps (assay time 10 min), a quantitative fluorescence polarization immunoassay (FPIA).
Results. A cut-off level of the developed MBA can vary wide from 0.8 ppb to 1 ppb. The FPIA method showed a linear working range of 8.6 ppb to 64 ppb, IC50 of FPIA is 24 ppb. The results were in good correlation with the ELISA results (IC50 = 0.1 ppb). LC–MS/MS was used to confirm the results, too.
Conclusion. MBA can be used for a quick on-site AFB1 detection in medical herbs (Herba Orígani vulgáris (Oríganum vulgáre), Folia Urticae (Urtíca dióica), Fructus Rubi idaei (Rúbus idáeus)), the developed test does not require special equipment and is not time-consuming (5-10min), includes several simple steps and can be performed directly on-site. The major advantages of the developed FPIA are its simplicity and suitability for a rapid screening of a large number of samples.
The combination of tomographic, microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on material and component properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. This logic thread equally holds for industrial and academic research and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated.
I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of damage evolution and microstructural properties, as well as for non-destructive testing. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
Additionally, I will show how Neutron Diffraction, which is extremely well suited to the study of internal stresses, both residual and under external load, can well be coupled to the microstructural framework gained by CT, allowing understanding the microstructure-property relationships in materials.
Finally, I will show that BAM is very active in standardization and certification, including production of Reference Materials and Methods.
The combination of tomographic, microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on material and component properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. This logic thread equally holds for industrial and academic research and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated.
I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of damage evolution and microstructural properties, as well as for non-destructive testing. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
Additionally, I will show how Neutron Diffraction, which is extremely well suited to the study of internal stresses, both residual and under external load, can well be coupled to the microstructural framework gained by CT, allowing understanding the microstructure-property relationships in materials.
Kaltrissprüfung hochfester Feinkornbaustähle beim Schweißen mit modifiziertem Sprühlichtbogen
(2019)
Sind in Stahlkonstruktionen hohe Tragfähigkeiten bei geringem Eigengewicht gefordert, finden hochfeste Feinkornbaustähle mit Streckgrenzen ≥ 960 MPa Anwendung. In der Vergangenheit wurde der konventionelle Übergangslichtbogen (Konv. LB) zur schweißtechnischen Fertigung von hochfesten Stählen eingesetzt. In den letzten Jahren wurde der modifizierte Sprühlichtbogen (Mod. SLB) entwickelt, welcher reduzierte Nahtöffnungswinkel bei erhöhter Abschmelzleistung ermöglicht. Jedoch treten höhere Wasserstoffkonzentrationen verbunden mit Mikro-(Kalt-)rissen unter reduziertem Nahtöffnungswinkel mit Mod. SLB auf. In diesem Beitrag wird die Kaltrissempfindlichkeit des hochfesten Feinkornbaustahles S960QL mit artgleichem Schweißzusatzwerkstoff untersucht.
Es besteht die grundsätzliche Anforderung, dass alle nichtmetallischen und metallischen Materialien nur dann in Sauerstoffanwendungen eingesetzt werden dürfen, wenn sie sicherheitstechnisch auch für die entsprechenden Betriebsbedingungen geeignet sind. Der Vortrag stellt nicht nur die gängigen Prüfverfahren und Beurteilungskriterien. Es werden auch die folgenden Fragen beantwortet, die häufig von Wirtschaftsunternehmen und Verbänden gestellt werden:
- Welchen praktischen Anwendungsfall bilden die Prüfungen ab?
- Welche Untersuchungsmethoden führt die BAM durch?
- Warum verwendet die BAM ergänzende Beurteilungskriterien bei der sicherheitstechnischen Interpretation von Prüfergebnissen?
- Warum empfiehlt die BAM chargenbezogene Materialprüfungen?
- Worin unterscheiden sich die zwei von der BAM verwendeten Methoden zur Beurteilung der Ausbrennsicherheit von Armaturen und Anlagenteilen und welche Vor- und Nachteile bietet jede dieser Methoden?
Grundsätzlich dürfen alle nichtmetallischen und metallischen Materialien nur dann in Sauerstoffanwendungen eingesetzt werden, wenn sie sicherheitstechnisch für die Betriebsbedingungen geeignet sind. Neben allgemeinen Sauerstoff-spezifischen Anforderungen stellt der Vortrag die standardisierten Prüfverfahren und die Untersuchungsmöglichkeiten der BAM vor. Die Beurteilungskriterien für die Prüfverfahren werden kritisch betrachtet und es wird erklärt, in welchen Fällen und aus welchen Gründen die BAM ergänzende Beurteilungskriterien verwendet. Um den tatsächlichen, praktischen Anwendungsfall abzubilden, ist unter gewissen Umständen die Anpassung des Prüfumfangs möglich. Außerdem wird dargestellt, warum die BAM chargenbezogene Materialprüfungen empfiehlt.
Auch Sauerstoff- Armaturen und Anlagenteile müssen sicherheitstechnisch für die Betriebsbedingungen geeignet sein. Zur Beurteilung der Ausbrennsicherheit werden die zwei an der BAM praktizierten Vorgehensweisen mit ihren jeweiligen Vor- und Nachteilen vorgestellt: Untersuchung der Armatur als komplette Funktionseinheit bzw. Beurteilung der Armatur auf Basis der Untersuchungen der eingesetzten Materialien. Neben den Anforderungen aus produktspezifischen Normen wird auch für diesen Fall kurz erklärt, in welchen Fällen und aus welchen Gründen die BAM ergänzende Beurteilungskriterien verwendet bzw. den Prüfumfang anwendungsfallbezogen anpasst.
Kaltrissprüfung hochfester Feinkornbaustähle beim Schweißen mit modifiziertem Sprühlichtbogen
(2019)
Der konstruktive Leichtbau erfordert den zunehmenden Einsatz hochfester Feinkornbaustähle mit Streckgrenzen bis zu 1300 MPa. Um darüber hinaus Schweißzeit, Schweißnahtvolumina und Schweißkosten zu minimieren, kam es zur Entwicklung moderner Lichtbogenprozesse mit erhöhter Abschmelzleistung, wie bspw. dem modifizierten Sprühlichtbogen (mod. SLB). Dieser Beitrag zeigt Kaltrissuntersuchungen beim Einsatz des mod. SLB unter reduziertem Nahtöffnungswinkel eines Hochfesten S960QL. Mit Hilfe des fremdbeanspruchten Implant-Tests konnte dargelegt werden, dass durch die erhöhte Abschmelzleistung ein tieferes Einbrandprofil entsteht und es dadurch zu einer zeitverzögerten Rissbildung kommt. Ergebnisse des selbstbeanspruchenden TEKKEN-Tests zeigen eine deutliche Rissbildung im Schweißgut unter reduziertem Nahtöffnungswinkel. Durch eine Nachwärmung unmittelbar nach dem Schweißen kann diese Rissbildung minimiert werden.
Force-distance curves have been recorded on thin films of lubricants. The lubricants wet the AFM tip, which causes a capillary force. This force depends on the shape of the tip, as well as on physical properties like viscosity and surface tension, which have been determined additionally with other methods. This way, their influence on the shape of the curves could be analyzed.
Photothermal radiometry with an infrared camera allows the contactless temperature measurement of multiple surface pixels simultaneously. A short light pulse heats the sample. The heat propagates through the sample by diffusion and the corresponding temperature increase is measured at the samples surface by an infrared camera. The main drawback in radiometric imaging is the loss of the spatial resolution with increasing depth due to heat diffusion, which results in blurred images for deeper lying structures. We circumvent this information loss due to the diffusion process by using blind structured illumination, combined with a non-linear joint sparsity reconstruction algorithm.
Der Vortrag zeigt aktuelle Entwicklungen und Betätigungsfelder des Fachbereichs Prozessanalytik zum Thema Automation in der Analytik. Dies Umfasst die Laborautomation am Beispiel der Probenpräparation für die Röntgenfluoreszenzanalyse und moderne Synthesekonzepte in der organischen Chemie. Außerdem wird die Rolle der Prozessanalytik in der kontinuierlichen Produktion thematisier. Als Anschauungsgegenstand dienen die Überwachung einer Hydroformylierung mittels Raman- und NMR-Spektroskopie und der Einsatz eines NMR-Sensors in einer modularen Produktionsanlage im Pilotmaßstab.
At BAM, which is a federal institute for materials research and testing in Germany, it is one of our tasks to evaluate the safety of casks designed for transport and/or storage of radioactive material. This includes assessment of elastomeric seals applied in the casks. One of the aims is to identify a suitable method for estimating the service lifetime of the seals with regard to the requirements for long-term safety (40 years and more) of the containers. Therefore, we started an accelerated ageing programme with selected rubbers often used for seals (HNBR, EPDM and FKM) which are aged at four different temperatures (75 °C, 100 °C, 125 °C and 150 °C) for up to five years. In order to assess sealability, O-rings were aged in compression by 25 % (corresponding to the compression during service) between plates as well as in flanges that allow leakage rate measurements. For comparison, uncompressed O-rings were aged as well. In order to understand the underlying ageing mechanisms in each material, material properties such as hardness, density and tensile properties were examined. Additionally, compression set (CS), which represents the recovery behaviour of a seal after release from compression, is measured. For obtaining results closely related to practical conditions, O-rings with a full-scale cord diameter of 10 mm were aged. However, this set-up can lead to heterogeneous ageing caused by diffusion-limited oxidation (DLO) effects especially for HNBR, resulting in distorted bulk properties such as compression set. However, if DLO-affected data is excluded, extrapolations of CS data are possible using time-temperature shifts.
For selecting an appropriate end-of-lifetime criterion, leakage rate measurements were performed, since leakage rate is the only characteristic directly correlated to the performance of the sealing system. A significant increase in leakage rate was considered as the end of the lifetime. However, the O-rings remained leak tight under static conditions even though material properties had already degraded strongly. For this reason, a modified, more demanding leakage test involving a fast small decompression of the seal was developed that allowed determining a more conservative end-of-lifetime criterion with a safety margin for EPDM seals. FKM, which is a very heat and oxidation resistant material, exhibited only little degradation, even though it had the smallest activation energy.
Seit dem 1. Januar 2019 müssen Hersteller alle ihre energieverbrauchrelevanten Produkte in der Europäischen Produktdatenbank für die Energieverbrauchskennzeichnung EPREL registrieren, bevor sie auf dem EU-Markt verkauft werden können. Nutzung, Aufbau und Admin-Struktur der Datenbank werden vorgestellt.
At the Stakeholder meeting of the EMPIR project “Multifunctional ultrafast microprobes for on-the-machine measurements”, details about two measurement modes were presented. Force distance curves and contact resonance measurements are compared. The basic principles are explained and exemplary measurements concerning mechanical properties of polymers are shown.
The motivation and the measurement setup for large fast-scanning piezoresistive cantilevers are presented. The theory behind the measurements of mechanical properties through contact resonance is explained. Results of such measurements on two kinds of polymer are compared to results from force distance curves. Noise, time-dependency and dependency of the results on the vibration mode are identified as challenges of contact resonance.
The geometry of the melt pool in laser beam welding plays a major role to understand the dynamics of the melt and its solidification behavior. In this study, a butt configuration of 20 mm thick structural steel and transparent quartz glass was used to observe the weld pool geometry in the partial penetration mode by means of a high-speed camera. The observations show that the dimensions of the weld pool vary depending on the depth. The areas close to the weld pool surface take a teardrop-shape. A bulge-region and its temporal evolution were observed approximately in the weld pool root. Additionally, a 3D transient thermal-fluid numerical simulation was performed to obtain the weld pool shape and to understand the formation mechanism of the observed bulging effect. The model considers the local temperature field, the effects of phase transition, thermo-capillary convection, natural convection and temperature-dependent material properties. The numerical results showed good accordance and were furthermore used to improve the understanding of the experimentally observed bulging effect.
High heat input leads to grain coarsening and softening in WM and HAZ; the tensile strength is reduced. Low heat input leads to inadmissible hardening in the WM; the impact strength is reduced.
The proposed t8/5-time of 3 s to 15 s could be achieved through the reduced welding velocity.
The concept of electromagnetic weld pool support system allowed single-pass welds in flat position without gravity drop-outs even for reduced welding speeds; in this way the heat input can be controlled.
The adaptation of the electromagnetic weld pool support system to laser and laser hybrid welding process can dramatically increase the potential field of application of these technologies for real industrial implementation.
Schwerpunkte:
Strategie zur Vermeidung von Schweißimperfektionen im Überlappbereich beilaserhybridgeschweißten Rundnähten für 9.5 mm dicke Rohre.
Anpassung der Laserleistung in Kombination mit der Defokussierung des
Laserstrahls sowie einer Endkraterfüllung am Ende der Schweißnaht führte zu einer besseren Nahtausbildung.
Herausrampung der Energie des Schweißprozesses, sodass ein Übergang von Durchschweißung zu einer Einschweißung mit gewünschter kelchförmiger Nahtgeometrie stattfand.
Einstellung eines Wärmestaus durch Defokussierung und Verschiebung des
Laserstrahls führt zu einem gut ausgebildeten Überlappbereich ohne Poren, Risse.
Schweißungen an Rohrabschnitten mit einer max. Wandstärke von 15 mm, bei gegebenenfalls weiteren Parameteranpassungen.
Advances and Applications of Molecular Absorption Spectrometry: from Non-Metals to Isotope Analysis
(2019)
The present work covers two main aspects of high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS), an analytical technique for elemental trace analysis.
First, a comprehensive mechanistic study of molecule formation in graphite furnaces is presented, which is a key step into the recovery of analytical signals. For this, the molecule formation of CaF was studied, which is used for the indirect analytical determination of fluorine in HR-CS-GFMAS. A zirconium coating catalyzes the CaF formation, and its structure was investigated. The kinetics of this reaction was established by monitoring its molecular spectrum at different atomisation temperatures. An Arrhenius plot showed a pseudo-first order reaction with respect to fluorine (n = 1). An intermediate state was isolated, and its structure was elucidated by spectroscopic methods: scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XANES and EXAFS), and Raman microspectroscopy. Here a mechanism is proposed, where ZrO2 works as a heterogeneous catalyst: after a pyrolytic step, an intermediate state of ZrO(OCaF) is activated, and at higher temperatures, CaF(g) is released from the zirconium-coated graphite surface.
Second, analytical methods were developed by using HR-CS-MAS as detector for non-metals and isotope analysis. Therefore, the determination of organic absorbable chlorine in water, the quantification of fluorine in consume care products with declared perfluorinated ingredients, and the determination of sulfur content in crude oils were investigated. Finally, the high resolution of the instrumentation allows to measure isotopic shifts with high precision in some observed molecular spectra. Consequently, the molecular spectra of enriched isotopes of boron and magnesium were investigated, establishing so the potential of HR-CS-MAS for the accurate and precise determination of isotopic amount ratios.
Zusammenfassung
Die vorliegende Arbeit befasst sich mit zwei zentralen Aspekten der High-Resolution-Continuum-Source-Molekülabsorptionsspektrometrie mit Graphitrohrtechnik (HR-CS-GFMAS), einer Analysetechnik für elementare Spurenanalyse.
Der erste Teil der Arbeit umfasst eine mechanistische Studie zur Molekülbildung auf Graphitoberflächen. Dies ist ein wichtiger Schritt, um analytische Signale zu entdecken. Dazu wurde die Molekülbildung von CaF analysiert, welches für die indirekte, analytische Bestimmung von Fluor in HR-CS-GFMAS genutzt wird. Die CaF Bildung wurde mittels einer Beschichtung aus Zirconium katalysiert und deren Struktur analysiert. Die Kinetik dieser Reaktion wurde durch Beobachtung des jeweiligen Molekülspektrums bei verschiedenen Atomisierungstemperaturen beobachtet. Ein Arrheniusplot zeigte für Fluor (n = 1) eine Reaktion Pseudo-erster Ordnung. Ein Übergangszustand wurde über die mit Zirconium überzogene Grafitoberfläche isoliert und seine Struktur mittels spektroskopischer Methoden Energiedispersive Rasterelektronenmikroskopie / Röntgenspektroskopie (REM-EDX), Röntgenphoto¬elektronenspektroskopie (XPS), Röntgenabsorptionsspektroskopie (XAS) und Raman Spektroskopie untersucht. Auf Grundlage dieser Ergebnisse wird ein Mechanismus vorgeschlagen, bei dem ZrO2 als heterogener Katalysator fungiert; in Folge einer Pyrolysestufe wird ein Übergangszustand des ZrO(OCaF) aktiviert, welcher bei höheren Temperaturen CaF(g) an der Zirconium-Graphitoberfläche freisetzt.
Im zweiten Teil der Arbeit werden Analysemethoden entwickelt, in dem HR-CS-MAS als Detektor für Nichtmetalle und Isotopanalyse angewandt wird. Hierfür wurde organisch gebundenes Chlor im Wasser bestimmt, der Fluorgehalt in Pflegeprodukten mit perfluorierten Inhaltsstoffen quantifiziert und der Schwefelgehalt in Erdöl untersucht. Weiterhin ermöglicht die hohe Auflösung der Messgeräte eine präzise Bestimmung der Isotopenverschiebung einiger untersuchter Molekülspektren. Daher wurden die Molekülspektren angereicherter Bor- und Magnesiumisotope untersucht. Auf diese Weise wurde das Potential von HR-CS-MAS für die akkurate und präzise Bestimmung von Isotop-Mengenverhältnissen nachgewiesen.
Magnesium is a major element in the hydrosphere and biosphere, and it is direct correlated with the carbon cycle. Therefore, the study of its isotopic fractionation in sediments and sea water helps to understand the earth’s climate and global warming. Mg has three stable isotopes, 24Mg, 25Mg and 26Mg, and traditionally isotope amount ratios are measured by mass spectrometric methods. Their drawbacks include the high costs for instruments and their operation, experienced operators and elaborate time-consuming chromatographic sample preparation. Recently, an optical spectrometric method has been proposed as faster and low-cost alternative for the analysis of isotope ratios: high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS).
For the determination of Mg isotope ratios in selected rock reference materials, the high-resolution molecular absorption spectrum of in-situ generated MgF molecule was studied applying multivariate analysis and the results compared with MC-ICP-MS. Samples were dissolved by acid digestion and Mg isotopes analyzed with and without matrix extraction. The absorption spectra were recorded for MgF for the electronic transition X 2Σ → B 2Σ+. The MgF spectrum is described as the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF. The isotope analysis was done by deconvolution of the MgF spectrum by partial least square regression (PLS). A PLS model was built and calibrated with enriched isotope spikes and certified reference materials. Spectra data was preprocessed by a derivate of second order and venetian blinds cross-validation was employed for finding the optimum latent variables. Finally, the model was refined by a genetic algorithm which identified the best subset of variables for a precise and accurate regression. Results are compatible with those obtained by MC-ICP-MS with an accuracy of ± 0.3‰ with uncertainties ranging between 0.02 to 0.6‰. This accuracy and precision discriminate the isotope fractionation in geological samples, and it is suitable for earth’s climate studies.
Residual stresses are crucial when assessing the performance of welded components. The present work deals with the possibilities of transferring the real-life boundary conditions of welding, which influence the residual stress, into the laboratory. The possibilities of a test system with a load capacity of 2 MN specifically developed for online monitoring of stress formation and cracking are shown. Due to the structural design, global process, geometry and material-dependent stresses are induced, which can be quantified in-situ during welding and post weld heat treatment. Examples are presented how the conditions to be found during production are simulated in the laboratory. It is shown how welding residual stresses in high-strength steels are affected by the heat control. Elevated working temperatures significantly increase the tensile residual stresses in the heat affected zone (HAZ). The effect of mechanical stresses resulting from welding on stress relief cracking is demonstrated by the example of a creep resistant steel. Reheat cracks were monitored online during post weld heat treatment.
Is it a parmesan cheese from Italy? Who painted the Mona Lisa? The determination of the place of origin is essential for consumer protection, detection of falsifications, and also to bring justice.
All the tangible possess an isotopic fingerprint. However, current technologies are too expensive. We work on the development of fast and low-cost optical instruments and methods for isotope analysis.
Microstructure ageing of stainless steel AISI 316L manufactured by selective laser melting (SLM)
(2019)
Additive manufacturing (AM) processes, such as SLM, offer a variety of advantages compared to conventional manufacturing. Today AM parts are still comparatively less cost-effective if they are manufactured in large quantities. To make the AM parts more cost-efficient, the AM process has to be improved. It requires a good understanding of microstructure formation, microstructure-property-relations and ageing processes affected by different loads.
In this work the ageing behavior of SLM manufactured AISI 316L stainless steel is evaluated. The microstructure effected by mechanical, thermal and corrosive loads are investigated and compared to as-built microstructure. Tensile tests are used for mechanical ageing. For thermal and corrosive loads the typical application conditions of 316L apply. The methods of microstructure investigation include SEM, TEM, CT and EBSD. The main object of this work is the description of microstructure and ageing processes of AM parts.
Simultaneous multielemental analysis of crude oils by high-resolutions absorption spectrometry
(2019)
When crude oil arrives at a refinery it needs a lot of processing before it is suitable for cracking into lighter fractions. Sulfur has to be extracted to meet ultra-low sulfur legislation for most of the fuel grades, and desalination is a crucial process as chlorine within salts is corrosive to refinery equipment. Measuring the amounts of sulfur and chlorine within crude oil is the first step in a complex clean-up process.
Heavy metals, such as vanadium, nickel and iron need to be removed too. These metals can poison the catalyst used to crack the oil into lighter fractions. This is costly as it reduces the useful life of the catalyst. Like chlorine, heavy metals also have a corrosive effect on the plant. There is some evidence that the presence of some metals in the final product can reduce performance.
A fast determination of elements and size of suspended particles is vital for diagnosis and safeguard of refinery equipment. However, sample preparation for current analytical methods consumes precious time and lost particle size information.
High-resolution continuum source graphite furnace absorption spectrometry (HR-CS-GFAS) is proposed as a fast analytical method for elemental determination in crude oils and potentially for simultaneous multielement and particle size analysis. This HR-CS-GFAS instrumentation is coupled to a modular simultaneous echelle spectrometer (MOSES) and provides a full optical window with high resolution (from 180 to 900 nm with bandwidth λ/170,000). By using this set-up, it is possible to generate a multiparameter 3D spectral image (atomic and molecular lines, isotopic shift, atomization delay, and intensities). The generated spectral images can be analyzed by multivariate regressions for the elemental and particle size analysis. Additionally, if several atomic and molecular lines are simultaneously measured, they may be used in multi-energy calibration (MEC), a method based on the use of many wavelengths of the same absorbing/emitting entity to improve the accuracy in analytical atomic spectrometry. This MEC approach combined with multivariate image analysis allows the quantification of selected elements (Si, Al, Ni, Fe, V, S, and Cl) and overcomes matrix effects.
We present our research on the development of a Brillouin optical frequency-domain analysis (BOFDA) using a perfluorinated graded-index polymer optical fiber (PFGI-POF) as a sensing fiber. The described works include investigations both on the selection of the setup components with respect to mode coupling effects and on the impact of the humidity cross-sensitivity. The suitability of the developed POF-based BOFDA is proved by a distributed measurement on an 86 m long PFGI-POF recorded with the spatial resolution of 6 m.
Society for Applied Spectroscopy (SAS) Atomic Section Student Award.
Magnesium is a major element in the hydrosphere and biosphere and plays important roles in (bio-) geochemical and physiological cycles. Mg has three stable isotopes, 24Mg, 25Mg and 26Mg. It is due to their relatively large mass difference (~8% between) that isotope fractionation leads to slight variations of isotope amount ratios in biological, environmental and geological samples. Traditionally, isotope ratios are measured by mass spectrometric methods. Their drawbacks include the high costs for instruments and their operation, experienced operators and elaborate time-consuming chromatographic sample preparation.
Recently, optical spectrometric methods have been proposed as faster and low-cost alternative for the analysis of isotope ratios of selected elements by means of high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS), and laser ablation molecular isotopic spectrometry (LAMIS).
For the determination of Mg isotope ratios in selected rock reference materials, the molecular spectrum of the in-situ generated MgF and MgO molecules were studied and their results compared with MC-ICP-MS. By HR-CS-MAS, samples were dissolved by acid digestion and Mg isotopes analyzed with and without matrix. The absorption spectrum was recorded for MgF for the electronic transitions X 2Σ → A 2 Πi, and X 2Σ → B 2Σ+. In the case of LAMIS, we investigated the MgF molecule for the electronic transition A 2Πi → X 2Σ, as well as direct analysis by the MgO molecule for the electronic transition A 1Π+ → X 1Σ. The MgF and MgO spectra are described as the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF for the MgF and 24MgO, 25MgO, and 26MgO for the MgO. The isotope analysis was done by deconvolution of the MgF spectrum by partial least square regression (PLS) calibrated with enriched isotope spikes. Results were accurate with precisions ranging between 0.2 ‰ and 0.8 ‰ (2 SD, n= 10) for HR-CS-GFMAS. No statistically significant differences were observed for samples w/o matrix extraction. On the other hand, LAMIS allows the direct analysis of solid samples with the extended possibility of direct analysis, however the precision is lower due the lack of solid isotopic calibration standards.
Is it a parmesan cheese from Italy? Who painted the Mona Lisa? The determination of the place of origin is essential for consumer protection, detection of falsifications, and also to bring justice.
All the tangible possess an isotopic fingerprint. However, current technologies are too expensive. We work on the development of fast and low-cost optical instruments and methods for isotope analysis.
The separation of two closely located 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.
The measured thermal waves can be transformed to virtual (ultrasound) waves that can be processed by applying ultrasound reconstruction algorithms and finally the super resolution algorithm. Otherwise, it is also possible to make use of a Fourier transform with a subsequent super resolution routine.
These super resolution thermographic image reconstruction techniques in post-processing are discussed and evaluated regarding performance, accuracy and repeatability.
Magnesium (Mg) is a major element in a range of silicate and carbonate minerals, the hydrosphere and biosphere and plays important roles in (bio-) geochemical and physiological cycles. Mg has three stable isotopes, 24Mg, 25Mg and 26Mg with natural abundances of 79 %, 10 %, and 11 %, respectively. It is due to their relatively large mass difference (~8% between 24Mg and 26Mg) that isotope fractionation leads to slight variations of isotope amount ratios n(26Mg)/n(24Mg) in biological, environmental and geological samples. Traditionally, isotope ratios are measured by mass spectrometric methods and isotope ratios are expressed as deviation from an internationally agreed upon material, i.e. the zero-point of the δ-value scale. Drawbacks of this method include the high costs for instruments and their operation, experienced operators and elaborate, time-consuming chromatographic sample preparation.
Recently, optical spectrometric methods have been proposed as faster and low-cost alternative for the analysis of isotope ratios of selected elements by means of high- resolution continuum source graphite furnace molecular absorption spectrometry (HR- CS-GFMAS) and laser ablation molecular isotopic spectrometry (LAMIS).
For the determination of Mg isotope amount ratios, the molecular spectrum of the in-situ generated MgF and MgO molecules were studied. In the case of HR-CS-GFMAS, the absorption spectrum was recorded for MgF for the electronic transitions X2Σ → A2Πi and X 2Σ → B2Σ+ around wavelengths 358 nm and 268 nm, respectively. In the case of LAMIS, we investigated the MgF molecule for the electronic transition A2Πi → X2Σ as well as the MgO molecule for the electronic transition A1Π+ → X1Σ around 500 nm. The MgF and MgO spectra are described by the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF for the MgF and 24MgO, 25MgO, and 26MgO for the MgO (F is monoisotopic, and the isotope composition of O is assumed as constant). By HR-CS-GFMAS the analysis of Mg was done by deconvolution of the MgF spectrum by partial least square regression (PLS) calibrated with enriched isotope spikes. Isotope amount ratios in rock samples with and without matrix separation were analyzed. Calculated δ-values were accurate and obtained with precisions ranging between 0.2 ‰ and 0.5 ‰ (1 SD, n = 10). On the other hand, LAMIS allows the direct analysis of solid samples with the extended possibility of in-situ analysis. Main advantages, limitations, and scopes of both optical techniques are going to be discussed and compared to MC-ICP-MS.
Additive manufacturing (AM) offers diverse advantages compared to conventional manufacturing. In this work the microstructure of austenitic steel 316L, manufactured with Selective Laser Melting (SLM), was analyzed and compared to microstructure of 316L hot rolled material. Methods used for analysis are microprobe, optical microscopy and electron backscatter diffraction.
Magnesium is a major element in the hydrosphere and biosphere and plays important roles in (bio-) geochemical and physiological cycles. Mg has three stable isotopes, 24Mg, 25Mg and 26Mg. It is due to their relatively large mass difference (~8% between) that isotope fractionation leads to slight variations of isotope amount ratios in biological, environmental and geological samples. Traditionally, isotope amount ratios are measured by mass spectrometric methods. Their drawbacks include the high costs for instruments and their operation, experienced operators and elaborate time-consuming chromatographic sample preparation. Recently, an optical spectrometric method has been proposed as faster and low-cost alternative for the analysis of isotope ratios: high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS).
For the determination of Mg isotope ratios in selected rock reference materials, the high-resolution molecular absorption spectrum of in-situ generated MgF molecule was studied applying multivariate analysis and the results compared with MC-ICP-MS. Samples were dissolved by acid digestion and Mg isotopes analyzed with and without matrix. The absorption spectra were recorded for MgF for the electronic transition X 2Σ → B 2Σ+. The MgF spectrum is described as the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF. The isotope analysis was done by deconvolution of the MgF spectrum by partial least square regression (PLS). A PLS model was built and calibrated with enriched isotope spikes and certified reference materials. Spectra data was preprocessed by a derivate of second order and venetian blinds cross-validation was employed for finding the optimum latent variables. Finally, the model was refined by a genetic algorithm which identified the best subset of variables for a precise and accurate regression. Results are compatible with those obtained by MC-ICP-MS with an accuracy of ± 0.3‰ with uncertainties ranging between 0.02 to 0.6‰.
Boron and Magnesium present two and three stable isotopes respectevely. It is due to their relatively large mass difference (~ 10%) that isotope fractionation leads to considerable isotope amount ratio variations in the nature. These have been used as a proof of provenance of mineral and biological samples, to estimate a contamination source and to the determination of geological processes by erosion or subduction. Additionally, boron is employed in the nuclear industry due to the capability of its isotope 10B to thermal-neutron capture and therefore 10B enriched boric acid solutions are used in the cooling system of thermonuclear facilities and in the alloying of steel and carbides for protective shielding. Traditionally, isotope ratio variations have been determined by mass spectroscopic methods.
Here an alternative faster and low cost method for isotope ratio determination is proposed: high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Isotope amount ratios have been determined by monitoring the absorption spectrum of boron monohydride (BH) for boron and Magnesium monofluoride (MgF) for magnesium in a graphite furnace HR-CS-MAS. Bands (0→0) and (1→1) were evaluated. Partial least square regression (PLS) for analysis of samples and reference materials were applied. For this, a spectral library with different isotopes ratios for PLS regression was built. Results obtained are metrologically compatible with those reported by mass spectrometric methods. Moreover, a precision and accuracy of the method of ± 0.5 ‰. This accuracy and precision is comparable with those obtained by thermal ionization mass spectrometry (TIMS) and multiple collector inductively coupled plasma mass spectrometry (MC-ICP-MS) for boron isotope ratio measurements
Magnesium is a naturally occurring element that can be found in several mineral forms in the earth crust. This element presents three stable isotopes 24Mg, 25Mg and 26Mg with a natural abundance of 79%, 10%, and 11% respectively. It is due to their relatively large mass difference (~8% between 24Mg and 26Mg) that isotope fractionation leads to slight isotope amount ratio variations n(26Mg)/n(24Mg) in biological and geological samples. Traditionally, isotope amount ratios have been measured by mass spectrometric methods. However, drawbacks of these methods include the high costs for instruments and their operation, experienced operators and elaborate chromatographic sample preparation which are time-consuming. Recently, optical spectrometric methods have been proposed as faster and low-cost alternative for the analysis of isotope ratios of selected elements by means of high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) and laser ablation molecular isotopic spectrometry (LAMIS). For the determination of Mg isotope amount ratios, the molecular spectrum of the in-situ generated MgF and MgO molecules were studied. In the case of HR-CS-GFMAS, the absorption spectrum was recorded for MgF for the electronic transitions X 2Σ → A 2 Πi and X 2Σ → B 2Σ+ around wavelengths 358 nm and 268 nm respectively. In the case of LAMIS, it was studied the MgF molecule for the electronic transitions A 2Πi → X 2Σ as well as the MgO molecule for the electronic transition A 1Π+ → X 1Σ around 500 nm. The MgF and MgO spectra are composed by the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF for the MgF and 24MgO, 25MgO, and 26MgO for the MgO (F is monoisotopic, and the isotope composition of O is assumed as constant). By HR-CS-GFMAS the analysis of Mg was done by deconvolution of the MgF spectrum by a partial least square regression (PLS) calibrated with enriched isotope spikes. The isotope amount ratios in rock samples with and without matrix separation were analyzed. Resulting delta values were obtained with precisions ranging between 0.2-0.5 ‰. On the other hand, LAMIS allows the direct analysis of solid samples with the extended possibility of in-situ analysis. Main advantages, limitations, and scopes of both optical techniques are going to be discussed and compared with MC-ICP-MS.
Crystalline molecular materials with mechanical flexibility are promising for technological development. This is particularly true for the development of advanced materials with optoelectronic and biomedical applications. While a growing number of mechanically flexible crystalline molecular materials are being reported,1 they remain scarce. At present, most discoveries are serendipitous, as limited design strategies are currently known. Amongst these strategies Desiraju et. al. suggested that elastic materials must contain herringbone structures.2 For plastic crystals, the so-called ‘shape-synthon’ strategy has been developed, in which weak non-covalent interactions are introduced into structures to facilitate mobility of molecules.3 This includes formation of slip planes. Generally, these models have performed very well at predicting and rationalizing the mechanical properties of new materials. Recently, however, a family of one-dimensional covalent networks (coordination polymers; CPs) has been described, which show mechanical elasticity. With drastically different structural chemistry, these systems do not seem to adhere to the currently established rules. Herein, we present the first such system: a plastically bendable crystal of a 1D CP, [Zn(-Cl)2(3,5-Cl2Py)2]n (where 3,5-Cl2Py = 3,5-dichloro pyridine). This CP crystallizes in a tetragonal, and can therefore be bent over two major faces to acute angles without fracturing. We conducted bending and indentation experiments to quantify the mechanical properties of the CP crystal. This was complimented by Vibrational (Raman and Terahertz) spectroscopy and theoretical calculations for deeper understanding of molecular level structural deformation.
Mass spectrometric Methods MC-ICP-MS and TIMS) are without doubt the working horse of stable isotope analysis. However, drawbacks of these methods include the high costs for instruments and their operation, experienced operators and elaborate chromatographic sample preparation which are time consuming.
Optical spectrometric methods are proposed as faster and low-cost alternative for the analysis of isotope ratios of selected elements by means of high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS) and laser ablation molecular isotopic spectrometry (LAMIS). First, stable isotope amount compositions of boron (B) and magnesium (Mg) were determined based on the absorption spectra of in-situ generated heteronuclear diatomic molecules (MH or MX) in graphite furnace HR-CS-MAS. The use of a modular simultaneous echelle spectrograph (MOSES) helps to find the maximal isotope shift in the diatomic molecular spectra produced in a graphite furnace by using isotopic spike solutions. Isotopes of boron (10B and 11B) were studied via their hydrides for the electronic transition X 1Σ+ → A 1Π. The spectrum of a given sample is a linear combination of the 10BH molecule and its isotopologue 11BH. Therefore, the isotopic composition of samples can be calculated by a partial least square regression (PLS). For this, a spectral library was built by using samples and spikes with known isotope composition. Boron isotope ratios measured by HR-CS-MAS are identical with those measured by mass spectrometric methods at the 0.15 ‰ level. Similar results were obtained for a multiple isotope system like Mg (24Mg, 25Mg, and 26Mg), where isotope shifts of their isotopologues can be resolved in the MgF molecule for the electronic transition X 2Σ → A 2 Πi. Finally, the application of molecular spectrometry via emission by LAMIS is compared and discussed.
Die vom BMBF unterstütze Forschungsinitiative BonaRes entwickelt Strategien um Boden als nachhaltige Ressource für die Bioökonomie zu nutzen. Das Projekt Intelligence for Soil (I4S) ist ein Teil dieser Initiative und beschäftigt sich mit der Entwicklung eines integrierten Systems zur ortsspezifischen Düngung. Ein Ziel dieses Projektes ist die Etablierung einer mobilen Sensorplattform zur Bodenkartierung. Aufgabe der BAM ist dabei das Installieren und die Optimierung eines RFA Sensors für die online Messung direkt auf dem Feld. Die RFA ist eine zerstörungsfreie Technik, die kaum Probenvorbereitung benötigt und einen schnelle Multielement Analyse ermöglicht. Das schnelle Kartieren des Bodens ermöglicht später eine ortsspezifische Düngung mit Nährstoffen wie z.B. K, Ca und P.
Die vom BMBF unterstütze Forschungsinitiative BonaRes entwickelt Strategien um Boden als nachhaltige Ressource für die Bioökonomie zu nutzen. Das Projekt Intelligence for Soil (I4S) ist ein Teil dieser Initiative und beschäftigt sich mit der Entwicklung eines integrierten Systems zur ortsspezifischen Düngung. Ein Ziel dieses Projektes ist die Etablierung einer mobilen Sensorplattform zur Bodenkartierung. Aufgabe der BAM ist dabei das Installieren und die Optimierung eines RFA Sensors für die online Messung direkt auf dem Feld. Die RFA ist eine zerstörungsfreie Technik, die kaum Probenvorbereitung benötigt und einen schnelle Multielement Analyse ermöglicht. Das schnelle Kartieren des Bodens ermöglicht später eine ortsspezifische Düngung mit Nährstoffen wie z.B. K, Ca und P.
The use of artificial neural networks (ANNs) is demonstrated for efficient real-time data processing in optical fiber sensing applications. Using ANN-based algorithms, two orders of magnitude improved computation time and improved measurement resolution is achieved for distributed strain sensing using the wavelength-scanning coherent optical time domain reflectometry technique.
The distributed measurement of relative humidity is a sought-after capability for a wide range of applications in civil engineering and structural health monitoring. We show that polymethyl methacrylate (PMMA) optical fi-bers can be employed as a sensor medium to conduct distributed humidity measurement by analyzing Rayleigh backscattering traces obtained by OTDR. We make use of the effect that water penetrates the fiber core and directly influences the local fiber attenuation and Rayleigh backscatter coefficient. We conducted distributed backscattering analysis for two different pulse wavelengths: 500 nm and 650 nm. The 650 nm results are susceptible to both, attenuation changes and backscatter changes, whereas backscatter results at 500 nm are not affected by humidity-induced attenuation and only exhibit a change of Rayleigh backscattered power as a function of humidity. The combined measurement and analysis of both parameters at these two wavelengths has the advantage that cross-sensitivities on backscatter change and attenuation, such as strain and tempera-ture changes, could be separated from the humidity response of the fiber. We present laboratory results for a humidity range between 30% and 90% for both pulse wavelengths: including step responses, humidity cycles and hysteresis analysis. In addition to the attenuation and backscatter coefficient dependence, we also analyze optical runtime changes as a function of humidity. POFs have the advantage that they can be directly embed-ded into materials such as concrete or soil to measure water content or localize water ingress. Standard step-index PMMA POFs can be used as a distributed relative humidity sensor up to 200 m distance.
We present our research on the development of a Brillouin optical frequency-domain analysis (BOFDA) using a perfluorinated graded-index polymer optical fiber (PFGI-POF) as a sensing fiber. The described works include investigations both on the selection of the setup components with respect to mode coupling effects and on the impact of the humidity cross-sensitivity. The suitability of the developed POF-based BOFDA is proved by a distributed measurement on an 86 m long PFGI-POF recorded with the spatial resolution of 6 m.
Polytetrafluorethylen (PTFE) ist ein Hochleistungskunststoff, der sich aufgrund seiner einzigartigen Eigenschaften als unverzichtbarer Werkstoff in der modernen Industriegesellschaft etabliert hat. PTFE, modifiziertes PTFE und PTFE-Compounds kommen bevorzugt bei systemtechnischen Lösungen im Umfeld komplexer Regelwerke mit hohen Kompatibilitäts- bzw. regulativen Anforderungen, z.B. im Sauerstoff-, Lebensmittel- bzw. Trinkwasserkontakt, zur Anwendung. Beim Einsatz in Sauerstoffanlagen sollten Verarbeiter eine Reihe von Hinweisen beachten.
Wir laden zum Trainingsworkshop Datenanalyse ein. Angetrieben durch die Digitalisierung und die sogenannte Industrie 4.0 steigt die Erwartungshaltung gegenüber der Nutzung von Daten. Die Unsicherheit, Widersprüchlichkeit und Redundanz separat verarbeiteter einzelner Quellen soll durch die synergetische Zusammenführung heterogener Datensätze überwunden werden. Dabei steht der zunehmenden Aufgabenkomplexität eine ebenso zunehmende Verfügbarkeit an Daten und Analyseverfahren gegenüber.
Der Workshop vermittelt ein konzeptionelles Verständnis für moderne Datenanalyseverfahren (Machine Learning (ML), Multivariate Statistik) und soll durch ein anschließendes Hands-On Training mit Python (https://www.python.org) einen einfachen Einstieg in die Thematik ermöglichen. Der Kurs richtet sich an den wissenschaftlichen Nachwuchs.
Die herkömmliche Bildgebung mit Röntgenstrahlung beruht auf unterschiedlicher Absorption durch verschiedene Materialien im Volumen eines Körpers. Es entsteht ein "Massebild". Die hier vorgestellten Verfahren benutzen die Brechung und Beugung von Röntgenstrahlen, um innere Oberflächen oder die Molekulartextur von Materialien und Bauteilen abzubilden. Im Vortrag werden die entsprechenden Messtechniken an der BAM im Labormaßstab sowie an Großforschungseinrichtungen vorgestellt und anhand einiger Anwendungsbeispiele die zusätzlichen Informationen zur herkömmlichen Durchstrahlung diskutiert.