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Eingeladener Vortrag
- nein (1102)
Three measurement campaigns of train-induced ground vibrations are evaluated for the vehicle-track-soil interaction. Ground vibrations, track vibrations and vehicle vibrations have been measured for train passages and impulse excitation and compared with theoretical results. The soil and the track-soil system are calculated by wavenumber integrals. The influence of the vehicle is introduced by a substructure method. By comparing theory and measurement the different components of excitation force and ground vibration can be analysed, the quasi-static excitation, track-alignment errors, the out-of-roundness of wheels, the wheel and rail roughness, and moreover, scattered axle impulses and ineffective high-frequency parts of the wheelset accelerations and Forces.
Three measurement campaigns of train-induced ground vibrations are evaluated for the vehicle-track-soil interaction. Ground vibrations, track vibrations and vehicle vibrations have been measured for train passages and impulse excitation and compared with theoretical results. The soil and the track-soil system are calculated by wavenumber integrals. The influence of the vehicle is introduced by a substructure method. By comparing theory and measurement the different components of excitation force and ground vibration can be analysed, the quasi-static excitation, track-alignment errors, the out-of-roundness of wheels, the wheel and rail roughness, and moreover, scattered axle impulses and ineffective high-frequency parts of the wheelset accelerations and forces.
Methods for the rapid and sensitive detection of target analytes are gaining importance in medical diagnostics and environmental monitoring, in the security, occupational health and safety as well as food sectors. Among all of the methods employed for rapid tests, lateral flow assays (LFAs) are the most commonly used, and hundreds of test kits based on this technique are available on the market. A major drawback is that most of these capture agents either indicate the analyte only indirectly, and in most cases a second binding agent able to bind directly or indirectly to the analytes is necessary (e.g., a secondary labeled antibody). Furthermore, in certain cases in which the (ultra)trace detection of an analyte is required, the traditional approach of a certain number of probe molecules being conjugated to a particular support is not sufficient. Therefore, novel concepts implementing steps of effective signal amplification are urgently required.
Keeping in mind these limitations, we thought that the sensitivity of these systems should be improvable through employment of gated reporter molecule-releasing hybrid nanoparticle materials on novel lateral flow devices. On one hand, the gated sensor material can produce a massive signal amplification, by releasing many reporter molecules only after chemical recognition of a few analyte molecules has taken place in an independent and separate step at the pore openings. On the other hand, the employment of tailored capture materials for the selective interaction with the released reporter molecules in a second arbitrary zone on the strip allows to concentrate or focus the latter for more efficient detection or to create selective multi-spot detection zones, which renders the simultaneous detection of several reporter molecules at the same time in multiplexed detection of various analytes possible.
For that purpose, we have prepared several stimuli-responsive materials for small-molecule sensing based on specific interactions between biomolecules such as antibodies with the corresponding analytes for the detection of certain explosives. In order to prepare these bio-capped materials, we have selected silica mesoporous nanoparticles (MSNs) as inorganic support due to their unique properties such as defined void structure, high inner surface area and flexible functionalization chemistry. These MSNs are loaded with a brightly fluorescent indicator dye, and the external surface is subsequently functionalized with suitable molecules able to interact with antibodies, efficiently inhibiting dye release. The opening protocol and delivery of the entrapped dye is reminiscent of a displacement reaction involving the presence of the target analyte, producing a displacement of the biomolecule and allowing the detection of the target analyte.
The presentation discusses general aspects of system design as well as analytical performance and highlights the integration into a lateral-flow assay, showing as an example the determination of the explosives TATP, TNT and PETN with fluorescence readout, in single-substance and multiplexing modes.
Es lässt sich feststellen, dass eine Vielzahl unterschiedlicher flüchtiger organischer Verbindungen aus Bauprodukten freigesetzt werden kann. Hierbei gibt es in den meisten Bauproduktgruppen sowohl emissionsarme als auch emissionsreiche Produkte.
Manche Verbindungen sind produktgruppenspezifisch; so werden beispielsweise Siloxane aus Silikondichtmassen freigesetzt, andere Verbindungen sind eher unspezifisch wie Formaldehyd und Essigsäure, die aber in unterschiedlichen Konzentrationen aus einer Vielzahl von Produkten abgegeben werden und zu den am häufigsten emittierten Verbindungen zählen.
Es ist darauf hinzuweisen, dass VOC-Analytik und Gerüche im Allgemeinen keinen Zusammenhang zeigen.
Gerade bei modernen, dichten Bauten mit geringem natürlichem Luftwechsel sind hohe Schadstoffkonzentrationen zu erwarten, wenn nicht emissionsarme Materialien und Produkte zum Einsatz kommen.
Explosionen in Rohrleitungen
(2019)
Deflagrationssicherungen sind Sicherheitseinrichtungen, die den Durchfluss von brennbaren Gasen und Dämpfen brennbarer Flüssigkeiten ermöglichen, den Flammendurchschlag und weitere Explosionsausbreitung nach der Zündung von explosionsfähigen Gas-/Dampf-Luftgemischen jedoch verhindern sollen.
Von besonderer Bedeutung für die Wirksamkeit der Deflagrationsrohrsicherung ist der Einbauort. Diesbezügliche Abweichungen von den normativen Anforderungen, die Grundlage der Prüfung und Zulassung von Deflagrationsrohrsicherungen sind, können zum Versagen der Sicherheitseinrichtung führen. Oft lassen sich allerdings aus betrieblichen bzw. verfahrenstechnischen Gründen der Norm entsprechende Einbaubedingungen nur schwer oder nicht realisieren.
Deshalb besteht das Ziel der Untersuchungen eines F&E-Vorhabens mit der Braunschweiger Flammenfilter GmbH darin, einen Beitrag zur Schaffung einer belastbaren Datenbasis zu leisten, um den Einfluss von Rohrleitungsverzweigungen auf deflagrative Gasexplosionen systematisch zu bewerten.
Considerations for nanomaterial identification of powders using volume-specific surface area method
(2019)
The EC’s recommendation for a definition of nanomaterial (2011/696/EU) should allow the identification of a particulate nanomaterial based on the number-based metric criterion according to which at least 50% of the constituent particles have the smallest dimension between 1 and 100 nm. However, it has been recently demonstrated that the implementation of this definition for regulatory purposes is conditioned by the large deviations between the results obtained by different sizing methods or due to practical reasons such as high costs and time-consuming.
For most measurement methods for particle size determination it is necessary to initially disperse the particles in a suitable liquid. However, as the particle size decreases, the adhesion forces increase strongly, making it more difficult to deagglomerate the particles and to assess accurately the result of this process. Therefore, the success of the deagglomeration process substantially determines the measurement uncertainty and hence, the comparability between different methods.
Many common methods such as dynamic light scattering (DLS), centrifugal liquid sedimentation (CLS) or ultrasound attenuation spectroscopy (US) can give good comparable results for the size of nanoparticles, if they are properly separated and stabilized (e.g. in reference suspensions).
In order to avoid the use of hardly available and expensive methods such as SEM / TEM for all powders, an agglomeration-tolerant screening method is useful.
One of the measurement methods well suited to probe the size of particulate powder is the determination of the volume-specific surface area (VSSA) by means of gas adsorption as well as skeletal density. The value of 60 m2/cm3 corresponding to spherical, monodisperse particles with a diameter of 100 nm constitutes the threshold for decisioning if the material is a nano- or non-nanomaterial. The identification of a nanomaterial by VSSA method is accepted by the EU recommendation.
However, the application of the VSSA method was associated also with some limitations. The threshold of 60 m2/cm3 is dependent on the particle shape, so that it changes considerably with the number of nano-dimensions, but also with the degree of sphericity of the particles. For particles containing micro-pores or having a microporous coating, false positive results are induced. Furthermore, broad particle size distributions made necessary to additionally correct the threshold. Based on examples of commercially available ceramic powders, the applicability of the VSSA approach was tested in relation with SEM and TEM measurements. The introduction of a correction term for deviations from sphericity and further additions improved the applicability of VSSA as a screening method.
Self-mated magnesia stabilized zirconia (Mg-PSZ) ceramic sliding couples have been investigated at 100 N load (P0max= 1324 MPa) in oscillating sliding conditions in different humidity conditions in air and in hot steam. Temperatures have been varied up to 400 °C and pressures up to 6 bars. The results show that the wear behavior of MgO-ZrO2 under high Hertzian contact pressures is strongly dependent on temperature and is similar for both dry oscillating and oscillating in hot steam. However, although the evolution in wear rates on temperature is similar and the wear rates of MgO-ZrO2 plunged above 300 °C in hot steam and air by nearly three orders of magnitude, SEM micrographs revealed in hot steam at 400 °C smooth wear tracks. In contrast, hot steam enhanced the tribochemistry of self-mated alumina couples and reduced wear rates. Hot steam decreased the coefficients of friction of MgO-ZrO2 with increasing temperature, but not the wear rates.
Powder bed -based technologies are amongst the most successful Additive Manufacturing (AM) techniques. "Selective laser sintering/melting" (SLS/SLM) and "binder jetting 3D printing" (3DP) especially are leading AM technologies for metals and polymers, thanks to their high productivity and scalability. In this context, the "layerwise slurry deposition" (LSD) has been developed as a layer deposition method which enables the use of SLS/SLM and 3DP technologies for advanced ceramic materials. LSD consists in the layer-by-layer deposition of a ceramic slurry by means of a doctor blade. Each layer is deposited and dried to achieve a highly packed powder layer, which can be used for SLM or for 3DP. This technique offers high flexibility in the ceramic feedstock used, especially concerning material and particle size, and is capable of producing parts with physical and mechanical properties comparable to traditionally shaped parts. In this presentation, the LSD technique will be introduced and several examples of application to porcelain, SiC and alumina products will be reported.
Powder bed -based technologies are amongst the most successful Additive Manufacturing (AM) techniques. "Selective laser sintering/melting" (SLS/SLM) and "binder jetting 3D printing" (3DP) especially are leading AM technologies for metals and polymers, thanks to their high productivity and scalability.
However, the flowability of the powder used in these processes is essential to achieve defect-free and densely packed powder layers. For standard powder bed AM technologies, this limits the use of many raw materials which are too fine or too cohesive.
This presentation will discuss the possibilities to either optimize the powder raw material to adapt it to the specific AM process, or to develop novel AM technologies which are able to process powders in a wider range of conditions.
In this context, the "layerwise slurry deposition" (LSD) has been developed as a layer deposition method which enables the use of very fine ceramic particles. Another technology, the Gas Flow Assisted Powder Deposition, can increase the stability of the powder bed and the packing density, even in extreme conditions such as in absence of gravitational forces.
The Scope of the Workshop was to provide a forum for discussion on progress in development, characterisation and application of reference nanomaterials. Results of recently finsihed national and international research projects have been presented. Moreover, the need for future developments have been addressed.
Attendees of teh Workshop were expected to be experts from academia, research institutes, regulatory bodies and industry working or interested in the area of reference nanomaterials.
The following structure of Workshop was planned: the main focus of the first day was on reference material needs and development, while teh second day was focussed on reference materials characterisation and standardisation.
Over 111 participants frm 13 countries and teh European Joint Research Centre have regsitered for the Workshop with 16 platform presentations and 42 poster contributions grouped in 2 sessions and 10 topical areas.
A summary of the observations, analysis and conclusions of the Workshop is made including an overview table of links to information on existing reference nanomaterials.
In powder bed Additive Manufacturing (AM) technologies, a part is produced by depositing and piling up thin powder layers. In each layer, the cross section of the object to build is defined by locally consolidating the powder, by sintering/melting the material (powder bed fusion technologies) or by ink jetting a binder (binder jetting technologies).
These are already leading AM technologies for metals and polymers, thanks to their high productivity and scalability. The application of these techniques to most ceramics has been challenging so far, because of the challenges related to the deposition of homogeneous powder layers when using fine powders.
In this context, the "layerwise slurry deposition" (LSD) has been developed as a layer deposition method which enables the use of SLS/SLM and 3DP technologies for advanced ceramic materials. LSD consists in the layer-by-layer deposition of a ceramic slurry by means of a doctor blade. Each layer is deposited and dried to achieve a highly packed powder layer. The LSD offers high flexibility in the ceramic feedstock used, especially concerning material and particle size, and enables the production of parts with physical and mechanical properties comparable to pressed or slip-casted parts. In this presentation, the LSD technique will be introduced and several examples of application to porcelain, SiC and alumina products will be reported.
Mykotoxine in Lebensmitteln stellen weltweit Probleme dar, Zearalenon in Speiseöl ist ein solches. Neue Hydrazinbasierte Analyseverfahren können jetzt helfen, den EU-Grenzwert besser zu kontrollieren. Aber auch die Strukturaufklärung von Transformationsprodukten und verlässliche Kalibrierstandards sind aktuelle Herausforderungen.
The lecture gives an overview of the core competencies of the department 8.5 Micro NDT (CT equipment, X-Ray Refraction, WAXS - Texture analysis, Data correction, Reconstruction algorithms, Image analysis, Dimensional control, Multi-Source Data Fusion and Combination, Micromechanical Properties by Neutron Diffraction) with regard to the characterization of lightweight materials (fibre composites, aluminum and titanium MMCs) used in aviation. The focus is on characterization by synchrotron and X-ray refraction techniques as well as computed tomography.
An overview of the activities in the field of surface and microbeam analysis at BAM-6.1 is given with focus on physico-chemical characterization at the nanoscale. Ideas of potential joint activities are presented: structural and chemical analysis of graphene, deposition techniques for nanoparticles, EBSD on steel for a broader range of methods, instruments and types of steel, soft X-ray Analysis of low-Z materials, analysis of mesoporous thin films, etc.
Das EMPIR-Förderprogramm wird kurz erläutert und laufende Projekte aus der Nanotechnologie werden vorgestellt. Der Schwerpunkt liegt auf Standardisierungsprojekten, die gemeinsam mit ISO/TC 229 'Nanotechnologies' und CEN/TC 352 'Nanotechnologies' zu neuen Normen führen sollten. Als Beispiel für laufende Nanotechnologie-Projekte mit Koordination aus Deutschland werden MagNaStand (PTB) und nPSize (BAM) gegeben.
Microbiologically influenced corrosion (MIC) of iron is usually attributed to sulfate-reducing microorganisms (SRM) in offshore industries, such as the oil and gas pipelines, due to the high concentrations of sulfate in the seawater. SRM act upon the metal by the reactiveness of hydrogen sulfide (HS-), and by withdrawal of the available electrons (Fe --> Fe2+ + 2e-; E° = -0.47 V) in electrical contact with the metal (EMIC). However, methanogenic archaea can also cause MIC. Because they do not produce HS-, withdrawal of electrons may be their main corrosive mechanism; however, mechanistic details and kinetics of the overall process are poorly understood.
To investigate the corrosion potential of methanogens, we studied the EMIC methanogenic strains isolated from marine sediments (Methanobacterium-affiliated strain IM1) and crude oil tanks (Methanococcus maripaludis Mic1c10), in an in-house developed flow-through cell to simulate a fluctuating environment. A co-culture of M. maripaludis and D. alaskensis was also established to study the effect of syntrophic growth on metal corrosion that may occur in industrial pipelines. Results indicate that the rates of iron corrosion due to coupled methanogenesis (up to 0.4 mm/yr) are higher to that caused by the marine SRM Desulfovibrio alaskensis (0.15 mm/yr). Surface analyses of the metal showed severe pitting with high methane production. Genomic analysis of the EMIC methanogen M. maripaludis Mic1c10 will provide an insight on the mechanisms of MIC. Such knowledge and deeper understanding also from an electrokinetic point of view may not only provide further models in microbial electrophysiology, but also contribute to mitigation strategies in MIC.zeige weniger
The lecture about gas sensor characterization and calibration contains the content of 3S: Sensitivity, selectivity and stability, sensor drift, aging and poisoning as well as gas mixing systems for laboratory and field calibration, measurement uncertainty for sensor calibration and traceable calibration of gas sensor systems.
Since cereals constitute a staple food worldwide, monitoring of growth, storage and processing represent a perseverative challenge of analytical sciences. Especially during storage infested grains breed fungal clusters (“hot spots”) in which mycotoxins accumulate and can highly exceed allowed maximum levels. Because of their unpredictable presence, analytical procedures – including representative sampling - contain invasive and time intensive steps.
To avoid erroneously negative results in mycotoxin analysis in cereals, the samples´ homogeneous headspace might be investigated instead of analyzing subsamples of the grains. So-called microbial volatile organic compounds (MVOC´s) provide information for instance about the fungal status of grains. Previous investigations revealed trichodiene to be a precursor of trichothecene mycotoxins which comprises more than 180 different compounds. Due to its non-functionalised sesquiterpene structure, quantification of trichodiene using Headspace GC-MS methods is possible. Thereby, it could be used as biomarker for trichothecene contamination of cereals.
Nevertheless, further investigations are necessary. To be able to draw conclusion about the trichothecene content in cereal samples, a possible correlation between trichodiene concentration in the gas phase and trichothecene concentration in the sample must be examined. Realizing this idea would widely extend the applicability of trichodiene and enormously simplify trichothecene detection. Hence, the first step of an ongoing study aims to develop a laboratory reference method using trichodiene as volatile biomarker to quantify trichothecenes in cereals. Both static headspace and SPME-enrichment coupled to gas chromatography with mass spectrometry (GC-MS) were tested and compared. In a second step, this reference method is intended to validate new approaches for fast on-site screening of trichodiene in cereals.
Die Bildgebung oder Analyse von Materialien mittels luftgekoppelten Ultraschalls profitiert von einer hohen Geschwindigkeit, Flexibilität und Materialschonung des assoziierten Verfahrens. Die Luftankopplung hat jedoch den wesentlichen Nachteil, dass die auftretenden Impedanzsprünge an Grenzflächen zu enormen Verlusten in den Signalamplituden führen. Ultraschallwandler, die laut genug senden und sensitiv genug empfangen, um die geringen Signalamplituden noch auswerten zu können, sind somit zentraler Gegenstand der aktuellen Forschung und Entwicklung. Vielversprechende Wandlertypen sind piezokeramische Wandler, Elektretwandler, aber auch passive, breitbandige Ultraschallempfänger, wie optische Mikrophone. Die quantitative Charakterisierung der Sensitivitäten solcher Wandler wird oft vernachlässigt, da kein simples, universelles Verfahren zur Verfügung steht. In diesem Beitrag geht es um die Methodik der Charakterisierung von Luftultraschallwandlern mittels thermoakustischer Ultraschallsender. Thermoakustische Wandler erzeugen Ultraschall durch das schnelle heizen eines finiten Volumens an Luft vor dem Wandler. Die erhöhte interne Energie führt zu einer Druckänderung, welche sich als akustische Welle fortpflanzen kann. Da keine mechanische Volumenarbeit vom Wandler erbracht wird, funktioniert das Verfahren resonanzfrei.
Die Charakterisierung wird am Beispiel von Elektretwandlern durchgeführt. Elektretwandler sind sensitive und immer verschleißresistentere Schallwandler, wodurch sie verbreitet Einsatz im Hör- und Ultraschallbereich finden. Geladene, zelluläre Polypropylen-Folien eignen sich besonders gut als Wandlermaterial aufgrund ihrer, verglichen mit Piezokompositen, hundertfach niedrigeren akustischen Impedanz bei gleichem piezoelektrischem Koeffizienten. Doch das winkel- und frequenzabhängige Verhalten der Wandler ist kaum untersucht und wenig quantifiziert. Es wird gezeigt, dass diese Folien eine schichtdickenabhängige Sensitivität in Größenordnungen zwischen 0.1 mV/Pa und 10 mV/Pa aufwiesen. Ein Maximum in der Sensitivität fand sich nahe ihrer mechanischen Resonanzfrequenz im Ultraschallbereich, aber auch im niederfrequenten Hörschallbereich. Darüber hinaus konnte die Winkelabhängigkeit der Sensitivität charakterisiert werden. Die Analyse konnte dabei zeiteffizient gestaltet werden, da pro Winkel eine Messung für die Berechnung der Übertragungsfunktion des Wandlers genügte. Quantifiziert wurden die Ergebnisse durch das einmalige Vermessen des Emitters mittels Laser-Doppler-Vibrometrie (LDV). Mit den erzielten Ergebnissen wurde zum einen das komplexe Sensitivitätsverhalten der Wandler untersucht, aber auch eine grundlegende Methodik aufgezeigt, wie Wandler quantitativ, multivariat charakterisiert werden können. Winkel- und frequenzaufgelöste Sensitivitäten erlauben zum einen die Analyse der Anwendbarkeit der Wandler für sämtliche Einsatzgebiete, zum anderen stehen so Rückschlüsse über die mechanische Dynamik von Elektretfolien in Aussicht, da deren Sensitivität direkt mit ihrem Elastizitätsmodul skaliert.
Shortly after founding the CCQM in 1993, the first key comparison (CCQM-K2) about the determination of Cd and Pb content in river water was hosted by IRMM. It has been clear from the beginning that for the determination of an element mass fraction in a matrix, accurate reference solutions would be the key point for a metrologically sound analysis. Triggered by the not entirely satisfactory results it was decided to investigate the basis of all measurements: the reference solutions. Thus in 1999, CCQM-K8, hosted by EMPA/LNE, started the tedious but indispensable work on elemental solutions standards.
Additionally, PTB, BAM and Merck KGaA initiated a project to establish a traceability system for inorganic analysis based on accurate monoelemental solutions. Within this unique approach ten high purity reference materials were fully characterized, and solutions were prepared gravimetrically thereof. These materials (forming the primary standards of elemental analysis) are available for NMIs/DIs from BAM.
CCQM-P46 (Cu, Mg, Rh) demonstrated the actuality of the topic and the challenges to prepare elemental solutions for every element. The accurate preparation and use of monoelemental solutions is consequently reflected in the recurrent conduct of (key) comparisons: CCQM-P149 (purity of zinc), CCQM-K87 (Co, Cr, Pb), and the current CCQM-K143/P181 (Cu solutions), to name only a few in a long series.
Is it necessary to put so much effort into the preparation of reference solutions? It clearly is! An example outside the world of academia: Recently, EDQM*, PTB, BAM and JRC have developed monoelemental reference standards traceable to the SI for toxic elements in support of the chapters of the European Pharmacopoeia, related to the analysis of elemental impurities in medicinal products. A new ICP OES method has been established allowing the comparison of two 1 g/kg mercury solutions with an outstandingly small uncertainty of Urel(w(Hg)) = 0.16 %. However, this technical progress would not have been possible without the ongoing effort of the metrological community within 25 years of research in the field of high accuracy monoelemental solutions.
* EDQM: European Directorate for the Quality of Medicines and HealthCare
Plasmas as atomization and ionization/excitation sources have been used for more than 50 years. The term plasma spectrochemistry was introduced in the 1980s and is nowadays a topic of annual reviews and different conferences such as the Winter Conference on Plasma Spectrochemistry (held in USA), the European Winter Conference on Plasma Spectrochemistry, and The Nordic conference on Plasma Spectrochemistry.
The development of advanced materials is inherently connected with improvements in analytical chemistry, and often is the driving force for method development in plasma-based spectrometry. Besides the determination of physical characteristics such as tensile strength, density, and conductivity, the investigation of their chemical constituents down to the trace and ultra-trace levels becomes more and more important and, therefore, the demand of sensitive and precise analytical methods is growing. In some cases, the determination of the average content is a sufficient result, for instance for the characterisation of raw material or waste management. However, lately laterally resolved analysis, depth profiling of layered materials and characterization of high purity materials are of growing importance. The aim of this article is to give an introduction into plasma spectrometry and its application in materials science. A theoretical overview of the used plasma techniques and a review on applications with a special focus on direct solid sampling will be presented.
Elemental impurities (EI) in medicinal products for human use are limited according to ICH guideline Q3D, which is in force since December 2017 in Europe and US.
As a consequenceconsequence, the relevant texts of the European Pharmacopoeia (Ph. Eur.) and the United States Pharmacopeia (USP) have been modified to reflect and complement ICH Q3D, providing details on the analytical methods to be used. In those chapters (Ph. Eur. 2.4.20., USP <233>), it is stated that for the quantification of elemental impurities, certified reference materials (CRM) from a national metrology institute (NMI) or reference materials that are traceable to the CRM of an NMI should be used.
The Ph. Eur. has so far implemented elemental impurity standards of this type for the four most important elemental impurities i.e. those corresponding to ICH Q3D Class 1: lead, cadmium, mercury and arsenic.
The poster provides details on the development of those four reference standards, which was undertaken in partnership with a major institute accredited CRM producer (JRC, European Commission), and a national metrology institute (BAM and PTB, Germany), and a Designated Institute and accredited CRM producer (BAM, Germany). The reference standards were established and characterised according to rigorous metrological principles and are supplied with extended supporting information as required for the intended use.
After successful completion of the project, the four reference standards have been added to the Ph.Eur. catalogue and are in distribution. It is expected that another three elemental impurity standards will be implemented and made available to users within the next three years.
Messergebnisse in der chemischen Analyse müssen vergleichbar sein. Dies wird durch die metrologische Rückführbarkeit (traceability) auf SI realisiert. In der Chemie dienen Reinststoffe als Primärnormale, deren Reinheit mit einer Unsicherheit von < 0.01% ermittelt werden soll. Ein eleganter Weg, die Reinheit eines realen Materials mit hoher Präzision zu bestimmen, ist, alle Verunreinigungen zu messen, diese aufzusummieren und von der idealen Reinheit von 100 Prozent abzuziehen. Die metallischen Verunreinigungen in Metallen lassen sich mittels hochauflösender Massenspektrometer ermitteln. Eine weit größere Herausforderung ist die Bestimmung von Nichtmetallen wie Sauerstoff, Wasserstoff und Stickstoff im Metall, zumal diese auch oft die Hauptverunreinigung darstellen. Für die quantitative Bestimmung von Verunreinigungen wurden mit Standards dotierte Pulverpresslinge und mit H, O und N dotierte, gesinterte Materialien auf ihre Eignung als Kalibrierstandards für die GD-OES und GD-MS untersucht. Dabei kamen unterschiedliche Plasmabedingungen (pulsed/ continuous mode; verschiedene Plasmagase) zum Einsatz. Ein Überblick über analytische Kenngrößen und Grenzen der verwendeten Kalibrierstrategien wird gegeben.
Für Bauteile (Komponenten) von Versorgungsanlagen für flüssige Brenn- und Kraftstoffe muss die Beständigkeit der metallenen Werkstoffe und Polymere nachgewiesen werden. Im Anwendungsfall von Heizöl mit 20 % biogenen Anteilen in Form von Rapsölfettsäuremethylester (FAME, Biodiesel) ist es für eine konservative Beurteilung des Korrosionssystems Werkstoff/Medium/Umgebung wichtig, die Alterungseffekte des Mediums einzubeziehen.
Entwicklung eines Prüfverfahrens für die Untersuchung der Beständigkeit von metallenen Werkstoffen und Polymeren in Heizöl und Heizöl-FAME-Blends, das für eine Vorauswahl der Werkstoffe und zum Nachweis der Beständigkeit im Hinblick auf die bauaufsichtlichen Zulassungsverfahren geeignet ist. Ein Schwerpunkt wird bei den metallenen Werkstoffen auf der Erprobung von Messmethoden liegen, mit denen sich in kurzer Versuchszeit ein Korrosionsangriff detektieren lässt.
Metallene Werkstoffe:
Weder örtliche Korrosion noch erhöhte Flächenkorrosion (Korrosionsrate:< 0,1 m/Jahr) sind bei den bisher geprüften Werkstoffen: Aluminium,
C-Stahl 1.0037, austenitischer CrNi-Stahl 1.4301, Kupfer und Messing in Heizöl und B20 (Heizöl mit 20% Biodiesel) aufgetreten. Diese Werkstoffe sind in den Prüfmedien Heizöl und B20 als beständig zu bewerten.
Es wurde keine signifikante Veränderung des pH-Wertes der Prüfmedien gemessen.
Polymere:
Massebestimmung:
Die Prüfkörper der Elastomere ACM, HNBR und PUR sowie in geringerem Maße PE neigten zur Quellung in Heizöl und B20 nach 42 d und 84 d Auslagerung; für PA 6, POM und PVC wurde keine Masseänderung gemessen. Die Masseänderung der Prüfkörper in Heizöl und B20 ist mit Ausnahme von PUR vergleichbar. Bei PE traten Verfärbungen durch die Brennstoffe auf.
Zugeigenschaften:
ACM, HNBR, PE und PVC sind in Heizöl und B20 beständig, da die Änderung der Zugfestigkeit und der Reißdehnung < 15 % beträgt. PA und POM sind bedingt beständig, da die Änderung der Zugfestigkeit und der Reißdehnung < 30% beträgt.
Metal phosphonates are metal-organic compounds consisting of a metal core and a phosphonate ligand. Depending on the nature of the ligand, metal phosphonates appear in different structures covering the range from molecular compounds to three-dimensional networks. Due to their structural diversity, the chemistry of metal phosphonates has gained great interest during the last decades. Metal phosphonates can be used for various applications as gas storage and separation, magnetism, and energy conversion. Especially transition metal phosphonates are promising candidates as electrocatalysts. Mechanochemistry is a versatile approach for green and fast synthesis of pure substances. By milling the reactants, various organic, inorganic, and metal-organic compounds can be obtained in high yields. Here, we present the synthesis of different new metal phosphonates obtained by grinding of metal acetates with respective phosphonic acids. By varying the ratio of the reactants, we are able to determine the composition of the final products. The addition of small amounts of liquid to the grinding process tends to increase the product’s crystallinity. The crystal structures of the new compounds were determined from powder X-ray data.
View into the depths of copolymer microstructure by a special approach of LC-MS data evaluation
(2019)
It is a well-known story that copolymers beside their molar mass distribution (MMD) can exhibit a functionality type distribution (FTD), a copolymer composition distribution (CCD), a monomer sequence distribution (MSD) and additionally different topologies within one sample. This is and will remain a challenge for analysts.
First a very short overview will be given concerning the common liquid separation techniques for polymers (SEC, LAC, LCCC, GELC) coupled to soft ionization mass spectrometric methods like MALDI and ESI-MS with focus on their limitations. For very broadly distributed samples or chemical very similar species the superposition of different separation mechanisms in chromatography is unavoidable or the separation efficiency cannot be optimized.
Different ionization probabilities and species of the same nominal mass with completely different structures are just two problems of mass spec of complex polymer mixtures.
Subsequently, different examples will be shown how these limitations in some cases could be outsmarted.
First example will be the separation of statistical EO-PO copolymers of different chemical compositions by end group functionality and the quantification of end group fractions over the whole CCD. Here an UP-LCCC / ESI-TOF-MS coupling is applied.
Further for different kinds of polymers it will be shown how it could be realized to obtain information on small isobaric/isomeric topological heterogeneities by coupling UP-SEC / ESI-TOF-MS.
All results are based on the data processing of reconstructed ion chromatograms of single mass traces of complex ESI-MS spectra.
This work investigates the fire phenomena of rigid polyurethane foams (RPUF) in detail. Rigid polyurethane foams (RPUF) are widely used in industry and daily life because of their outstanding mechanical and thermal insulating properties. In case of fire, cellular polymers like RPUF behave differently from bulk materials, the reason for this is their low thermal inertia. The aim of this study is to investigate the fire phenomena of RPUF in detail. Characterized by simultaneous physical and chemical processes which interact, depend, and compete with each other, the combustion of RPUF is a highly complex occurrence. Therefore it is necessary to study all aspects in detail. The fire phenomena that were examined are gasification, liquefaction, charring and structural integrity as well as collapse. The comprehensive understanding of the processes taking place during combustion is the foundation of customized development of successful flame retardant approaches. Advanced cone calorimeter investigations provide insight into the fire behavior under forced flaming conditions. Thermocouples in the inside of specimens give information about the temperature gradient and temperature of the pyrolysis zone during combustion. Changes in the morphology and thickness of the pyrolysis zone were examined using a hot-stage microscope, as well as SEM images of cross-sections of quenched foam specimens. Furthermore, fire phenomena were characterized using LOI and thermal analysis. By using a multimethodological approach and systematically varied sets of Polyurethane and Polyisocyanurate foams, new insights into the burning of RPUF were won. The detailed knowledge of fire phenomena is essential for future development of tailored flame retardant strategies for RPUF.
Nominal-actual comparisons are routinely performed to compare a manufactured specimen to a reference specimen. X-ray Computed Tomography (CT) has brought a profound change in the way that tolerance verifications are performed in industry, by allowing the inner and outer geometries of an object to be measured, without the need for external access or destructive testing. As a results, CT is increasingly used in additive manufacturing applications, where a nominal-actual comparison performed between the digital model (CAD file), used as an input for the 3D printer, and the CT volume from the printed part, can provide invaluable information as to the accuracy of the printing process. However, the nominal-actual comparison process is somewhat different when applied to additively manufactured specimens by comparison to conventionally manufactured specimens.
Nominal-actual comparisons are routinely performed to compare a manufactured specimen to a reference specimen. X-ray Computed Tomography (CT) has brought a profound change in the way that tolerance verifications are performed in industry, by allowing the inner and outer geometries of an object to be measured, without the need for external access or destructive testing. As a results, CT is increasingly used in additive manufacturing applications, where a nominal-actual comparison performed between the digital model (CAD file), used as an input for the 3D printer, and the CT volume from the printed part, can provide invaluable information as to the accuracy of the printing process. However, the nominal-actual comparison process is somewhat different when applied to additively manufactured specimens by comparison to conventionally manufactured specimens.
One of the great strengths of X-ray computed tomography over conventional inspection methods (ultrasound, thermography, radiography) is that it can image damage in 3D. However for curved or deformed composite panels, it can be difficult to automatically ascribe the damage to specific plies or inter-ply interfaces. An X-ray computed tomography (CT) data processing methodology is developed to extract the through-thickness distribution of damage in curved or deformed composite panels. The method is applied to [(0°/90°)2]s carbon fibre reinforced polymer (CFRP) panels subjected low velocity impact damage (5 J up to 20 J) providing 3D ply-by-ply damage visualisation and analysis. Our distance transform approach allows slices to be taken that approximately follow the composite curvature allowing the impact damage to be separated, visualised and quantified in 3D on a ply-by-ply basis. In this way the interply delaminations have been mapped, showing characteristic peanut shaped delaminations with the major axis oriented with the fibres in the ply below the interface. This registry to the profile of the panel constitutes a significant improvement in our ability to characterise impact damage in composite laminates and extract relevant measurements from X-ray CT datasets.
The ubiquitous presence of unwanted plastics in the environment, especially microscale particles, has been an issue in scientific studies and public debate in the last years. It is well known that oxidative degradation and subsequent fragmentation, caused by UV-radiation, oxidative aging and abrasion lead to the decomposition of larger plastic products into microplastics (MP). Possible effects of these MP on ecosystems are still unclear. Recent studies on MP findings are focused mainly on aquatic systems, while little is known about MP in terrestrial ecosystems.
A possible source of MP input into the soil is compost from domestic bio-waste. Inappropriate waste separation causes plastic fragments in the bio-waste, some of which end up in the compost. In Germany compost is used as fertilizer in agriculture, hence MP could enter the soil by this pathway. So far, there have been only a few studies on this object. For this reason, analysis of compost as a sink and source of MP in ecosystems is of high interest.
To estimate and monitor the MP content in compost and soil, fast and harmonised analytical methods are essential, which not only measure the polymer type and number of particles, but also the mass content. The most common spectroscopic methods are very time-consuming, often require complex sample preparation steps and cannot determine mass contents. Therefore, we used ThermoExtractionDesorption-GasChromatography-MassSpectrometry (TED-GC-MS) as a fast, integral analytical technique. The sample is pyrolyzed to 600°C in a nitrogen atmosphere and an excerpt of the pyrolysis gases is collected on a solid phase adsorber. Afterwards, the decomposition gases are desorbed and measured in a GC-MS system. Characteristic pyrolysis products can be used to identify the polymer type and determine the mass contents. This method is well established for the analysis of MP in water filtrate samples.
In the present work we optimized the TED-GC-MS method for compost and compost/soil matrix and very common polymers, such as polyethylene, polypropylene, polyethylene-terephthalate and polystyrene (sample mass, detection limits, interfering signals, etc.). Additionally, specific pyrolysis products of polymers used for bio-waste bags, such as polylactide (PLA) and polybutylenadipat-terephthalat (PBAT) had to be identified and evaluated.
First measurements were carried out on model and real samples from prepared mixtures and composting plant. The samples were sterilized, fractionated, filtered and dried. In addition, half of the sample material was treated with hydrogen peroxide to investigate a possible effect on detection.
In this study, the molecular dynamics of a series of dipole functionalized triphenylene-based discotics, forming a columnar mesophase, were investigated by broadband dielectric spectroscopy (BDS). In addition to conductivity and localized dynamics, glassy dynamics were also observed. At higher temperatures an α1-processes and at low temperatures an α2 processes were detected having a completely different temperature dependence of its relaxation times. Different molecular assignments of α1- and α2-processes are suggested. The phase behavior of the material was explored under helium purge down to 100 K by differential scanning calorimetry (DSC). Besides the phase transition temperatures and enthalpies, one or two thermal glass transitions were found for all the materials. Moreover, the glassy dynamics were further investigated by Flash DSC, which is a chip-based calorimetry technique allowing for fast heating and cooling rates as high as 10000K/s.
Despite abundant evidence of the occurrence of microplastics (MP) – these are particles smaller 5 mm – in aquatic environments, little is known about the accumulation of plastic in terrestrial environments, especially in soils.
Possible major input pathways could be the use of plastic mulching, the use of compost, sewage sludge or residues from biogas facilities as fertilizers, as well as littering in urban areas. To estimate the MP pollution, the development of reliable, fast methods for sampling, sample preparation, and detection is needed. The obtained data must be representative of the sampled environmental compartment and measurements from different environmental compartments must be comparable. A first breakthrough is an application of ThermoExtractionDesorption-Gas Chromatography-MassSpectrometry (TED-GC-MS) for the detection of MP, including tire abrasives. This method allows the determination of mass content within a few hours and only a minimum of sample preparation for samples from aquatic environments is needed.
However, in contrast to filtrate samples from aquatic environments, sediment or soil samples need an enrichment of MP. Whereas MP concentration from marine sediments can be obtained by floatation and density Separation techniques using NaCl solutions, the extraction or separation from soils proves to be more difficult, as plastic particles are often part of organo-mineral aggregates within the soil matrix.
The aim of this study is the development of a practicable processing guideline for representatively taken soil samples in order to concentrate microplastics, without complex and time-consuming treatment steps. Dispersants or detergents can be applied to decompose the soil matrix, but each preparation step carries the risk of crosscontamination of the sample and prolongs the preparation procedure.
For this reason, we choose ZnCl2-solution with a density of 1.7 g/cm3, which include the densities of relevant MP types (0.9-1.7 g/cm3). It was tested to achieve both, disaggregation and separation as it decomposes organic material and dissolves carbonates. Also, ZnCl2 is inert to the precipitation of undesirable salts and Carbonates during the process of density separation, as polytungstate solution does. ZnCl2 can be reused after stepwise filtering (7 µm, 1.5 µm, 0.7 µm). Thus, disposal costs can be reduced. Efficiency and reproducibility of the sample preparation as well as the degradation behavior of MP under the present conditions were demonstrated with model samples.
Real sampling campaigns were conducted at several agricultural sites and floodplains in south-west Germany. The sampling was performed according to practice for soil sampling, using adequate sampling strategies (pattern of sampling, number of field samples, homogenization, etc). The lab sample was fractioned into three size classes (5-100 µm, 100-1000 µm, and 1-5 mm). The identification and determination of mass fraction were done using TED-GC-MS.
While plastics have become indispensable in our daily lives over the last decades, the input into the environment has been increasing concurrently. Plastics often end up in the environment because of intensive use and poor waste management practice. They are subjected to aging and fragmentation and finally be deposited as microplastic particles or in short microplastics (MP). MP are defined as particles originating from synthetic polymers between 1 µm and 5 mm.
Although the pervasive abundance of MP in aquatic environments has been demonstrated comprehensively, less is known about the occurrence and fate of MP in terrestrial ecosystems. It is still unclear if soil functions as a MP source or a sink for aquatic environments. MP can either be transported into water bodies by soil erosion or be retained in soils. The few studies published are not comparable because of non-existent harmonized and standardized methods for sampling, sample preparation, and analysis.
For an assessment of a potential exposure situation of MP, the determination of a mass content in the soil is crucial. Consequently, spectroscopic methods like Raman or FTIR are not suitable, as they deliver information about the shape and size of individual particles. Therefore, we show the application of ThermoExtractionDesorption-GasChromatography-MassSpectrometry (TED-GC-MS) for MP analysis in the soil. In this method, the soil sample is heated up to 600 °C in a nitrogen atmosphere. The decomposition gases are sorbed on a solid phase, then transferred to a GS-MS system where they are desorbed, separated and identified. The method allows the rapid identification of individual polymers through the detection of specific decomposition products, but also the quantitative determination of the MP mass. Besides thermoplastics, elastomers originated from tire abrasion, can be detected.
In the present study, several terrestrial ecosystems in south-west Germany were systematically sampled. Subsequent sample preparation included sieving in fractions of 5-100 µm, 100-1000 µm, and 1-5 mm. MP were extracted by density separation using ZnCl2 solutions. The detection was done by TED-GC-MS measurements. Data of agricultural areas and floodplains are presented exemplarily. A quantitative assessment of highly occurring MP from littering as well as tire abrasion is conducted.
Particle scattering simulations are an useful tool to plan experiments, design detectors, estimate doses in irradiated materials and medical treatment planning.
Geant4 is a Monte-Carlo toolkit for the simulation of of particles scattering in matter. Photons, electrons, ions etc can be simulated with energies in the eV to GeV range. Their interactions with matter in arbitrary scattering geometries be studied. Scattering models, cross sections and material parameters can be set to cover interactions in gas, liquid and solid state. The import of geometries from computer aided design files or the protein data base is possible.
It is currently being applied in high energy and nuclear physics, accelerator and detector design, space application, dosimetry and medical sciences.
In this first part of the talk a brief overview over the structure, functionality and possible applications of Geant4 will be given. In the second part an example application will be presented: The determination of the microscopic dose-damage relations in aqueous environment for electron irradiated plasmid DNA will be explained. Therefore, we combine electron scattering simulations in water with calculations concerning the movement of biomolecules to obtain the energy deposit in the biologically relevant nanoscopic volume. We present, how to combine these simulational results and experimental data via a generalized damage model to determine the microscopic dose-damage relation at a molecular level.
The reassessment of bridges is becoming increasingly important. The basic requirement for analyses of structural safety is reliable knowledge about individual structures. This paper introduces the new approach to evaluate the quality of measured data gained from non-destructive testing (NDT) to provide reliable, objective, and relevant information about existing bridges. The purpose is to relate this validated knowledge to probabilistic analyses. Bridging the gap between NDT and numerical reassessments indicates reduced numerical uncertainties and residual service time extensions. This paper deals with an application of this approach using measurement data collected by ultrasonic technique at a prestressed concrete bridge.
The determination of microscopic dose-damage relations in aqueous environment is of fundamental interest for dosimetry and its application in radiation-therapy and protection. We present a combined experimental and simulational approach to quantify the microscopic energy deposit at biomolecules in liquid environment which is applicable to a wide range of primary radiation sources, e.g. photons, electrons or ions, and targets, such as DNA, proteins or cells.Therefore, we combine Geant4 particle-scattering simulations in water with calculations concerning the movement of biomolecules to obtain the energy deposit in the biologically relevant nanoscopic volume. We present, how to combine these simulational results and experimental data via a generalised damage model to determine the microscopic dose-damage relation at a molecular level.
To show the viability of this approach, we apply this method to an experimentally challenging system, the direct irradiation of plasmid DNA (pUC19) in water with electrons as primary particles. Here we combine electron-scattering simulations with calculations concerning the diffusion and convection induced movement of the DNA, within a coarse-grained model of the irradiated liquid. Additionally a microscopic target model for DNA molecules based on the relation of lineal energy and radiation quality is used to calculate their effective target volume.
It was found that on average fewer than two ionisations within a 7.5\,nm radius around the sugar-phosphate backbone are sufficient to cause a single strand break, with a corresponding median lethal energy deposit being E\textsubscript{1/2}=6+-4\,eV. The presented method is applicable for all types of ionising radiation and a broad variety of biological targets.
High performance polymers of intrinsic microporosity (PIMs) have emerged as novel materials with broad applications from gas separation to electronic devices. Sufficiently rigid, even contorted polymer chains show only limited molecular mobility, therefore undergo inefficient packing and give rise to intrinsic microporosity with pore size generally smaller than 1 nm and BET surface areas larger than 700 m2/g. Further performance optimization and long-term stability of devices incorporating PIMs rely on our understanding of structure-processing-property relationships and physical aging, in which glass transition plays a key role. Up to now no glass transition temperature (Tg) of PIMs could be detected with conventional thermal analysis techniques before degradation. Decoupling the time scales responsible for the glass transition and the thermal decomposition is a reliable strategy to overcome this. This was achieved by employing fast scanning calorimetry (FSC) based on a chip sensor, which is capable to heat and cool a small sample (ng-range) with ultrafast rates of several ten thousand K/s. FSC provides definitive evidence of glass transition of a series of PIMs with a special consideration on the chain rigidity. The determined glass transition temperature of these PIMs follows the order of the rigidity of their backbone structures. FSC provides the first clear-cut experimental evidence of the glass transition of PIM-EA-TB with a Tg of 663 K, PIM-1 of 644 K and PIM-DMDPH-TB of 630 K at a heating rate of 1Χ104 K/s. Local fluctuations are featured in glass transition of highly rigid PIMs. As conformational changes are prevented by the backbone rigidity, the glass transition must rather be assigned to local small scale fluctuations.
Polymeric membranes represent a low-cost, energy efficient solution for gas separation. Recently polymers of intrinsic microporosity (PIMs) have emerged as prestigious membrane materials featuring a large concentration of pores smaller than 1 nm, a BET surface area larger than 700 m2/g and high gas permeability and selectivity. Unusual chain structure combining rigid segments with sites of contortion gives rise to the intrinsic microporosity. However, this novel class of glassy polymers are prone to pronounced physical aging. The initial microporous structures approach a denser state via local small scale fluctuataions, leading to a dramatic reduction in the gas permeabilities. For the first time, dielectric relaxation spectroscopy with state-of-the-art high-resolution analyzers was employed to investigate three representative PIMs with a systematic change in chain rigidity: PIM-EA-TB 〉 PIM-1 〉 PIM-MDPH-TB. The molecular mobility, the charge transport and their response upon heating (aging) in the polymers were measured in a broad temperature range through isothermal frequency scans during different heating / cooling cycles. Multiple dielectric processes following Arrhenius behavior were observed for the investigated polymers. Local fluctuations, Maxwell-Wagner-Sillars (MWS) polarization and structural relaxation phenomena were discussed and attempted to be correlated with the structural features of PIMs. Moreover, all PIMs showed conductivity in the glassy state. The significant increase in the conductivity with increasing temperature far below the glass transition temperature of PIMs is explained in terms of the loosely packed microporous structure and the formation of local intermolecular agglomerates due to interaction of π-electrons in aromatic moieties of the polymer backbone.
An equation for wind vector estimation using a multirotor aircraft as a flying anemometer is shown. To compute the wind vector an estimate of the thrust of the aircraft is required, which is related to the rotational speed of the rotors. Hence, a sensing system for the rotational speed using phototransistors is presented.
In this paper, we present an autonomous aerial robot to reconstruct tomographic 2D slices of gas plumes in outdoor environments. Our platform, the so-called Unmanned Aerial Vehicle for Remote Gas Sensing (UAV-REGAS) combines a lightweight Tunable Diode Laser Absorption Spectroscopy (TDLAS) sensor with a 3-axis aerial stabilization gimbal for aiming on a versatile octocopter. The TDLAS sensor provides integral gas concentration measurements but no information regarding the distance traveled by the laser diode's beam or the distribution of the gas along the optical path. We complemented the set-up with a laser rangefinder and apply principles of Computed Tomography (CT) to create a model of the spatial gas distribution from these integral concentration measurements. To allow for a rudimentary ground truth evaluation of the applied gas tomography algorithm, we set up a unique outdoor test environment based on two 3D ultrasonic anemometers and a distributed array of 10 infrared gas transmitters. We present first results showing the 2D plume reconstruction capabilities of the system under realistic conditions.
In industrial environments, airborne by-products such as dust and (toxic) gases, constitute a major risk for the worker’s health. Major changes in automated processes in the industry lead to an increasing demand for solutions in air quality management. Thus, occupational health experts are highly interested in precise dust and gas distribution models for working environments. For practical and economic reasons, high-quality, costly measurements are often available for short time-intervals only. Therefore, current monitoring procedures are carried out sparsely, both in time and space, i.e., measurement data are collected in single day campaigns at selected locations only. Real-time knowledge of contaminant distributions inside the working environment would also provide means for better and more economic control of air impurities. For example, the possibility to regulate the workspace’s ventilation exhaust locations can reduce the concentration of airborne contaminants by 50%.
To improve the occupational health and safety of (industrial) workplaces, this work aims for developing a swarm of gas-sensitive aerial nano robots for monitoring indoor air quality and for localizing potential emission sources.
Luminescence techniques are amongst the most commonly used analytical methods in life and material sciences due to their sensitivity and their nondestructive and multiparametric character. Photoluminescence signals are, however, affected by wavelength, polarization and time dependent instrument specific effects, and provide only relative intensities. This hampers the comparability of fluorescence measure-ments and calls for simple tools for instrument characterization and the quantification of measured fluorescence intensities. Well characterized fluorescence standards for instrument calibration and performance validation (IPV) can be used as references for fluorescence signals. Of special importance is the correct determination of photoluminescence quantum yields (QF) (number of emitted per absorbed photons) that provides a direct comparison of the fluorescence efficiency of emitters. Such well characterized standards have been successfully developed by BAM for the relative determination of f values of transparent solutions of molecular and nanoscale emitters in the wavelength range from 350 and 1100 nm and will be soon certified. These standards can also be used to evaluate integrating sphere setups, which are increasingly being used for absolute measurements of QF values.
Digital holographic cytometry (DHC) is a state-of-the-art quantitative Phase imaging (QPI) method that permits time-lapse imaging of cells without induced cellular toxicity. DHC platforms equipped with semi-automated image segmentation and analysis software packages for assessing cell behavior are commercially available. In this study we investigate the possible uptake of nanoprobes in macrophages in vitro over time.
The European building sector is moving towards more complex and high-tech building approaches. While focusing on energy efficiency, aspects e.g. occupant health, sustainability and life cycle costing are often neglected. This study highlights the potential of earthen plasters in combination with natural ventilation for low-tech solutions.
The EU funded project [H]house established the outstanding performance of earthen materials in light of hygrothermal and air purifying properties, which were further supported by experimental data from monitoring of naturally ventilated pilot buildings in Berlin. Additionally, [H]house demonstrated through LCC an increased cost efficiency of earth based low-tech solutions in comparison to conventional constructions relying on mechanical ventilation.
Während des Entladungsprozesses interagieren Mikrohohlkathodenentladungen (engl. micro hollow cathode discharges) durch verschiedenste physikalische Phänomene mit ihrer Umgebung. Analog zu Funken- und Koronaentladung treten neben den optischen Erscheinungen auch akustische Wechselwirkungen bis in den Ultraschallbereich auf. Diese Wechselwirkungen sind bisher jedoch nur selten Gegenstand der Forschung gewesen. Durch elektro-chemischen Prozesse und die Stromdichteverteilung während des Zündvorgangs erfährt das angrenzende Fluid eine, durch den thermoakustischen Effekt hervorgerufene, rapide Dichteänderung und erzeugt somit eine akustische Emission. Dieser Beitrag gibt einen Überblick über den letzten Stand der akustischen Beschreibung der Mikrohohlkathode. Weiterhin wird anhand von Anwendungsbeispielen, wie der Charakterisierung von akustischen Sensoren, sowie der Nutzung innerhalb der zerstörungsfreien Werkstoffprüfung, die Nutzung dieser Entladungsart präsentiert. Darüber hinaus erlaubt die Kenntnis hinsichtlich der akustischen Eigenschaften der Entladung wichtige Rückschlüsse im Rahmen der Plasmadiagnostik.
Die Brücken im Netz der Bundesverkehrswege sind überwiegend in einem ausreichenden bis guten Zustand. Allerdings steigt der Unterhalts- und Sanierungsaufwand aufgrund des inzwischen hohen Alters vieler Brücken sowie des ständig wachsenden Schwerlastverkehrs. Techniken zur Einschätzung der verbleibenden Lebensdauer von Brücken sowie zur dauerhaften Beobachtung des Tragverhaltens bzw. des Erfolges von Sanierungsmaßnahmen werden daher für den sicheren und wirtschaftlichen Betrieb dringend benötigt. Zur Evaluierung dafür geeigneter holistischer Ansätze wurde in der BAM das Projekt BLEIB - Bewertung, Lebensdauerprognose und Instandsetzung von Brückenbauwerken - ins Leben gerufen.
Ein zentrales Ergebnis des Projektes ist eine extern vorgespannte Stahlbetonbrücke als Zweifeldträger mit einer Gesamtlänge von 24 m, die für den Test verschiedenster Sensorsysteme, zur Validierung numerischer Modelle und zur Erprobung von Sanierungs- und Verstärkungsmaßnahmen entwickelt wurde. Für die Simulation unterschiedlicher Schädigungsgrade kann die Vorspannung der Brücke variiert werden. Die Brücke wird mit beweglichen Gewichten belastet und über einen Shaker zum Schwingen angeregt.
Das Brückenmodell wurde bewusst geschädigt, indem die Vorspannung der Struktur erstmalig schrittweise bis auf null reduziert wurde. Unter der Eigenlast verformte sich die Brücke, wodurch eine Rissbildung im Beton einsetzte. Die Zugspannung, die zuvor durch die Vorspannung aufgenommen wurde, übernahm Schritt für Schritt der Beton. Als die Zugspannungen die relativ geringe Zugfestigkeit des Betons überstiegen, begann dieser zu reißen und die schlaffe Bewehrung der Struktur nahm die Spannungen auf. Dieser Versuch wurde unter anderem von Schallemissionsmessungen begleitet. Der Rissbildungsprozess konnte damit, bei gleichzeitiger Aufzeichnung der Vorspannung, früh detektiert und die Risse geortet werden. Die Ergebnisse korrelieren gut mit den Ergebnissen der stereophotogrammetrischen Verformungsmessungen der Struktur.
Bestimmung der Rissgeometrie bei der zerstörungsfreien Ultraschallprüfung mit geführten Wellen
(2019)
In der zerstörungsfreien Prüfung werden in zunehmendem Maße geführte Ultraschallwellen zur Lokalisation von Fehlstellen genutzt. Geführte Ultraschallwellen zeichnen sich dadurch aus, dass sie große Distanzen innerhalb des zu prüfenden Bauteiles zurücklegen können. Das Ultraschallwellenfeld setzt sich dabei aus verschieden Moden zusammen. Etablierte Prüfverfahren mit geführten Wellen ermitteln häufig nur die Position der Fehlstelle, wobei die Laufzeiten der reflektierten Signale ausgewertet wird. Modenumwandlung bleibt dabei zumeist unberücksichtigt.
Die Charakterisierung der Fehlstelle, zum Beispiel hinsichtlich der Länge eines Risses, ist dagegen herausfordernd. Aussagekräftige Zusammenhänge zwischen der Dimension oder Geometrie der Fehlstelle und ihrer Interaktion mit der Ultraschallwelle zu finden, ist Teil aktueller Forschung. Insbesondere eine Betrachtung der Moden höherer Ordnung und deren Amplitudenverhältnisse kann beim Aufspüren dieser Zusammenhänge hilfreich sein.
Im Beitrag werden zunächst die Zusammenhänge zwischen den beiden fundamentalen Moden in einer isotropen Platte und der Länge eines Risses untersucht. Aus den Ergebnissen wird ein inverses Verfahren motiviert. Ein Algorithmus wird vorgestellt, der die Risslänge im Modell solange variiert, bis er die modalen Zusammenhänge einer Vorgabe oder einer Messung rekonstruiert. Die eingesetzte Scaled Boundary Finite Element Method ermöglicht dabei eine sehr kurze Rechenzeit in jeden Optimierungsschritt. Zusätzlich ermöglicht die Methode eine Auswertung der modalen Zusammenhänge ohne Postprocessing, was die Rechenzeiten weiter verkürzt.
Die Messung von Flüssigkeitskonzentrationen in Rohrsystemen ist von großem Interesse für viele unterschiedliche Anwendungen. Die meisten Messsysteme sind jedoch nicht in der Lage, die Flüssigkeit direkt im Rohr zu untersuchen und es muss eine zusätzliche Vorrichtung, wie z.B. einem Bypass, angebracht werden, welche den Kontakt zwischen Flüssigkeit und Sensor ermöglicht.
Um den Einbauaufwand gering zu halten und die Strömungseigenschaften des Rohres nicht zu beeinflussen, wird ein neuartiges Messsystem entwickelt, welches als Teil der Rohrwand ausgeführt werden kann. Dieses neuartige System ist angelehnt an die Idee der phononischen Kristallen (PnK). PnK’s bestehen im Allgemeinen aus einem Matrixmaterial, in welchem Streuzentren periodisch angeordnet sind. Dies führt beim Eintreffen einer akustischen Welle in definierten Frequenz-bereichen, sogenannter Bandlücken, zu zunehmender destruktiven Interferenz. Wird innerhalb einer solchen Bandlücke durch Einbringen einer flüssigkeitsgefüllten Kavität ein Resonanzverhalten erzeugt, kann dies genutzt werden, um die Flüssigkeit zu analysieren.
Im Rahmen von Voruntersuchung wird zunächst das akustische Verhalten des PnK’s, welcher für die Sensorentwicklung genutzt werden soll, unter Vernachlässigung der Flüssigkeit ausführlich untersucht. Hierbei werden zunächst die Bandlücken ermittelt und das Übertragungsverhalten betrachtet. Dieses wird im Anschluss experimentell überprüft.
New Focus On Boehmite-Reinforced Nanocomposites Molecular Approach With Advanced FTIR-Techniques
(2019)
By FTIR-study it was possible to proof a chemical reaction between boehmite and the hardener of anhydride cured epoxy resins. Future studies can assume that the chemical environment of the resin system is changed in the surrounding of boehmite nanoparticles. This highly affects especially localized properties.
Fibreoptic sensors (FOS) represent sensing technology with small footprint, low invasiveness, electromagnetic passivity and immunity, plus potential for remote and real-time monitoring. Modern FOS techniques allow truly temporally- and spatially-continuous monitoring over extended distances; a feature not attainable with any other sensing technology. Moreover, depending on their particular material composition and design, optical fibres can be made resistant to high temperatures, chemicals and ionizing radiation. Due to this unique combination of advantageous properties, ever since their emergence, FOS have been attracting considerable attention for monitoring tasks in harsh, hazardous and difficult-to-access locations. The potential of FOS has been recognized also in the field of radioactive waste management and fibreoptic sensors belong to the most promising technologies for nuclear waste repositories (NWR) monitoring.
Vast majority of distributed fibreoptic sensor applications rely on use of silica-based optical fibres as sensing elements. At the same time, distributed measurement of local temperature and strain along the fibre are the most common monitoring tasks addressed by fibreoptic sensors. Nevertheless, FOS offer much larger flexibility both in terms of utilized sensing fibre as well as targeted measurand. In this contribution, we will review some of more alternative implementations of FOS that are being explored at “Fibre Optic Sensors” division of Federal Institute for Material Research and Testing (BAM), in Berlin. The main focus will be twofold. On one side, we will address FOS applications with polymer optical fibres (POF), that may enable monitoring of large strains (>100%) and high-sensitivity radiation detection. On the other side, we will present our activities in the area of distributed acoustic sensing (DAS); one of the most recent developments in the fibreoptic sensing field enabling highly-dynamic vibration sensing with nanostrain sensitivity. We will introduce the principles of the addressed FOS technologies, present application examples from our case studies, discuss advantages and limitations of the techniques and highlight their potential for NWR monitoring.
Ultrashort laser pulse micromachining features a high precision. By increasing the repetition rate of the applied laser to several 100 kHz, laser processing becomes quick and cost-effective and make this method attractive for industrial applications. Upon exceeding a critical laser intensity, hard X-ray radiation is generated as a side effect. Even if the emitted X-ray dose per pulse is low, the accumulated X-ray dose becomes significant for high-repetition-rate laser systems so that radiation safety must be considered.
Der vorliegende Vortrag gibt einen Überblick über Probenpräparationen mit der Focused Ion Beam (FIB) für AFM-basierte Untersuchungsverfahren. Anhand zweier Beispiele wird gezeigt, wie ionenstrahlpolierte Lamellen aus Halbleiter-Schichtsystemen elektrisch leitfähig auf Substrate platziert werden, so dass in-situ und in-operando Messungen mit Scanning Microwave Microscope (SMM) bzw. Spectroscopic infrared scanning near-field optical microscope (IR-SNOM) durchgeführt werden können.
The closure of underground nuclear waste disposal facilities requires reliable gas- and water-tight engineered barriers. In Germany, barriers made from salt concrete have been evaluated in full scale. While the barriers seem to fulfill the requirements regarding permeability, some unexpected cracks have been detected at the surface and at depth. In cooperation between the Federal Company for Radioactive Waste Disposal (BGE) and the Federal Institute for Materials Research and Testing (BAM), several experiments have been carried out to evaluate the applicability for ultrasonic measurements in crack detection and general quality assurance. Both commercial instruments and specially developed devices have been tested on site.
Using commercial ultrasonic echo devices designed for concrete inspection it was possible to detect cracks and objects in salt concrete up to a depth of 2 m. The check for delamination in shotcrete is another field of application. A unique device available at BAM, the wide aperture, deep penetration instrument LAUS, was able to locate cracks and objects up to a depth of 8 m so far, which is thought to be a record for ultrasonic echo measurements in concrete. Adapted imaging procedures, partly adopted from geophysics, helped to reveal 3D structure at depth.
In addition, we have developed ultrasonic probes to be deployed in boreholes, currently at up to 20 m depth. They can collect information on cracks and other features in a radius of about 1.5 m around the borehole in the current version and might be used in echo or transmission mode. Evaluation experiments have been performed at an experimental barrier at the ERAM site in Morsleben, Germany. The results showed several empty and injected cracks as well as built-in instrumentation. The results have been verified using borehole endoscopy as well as core examination and will be used to set up a reliable quality assurance system for engineered barriers. All instruments are based on ultrasonic shear wave transducers with a frequency range between 25 kHz and 100 kHz. Current research focuses on the improvement of the hardware (e. g. optimization of array characteristics) and imaging techniques such as Reverse Time Migration, both aiming at the improvement of depth of penetration, resolution and probability of detection.
Evolution of a friction material with braking sequence: properties related to the microstructure
(2019)
The microstructural complexity (multi-component and multi-scale) of friction materials, such as those used in braking applications,usually limits the characterization to the pristine state, even when they are to be submitted to high loading brake sequences. The understanding of properties ageing as a function of load history and microstructure is an important step to gain further knowledge on the tribological mechanisms occurring at the contact surface, as well as on the braking performances. To do so, the bulk mechanical and microscopical properties of a semi-metallic friction material are investigated before and after a braking sequence. Uniaxial compression tests combined with DIC are used to study the axial evolution of the mechanical behaviour (i.e., from the contact surface to the backplate). A significant mechanical evolution is observed in the after-braking material, which develops a layered behaviour along the depth. The layers (three) exhibit distinct mechanical/microstructural features that can be related to the braking thermal gradients and the occurrence of local damage.
The proposed BAM project SealWasteSafe will advance the state of the art for the construction and monitoring of safe sealing systems for underground repositories of radioactive or toxic waste. During this project, a novel salt concrete exhibiting neither significant cracking nor shrinkage will be optimized for use in the sealing systems. The composition of this material will be based on alkali-activated materials, which are characterized by particularly small thermal deformations during the hardening reaction. Quality assurance and continuous monitoring systems developed during this project will be demonstrated not only for high reliability, but also for resistance to highly alkaline environments and to water intrusion along cables or at sensor locations. A variety of sensors will be used in combination with wireless Radio Frequency Identification (RFID) technology to record moisture, temperature, and, if necessary, corrosion activity within the sealing system. Distributed Fibre Optic Sensor (FOS) technology will also be used for strain, temperature, and moisture content measurement. Ultrasound-based measuring methods will be utilized for the detection of cracks and delaminations. Additionally, digital image correlation and acoustic emission analysis will be used for deformation measurements and crack detection. A novel borehole probe and advanced ultrasound imaging techniques will be further developed to track cracks and delaminations within the host rock in 3D. The surface-based Large Aperture Ultrasound System (LAUS) will also be utilized to detect cracks and delaminations deep below the exterior surface of the sealing system. Although the focus of this project will be on the host rock salt, the resulting technologies will be intentionally developed in a way that facilitates their adaptation to other host rocks.
In this work, the structural integrity of LBM fabricated IN625 small cylinders (d = 1 mm, h = 6 mm) was investigated regarding the porosity and the surface roughness by means of computed tomography. The measurements were carried out on a GE v|tome|x L 300/180 with a reconstructed voxel size of 2 µm. The pores were analyzed for size, shape and spatial distribution. The correlation between compactness C and spatial distribution showed that elongated pores (C < 0.2) appear exclusively within a distance of 80 µm to the sample surface. The reconstructed surface was digitally meshed and unwrapped to evaluate the mean roughness Ra. Since the gravity correlates linearly with the sine of the build angle, the influence of gravity on porosity and surface roughness was determined.
Die Brücken im Netz der Bundesverkehrswege sind überwiegend in einem ausreichenden bis guten Zustand. Allerdings steigt der Unterhalts- und Sanierungsaufwand aufgrund des inzwischen hohen Alters vieler Brücken sowie des ständig wachsenden Schwerlastverkehrs. Techniken zur Einschätzung der verbleibenden Lebensdauer von Brücken sowie zur dauerhaften Beobachtung des Tragverhaltens bzw. des Erfolges von Sanierungsmaßnahmen werden daher für den sicheren und wirtschaftlichen Betrieb dringend benötigt. Zur Evaluierung dafür
geeigneter holistischer Ansätze wurde in der BAM das Projekt BLEIB - Bewertung, Lebensdauerprognose und Instandsetzung von Brückenbauwerken - ins Leben gerufen.
Ein zentrales Ergebnis des Projektes ist eine extern vorgespannte Stahlbetonbrücke als Zweifeldträger mit einer Gesamtlänge von 24 m, die für den Test verschiedenster Sensorsysteme, zur Validierung numerischer Modelle und zur Erprobung von Sanierungs- und Verstärkungsmaßnahmen entwickelt wurde. Für die Simulation unterschiedlicher Schädigungsgrade kann die Vorspannung der Brücke variiert werden. Die Brücke wird mit beweglichen Gewichten belastet und über einen Shaker zum Schwingen angeregt.
Das Brückenmodell wurde bewusst geschädigt, indem die Vorspannung der Struktur erstmalig schrittweise bis auf null reduziert wurde. Unter der Eigenlast verformte sich die Brücke, wodurch eine Rissbildung im Beton einsetzte. Die Zugspannung, die zuvor durch die Vorspannung aufgenommen wurde, übernahm Schritt für Schritt der Beton. Als die Zugspannungen die relativ geringe Zugfestigkeit des Betons überstiegen, begann dieser zu reißen und die schlaffe Bewehrung der Struktur nahm die Spannungen auf. Dieser Versuch wurde unter anderem von Schallemissionsmessungen begleitet. Der Rissbildungsprozess konnte damit, bei gleichzeitiger Aufzeichnung der Vorspannung, früh detektiert und die Risse geortet werden. Die Ergebnisse korrelieren gut mit den Ergebnissen der stereophotogrammetrischen Verformungsmessungen der Struktur.
Nanocomposites are extremely versatile due to their physicochemical properties, which differ significantly from bulk homopolymers. One of the inorganic nanomaterials which are increasingly used as a filler in polymer matrices is boehmite, typically used as an inexpensive flame retardant. Here, it is used as a nanofiller in polycarbonate and polyamide, expecting to improve their mechanical properties. For industrial use boehmite is obtained by the solvothermal method, resulting in a layered nanomaterial, whereas naturally it occurs as single crystals with the size of <100µm. In this work we are obtaining and isolating boehmite crystals by a bottom-up method, in which a reaction between aluminum nitride and sodium hydroxide. Obtaining boehmite as microcrystals is necessary for its analysis and characterization, as well as to investigate its interaction with polymer matrices at the polymer/particle interface. Here, the obtained particles in polymer matrices are characterized with differential scanning calorimetry and thermogravimetry analysis.
Nanocomposites are extremely versatile due to their physicochemical properties, which differ significantly from bulk homopolymers. One of the inorganic nanomaterials which are increasingly used as a filler in polymer matrices is boehmite, typically used as an inexpensive flame retardant. Here, it is used as a nanofiller in polycarbonate and polyamide, expecting to improve their mechanical properties. For industrial use boehmite is obtained by the solvothermal method, resulting in a layered nanomaterial, whereas naturally it occurs as single crystals with the size of <100µm. In this work we are obtaining and isolating boehmite crystals by a bottom-up method, in which a reaction between aluminum nitride and sodium hydroxide. Obtaining boehmite as microcrystals is necessary for its analysis and characterization, as well as to investigate its interaction with polymer matrices at the polymer/particle interface. Here, the obtained particles in polymer matrices are characterized with differential scanning calorimetry and thermogravimetry analysis.
In well-annealed thin polymer films, with non-repulsive polymer/substrate interactions, an irreversibly adsorbed layer is formed. These adsorbed layers have shown enormous potential for technological applications. The growth kinetics and molecular dynamics of these buried layers in thin films are still not fully investigated due to the hard accessibility. Here, the irreversibly adsorbed layers of homopolymer thin films are revealed by solvent-leaching experiments. The growth kinetics of these layers is investigated as a function of original film thickness and annealing times. The thickness, topography and quality of the adsorbed layer is determined with Atomic Force Microscopy (AFM) and spectroscopic ellipsometry. Additionally, the molecular mobility of the adsorbed layer is investigated with Broadband Dielectric Spectroscopy (BDS). A recently developed nanostructured capacitor (NSC) is employed to measure the adsorbed layers with a free surface layer depending on annealing and solvent-leaching time. The results are quantitatively compared and discussed with respect to recently published work.
In well-annealed thin polymer films, with non-repulsive polymer/substrate interactions, an irreversibly adsorbed layer is formed. These adsorbed layers have shown enormous potential for technological applications. Due to the hard accessibility of these layers, their growth kinetics and molecular dynamics are still not fully understood. Here, the irreversibly adsorbed layers of Poly(2-vinylpyridine) (P2VP) and Poly(vinyl methyl ether) (PVME) thin films are revealed by solvent-leaching experiments. The growth kinetics of these layers is investigated as a function of original film thickness and annealing times. The thickness, topography and quality of the adsorbed layer is determined with Atomic Force Microscopy (AFM) and spectroscopic ellipsometry. Additionally, the molecular mobility of the adsorbed layer is investigated with Broadband Dielectric Spectroscopy (BDS). A recently developed nanostructured capacitor (NSC) is employed to measure the adsorbed layers with a free surface layer depending on annealing and solvent-leaching time. The results are quantitatively compared and discussed with respect to recently published work.
KonSens (Kommunizierende Sensorsysteme für die Bauteil- und Umweltüberwachung) - Projektergebnisse
(2019)
Im Projekt KonSens werden für die Anwendungsbeispiele bauteilintegrierte Sensorik für Betonkomponenten und mobile Multigassensorik Sensorsysteme in Form von Funktionsmustern entwickelt, validiert und angewendet. Schwerpunkte liegen einerseits in der Detektion und Bewertung von Korrosionsprozessen in Beton und andererseits in der Detektion und Quantifizierung sehr geringer Konzentrationen toxischer Gase in der Luft. Dabei ist die Adaption der sensorischen Methoden aus dem Labor in reale Messumgebungen inklusive geeigneter Kommunikationstechnik ein wichtiger Aspekt.
Over the past decades research on the molecular dynamics of miscible polymer blends is of topical interest in the literature, to understand the segmental mobility of individual components, as it is affected by blending. In general, miscible polymer blends exhibit a complex dynamic behavior. For an A/B blend the relaxation times of component A and component B are affected by the spatial local compositional heterogeneity, present in binary systems on a microscopic level, regardless of the macroscopic homogeneity. Here, a combination of broadband dielectric and specific heat spectroscopy was employed to study the dynamically asymmetric PVME/PS blend with seven different compositions, focusing on samples with high PS contents. Considering that PS is dielectrically invisible, BDS is a powerful technique to study the response of PVME, as it is affected by PS segments. Here, three separate relaxation processes were found by dielectric investigations, related to confined or constrained PVME segments due to the spatial local compositional heterogeneities, which is in contrary to the previous literature findings [1]. Moreover, the dielectric data was compared with results obtained by specific heat spectroscopy, where a fourth relaxation process was found, due to the cooperative fluctuations of PVME and PS.
[1] Colmenero, J., Arbe, A. Soft Matter, 2007, 3, 1474.
For inorganic/polymer nanocomposites a so-called Rigid Amorphous Phase (RAF) is formed in the interfacial region by adsorption of polymer segments onto the nanoparticles. The segmental dynamics of RAF is expected to be altered, as compared to the pure matrix, which might percolate to the entire system, affecting the overall nanocomposite properties. A combination of two relaxation spectroscopy techniques (Broadband Dielectric Spectroscopy (BDS) and Temperature Modulated DSC (TMDSC)) as well as Fast Scanning Calorimetry (FSC) was employed to investigate the structure and molecular mobility of nanocomposites based on Epoxy and Layered Doubled Hydroxides with different nanoparticle content. First, BDS investigations proved the existence of a process, which is present only for nanocomposites, assigned to the dynamics of polymer segments within RAF. Second, the amount of RAF was quantified by analyzing the change of specific heat capacity step of nanocomposites, comparing to the pure material. Thirdly, the glass transition of nanocomposites was studied with FSC, applying high heating rates (0.5-10 kK/s). Considering that all techniques probe essentially the same molecular process, an activation plot was constructed, delivering a complete picture of the molecular mobility and structure of the polymer nanocomposites including RAF.
Die zeitaufgelöste THz-Spektroskopie (THz-TDS) operiert mit elektromagnetischen Impulsen, die ein Amplitudenspektrum im unteren THz-Bereich aufweisen. Die THz-TDS ist in der Lage, dielektrische Volumina zerstörungs- und kontaktfreie zu durchstrahlen. Um eine 3D-THz Bildung zu ermöglichen, wurde für die THz-TDS ein rechnergestütztes Mess- und Rekonstruktionsverfahren (THz-TD-SAFT) entwickelt, mit dem es gelingt, unter Verwendung der im Zeitbereich registrierten THz-TDS-Daten das Volumeninnere in Form eines dreidimensionalen Tomogramms zu rekonstruieren. Die THz-TD-SAFT basiert auf die für die Ultraschalltechnik entwickelte Synthetische Apertur Fokussierung (SAFT) bzw. des heuristisch begründeten Algorithmus des Synthetischen Apertur Radars (SAR). Anhand von Beispielen wird die Möglichkeiten der THz-TD-SAFT demonstriert und nachgewiesen, dass mit dem Rekonstruktionsansatz die künstlich eingebauten Fehlstellen bezüglich der Position und Größe geometrisch richtig im Tomogramm abgebildet werden können.
The Spectral Element Method (SEM) has been proven to be an efficient numerical method for solving the wave equation in linear elastic bodies. This efficiency is reduced if a stress singularity is present in the body. For example, re-entrant corners, material interfaces, fixed boundaries, and especially crack tips can cause stress singularities. To preserve the efficiency of the SEM, special solution strategies are required. There are many approaches which consider stress singularities, but comparisons are rare for dynamic problems. Finding an efficient model is an important step for many applications. In particular, applications for structural health monitoring and non-destructive evaluation rely on accurate and efficient crack models.
In this contribution, we present several models to capture singularities in combination with the SEM. The theory behind the models are shortly summarized and we show results for different benchmark problems in two dimensions. The first model deploys a new class of singular elements. For these singular elements, the crack tip approximation is computed based on the static Scaled Boundary Finite Element Method (SBFEM). The second model uses the continued‐fraction‐based SBFEM, while the third model uses an hp-refinement near the singularity. The models are compared among each other and evaluated in terms of their respective efficiency and accuracy.
Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is nowadays an established multi-elemental analysis and mapping technique. It was shown that LA-ICP-MS can visualize the elemental distribution within tissue thin sections or cell samples. Quantification is possible by using appropriate matrix-matched calibration samples. Besides naturally occurring elements and metals from contrast agents, biomolecules using metal-tagged antibodies were detected in different bio-medical samples. By combining the results with findings from histology, magnetic resonance imaging (MRI) and other techniques disease related changes like alterations of the extracellular matrix can be investigated.
Therapeutische Antikörper sind innerhalb weniger Jahre zur wichtigsten pharmazeutischen Produktklasse aufgestiegen. Für 2023 werden weltweite Umsätze von über 200 Milliarden USD erwartet. Auch diagnostische Antikörper sind mittlerweile unverzichtbare Produkte, auf deren Basis zahllose Immunoassays und andere Schnelltests entwickelt wurden. Neben der bereits sehr aufwendigen Herstellung von Antikörpern ist deren Aufreinigung aus komplexen Zellkulturmedien oder Blutseren und -plasmen zu einem Engpass in der Produktion und Nutzung dieser komplexen Proteine geworden. Schnelle und einfache Reinigungsmethoden für Antikörper sind daher sehr gefragt.
The successful off-line coupling of asymmetrical flow field flow fractionation (AF4) and capillary electrophoresis (CE) for Separation of nanoparticles (NPs) with different surface coatings was shown.
Two mixtures of polystyrene nanoparticles (PS-NPs) with comparable core sizes (20 nm and 50 nm) but different coatings (no coating/carboxyl-coated) were studied. Separation in either method resulted in non-baseline resolved or non-separated peaks. In contrast, two-dimensional off-line coupling of AF4 and CE resulted in clearly separated regions in their 2 D plots and can obviouly improve separation resolution.
An affinity column, which removed up to 99 % of high affinity Anti-TNT antibody at high antibody concentrations, was manufactured based on a monolithic glass core and a trinitroaniline-BSA conjugate. To detect the label Dy654 in the nM range an epi-fluorescence microscope setup with a CMOS camera was established to serve as online fluorescence detector with multiplexing capabilities.
Screening of one-bead-one-peptide libraries is a powerful analytical tool for the identification of protein ligands. However, the traditional peptide screening procedure involves tedious steps such as manual selection, sequencing, and characterization. We present a high-throughput “all in one chip” system, allowing the screening of a high number of resin beads in short time. Here, beads of a combinatorial one-bead one compound peptide library are immobilized on an in-house produced chip, on which every bead has a well-defined position. The chip is then incubated with a fluorophore-labeled protein, identifying suitable peptides by a high-resolution fluorescence scan. The screening is followed by MALDI-MS experiments directly on the respective glass chip. To circumvent the need for peptide fragmentation normally used for peptide de novo sequencing, which can result in incomplete sequence information, an approach based on ladder sequencing has been used. This allows the peptide sequence identification by fragmentation-free MS with almost 100 % accuracy. For this purpose, a software tool was developed automatically translating MALDI-MS spectra into the corresponding peptide sequences.
Bestimmung der Rissgeometrie bei der zerstörungsfreien Ultraschallprüfung mit geführten Wellen
(2019)
In der zerstörungsfreien Prüfung werden in zunehmendem Maße geführte Ultraschallwellen zur Lokalisation von Fehlstellen genutzt. Geführte Ultraschallwellen zeichnen sich dadurch aus, dass sie große Distanzen innerhalb des zu prüfenden Bauteiles zurücklegen können. Das Ultraschallwellenfeld setzt sich dabei aus verschieden Moden zusammen. Etablierte Prüfverfahren mit geführten Wellen ermitteln häufig nur die Position der Fehlstelle, wobei die Laufzeiten der reflektierten Signale ausgewertet wird. Modenumwandlung bleibt dabei zumeist unberücksichtigt.
Die Charakterisierung der Fehlstelle, zum Beispiel hinsichtlich der Länge eines Risses, ist dagegen herausfordernd. Aussagekräftige Zusammenhänge zwischen der Dimension oder Geometrie der Fehlstelle und ihrer Interaktion mit der Ultraschallwelle zu finden, ist Teil aktueller Forschung. Insbesondere eine Betrachtung der Moden höherer Ordnung und deren Amplitudenverhältnisse kann beim Aufspüren dieser Zusammenhänge hilfreich sein.
Im Beitrag werden zunächst die Zusammenhänge zwischen den beiden fundamentalen Moden in einer isotropen Platte und der Länge eines Risses untersucht. Aus den Ergebnissen wird ein inverses Verfahren motiviert. Ein Algorithmus wird vorgestellt, der die Risslänge im Modell solange variiert, bis er die modalen Zusammenhänge einer Vorgabe oder einer Messung rekonstruiert. Die eingesetzte Scaled Boundary Finite Element Method ermöglicht dabei eine sehr kurze Rechenzeit in jeden Optimierungsschritt. Zusätzlich ermöglicht die Methode eine Auswertung der modalen Zusammenhänge ohne Postprocessing, was die Rechenzeiten weiter verkürzt.
We compare four different sensing solutions suitable for distributed fiber optic humidity sensing in per uorinated graded-index polymer optical fibers (PFGI-POFs). Compared to silica fbers, polymer optical fibers over advantageous beneffits including signifficantly higher break down strain, fracture toughness and humidity sensitivity. Various humidity-related effects in PFGI-POFs have been reported in the last years including measured attenuation and length changes as well as Brillouin frequency and Bragg wavelength shifts. The four aforementioned methods could serve as a basis for distributed and quasi-distributed humidity sensing and are described here closely with an emphasis on plausible cross effects to temperature and strain. The main focus of this paper lies on the comparison of four approaches with regard to method complexity, sensitivity to humidity, spatial resolution, real-time capability and effort to compensate for cross effects.
Microbiologically influenced corrosion (MIC) of iron is usually attributed to sulfate-reducing microorganisms (SRM) in offshore industries, such as the oil and gas pipelines, due to the high concentrations of sulfate in the seawater. SRM act upon the metal by the reactiveness of hydrogen sulfide (HS-), and by withdrawal of the available electrons (Fe --> Fe2+ + 2e-; E° = -0.47 V) in electrical contact with the metal (EMIC). However, methanogenic archaea can also cause MIC. Because they do not produce HS-, withdrawal of electrons may be their main corrosive mechanism; however, mechanistic details and kinetics of the overall process are poorly understood.
To investigate the corrosion potential of methanogens, we studied the EMIC methanogenic strains isolated from marine sediments (Methanobacterium-affiliated strain IM1) and crude oil tanks (Methanococcus maripaludis Mic1c10), in an in-house developed flow-through cell to simulate a fluctuating environment. A co-culture of M. maripaludis and D. alaskensis was also established to study the effect of syntrophic growth on metal corrosion that may occur in industrial pipelines. Results indicate that the rates of iron corrosion due to coupled methanogenesis (up to 0.4 mm/yr) are higher to that caused by the marine SRM Desulfovibrio alaskensis (0.15 mm/yr). Surface analyses of the metal showed severe pitting with high methane production. Genomic analysis of the EMIC methanogen M. maripaludis Mic1c10 will provide an insight on the mechanisms of MIC. Such knowledge and deeper understanding also from an electrokinetic point of view may not only provide further models in microbial electrophysiology, but also contribute to mitigation strategies in MIC.
Digital Analytical Sciences
(2019)
Based on inductive reasoning scientific inquiry in Analytical Sciences has a long tradition. The talk addresses in which way the digital transformation will change the scientific paradigm in Analytical Sciences to a data-driven discipline. Three main areas, integration, instruments, and methods, are discussed in their transformation through machine learning and other digital tools. Finally, some shortcomings and pitfalls in the deployments of algorithmic shortcuts are illustrated.
Durch eine breite Beteiligung von Schleifmittelherstellern, -anwendern und wissenschaftlichen Einrichtungen im projektbegleitenden Ausschuss (PA) konnte der vielschichtige Themenkomplex „Schleifen“ im Kontext zu den Projektzielen umfassend untersucht werden. Es wurden praxisrelevante Parameterfelder definiert, die eine erfolgreiche Aufklärung der Projektfragestellung ermöglichten.
Im Zuge der Untersuchungen wurde ein signifikanter Einfluss beim Einsatz von Granulatschleifbändern auf das Korrosionsverhalten geschliffener Oberflächen festgestellt. Damit zeigten geschliffene Oberflächen regelmäßig eine schlechtere Korrosionsbeständigkeit als Oberflächen, die mit sonst gleichen Parametern mit einlagig gestreuten Bändern bearbeitet wurden.
Die durch einige Untersuchungsergebnisse aus vorangegangenen AiF-Vorhaben ursprünglich verfolgte These, dass Unterschiede in der Korrosionsbeständigkeit auf die Kornart der Schleifmittel Korund bzw. SiC zurückzuführen ist, konnte nur bedingt bestätigt werden. Bei den systematischen Untersuchungen innerhalb dieses Projektes erwies sich der Einfluss der Kornart im Vergleich zum Einfluss des Schleifbandtyps (Granulat bzw. einlagig gestreutes Korn) als weniger relevant.
Durch weiterführende Untersuchungen konnten auf Oberflächen, die mit Granulatschleifbändern bearbeitet wurden, große Materialaufplattungen aus Eigenmaterial festgestellt werden. Das Eigenmaterial wird dabei im Schleifprozess zunächst abgetragen und aufgrund der Topografie des Schleifbandes zeitweise auf den Bändern festgehalten. Später lösen sich diese Materialanhäufungen vom Band ab und können prozessbedingt durch Wärme- und Krafteinwirkung auf den bearbeiteten Oberflächen aufgeplattet werden. Durch REM und KorroPad Untersuchungen ließen sich Bereiche mit solchen Eigenmaterialaufplattungen eindeutig als wesentliche Ausgangspunkte für Korrosionsprozesse identifizieren. Das aufgeplattete Material ist stark verformt, thermisch beeinflusst und bildet eine Spaltgeometrie zur Bauteiloberfläche aus. Diese Veränderungen führen zur Störung der Passivschichtausbildung in diesen Bereichen und verursachen damit eine erhöhte Korrosionsanfälligkeit der Oberflächen.
Durch gezielte Nachbearbeitungsprozesse ist es möglich, die Eigenmaterialaufplattungen von den Oberflächen zu entfernen. Im Rahmen des Vorhabens wurde dazu eine Nachbearbeitung mittels Schleifvlies geprüft, die zu einer Entfernung der Eigenmaterialaufplattungen und damit zu einer Wiederherstellung der erwarteten Korrosionsbeständigkeit führte. Wird der Endschliff von Oberflächen mit einlagig gestreutem Korn ausgeführt, sind ebenfalls keine korrosionsrelevanten Materialaufplattungen zu erwarten.
Die in einem vorhergehenden AiF Vorhaben IGF 17136 N/1 entwickelte Methode der KorroPad-Prüfung konnte auch hier erfolgreich für die Untersuchung der Auswirkung unterschiedlicher Prozessparameter auf die Korrosionsbeständigkeit der Oberflächen eingesetzt werden. Zudem erwies sich das EPR-SL-Verfahren als ein weiterer Ansatz, um die Passivschichtstabilität verschieden geschliffener Oberflächen vergleichend untersuchen zu können.
Mit den nun vorliegenden Erkenntnissen können kmU künftig durch Anpassungen und Optimierung von Schleifprozessen eine gute Korrosionsbeständigkeit der bearbeiteten Oberflächen sicherstellen. Die Optimierung der Prozessparameter und -schritte kann durch den Einsatz der KorroPad-Prüfung Inhouse erfolgen und somit die laufende Fertigung im Rahmen der Qualitätsprüfung überwacht und dokumentiert werden.
Heute werden in Stahlkonstruktionen zunehmend hochfeste Baustähle (Streckgrenze ≥ 960 MPa) eingesetzt. Daher sind auch in Schweißnähten solche hohen Festigkeiten gefordert. Jedoch können hohe Eigenspannungen aufgrund geringerer plastischer Dehnungsreserven in diesen Schweißnähten die Sicherheit der Bauteile vermindern. Diese sind insbesondere im Zusammenhang mit Wasserstoff und Härtegefügen risskritisch. Niedrige Bauteilbeanspruchungen und Kosteneinsparungen lassen sich heutzutage mit modernen fokussierten Lichtbogenvarianten und engeren Nahtspalten erreichen. Die vorliegende Studie zeigt allerdings, dass diese modernen Schweißprozesse und die angepasste Nahtgeometrie höhere Wasserstoffkonzentrationen und signifikant gesteigerte oberflächennahe Zugeigenspannungsniveaus bedingen. Anhand mehrlagiger Schweißversuche an S960QL unter Variation von Wärmeführung, Lichtbogenvariante und Nahtöffnungswinkel wurden die Effekte und Wechselwirkungen unter Zuhilfenahme von Eigenspannungsanalytik mittels Röntgendiffraktometrie und Wasserstoffanalytik mittels Trägergasheißextraktion systematisch untersucht. Das Schweißgefüge führte unter kritischer mechanischer Beanspruchung und erhöhtem Gehalt an diffusiblem Wasserstoff insbesondere bei geringem Nahtöffnungswinkel und fokussiertem Lichtbogen zu einer deutlichen Ausbildung von Mikrorissen. Die Mikrorisse führten teils zu einer makroskopischen Ausprägung. Durch Analysen zur Nachwärmung aus der Schweißwärme heraus konnten suffiziente Wärmeführungsparameter für eine effektive Prävention solcher Risse erarbeitet werden. Die vorliegende Arbeit zeigt anhand des Interaktionssystems bei der wasserstoffunterstützten Kaltrissbildung Gefüge-Beanspruchung-Wasserstoff, welche Wärmeführungs- und Schweißparameter sich für die hochfesten Feinkornbaustähle zur Kaltrissvermeidung eignen.
Permitted explosives have a tradition of many decades in Germany and had been designed to the needs of the underground coal mining in the Ruhr. In neighboring countries of Germany similar provisions were made to prevent hazards from fire damp and coal dust explosions in underground coal mines. Due to the termination of coal mining in Germany and most other European countries, also the testing facilities are disappearing. This presentation outlines the current situation of testing regimes and facilities.
Der Vortrag berichtet über die Auslagerung von Standardproben nach DIN EN ISO 9223 bis 9226 aus Zink, Stahl, Kupfer und Aluminium auf den verschiedenen atmosphärischen Bewitterungsständen der Bundesanstalt für Materialforschung und -prüfung (BAM). Im Vortrag werden die Masseverluste, Korrosionsgeschwindigkeiten und Korrosivitätskategorien der Standardproben im freibewitterten und überdachten Bereich nach einem Jahr vorgestellt und Unterschiede hinsichtlich der Atmosphärenbedingungen aufgezeigt. Freibewitterte Proben zeigen dabei deutliche Unterschiede hinsichtlich ihres Korrosionsverhaltens im Vergleich zu überdachten Proben. Die ermittelten Korrosivitätskategorien sind sowohl standort- als auch materialspezifisch.