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- 1 Analytische Chemie; Referenzmaterialien (9)
- 6 Materialchemie (6)
- 1.5 Proteinanalytik (5)
- 6.5 Synthese und Streuverfahren nanostrukturierter Materialien (4)
- 8 Zerstörungsfreie Prüfung (4)
- 1.7 Organische Spuren- und Lebensmittelanalytik (3)
- 8.0 Abteilungsleitung und andere (3)
- 1.4 Prozessanalytik (2)
- 6.3 Strukturanalytik (2)
- 6.6 Physik und chemische Analytik der Polymere (2)
Homochirality is an obvious feature of life on Earth. On the other hand, extraterrestrial samples contain largely racemic compounds. The same is true for any common organic synthesis. Therefore, it has been a perplexing puzzle for decades how these racemates could have formed enantiomerically enriched fractions as a basis for the origin of homochiral life forms. Numerous hypotheses have been put forward as to how preferentially homochiral molecules could have formed and accumulated on Earth. In this article, it is shown that homochirality of the abiotic organic pool at the time of formation of the first self-replicating molecules is not necessary and not even probable. It is proposed to abandon the notion of a molecular ensemble and to focus on the level of individual molecules. Although the formation of the first self-replicating, most likely homochiral molecule is a seemingly improbable event, on a closer look, it is almost inevitable that homochiral molecules have formed simply on a statistical basis. In this case, the non-selective leap to homochirality would be one of the first steps in chemical evolution directly out of a racemic “ocean”. Moreover, most studies focus on the chirality of the primordial monomers with respect to an asymmetric carbon atom. However, any polymer with a minimal size that allows folding to a secondary structure, would spontaneously lead to asymmetric higher structures (conformations). Most of the functions of these polymers would be influenced by this inherently asymmetric folding. To summarize, simple and universal mechanisms may have led to homochiral self-replicating systems in the context of chemical evolution. A homochiral monomer pool is deemed unnecessary and probably never existed on primordial Earth.
The use of renewable energy technologies, such as photovoltaics (PV) should be sustainable and environmentally compatible and therefore protect the environment from risks and damaging impacts. Regarding the growing number of installed photovoltaic systems, the end-of-life management of the pv-modules will become increasingly important. Thin film panels contain hazardous substances that may harm the environment if they are not recycled or disposed properly after reaching the end of their service life. Heavy metals, for example, can be toxic as well as carcinogenic or teratogenic. Processing methods for the recycling of PV thin film modules have to take these facts into account. Currently the available recycling techniques usually utilise chemicals such as acids for a wet-chemical treatment of end-of-life modules. The aim of RESOLVED was to identify and test alternative methods for a wet-mechanical treatment in order to reduce the consumption of chemicals in the recycling of thin film modules. Furthermore, the recovered Cadmium-Telluride (CdTe) and Copper-Indium-Diselenide/Disulfide (CIS) should be helping to save scare resources especially for limited elements such as tellurium and indium. The project RESOLVED investigated the recovery of semiconductors material as secondary raw material and the decontamination of the residues of the PV thin film modules. These goals were achieved by testing and optimising existing technologies for the recycling process as well as for the enrichment of the semiconductor materials. The target is to re-use the enriched recovered material in the production of new PV modules. Special efforts were made to look into life cycle analysis, process sustainability, economical aspects, and resource availability.
In dem Projekt sollten die Aufbereitung der Betonbrechsandfraktion aus Bauschutt mittels eines Nassverfahrens zu einer geeigneten Gesteinskörnung für die Betonherstellung sowie die vollständige Verwertung der bei diesem Verfahren anfallenden Reststoffe demonstriert werden.
Der im Rahmen der geordneten Vorsortierung mit zahlreichen Schritten zur Qualitätssicherung hergestellte Betonbrechsand war qualitativ hochwertig und wies nur geringe Schadstoffgehalte auf. Für die Nassaufbereitung des Betonbrechsands wurde vom Projektpartner Allmineral der Prototyp einer Sandsetzmaschine zur Dichtetrennung designt und konstruiert. Diese Sandsetzmaschine wurde für die umfangreichen Betonbrechsandversuche in die Aufbereitungsanlage der BAM integriert. Begleitend zur Aufbereitung wurden die eingesetzten Materialien, Bauschutt und Prozesswasser, sowie die Austragsprodukte chemisch-physikalisch und mineralogisch untersucht.
Die anschließenden Baustoffuntersuchungen zeigten, dass durch das im Demonstrationsprojekt angewandte Nassaufbereitungsverfahren eine deutliche Verbesserung der Materialeigenschaften des Betonbrechsandes erzielt werden konnte. Die Qualität von Natursteinkörnungen wurde (z.B. aufgrund von Kornschädigungen durch den Bruch des Altbetons und noch verbleibende Zementanhaftungen) gleichwohl nicht erreicht. Gerade die Betonprüfungen (mit Anteilen von bis zu 50% Betonbrechsand an der gesamten Gesteinskörnung) haben jedoch gezeigt, dass es dennoch sehr wohl möglich wäre, größere Mengen von aufbereitetem Betonbrechsand in der Betonherstellung zu verwerten und so im Sinne der Nachhaltigkeit den Verbrauch von natürlichen Sandvorkommen zu reduzieren.
Die bei der Nassaufbereitung des Betonbrechsands anfallenden Restsstoffe, nämlich die Fraktionen Leichtgut und Feinstfraktion wurden separat erfasst und bilanziert. Diese Materialien wurden auf die Eignung als Kompostzugabe in Hinblick auf Schadstoffanreicherungen und Pflanzenverträglichkeit untersucht (Projektpartner Deisl). Nach der Kompostierung in Rotteboxen wurden Wachstumsversuche mit dem Referenzgewächs Kresse (Kressetest nach ÖNORM) mit zufriedenstellenden Ergebnissen durchgeführt. Die Reststoffe Feinstgut und Leichtgut aus dem Nassaufbereitungsprozess könnten – sofern die Schadstoffgehalte nachweislich unter den vorgegebenen Grenzwerten liegen – als Zugabe zur Vererdung in der Kompostierung eingesetzt werden.
Die Verwendung hochfester Feinkornbaustähle hat für viele Anwendungen des Stahlbaus ein großes Potenzial für gewichtsoptimierte, effiziente Strukturen mit ho-her mechanischer Beanspruchbarkeit. Weitere Zugewinne an Effizienz sind durch generative Fertigungsschritte sowie bionische Bauweisen erzielbar. Hierzu stehen bereits kommerzielle hochfeste drahtförmige Zusatzwerkstoffe für formgebendes MSG-Schweißen zur Verfügung. Dem Einsatz stehen noch fehlende quantitative Aussagen zu den fertigungsbedingten Beanspruchungen und der Bauteilsicherheit während Herstellung und Betrieb im Wege. Dies betrifft insbesondere prozess- sowie materialbedingte Einflüsse und die konstruktive Schrumpfbehinderung verbunden mit der Ausbildung hoher Zugeigenspannungen und damit zusammenhängenden Kaltrissbildung.
Hierfür wurden im Projekt detaillierte und anwenderbezogene Kenntnisse zu den komplexen Wechselwirkungen zwischen Schweißprozess und Wärmeführung während der Fertigung, der metallurgischen Vorgänge und insbesondere der vorliegenden konstruktiven Einflüsse auf die entstehenden Eigenspannungen erarbeitet, um ein frühzeitiges Bauteilversagen aufgrund eines hohen fertigungsbedingten Beanspruchungsniveaus bis hin zu einer Rissbildung während der Fertigung sicher zu vermeiden. Gleichzeitig wurden die Einflüsse auf die mechanisch-technologischen Gütewerte systematisch analysiert. Zudem wurden die Auswirkungen trennender Verfahren durch Entfernen der Substratplatte sowie durch die spanende Bearbeitung der Vorformlinge zu Endbauteilgeometrien geklärt, da diese unmittelbar den Eigenspannungszustand beeinflussen und deutlichen Verzug der Bauteile auslösen.
Für das generative Schweißen konnten Verarbeitungsempfehlungen sowie Normenvorgaben erarbeitet werden. Dies hilft insbesondere KMU eine wirtschaftliche, beanspruchungsgerechte und risssichere generative Fertigung von Bauteilen aus hochfesten Feinkornbaustählen zu ermöglichen.
Nonporous corundum powder, known as an abrasive material in the industry, was functionalized covalently with protein binders to isolate and enrich specific proteins from complex matrices. The materials based on corundum were characterized by TEM, ESEM, BET, DLS, and zeta potential measurements. The strong Al-O-P bonds between the corundum surface and amino phosphonic acids are used to introduce functional groups for further conjugations. The common cross-linker glutaraldehyde was compared with a hyperbranched polyglycerol (PG) of around 10 kDa. The latter is oxidized with periodate to generate aldehyde groups that can covalently react with the amines of the surface and the amino groups from the protein via a reductive amination process. The amount of bound protein was quantified via aromatic amino acid analysis (AAAA). This work shows that oxidized polyglycerol can be used as an alternative to glutaraldehyde. With polyglycerol, more of the model protein bovine serum albumin (BSA) could be attached to the surface under the same conditions, and lower nonspecific binding (NSB) was observed. As a proof of concept, IgG was extracted with protein A from crude human plasma. The purity of the product was examined by SDS-PAGE. A binding capacity of 1.8 mg IgG per g of corundum powder was achieved. The advantages of corundum are the very low price, extremely high physical and chemical stability, pressure resistance, favorable binding kinetics, and flexible application.
We introduce a novel adaptive Gaussian Process Regression (GPR) methodology for efficient construction of surrogate models for Bayesian inverse problems with expensive forward model evaluations. An adaptive design strategy focuses on optimizing both the positioning and simulation accuracy of training data in order to reduce the computational cost of simulating training data without compromising the fidelity of the posterior distributions of parameters. The method interleaves a goal-oriented active learning algorithm selecting evaluation points and tolerances based on the expected impact on the Kullback-Leibler divergence of surrogated and true posterior with a Markov Chain Monte Carlo sampling of the posterior. The performance benefit of the adaptive approach is demonstrated for two simple test problems.
The project addresses chemical and topographical metrology at surfaces. The new methodologies of measurements at surfaces will be developed as good practice guides and new work item proposals for industrial ISO standards. The objectives of the Joint research project (JRP) are to provide measurement standards and methods with traceability wherever it is practicable to do so for quantitative surface chemical analysis for industrial applications.
MALDI-TOF-MS-based identification of monoclonal murine anti-SARS-CoV-2 antibodies within one hour
(2022)
During the SARS-CoV-2 pandemic, many virus-binding monoclonal antibodies have been developed for clinical and diagnostic purposes. This underlines the importance of antibodies as universal bioanalytical reagents. However, little attention is given to the reproducibility crisis that scientific studies are still facing to date. In a recent study, not even half of all research antibodies mentioned in publications could be identified at all. This should spark more efforts in the search for practical solutions for the traceability of antibodies. For this purpose, we used thirty-five monoclonal antibodies against SARS-CoV-2 to demonstrate how sequence-independent antibody identification can be achieved by simple means applied onto the protein. First, we examined the intact and light chain masses of the antibodies relative to the reference material NIST-mAb 8671. Already half of the antibodies could be identified based solely on these two parameters. In addition, we developed two complementary peptide mass fingerprinting methods with MALDI-TOF-MS that can be performed in 45 minutes and had a combined sequence coverage of over 80%. One method is based on the partial acidic hydrolysis of the protein by 5 mM of sulfuric acid at 99 °C. Furthermore, we established a fast way for a tryptic digest without an alkylation step. We were able to show that the distinction of clones is possible simply by a brief visual comparison of the mass spectra. In this work, two clones originating from the same immunization gave the same fingerprints. Later, a hybridoma sequencing confirmed the sequence identity of these sister clones. In order to automate the spectral comparison for larger libraries of antibodies, we developed the online software ABID 2.0 (https://gets.shinyapps.io/ABID/). This open-source software determines the number of matching peptides in the fingerprint spectra. We propose that publications and other documents critically relying on monoclonal antibodies with unknown amino acid sequences should include at least one antibody fingerprint. By fingerprinting an antibody in question, its identity can be confirmed by comparison with a library spectrum at any time and context.
This document presents the specification for the execution and evaluation of high-speed tensile tests on reinforcement bar coupler systems. This specification was developed at BAM - Bundesanstalt für Materialforschung und -prüfung (Federal Institute for Materials Research and Testing, Germany) - following test principles from related international standards.
The present document represents the latest status of the test specification. It is noted that until 2010 the test procedure was characterised on a test velocity based on L0. In an improved test conception and after intensive investigations in cooperation with industry partners, this procedure has been updated to consider instead a test velocity based on Lr, since this warrants more comparable and meaningful results.
Protein immobilization for the functionalization of particles is used in various applications, including biosensors, lateral-flow immunoassays (LFIA), bead-based assays, and others. Common methods for the quantification of bound protein are measuring protein in the supernatant before and after coating and calculating the difference. This popular approach has the potential for a significant overestimation of the amount of immobilized protein since layers not directly bound to the surface (soft protein corona) are usually lost during washing and handling. Only the layer directly bound to the surface (hard corona) can be used in subsequent assays. A simplified amino acid analysis method based on acidic hydrolysis and RP-HPLC-FLD of tyrosine and phenylalanine (aromatic amino acid analysis, AAAA) is proposed to directly quantify protein bound to the surface of gold nano- and latex microparticles. The results are compared with indirect methods such as colorimetric protein assays, such as Bradford, bicinchoninic acid (BCA), as well as AAAA of the supernatant. For both particle types, these indirect quantification techniques show a protein overestimation of up to 1700% compared to the direct AAAA measurements. In addition, protein coating on latex particles was performed both passively through adsorption and covalently through EDC/sulfo-NHS chemistry. Our results showed no difference between the immobilization methodologies. This finding suggests that usual protein determination methods are no unambiguous proof of a covalent conjugation on particles or beads.
Quantitative 1H Nuclear Magnetic Resonance (qNMR) of Aromatic Amino Acids for Protein Quantification
(2022)
qNMR is a valuable technique for metrological studies due to the uniformity of its signal response for all chemical species of an isotope of interest, which enables compound-independent calibration. However, protein quantification remained challenging as large molecules produce wide, low-intensity signals that reduce the already low sensitivity. Combining qNMR with the hydrolysis of protein samples into amino acids circumvents many of these issues and facilitates the use of NMR spectroscopy for absolute protein and peptide quantification.In this work, different conditions have been tested for quantifying aromatic amino acids and proteins. First, we examined the pH-based signal shifts in the aromatic region. The preferable pH depends on the selection of the amino acids for quantification and which internal standard substance should be used to avoid peak overlap. Several aromatic compounds, such as terephthalic acid, sulfoisophthalic acid, and benzene tricarboxylic acid, have been applied as internal standards. The quantification of amino acids from an amino acid standard, as well as from a certified reference material (bovine serum albumin), was performed. Using the first two suggested internal standards, recovery was ~ 97 % for histidine, phenylalanine, and tyrosine at a concentration of approximately 1 mM in solution. Acidic hydrolysis of a certified reference material (CRM) of bovine serum albumin (BSA) and subsequent quantification of Phe and Tyr yielded recoveries of 98 ± 2 and 88 ± 4 %, respectively, at a protein concentration of 16 g/L or 250 µM.
Four cement-based and four calcium-sulphate-based screed types are investigated. The samples have a diameter of 300 mm and a height of 35 or 70 mm. Up to ten humidity sensors are embedded directly during the concreting of the screed samples. Thus, the humidity over the sample height is monitored during hardening, hydration, evaporation, and oven drying. Furthermore, the screed samples are weighted during every measurement to determine the total mass and the corresponding moisture loss.
To define the pore system precisely, mercury intrusion porosimetry as well as gas adsorption is performed. According to the data, the entire pore volume distribution is known. The measured pore diameters range from 0.8 nm to 100 μm and the total porosity of the examined screeds ranges between 11 % and 22 %.
Based on these measurement data, moisture transport, pore saturation as well as sorption isotherms and their hysteresis may be calculated quantitatively as described by Strangfeld et al.
Contaminated land, landfills and sediments pose a serious environmental threat by polluting groundwater in the surrounding area. In 14 European countries contamination caused by uranium represents a particularly serious danger where drinking water resources might be affected. Other heavy metals and organic pollutants can also have a strongly deleterious effect on groundwater. Available technologies (e.g. pump- and-treat) fall short of solving the problem because their performance is not yet adequate for effective remediation. The aim of the project is to elaborate the scientific basis for laboratory and pilot-scale testing of and the practical application of a considerably more efficient and cost-effective in-situ reactive barrier technology targeting the above contaminants. The primary model test site will be an area in Southern Hungary contaminated by uranium mining- thus including a region which is due to become part of the European Union.
The approach taken to meet the project objectives was the characterisation of different reactive materials and relevant attenuation processes in the reactive matrix of the permeable barrier with special respect to their long-term behaviour. The experimental work included laboratory experiments at different scales, going from bench-scale tests up to pilot-scale, and field-scale experiments. Experimental conditions were predetermined by the characteristics of the model site, such as geologic and hydrogeological settings, soil composition, and type, extent and spreading of the contamination. Technological methods to enhance the long-term efficacy and cost-effectiveness of permeable reactive barrier systems were developed and tested under realistic conditions.
Bei der Montage von Stahlkonstruktionen kommt es trotz anforderungsgerechter schweißtechnischer Fertigung vereinzelt zur Detektion von unzulässigen Unregelmäßigkeiten im Schweißbereich.
In einem Forschungsprojekt (FOSTA P1311) wurden Untersuchungen durchgeführt und Kenntnisse erarbeitet, um mittelfristig vor allem KMU beanspruchungsgerechte Reparaturkonzepte zur Verfügung zu stellen. Damit können letztlich Schäden und zumeist teure Nacharbeiten verhindert und eine verbesserte Ausnutzung des hohen Festigkeitspotentials hochfester Stähle erreicht werden. Gerade KMU können mit Blick auf die Kosten für Fertigung, Schweißarbeit und Material von den Erkenntnissen beim Einsatz hochfester Stähle, die für eine effiziente Realisierung der Energiewende in Deutschland notwendig sind, profitieren.
ISO 10156:2010 contains a test method and a calculation method for flammability of gases and gas mixtures for the selection of cylinder valve outlets. The calculation method is used also to classify gas mixtures according to the national and international dangerous goods and dangerous substances regulations, e.g. according to the UN Recommendations on the Transport of Dangerous Goods (UN TDG) and the Globally Harmonized System of Classification and Labelling of Chemicals (UN GHS). The calculation method for gas mixtures requires substance parameters of the single components. These are the coefficients for the fire potential (Tci) and for inerting ability, the so-called nitrogen equivalence (Kk), which have been estimated conservatively by means of flammability data.
BAM checked Tci and Kk values of ISO 10156:1996 using three-component diagrams (Flammable gas-Inert-Air) of the CHEMSAFE® database. The experimental fundamentals and the principles of the calculation method are summarized in this paper. The revised data for Tci and Kk values were adopted in the tables of ISO 10156:2010.
Furthermore, subcategorization of flammable gases has been proposed by a UN working group and shall be implemented in the GHS in the meantime. The subcategorization requires the lower flammability limit (LFL) as an additional indicator. Therefore, a test method and a calculation method for LFL were proposed by BAM and have been implemented in the new draft of ISO/CD 10156:2016.
The calculation method for gas mixtures is based on Le Chatelier’s rule and was extended by using the Kk values for inert components in the mixture. The calculated LFLs of methane-inert gas mixtures were compared with experimental values for different types of inert gases. It could be shown that calculated LFLs are in good agreement with experimental values if the Kk values derived from three-component flammability diagrams are used. Although using the Kk values of ISO 10156:2010 leads to higher deviations, the results are still on the safe side.
Recently, we suggested an unconventional approach [the so-called Internal-Field-Guarded-Active-Region Design (IFGARD)] for the elimination of the crystal polarization field induced quantum confined Stark effect (QCSE) in polar semiconductor heterostructures. And in this work, we demonstrate by means of micro-photoluminescence techniques the successful tuning as well as the elimination of the QCSE in strongly polar [000-1] wurtzite GaN/AlN nanodiscs while reducing the exciton life times by more than two orders of magnitude. The IFGARD based elimination of the QCSE is independent of any specific crystal growth procedures. Furthermore, the cone-shaped geometry of the utilized nanowires (which embeds the investigated IFGARD nanodiscs) facilitates the experimental differentiation between quantum confinement- and QCSE-induced emission energy shifts. Due to the IFGARD, both effects become independently adaptable.
„Getränkekühler optimal einsetzen“: So sparen Sie die Energiekosten und schonen das Klima.
Wussten Sie, dass Sie durch den Einsatz eines effizienten Getränkekühlers (Energieeffizienzklasse B) ca. 114 € pro Jahr sparen im Vergleich zu einem weniger effizienten Gerät (Energieeffizienzklasse D)? Aber nicht immer gibt es die Möglichkeit ein Neugerät anzuschaffen. Oft werden die Kühlgeräte von Getränkeherstellern zur Präsentation ihrer Waren zur Verfügung gestellt. Trotzdem tragen am Ende die Betreiber:innen die Betriebskosten der Geräte.
Aber auch beim Einsatz Ihres weniger effizienten Getränkekühler gibt es verschiedene Möglichkeiten, die Energiekosten zu senken. Beispielsweise kann schon der Einsatz einer Zeitschaltuhr zu einer Stromreduzierung von bis zu 50 Prozent oder auch die richtige Platzierung der Geräte an kühlen Orten ohne Zugluft zu einem geringeren Strombedarf von bis zu 30% führen.
In unserer Checkliste für die Aufstellung und das Betreiben von Getränkekühlgeräten zeigen wir Ihnen einfache Schritte, um den Energieverbrauch schnell zu senken.