Analytische Chemie
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- 4 Material und Umwelt (12)
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- 1.1 Anorganische Spurenanalytik (2)
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- 6.1 Oberflächen- und Dünnschichtanalyse (1)
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- 7.1 Baustoffe (1)
- 7.4 Baustofftechnologie (1)
- 8.5 Röntgenbildgebung (1)
- 8.6 Faseroptische Sensorik (1)
- S Qualitätsinfrastruktur (1)
- S.2 Digitalisierung der Qualitätsinfrastruktur (1)
This paper addresses the sensitive issue of authenticating unprovenanced manuscripts of high monetary value to certify they are genuine. Over the last decade, the popularity of material studies of manuscripts using non-destructive testing (NDT) has increased enormously. These studies are held in especially high esteem in the case of suspicious writings due to the methodological rigour they are reputed to contribute to debate. We would like to stress that materials analysis alone cannot prove that an object is genuine. Unfortunately, audiences with a humanities background often tend to disregard the technical details and treat any published interpretation of instrumental analysis as an objective finding. Four examples are outlined here to illustrate what questionable contributions the natural sciences can make in describing manuscripts that have actually been forged.
Ultrasonic monitoring, making use of the sensitivity of the coda of repeated transmission meas-urements to changes in stress, temperature, moisture, as well as localized or distributed damage, has gotten at-tention in structural health monitoring (SHM) research recently. Analysis methods such as coda wave inter-ferometry (CWI), including its nonlinear extension, have been shown to be able to measure ultrasonic wave velocity changes with a 1∙10-5 resolution, while indicators such as cross-correlation or cross-coherence have been used to distinguish between reversible and irreversible changes. Several small- and large-scale laboratory experiments have demonstrated that stress changes in structures can be captured or damage detected in a very early stage. The use of this technique for pre-warning before failure are currently under investigation, as well as detailed research on the physical causes and the connection between ultrasonic wave properties and materi-al/structural behavior. Recently, several of large-scale laboratory and real structures have been instrumented with embedded ultrasonic transducers to gather experience and evidence on how to use this technology in re-al-world applications. Preliminary results from installations on a new bridge, an existing bridge, a tunnel, a la-boratory earthquake test as well as a historic stadium in Germany, Poland, and the United States, respectively, are presented. Environmental influences (mainly temperature) and validation by load tests are discussed.
NDE 4.0 in Civil Engineering
(2021)
Civil engineering industry is one of the most important industry sectors in the worldwide economy. It contributes significantly to the gross economic product and general employment. Even more important, it provides many of the basic needs of the society (e.g., housing, infrastructure, and protection from natural hazards). The concept of “Industry 4.0” or “Smart Production” has not yet made significant progress in the civil engineering industry. The designing, building, and operating processes are still widely dominated by the exchange of printed documents and drawings. Most objects (buildings and other constructions) are unique, and a large part of the production still requires a large amount of manual labor. As-built documentation and quality assurance are often neglected. Civil engineering is among the industry sectors with the lowest level of digitalization and the lowest gain in productivity. However, this is going to change. In the past decade, several drivers have challenged the ways clients, contractors, and authorities currently operate. These drivers include but are not limited to an increasing demand for serialization and automatization or the mandatory introduction of “Building Information Modeling” (BIM) in public procurement as well as the upcoming use of digital twins. NDE plays an increasing role in quality assurance, condition assessment, and monitoring of structures. However, with very few exceptions, applications are mostly nonstandardized and performed only at selected sites. To change this, the NDT-CE community including manufacturers, service providers, clients, and the scientific community must work consistently on open data formats, interfaces to BIM, standardization, and validated ways for a quantitative use of the results in the assessment of constructions.
Our standard protocol for the characterisation of writing materials within advanced manuscript studies has been successfully used to investigate manuscripts written with a pure ink on a homogeneous writing surface. However, this protocol is inadequate for analysing documents penned in mixed inks. We present here the advantages and limitations of the improved version of the protocol, which now includes imaging further into the infrared region (1100−1700 nm).
In this paper, we discuss the importance of scientifically investigating cultural artefacts in a non-invasive way. Taking as test case Leonardo da Vinci’s Manuscript with anatomic drawings and notes, which is stored in Weimar, we clarify fundamental steps in the chronology of this folio. By means of microscopy, infrared reflectography, UV photography, and X-ray fluorescence analysis, we were able to identify various types of sketching material and several varieties of iron gall ink. For his sketches, Leonardo used two different sketching tools, a lead pencil and a graphite pencil, as well as several types of ink for developing these sketches into drawings. With regard to ink, it is important to observe that there is no difference between the ink Leonardo used for drawing and the ink he used for writing text. Based on the materials analysed, we suggest a chronology for the creation of this unique folio.
High-temperature corrosion is a widespread problem in various industries.
As soon as a hot and reactive gas (CO2, O2, H2O, SO2, NOx, etc.) is in contact with a solid, physico-chemical processes at the surface and interfaces lead to material degradation. The processes are dynamic and controlled by thermodynamic and kinetic boundary conditions. Whether a reaction product is protective or not depends on various factors, such as chemical composition of the solid and the reactive media, surface treatment as well as diffusion and transport paths of cations and anions. Resulting chemical and structural inhomogeneities with the corrosion layers are characterized by off stoichiometry within cationic and anionic sub lattices. The competitive processes can be studied by various techniques of applied crystallography.
This chapter gives an overview on the challenges of chemical-structural Analysis of reaction products by crystallographic methods such as X-ray diffraction and X-ray near-edge structure spectroscopy and scanning electron microscopy electron backscatter diffraction (SEM-EBSD) for corrosion science.
Nondestructive evaluation (NDE) is entering an era of the fourth industrial revolution and will undergo a major transformation. NDE is a vital part of industry and a successful move to NDE 4.0, it will require not just developing and embracing new technologies, but also developing and adopting new ways of working and becoming an integral part of the overall Industry 4.0. This will pose new challenges for the inspection personnel. To ensure the expected benefits from NDE 4.0, inspectors need stay in charge of the changing inspections. The promised autonomy and interconnectedness of NDE 4.0 will supersede the majority of traditional inspector tasks and will in turn require a different set of skills and raise different demands and challenges for the inspection personnel, thus conflicting the current “procedure-following”-“level I-III” paradigm. The new industry 4.0 technologies can be integrated into the current framework, but exploiting their full potential requires changes in the role of the inspectors. The inspectors will be relieved from the tedious and error-prone aspects of the current system. At the same time, they will need to take responsibility for increasingly complex automated systems and work in closer collaboration with other experts. We propose that the traditional inspector roles will be transformed into that of the system developer, caretaker, and problem solver, each requiring a specific set of skills and assuming different responsibilities. For full NDE 4.0, NDE must abandon its traditional role as a self-contained entity with well-defined boundaries and take its role in the wider system that is the industry 4.0.
Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is nowadays a versatile and powerful analytical method for direct solid sample analysis. The applicability has been demonstrated for a wide variety of samples covering hard and soft materials. In an imaging mode the technique provides quantitative information on the elemental distribution within a sample. LA-ICP-MS imaging is of particular interest in biomedical research as the distribution of an element gives valuable insight on uptake and distribution of essential and toxic trace elements, administered contrast agents as well es nanoparticles. LA-ICP-MS is therefore a powerful complement to other imaging techniques. Recent instrumental improvements, especially in sample chamber design, have contributed to better sensitivity and spatial resolution enabling subcellular imaging. The book chapter provides a comprehensive overview about spatially resolved localisation and quantification of various nanoparticles in cells and tissue thin sections by LA-ICP-MS. Furthermore, different sample preparation strategies and internal standardisation and calibration approaches for bioimaging by LA-ICP-MS are summarized and discussed.
Metal-containing nanomaterials are used in numerous fields ranging from industrial applications to nanomedicine. Several studies have demonstrated that the physicochemical properties of nanoparticles have an impact on their pharmacokinetics, transfer and clearance. The high sensitivity and multielement capability of LA-ICP-MS enables the elucidation of interactions between tissue components and nanomaterials used as imaging probes or drug carriers. Potential toxic effects are investigated as well. Thus, LA imaging significantly supports the clinical translation of safe and efficient nanoparticles for diagnostic and therapeutic purposes.
The purpose of this contribution is to introduce and to apply the developed approach of incorporating non-destructively gathered measurement results (instead of deterministic information and assumptions) into a reassessment model of a typical prestressed concrete road bridge and to outline the advantages. An essential part is the quality evaluation of the non-destructively measured information, that deals primarily with two questions. Could the object or parameter to be obtained reliably detected and if, how accurate are the inspection results achieved? Therefore, the importance of the combination of a probability of detection (POD)-approach and measurement uncertainty calculations is emphasized. With regard to the introduced case-study it is shown, for which structure parameters an assumption deviating from the actual (and measurable) situation has a particularly strong (and possibly arithmetically unfavorable) influence on the structural reliability. Measurements on such parameters are particularly beneficial for a reliable and robust reassessment. In conclusion, the individual reassessment results without consideration and with consideration of evaluated non-destructive inspection results are compared.
Der Sensorik kommt bei der Digitalisierung der Prozessindustrie eine Schlüsselrolle zu. Entsprechend ist sie ein zentraler Baustein der NAMUR Open Architecture Konzepts (NOA). M+O-Sensoren (Monitoring + Optimization) - stellen eine neue Geräteklasse für die zusätzliche Überwachung und Optimierung von Anlagen der Prozessindustrie dar. Diese deckt klassische und alternative Messprinzipien bis hin zur Nachbildung der menschlichen Sinne ab. Hier werden die Anforderungen an M+O-Sensoren als Bestandteile der NOA beschrieben.
Inductively coupled plasma-mass spectrometry (ICP-MS) is a well-established analytical method offering high sensitivity and multi-element analysis. ICP-MS has found acceptance in various application areas ranging from material analysis to applications in the life sciences. Within the last 15 years new strategies for the sensitive detection and accurate quantification of biomolecules in complex biomedical samples have been developed. Recent instrumental improvements have contributed to this progress.
As most of the biomolecules do not contain endogenous metals etectable with ICP-MS, bioconjugation with artificial metal-containing tags based on metal-loaded chelate complexes or nanoparticles is increasingly applied to determine biomolecules indirectly. Especially, the combination of immunohistochemical workflows using lanthanoid-tagged antibodies and ICP-MS detection provides new insights in the complexity and interdependency of cellular processes. Single-cell ICP-MS, also termed as mass cytometry, allows high-dimensional analysis of biomarkers in cell populations at single-cell resolution. For that purpose, lanthanoid isotope labelled antibodies are used to detect their corresponding target molecules. The visualisation of the elemental distribution is possible with laser ablation ICP-MS (LA-ICPMS) at high spatial resolution. Especially, the combination of LA with ICP time-of-flight mass spectrometry, also referred to as imaging mass cytometry (IMC), opens new possibilities for multiparametric tissue imaging at the single-cell level and even below. The lanthanoid localisation and concentration can be linked to their conjugated antibody target providing valuable information about surface markers, intracellular signalling molecules to measure biological function, and the network state of an individual cell in a tissue.
This book chapter focuses on new applications, where the multi-element capabilities of ICP-MS are used for the detection of lanthanoids applied as artificial elemental stains or tags for biomolecules and in particular antibodies.
Der fabelhafte Möglichmacher
(2022)
Calibration-free methods in laser-induced breakdown spectroscopy, CF LIBS, serve as an alternative to calibration-based LIBS techniques. Their major advantage is the ability for fast chemical analysis in situations where matrix-matched standards are not readily available (as, e.g., in the analysis of biological materials and remote analysis) or amount of samples are limited. Their main applications are in the industry, geology, biology, archeology, and even space exploration. This chapter overviews the principle of operation and performance of CF LIBS techniques.
"The reassessment of bridges continues to take great importance both nationally and internationally. A major challenge is to find computation models reflecting the actual properties of the considered structures sufficiently accurate. Besides regular inspections, the conduction of advanced measurements is suitable to generate reliable information about a structure to be assessed. Prior to incorporating measurement results in reassessment, the relevance, the trueness, and the precision of the measured information needs to be stated. On the one hand, the use of information whose quality has not been assessed can lead to errors with serious consequences. On the other, the measurement of irrelevant information is inefficient. Although the use of measured data in assessment is currently mostly unregulated, their appreciation in reliability analyses is beneficial since the built environment can be assessed more realistically. Utilizing NDT in reassessment has the potential to extend remaining lifetimes of a structure, save resources, and improve infrastructural availabilities. The power of judgment regarding the decision on the reliability of an existing structure can be increased.
In this contribution, an approach is outlined to process non-destructively gathered measurement data in a comparableway in order to include themeasured information in probabilistic reliability assessments of existing structures. An essential part is the calculation of measurement uncertainties. The effect of incorporating evaluated NDT-results is demonstrated by means of a prestressed concrete bridge and GPR measurements conducted on this bridge as a case-study. The bridge is assessed regarding SLS Decompression using the NDT-results."
Per- and polyfluoroalkyl substances (PFAS) are a group of more than 4700 anionic and cationic anthrophonic substances which have been used extensively in a variety of products and industries due to their inert chemical stability and resistance to degradation by heat or acids. As a result of continuous use, mainly in aviation firefighting foams, thousands of industrial and military installations have been found to contain contaminated soil and groundwater resources. However, because of the continuous use of fluorinated consumer products, also effluents and sewage sludge from wastewater treatment plants (WWTPs) have been shown to be an important source of PFAS contamination into the aquatic environment. Resulting from recent stricter regulations and restrictions in the last years on the use of long chain (≥C8) PFAS, there is a significant shift in the chemical industry towards production of short (C4-C7) and ultrashort (C1-C3) chain alternatives. With the amendment of the Sewage Sludge Ordinance in 2017 the German legislation banned sewage sludge application on agricultural land, and by 2029/2032 sewage sludge will be completely prohibited from agricultural application. While environmental exposure of organic pollutants like PFAS, pesticides and pharmaceuticals are no longer desirable, phosphorus (P) from sewage sludge must still be used to produce high-quality P-fertilizers for a circular economy. Currently, plant-available P-fertilizers from sewage sludge/wastewater can be produced using a variety of treatment approaches including precipitation, leaching, and thermal treatment. However, the fate of legacy and emerging PFAS compounds during P leaching, precipitation and treatment from sewage sludge and wastewater is for the most parts still unknown.
Der Beitrag beschäftigt sich mit zerstörungsfreien Untersuchungen an den Farbmitteln früher Bauhauszeichnungen. Mit welchen Farbmitteln wurden diese Zeichnungen gestaltet? Wurden hier neueste Zubereitungen genutzt, von denen viele im ersten Drittel des 20. Jahrhunderts gerade auf den Markt kamen, oder fanden – der ebenfalls am Bauhaus propagierten Materialökonomie folgend – althergebrachte Materialien Verwendung, die günstiger zu beschaffen waren? Weitere Fragen widmen sich dem Themenkomplex Original, Kopie und Nachahmung sowie der Auffindung von Fälschungen. Restauratorische, konservatorische und kuratorische Fragestellungen und Entscheidungen sind grundsätzlich damit verknüpft. Zwölf exemplarisch vorgestellte Zeichnungen ermöglichen einen guten Über blick über die verwendeten Farbmittel des frühen Bauhauses von 1919 bis 1925. Trotz der Vielfalt der betrachteten Studien, Entwürfen und Arbeitsblättern, ergibt sich ein homogenes Gesamtbild. Bis auf wenige Ausnahmen dominieren anorganische Pigmente die Farbmittelpalette. Dieser Befund wird durch eine weitaus größere Stichprobe materialtechnologisch untersuchter Zeichnungen aus dem Bestand des Bauhaus-Museums Weimar bestätigt
Process analytical technology (PAT) is a cross-sectional technology and thus essential for future smart production. While in the past decades, the focus of process optimization strategies was on increasing efficiency, in the future, the focus will be on the sustainability of a production and its products. In addition, products will be increasingly personalized in order to match the property profile exactly to the intended use. PAT is able to provide context-sensitive information at the molecular level for process control. Spectroscopic sensors can determine inline and simultaneously both the chemical composition and its sub-microscopic morphology. The article will focus on the optical spectroscopy and therefore starts with a brief introduction on the basic concepts of molecular spectroscopy. In addition, the particularities of measuring liquids, surfaces, or particulate systems in PAT applications are described. This should enable the reader to select the appropriate method for the specific problem. Many examples from everyday industrial practice illustrate the applications. The areas covered are the manufacturing industry, process and pharmaceutical industry, food industry, as well as biotechnology and medical technology. Future will show that PAT is especially important for applications in the field of medicine (point of care) circular economy (recycling, water–wastewater, etc.). It is important to emphasize that sustainability in industrial production can only be successful with an inter- and transdisciplinary close exchange between the different disciplines.
The through-life management of our constantly ageing infrastructure is a basic requirement in order to ensure their structural safety and serviceability. Each structure experiences deterioration processes with time leading to a decrease of structural safety and serviceability. The design of new structures considers the expected deterioration for a defined period, the design service life. However, a frequent survey of structural safety controlling structural condition should be mandatory and a maintenance plan should be an integral part of the design. In addition, many structures have exceeded their design service life already or are very close to it leading to an increasing demand for condition assessment. On the one hand, assumptions made during design are not valid any more due to change of the loads, e.g., increasing traffic loads in terms of number and weights. On the other hand, design codes evolved over time in such a way that existing structures do not comply with today’s standards. In all these cases, the through-life management is an important tool to maintain the accessibility of existing structures with known reliability.
In line with the new Model Code for Concrete Structures, which includes guidance for both – design of new structures and assessment of existing structures, the Task Group 3.3 focused on the compilation of a state-of-the-art guideline for the through-life management of existing concrete structures, including:
Data acquisition by testing and monitoring techniques;
Condition assessment for the evaluation of existing structures;
Performance prediction using advanced methods;
Decision-making procedures to perform a complete assessment of existing structure.
The overall objective of the through-life management is the assessment of the current condition and the estimation of the remaining service life under consideration of all boundary conditions.
The structure and composition of ancient gold objects retain information about their long history of manufacture, from the exploitation of the ore to the finishing touches, as well as evidence of their use, deposition, and degradation. By developing an efficient analytical strategy, it is possible to retrieve that information. This chapter sets the necessary foundation 131to explore fully the analytical results presented in the following chapters of this volume. The techniques employed in the analyses of the Egyptian jewellery are described and the analytical parameters provided. For more established techniques, only brief introductions are presented, while more recent developments are presented in greater detail.
Bio-panning is a common process involved in recombinant antibody selection against defined targets. The biopanning process aims to isolate specific antibodies against an antigen via affinity selection from a phage display library. In general, antigens are immobilized on solid surfaces such as polystyrene plastic, magnetic beads, and nitrocellulose. For high-throughput selection, semi-automated panning selection allows simul-taneous panning against multiple target antigens adapting automated particle processing systems such as the KingFisher Flex. The system setup allows for minimal human intervention for pre-and post-panning steps such as antigen immobilization, phage rescue, and amplification. In addition, the platform is also adaptable to perform polyclonal and monoclonal ELISA for the evaluation process. This chapter will detail the protocols involved from the selection stage until the monoclonal ELISA evaluation with important notes attached at the end of this chapter for optimization and troubleshooting purposes.