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Eingeladener Vortrag
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Mechanically stable structures with interconnected hierarchical porosity combine the benefits of both small
and large pores, such as high surface area, pore volume, and good mass transport capabilities. Hence, lightweight micro-/meso-/macroporous monoliths are prepared from ordered mesoporous silica COK-12 by means of spark plasma sintering (SPS, S-sintering) and compared to conventionally (C-) sintered monoliths. A multi-scale model is developed to fit the small angle X-ray scattering data and obtain information on the hexagonal lattice parameters, pore sizes from the macro to the micro range, as well as the dimensions of the silica population. For both sintering techniques, the overall mesoporosity, hexagonal pore ordering, and amorphous character are preserved. The monoliths' porosity (77–49%), mesopore size (6.2–5.2 nm), pore volume (0.50–0.22 g cm-3
), and specific surface area (451–180 m2 g-1) decrease with increasing processing temperature and pressure. While the difference in porosity is enhanced, the
structural parameters between the C-and S-sintered monoliths are largely converging at 900 C, except for the mesopore size and lattice parameter, whose dimensions are more extensively preserved in the
S-sintered monoliths, however, coming along with larger deviations from the theoretical lattice. Their higher mechanical properties (biaxial strength up to 49 MPa, 724 MPa HV 9.807 N) at comparable porosities and ability to withstand ultrasonic treatment and dead-end filtration up to 7 bar allow S-sintered monoliths to reach a high permeance (2634 L m-2 h-1 bar-1), permeability (1.25 x 10^-14 m2), and ability to reduce the chemical oxygen demand by 90% during filtration of a surfactant-stabilized oil in water emulsion, while indicating reasonable resistance towards fouling.
Formalin-fixed paraffin-embedded (FFPE) specimen from biopsy materials are a widespread sample format for pathologists and medical researchers. Pathologists are archiving vast numbers of FFPE samples which can be stored for decades. Conventional immunohistochemical staining (IHC) of biomarkers on FFPE tissue sections is one of the most important analytical techniques for cancer diagnosis and pathology in general. However standardization for IHC samples and quality management is tedious and differs significantly from clinic to clinic. Combining established IHC staining strategies with modern mass spectrometry mediated methods would increase it`s potential and enable access of large FFPE archives for multiplexed quantitation purposes. In this work element mass spectrometry and a new ink-jet printed internal standardization approach was successfully combined with IHC staining to facilitate quantitative multiplex assays for archived FFPE samples. The printing strategy improves elemental image resolution and reproducibility of paraffin embedded breast cancer tissue sections in laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) using conventional IHC staining as a model system to investigate the new capabilities of this technique. For the internal standardization we applied a conventional CD-ink-jet printer to print a metal spiked ink onto the top of thin layer tissue sections with constant density. Printing was carried out in a direct comparison to an iodination of the tissue section as previously described as an alternative standardization method. The use of the printed internal standard allowed correction of the fluctuation during the laser ablation process and compensated instrumental drift effects. Mediated by the ink correction approach we achieved better signal-to-background-ratios (SBR) of 74 and better spatial resolution of 30 µm compared to iodination (SBR=23). This improved performance was demonstrated on tumorous areas in FFPE breast cancer tissue sections and allowing detection of Her-2 in tumorous areas of this tissue with significantly improved contrast.
Industry 4.0 is all about interconnectivity, sensor-enhanced process control, and data-driven systems. Process analytical technology (PAT) such as online nuclear magnetic resonance (NMR) spectroscopy is gaining in importance, as it increasingly contributes to automation and digitalization in production. In many cases up to now, however, a classical evaluation of process data and their transformation into knowledge is not possible or not economical due to the insufficiently large datasets available. When developing an automated method applicable in process control, sometimes only the basic data of a limited number of batch tests from typical product and process development campaigns are available. However, these datasets are not large enough for training machine-supported procedures. In this work, to overcome this limitation, a new procedure was developed, which allows physically motivated multiplication of the available reference data in order to obtain a sufficiently large dataset for training machine learning algorithms. The underlying example chemical synthesis was measured and analyzed with both application-relevant low-field NMR and high-field NMR spectroscopy as reference method. Artificial neural networks (ANNs) have the potential to infer valuable process information already from relatively limited input data. However, in order to predict the concentration at complex conditions (many reactants and wide concentration ranges), larger ANNs and, therefore, a larger Training dataset are required. We demonstrate that a moderately complex problem with four reactants can be addressed using ANNs in combination with the presented PAT method (low-field NMR) and with the proposed approach to generate meaningful training data.
Data set of low-field NMR spectra of continuous synthesis of nitro-4’-methyldiphenylamine (MNDPA). 1H spectra (43 MHz) were recorded as single scans.
Two different approaches for the generation of artificial neural networks training data for the prediction of reactant concentrations were used: (i) Training data based on combinations of measured pure component spectra and (ii) Training data based on a spectral model.
Synthetic low-field NMR spectra
First 4 columns in MAT-files represent component areas of each reactant within the synthetic mixture spectrum.
Xi (“pure component spectra dataset”)
Xii (“spectral model dataset”)
Experimental low-field NMR spectra from MNDPA-Synthesis
This data set represents low-field NMR-spectra recorded during continuous synthesis of nitro-4’-methyldiphenylamine (MNDPA). Reference values from high-field NMR results are included.
Hierarchically porous, high‐surface‐area silica materials are excellent candidates for multiple applications like catalysis and environmental remediation. Shaping these materials with additive manufacturing (AM) techniques, like robocasting, could enable their use with the benefit of on‐demand, customized shaping and maximizing performance. Herein, ordered mesoporous silica COK‐12 slurries were robocasted into monoliths, containing different ratios of uncalcined COK‐12 and sodium bentonite (0–25 wt.%). The rheology of the mixed slurries is characterized by lower flow indexes (0.69 vs. 0.32) and higher yield stresses (96 vs. 259 Pa) compared to pure COK‐12 ones. Monoliths were printed in woodpile structures and calcined at 600°C. Micro‐CT measurements showed a linear shrinkage of 25% after calcination. Mechanical characterization showed increased uniaxial strength (0.20 ± 0.07 to 1.0 ± 0.3 MPa) with increasing binder/solids ratio from 13 to 25%. The amorphous, mesoporous structure of COK‐12 was retained. The structures exhibited open porosities of 52 ± 4% and showed higher specific mesopore volumes, and increased average mesopore size (6 vs. 8 nm) compared to COK‐12. Small‐angle x‐ray scattering analysis revealed an increased lattice parameter (10.3 vs. 11.0 nm) and reduced wall thickness (3.1 nm vs. 4.1 nm) of the COK‐12 in the monoliths. These properties indicate suitability for their application as porous supports and adsorbents.
Weltweit stellen Waldbrände eine große Bedrohung für Umwelt, Wirtschaft und menschliches Leben dar. Der fortschreitende Klimawandel verstärkt Trockenheit und Dürre, wodurch die Größe und Intensität von Waldbränden sowie das daraus resultierende Gefahrenpotential zusätzlich erhöht werden. Um im Risikofall eine schnelle und effektive Waldbrandbekämpfung zu gewährleisten, sollen Einsatzkräfte in Zukunft von KI-basierten Ausbreitungsmodellen unterstützt werden.
Der Einsatz von maschinellem Lernen ermöglicht dabei schnelle und zielgerichtete Ausbreitungsvorhersagen in Echtzeit, die in den Prozess der Brandbekämpfung als zusätzliche Information einfließen können. Im Rahmen des durch das EU-Förderprogram Horizon 2020 finanzierte Projekt TREEADS wird ein solches Modell für Europa entwickelt.
Dazu wird mit verschiedenen Satellitendaten des Copernicus-Programms und der NASA ein auf räumlicher und zeitlicher Ebene aufgelöster Datensatz zu europäischen Waldbränden aufgebaut. Zu den erfassten Waldbränden werden wichtigen Faktoren, die Einfluss auf die Brandausbreitung haben, ergänzt. Dazu gehören das von Copernicus bereitgestellte, digitale Geländemodell Europas und verschiedene, von Sentinel-2 Messungen abgeleitete Informationen zu Vegetation und Landnutzung. Dieser 2D-Trainingsdatensatz zu realen Waldbränden wird durch die zeitlich hochaufgelösten, meteorologischen Reanalyse-Produkte – Copernicus European Regional ReAnalysis (CERRA) und ERA5-Land – vervollständigt und ist die Grundlage für ein Modell zur Ausbreitungsvorhersage von Waldbränden.
Methoden des Maschinellen Lernens können komplexe Muster in den gesammelten Daten erkennen und so zu einer verbesserten Vorhersage der Brandausbreitung beitragen. Die vielfältigen, von Copernicus bereitgestellten Daten sind dabei ein unabdingbarer Bestandteil des Modells, mit dem den Einsatzkräften ein zusätzliches Tool für den effizienten Einsatz ihrer limitierten Ressourcen zur Verfügung steht.
Engineered capping systems are in most cases an indispensable and often the only efficient component required by the long-term safety concept for landfills, mine tailings tips and contaminated land. In Germany the composite liner is the main component of standard landfill cappings for municipal and hazardous waste landfills and the compacted clay liner (CCL) for landfills for inert or low-contamination waste. The composite liner is a technically highly effective but very expensive system. Research and experience has given rise to concern about the proper long-term performance of a conventional single CCL as a landfill capping. Therefore, alternative capping systems are discussed and applied for landfills and for the containment of contaminated sites. This paper gives an overview on various alternative engineered cappings and suitable systems for capping reflecting the state of the art and the expert view in Germany. According to the European Council Directive on the landfill of waste an impermeable mineral layer is recommended for the surface sealing of non-hazardous landfills and a composition of artificial sealing liner and impermeable mineral layer for hazardous landfills. In both cases a drainage layer thickness of at least 0.5 m is suggested. These recommendations should be interpreted flexibly and to some extent modified in the light of the experience and results presented in this paper.
In absehbarer Zeit werden CE-gekennzeichnete Geovliesstoffe, Geogewebe, geosynthetische Dränelemente und Geogitter aus Kunststoff erhältlich sein, bei denen die CE-Leistungserklärung den Hinweis enthält 'dauerhaft für bis zu 100 Jahre' oder sogar 'dauerhaft für mindestens 100 Jahre'. Hersteller, Bauherren, Planer und zuständige Behörden werden sich daher die Frage stellen, ob diese Produkte auf der Grundlage von Anhang 1 Nummer 2.1 Satz 7 Ziffer 1 der Deponieverordnung (DepV) im Deponiebau auch ohne Zulassung verwendet werden dürfen. Ein Vergleich der europäisch harmonisierten Bauproduktnormen DIN EN 13252 und DIN EN 13257, die der CE-Kennzeichnung der Geotextilien und geotextilverwandten Produkte zugrunde liegen, mit den Anforderungen der DepV zeigt nun aber, dass nur ein Teil der für den Deponiebau wesentlichen technischen Eigenschaften in diesen Normen erfasst werden. Daher sind für CE gekennzeichnete Produkte zusätzliche Prüfungen auf der Grundlage der DepV-Liste der Kriterien und Einwirkmechanismen erforderlich. Die in den Produktnormen beschriebene Qualitätssicherung ist nach Anhang 1 Nummer 2 Satz 14 ff der DepV ebenfalls für die Gleichwertigkeit nicht ausreichend. Eine CE-Kennzeichnung ist deshalb noch kein Nachweis, dass die Produkte dem Stand der Technik nach der DepV entsprechen und die Eigenschaften der Produkte den geforderten Eigenschaften im Wesentlichen gleichwertig sind, auch wenn mit Bezug auf den Anhang B der genannten Normen deren Dauerhaftigkeit für 100 Jahre vom Hersteller deklariert wird.----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
In the near future, CE-marked woven and nonwoven geotextiles, geocomposite drains and geogrids will be available on the market, whose declaration of performance will contain the qualification 'predicted service life up to 100 years' or even 'predicted service life minimum 100 years'. Manufacturer, principals and their design engineers as well as the responsible authorities will have to deal with the question, whether such products can be used on the basis of Annex 1, no. 2.1, sentence 7, cipher 1 of the German landfill ordinance (DepV) as components of landfill liner and capping systems. A comparison of the harmonized European standards hEN 13252 and 13257, on which the CE-marking of geotextiles and geotextile-related products is based, with the DepV, shows that only a few of the essential technical characteristics actually relevant for landfill constructions are considered in these standards. Therefore, additional tests based on the DepV-list of criteria and mechanisms of action are necessary for CE-marked products. Requirements on quality managements in the hEN are likewise not adequate for essential equivalence with respect to annex 1, No. 2.1, sentence 14 ff, DepV. Therefore, CE-marking is actually no proof of the fulfilment of the state of the techno logy according to the DepV and of the essential equivalence of product properties to the required properties, albeit the declaration of performance indicates a predicted service life of 100 years.
Phoenician ivory objects (8th century B.C., Syria) from the collections of the Badisches Landesmuseum, Karlsruhe, Germany, have been studied with full field X-ray fluorescence microimaging, using synchrotron radiation (SR-FF-microXRF). The innovative Color X-ray Camera (CXC), a full-field detection device (SLcam), was used at the X-ray fluorescence beamline of the ANKA synchrotron facility (ANKA-FLUO, KIT, Karlsruhe, Germany) to noninvasively study trace metal distributions at the surface of the archeological ivory objects. The outstanding strength of the imaging technique with the CXC is the capability to record the full XRF spectrum with a spatial resolution of 48 µm on a zone of a size of 11.9 × 12.3 mm² (264 × 264 pixels). For each analyzed region, 69696 spectra were simultaneously recorded. The principal elements detected are P, Ca, and Sr, coming from the ivory material itself; Cu, characteristic of pigments; Fe and Pb, representing sediments or pigments; Mn, revealing deposited soil minerals; Ti, indicating restoration processes or correlated with Fe sediment traces; and Au, linked to a former gilding. This provides essential information for the assessment of the original appearance of the ivory carvings. The determined elemental maps specific of possible pigments are superimposed on one another to visualize their respective distributions and reconstruct the original polychromy and gilding. Reliable hypotheses for the reconstruction of the original polychromy of the carved ivories are postulated on this basis.
Vor 30 Jahren wurde die erste BAM-Zulassung für ein Geokunststoffprodukt in der Deponietechnik ausgestellt. Seither wurden immer wieder eigene wissenschaftliche Untersuchungen durchgeführt, neue Forschungsergebnisse herangezogen und die Prüftechnik weiterentwickelt, um die Eignung und Funktionsdauer von Kunststoffdichtungsbahnen, Schutzschichten, Kunststoff-Dränelementen, geotextilen Filtern oder Bewehrungsgittern beurteilen zu können. Einige dieser Entwicklungen werden hier diskutiert.
Im ersten Teil dieses Aufsatzes wurde gezeigt, dass nur ein Teil der für den Deponiebau wesentlichen technischen Eigenschaften in den europäisch harmonisierten Bauproduktnormen DIN EN 13252 und DIN EN 13257, die der CE-Kennzeichnung der Geotextilien (GTX) und geotextilverwandten Produkte (GTP) zugrunde liegen, erfasst werden. Um eine im Wesentlichen vorhandene Gleichwertigkeit der Produkteigenschaften überhaupt abwägen zu können, müssen aber sämtliche relevanten Eigenschaften bekannt sein. Dies erfordert für CE-gekennzeichnete Produkte zusätzliche Prüfungen auf der Grundlage der DepV-Liste der Kriterien und Einwirkmechanismen (Anhang 1, Nummer 2.1.1, DepV). In diesem Teil werden die Tabellen C1 und C2 sowie die Tabelle D aus dem ersten Teil, in denen die Eigenschaften der harmonisierten europäischen Normen (hEN) den Anforderungen der DepV gegenübergestellt wurden, in technischer Hinsicht näher erläutert.