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Eingeladener Vortrag
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Determining the influence of impurities on the fixed-point emperatures
of the ITS-90 requires the completion of several tasks. In this paper, the Progress made at Physikalisch-Technische Bundesanstalt (PTB) and BAMFederal Institute for Materials Research and Testing is presented and remaining questions are discussed.
The projected characterization procedure at PTB, which is based on the established SIE method (sum of the individual estimates), using a new indium fixed-point cell is described as an example. This procedure includes an SI-traceable chemical Analysis of the material in the fixed-point cell with sufficiently low uncertainties, the individual experimental determination of the influence of the quantified impurities on the fixed-point temperature, and the establishment of direct links to the phase-transition temperatures of the national standard and of an assumed material of ideal purity.
A characteristic difference to the common practice is the chemical analysis of the fixed-point metal being done after determining the cells freezing temperature. This allows for the detection and consideration of contamination and purification effects due to the filling process, or due to the contact with the carbon crucible and other parts of the fixed-point cell. A chemical analysis of an indium fixed-point was carried out by BAM with relative measurement uncertainties below 30 % which have not been previously achieved. The results provide evidence for the precipitation of some impurities,
which is apparently inconsistent with the corresponding binary phase diagrams, but was explained in a recent publication. Implications for the use of the SIE method shall be described briefly at the end.
To set up recommendations on how to define “reasonable minimum composition thresholds” for CO2 streams to access CO2 pipeline networks, we investigated potential impacts of CO2 streams with different and temporally variable compositions and mass flow rates along the CCS chain. All investigations were based on a generic “CCS cluster scenario” in which CO2 streams captured from a spatial cluster of eleven emitters (seven fossil-fired power plants, two cement plants, one refinery and one steel mill) are collected in a regional pipeline network. The resulting CO2 stream (19.78 Mio t impure CO2 per year) is transported in a trunk line (onshore and offshore) and injected into five generic replicate storage structures (Buntsandstein saline aquifers) offshore. Experimental investigations and modeling of selected impacts revealed beneficial as well as adverse impacts of different impurities and their combinations. Overall, no fundamental technical obstacles for transporting, injecting and storing CO2 streams of the considered variable compositions and mass flow rates were observed. We recommend to define minimum composition thresholds for each specific CCS project through limiting
i) the overall CO2 content,
ii) maximum contents of relevant impurities or elements,
iii) acceptable variability of concentrations of critical impurities, and defining impurity combinations to be avoided.
The collaborative project “Impacts of impurities in CO2 streams captured from different emitters in a regional cluster on transport, injection and storage (CLUSTER)” aimed to set up recommendations on how to define “reasonable minimum composition thresholds” that CO2 streams should meet when accessing CO2 transport pipeline networks. Within CLUSTER, we investigated potential impacts of CO2 streams with different and temporally variable compositions and mass flow rates along the whole CCS chain. Investigations included, amongst others, impacts on: Corrosion of pipeline steel, pipeline network design and related transport costs, alteration of well bore cements, pressure development and rock integrity, geochemical reactions, and petrophysical and geomechanical rock properties.
All investigations are based on a generic CCS chain scenario. In this scenario, CO2 streams are captured from a spatial cluster of eleven emitters and collected in a regional pipeline network. Emitters comprise seven fossil fuel-fired power plants equipped with different capture technologies, two cement plants, one refinery and one integrated iron and steel plant. In total, 19.78 Mio t CO2 (including impurities) are captured in the emitter cluster annually. The combined CO2 stream is transported in a trunk line with a length of 400 km (100 km of these offshore) and is injected into five generic storage structures. The storage reservoirs are saline aquifers of the Buntsandstein.
The investigations revealed beneficial and deteriorating impacts of different impurities and combinations thereof. Overall, no fundamental technical obstacles for transporting, injecting and storing CO2 streams of the modelled variable compositions and mass flow rates were observed. Based on the results, the CLUSTER project team recommends not to define “minimum composition thresholds” for CO2 streams as strict threshold values for each individual impurity in the stream. Instead, CO2 stream compositions and variabilities for specific CCS projects should be constrained with regard to a set of parameters including i) the overall CO2 content, ii) maximum contents of relevant impurities or elements, iii) acceptable variability of CO2 stream composition, and iv) impurity combinations to be avoided.
A software prototype is developed for assessing and updating the reliability of single-cell prestressed concrete box girders subjected to chloride-induced reinforcement corrosion. The underlying system model consists of two integrated sub-models: a condition model for predicting the deterioration state of the box girder and a structural model for evaluating the overall system reliability. The condition model is based on a dynamic Bayesian network (DBN) model which considers the spatial variation of the corrosion process. Inspection data are included in the calculation of the system reliability through Bayesian updating on the basis of the DBN model. To demonstrate the effect of partial inspections, the software prototype is applied to a case study of a typical highway bridge with six spans. The case study illustrates that it is possible to infer the condition of uninspected parts of the structure due to the spatial correlation of the corrosion process.
Dieser Bericht beschreibt ein Systemmodell für eine integrale Ermittlung und Prognose der Schadens- und Zustandsentwicklung der Elemente eines Brückensystems unter Berücksichtigung von Ergebnissen aus Inspektionen und Überwachung. Das Systemmodell wurde anhand eines ausgesuchten Spannbetonüberbaus in einzelliger Kastenbauweise entwickelt. Es besteht aus zwei integralen Teilmodellen: ein Modell zur Beschreibung des Systemschädigungszustandes und ein Modell zur Beschreibung der Standsicherheit. Für die Modellierung des stochastischen Systemschädigungszustandes eines Brückensystems werden dynamische Bayes'sche Netze (DBN) vorgeschlagen. Dieser Ansatz ermöglicht es, alle relevanten Schädigungsprozesse und deren stochastische Abhängigkeiten zu berücksichtigen. Ein wesentlicher Vorteil dieses Ansatzes ist es, dass DBN ideal dafür geeignet sind, Bayes'sche Aktualisierungen auf Grundlage von Informationen aus Inspektionen und Überwachungsmaßnahme auf eine effiziente und robuste Art und Weise durchzuführen. Der DBN-Ansatz ist deshalb für die Entwicklung von Software für das Erhaltungsmanagement von alternden Brückenbauwerken, die vom Benutzer keine vertieften Kenntnisse der Zuverlässigkeitstheorie verlangt, ideal geeignet. Für die Modellierung der Standsicherheit eines alternden Kastenträgers wird vereinfachend Biegeversagen des globalen Längssystems betrachtet. Zur Berechnung der maximalen Traglast eines Kastenträgers infolge des Systemschädigungszustandes wird ein plastisch-plastisches Verfahren eingesetzt, wobei die Beanspruchungen mittels der Fließgelenktheorie unter Ausnutzung der plastischen Beanspruchbarkeit der Querschnitte des Kastenträgers ermittelt werden. Ein Kastenträger versagt, wenn sich durch die Ausbildung einer ausreichend großen Anzahl von Fließgelenken eine kinematische Kette ausbildet. Dieser Modellierungsansatz berücksichtigt Redundanzen, die sich aus der plastischen Beanspruchbarkeit der Querschnitte und der statischen Unbestimmtheit eines Kastenträgers ergeben. Zum Nachweis der praktischen Einsetzbarkeit des entwickelten Systemmodells wurde ein Software-Prototyp entwickelt, der eine intuitiv benutzbare graphische Benutzeroberfläche (Front-End) mit einem Berechnungskern (Back-End) koppelt. Die aktuelle Version des Software-Prototyps implementiert ein Modell der chloridinduzierten Bewehrungskorrosion und ein Tragwerksmodell, welches das Verfahrens der stetigen Laststeigerung zur Bestimmung der maximalen Traglast des Kastenträgers auf der Grundlage eines Finite-Elemente-Modells umsetzt. Zur Durchführung von Bayes'schen Aktualisierungen des Systemschädigungszustandes auf der Grundlage des DBN-Modells implementiert der Prototyp den Likelihood-Weighting-Algorithmus. Die entwickelte Architektur des Prototyps ermöglicht eine Erweiterung der Software um weitere Schädigungsprozesse. Der entwickelte Software-Prototyp ermöglicht Benutzern ohne vertiefte Kenntnisse der Zuverlässigkeitstheorie eine Berechnung des Einflusses von Bauwerksinformationen auf den Systemschädigungszustand und die Tragsicherheit eines Kastenträgers. Auf dieser Grundlage können effiziente Inspektions- und Überwachungsmaßnahmen identifiziert und das Erhaltungsmanagement optimiert werden.
The analytical utility of a new and simple to use ionization method, matrix-assisted ionization (MAI), coupled with ion mobility spectrometry (IMS) and mass spectrometry (MS) is used to characterize a 2-armed europium(III)-containing poly(ethylene glycol) (Eu-PEG) complex directly from a crude sample. MAI was used with the matrix 1,2-dicyanobenzene, which affords low chemical background relative to matrix-assisted laser desorption/ionization (MALDI) and electrospray ionization (ESI). MAI provides high ion abundance of desired products in comparison to ESI and MALDI. Inductively coupled plasma-MS measurements were used to estimate a maximum of 10% of the crude sample by mass was the 2-arm Eu-PEG complex, supporting evidence of selective ionization of Eu-PEG complexes using the new MAI matrix, 1,2-dicyanobenzene. Multiply charged ions formed in MAI enhance the IMS gas-phase separation, especially relative to the singly charged ions observed with MALDI. Individual components are cleanly separated and readily identified, allowing characterization of the 2-arm Eu-PEG conjugate from a mixture of the 1-arm Eu-PEG complex and unreacted starting materials. Size-exclusion chromatography, liquid chromatography at critical conditions, MALDI-MS, ESI-MS, and ESI-IMS-MS had difficulties with this analysis, or failed.
Layered silicate epoxy nanocomposites: formation of the inorganic-carbonaceous fire protection layer
(2011)
The layered silicate (LS) modification and processing parameters applied control the morphology of the LS/polymer composites. Here, increasing the surface area of the LS particles by using alternative drying processes increases dispersion towards a more typical nanocomposite morphology, which is a basic requirement for promising flame retardancy. Nevertheless, the morphology at room temperature does not act itself with respect to flame retardancy, but serves as a prerequisite for the formation of an efficient surface protection layer during pyrolysis. The formation of this residue layer was addressed experimentally for the actual pyrolysis region of a burning nanocomposite and thus our results are valid without any assumptions or compromises on the time period, dimension, surrounding atmosphere or temperature. The formation of the inorganic-carbonaceous residue is influenced by bubbling, migration, reorientation, agglomeration, ablation, and perhaps also delamination induced thermally and by decomposition, whereas true sintering of the inorganic particles was ruled out as an important mechanism. Multiple, quite different mechanisms are relevant during the formation of the residue, and the importance of each mechanism probably differs from one nanocomposite system to another. The main fire protection effect of the surface layer in polymer nanocomposites based on non-charring or nearly non-charring polymers is the increase in surface temperature, resulting in a substantial increase in reradiated heat flux (heat shielding).
The synthesis and properties of a series of new structure-directing triblock copolymers with PEO-PB-PEO structure (PEO = poly(ethylene oxide) and PB = polybutadiene) and their application as superior pore-templates for the preparation of mesoporous titania coatings are reported. Starting from either TiCl4 or from preformed TiO2 nanocrystalline building blocks, mesoporous crystalline titanium oxide films with a significant degree of mesoscopic ordered pores are derived, and the pore size can be controlled by the molecular mass of the template polymer. Moreover, the triblock copolymers form stable micelles already at very low concentration, i.e., prior to solvent evaporation during the evaporation-induced self-assembly process (EISA). Consequently, the thickness of pore walls can be controlled independently of pore size by changing the polymer-to-precursor ratio. Thus, unprecedented control of wall thickness in the structure of mesoporous oxide coatings is achieved. In addition, the micelle formation of the new template polymers is sufficiently distinct from that of typical commercial PPO-PEO-PPO polymers (Pluronics; PPO = poly(propylene oxide)), so that a combination of both polymers facilitates bimodal porosity via dual micelle templating.
The collaborative project “Impacts of impurities in CO2 streams captured from different emitters in a regional cluster on transport, injection and storage (CLUSTER)” aimed to set up recommendations on how to define “reasonable minimum composition thresholds” that CO2 streams should meet when accessing CO2 transport pipeline networks. Within CLUSTER, we investigated potential impacts of CO2 streams with different and temporally variable compositions and mass flow rates along the whole CCS chain. Investigations included, amongst others, impacts on:
• corrosion of pipeline steel,
• pipeline network design and related transport costs,
• alteration of well bore cements,
• pressure development and rock integrity,
• geochemical reactions, and
• petrophysical and geomechanical rock properties.
All investigations are based on a generic CCS chain scenario. In this scenario, CO2 streams are captured from a spatial cluster of eleven emitters and collected in a regional pipeline network. Emitters comprise seven fossil fuel-fired power plants equipped with different capture technologies, two cement plants, one refinery and one integrated iron and steel plant. In total, 19.78 Mio t CO2 (including impurities) are captured in the emitter cluster annually. The combined CO2 stream is transported in a trunk line with a length of 400 km (100 km of these offshore) and is injected into five generic storage structures. The storage reservoirs are saline aquifers of the Buntsandstein.
The investigations revealed beneficial and deteriorating impacts of different impurities and combinations thereof. Overall, no fundamental technical obstacles for transporting, injecting and storing CO2 streams of the modelled variable compositions and mass flow rates were observed. Based on the results, the CLUSTER project team recommends not to define “minimum composition thresholds” for CO2 streams as strict threshold values for each individual impurity in the stream. Instead, CO2 stream compositions and variabilities for specific CCS projects should be constrained with regard to a set of parameters including i) the overall CO2 content, ii) maximum contents of relevant impurities or elements, iii) acceptable variability of CO2 stream composition, and iv) impurity combinations to be avoided.