Filtern
Dokumenttyp
Sprache
- Englisch (16)
Schlagworte
Organisationseinheit der BAM
- 7 Bauwerkssicherheit (5)
- 8 Zerstörungsfreie Prüfung (4)
- 8.5 Röntgenbildgebung (4)
- 1 Analytische Chemie; Referenzmaterialien (3)
- 1.7 Organische Spuren- und Lebensmittelanalytik (2)
- 1.8 Umweltanalytik (2)
- 7.2 Ingenieurbau (2)
- 7.4 Baustofftechnologie (2)
- S Qualitätsinfrastruktur (2)
- S.1 Qualität im Prüfwesen (2)
- 7.0 Abteilungsleitung und andere (1)
The demonstration of competency and equivalence for the assessment of levels of contaminants and nutrients in primary foodstuffs is a priority within the 10-year strategy for the OAWG Track A core comparisons. The measurements are core challenges for reference material producers and providers of calibration Services. This key comparison related to low polarity analytes in a high fat, low protein, low carbohydrate food matrix and Benzo[a]pyrene in edible oil was the model System selected to align with this class within the OAWG strategy. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims (CMCs) made by national metrology institutes (NMIs) and designated institutes (Dis). 16 National Metrology Institutions participated in the Track A Key Comparison CCQM-K146 Low-Polarity Analyte in high fat food: Benzo[a]pyrene in Olive Oil. Participants were requested to evaluate the mass fractions, expressed in µg/kg, of Benzo[a]pyrene in the olive oil material. The KCRV was determined from the results of all NMIs/DIs participating in the key comparison that used appropriately validated methods with demonstrated metrological traceability. Different methods such as liquid-liquid extraction, GPC and SPE were applied in the sample pretreatment and HPLC-FLD, HPLC-MS/MS, and GC-MS or GC-MS/MS were applied for detection by the participants. The mass fractions for BaP were in the range of (1.78 to 3.09) µg/kg with Standard uncertainties of (0.026 to 0.54) µg/kg, with corresponding relative Standard uncertainties from 0.9% to 21%. Five labs withdrew their result from the Statistical evaluation of the KCRV for technical reasons. One lab was excluded from the KCRV evaluation, as they did not meet the CIPM metrological traceability requirements. A Hierarchical Bayes option was selected for the KCRV value, which was determined as 2.74 µg/kg with a Standard uncertainty of 0.03 µg/kg. The 10 institutes those were included in the calculation of the consensus KCRV all agreed within their Standard uncertainties. Successful participation in CCQM-K146 demonstrates the measurement capabilities in determining mass fraction of organic compounds, with molecular mass of 100 g/mol to 500 g/mol, having low polarity pKow < -2, in mass fraction range from 0.1 µg/kg to 1000 µg/kg in a high fat, low protein, low carbohydrate food matrix.
Extraction, chromatographic separation, and quantification of low-concentration organic compounds in complex matrices are core challenges for reference material producers and providers of calibration services. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims made by national metrology institutes (NMIs) and designated institutes (DIs). To enable NMIs and DIs to update or establish their claims, in 2014 the Organic Analysis Working Group (OAWG) initiated CCQM-K95.1 "Low-Polarity Analytes in a Botanical Matrix: Polycyclic Aromatic Hydrocarbons (PAHs) in Tea". This was a follow-on comparison from CCQM-K95 which was completed in 2014.
The polycyclic aromatic hydrocarbons (PAHs) benz[a]anthracene (BaA) and benzo[a]pyrene (BaP) are considered priority pollutants by U.S. Environmental Protection Agency and are regulated contaminants in food, pose chromatographic separation challenges, and for which exist well-characterized measurement procedures and standard materials. BaA and BaP in a smoked tea were therefore selected as representative target measurands for CCQM-K95.1. Ten NMIs participated in CCQM-K95.1. The consensus summary mass fractions for the two PAHs are in the range of (50 to 70) ng/g with relative standard deviations of (6 to 10) %.
Successful participation in CCQM K95.1 demonstrates the following measurement capabilities in determining mass fraction of organic compounds, with molar mass of 100 g/mol to 500 g/mol and having polarity pKow −2, in a botanical matrix ranging in mass fraction from 10 ng/g to 1000 ng/g: (1) value assignment of primary reference standards (if in-house purity assessment carried out), (2) value assignment of single and/or multi-component organic solutions, (3) extraction of analytes of interest from the matrix, (4) cleanup and separation of analytes of interest from interfering matrix or extract components, and (5) separation and quantification using gas chromatography or liquid chromatography.
Solutions of organic analytes of known mass fraction are typically used to calibrate the measurement processes used to determine these compounds in matrix samples. Appropriate value assignments and uncertainty calculations for calibration solutions are critical for accurate measurements. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims (CMCs) made by national metrology institutes (NMIs) and designated institutes (DIs). To enable NMIs and DIs to update or establish their claims, in 2015 the Organic Analysis Working Group (OAWG) sponsored CCQM-K131 "Low-Polarity Analytes in a Multicomponent Organic Solution: Polycyclic Aromatic Hydrocarbons (PAHs) in Acetonitrile".
Polycyclic aromatic hydrocarbons (PAHs) result from combustion sources and are ubiquitous in environmental samples. The PAH congeners, benz[a]anthracene (BaA), benzo[a]pyrene (BaP), and naphthalene (Nap) were selected as the target analytes for CCQM-K131. These targets span the volatility range of PAHs found in environmental samples and include potentially problematic chromatographic separations. Nineteen NMIs participated in CCQM-K131. The consensus summary mass fractions for the three PAHs are in the range of (5 to 25) μg/g with relative standard deviations of (2.5 to 3.5) %.
Successful participation in CCQM-K131 demonstrates the following measurement capabilities in determining mass fraction of organic compounds of moderate to insignificant volatility, molar mass of 100 g/mol up to 500 g/mol, and polarity pKow < −2 in a multicomponent organic solution ranging in mass fraction from 100 ng/g to 100 μg/g: (1) value assignment of primary reference standards (if in-house purity assessment carried out), (2) value assignment of single and/or multi-component organic solutions, and (3) separation and quantification using gas chromatography or liquid chromatography.
A thorough characterization of starting materials is the precondition for further research, especially for cement, which contains various phases and presents quite a complex material for fundamental scientific investigation. In the paper at hand, the characterization data of the reference cement CEM I 42.5 R used within the priority program 2005 of the German Research Foundation (DFG SPP 2005) are presented from the aspects of chemical and mineralogical compositions as well as physical and chemical properties. The data were collected based on tests conducted by nine research groups involved in this cooperative program. For all data received, the mean values and the corresponding errors were calculated. The results shall be used for the ongoing research within the priority program.
Two types of cements were selected as the reference cement in the priority program 2005 of the German Research Foundation (DFG SPP 2005). A thorough characterization of CEM I 42.5 R has been made in a recent publication. In this paper, the characterization data of the other reference cement CEM III/A 42.5 N are presented from the aspects of chemical and mineralogical compositions as well as physical and chemical properties. The characterization data of the slag, which is the second main constituent of this specific cement besides the clinker, are presented independently. For all data received, the mean values and the corresponding errors were calculated. The data shall be used for the ongoing research within the priority program. Also, researchers from outside this priority program can benefit from these data if the same materials are used.
A systematic, nature-inspired chemical engineering approach is employed to solve the issue of flooding in electrochemical devices. The mechanism of passive water transport utilized by lizards living in arid environments is leveraged to design flow-fields with a microchannel structure on their surface, through which capillary pressure rapidly removes the water generated in the electrochemical device. This water management strategy is implemented in proton exchange membrane fuel cells (PEMFCs) with a lunginspired flow-field, which ensures uniform distribution of reactants across the catalyst layer. Jointly, this nature-inspired approach results in flood-free, stable operation at 100% RH and a B60% increase in current (B1.9 A cm-2) and peak power density (B650 mW cm−2) compared to current PEMFCs with a flood-prone, serpentine flow-field (B0.8 A cm-2 and 280 mW cm-2, respectively). This significant advance allows for PEMFC operation at fully humidified conditions.
Rechargeable alkali metal−CO2 batteries, which combine high theoretical energy density and environmentally friendly CO2 fixation ability, have attracted worldwide attention. Unfortunately, their electrochemical performances are usually inferior for practical applications. Aiming to reveal the underlying causes, a combinatorial usage of advanced nondestructive and postmortem characterization tools is used to intensively study the failure mechanisms of Li/Na−CO2 batteries. It is found that a porous interphase layer is formed between the separator and the Li/Na anode during the overvoltage rising and battery performance decaying process. A series of control experiments are designed to identify the underlying mechanisms dictating the observed morphological evolution of Li/Na anodes, and it is found that the CO2 synergist facilitates Li/Na chemical corrosion, the process of which is further promoted by the unwanted galvanic corrosion and the electrochemical cycling conditions. A detailed compositional analysis reveals that the as-formed interphase layers under different conditions are similar in species, with the main differences being their inconsistent quantity. Theoretical calculation results not only suggest an inherent intermolecular affinity between the CO2 and the electrolyte solvent but also provide the most thermodynamically favored CO2 reaction pathways. Based on these results, important implications for the further development of rechargeable alkali metal−CO2 batteries are discussed. The current discoveries not only fundamentally enrich our knowledge of the failure mechanisms of rechargeable alkali metal−CO2 batteries but also provide mechanistic directions for protecting metal anodes to build high-reversible alkali metal−CO2 batteries.
Rechargeable sodium–oxygen batteries (NaOBs) are receiving extensive research interests because of their advantages such as ultrahigh energy density and cost efficiency. However, the severe failure of Na metal anodes has impeded the commercial development of NaOBs. Herein, combining in situ synchrotron X-ray computed tomography (SXCT) and other complementary characterizations, a novel electro-chemo-mechanical failure mechanism of sodium metal anode in NaOBs is elucidated. It is visually showcased that the Na metal anodes involve a three-stage decay evolution of a porous Na reactive interphase layer (NRIL): from the initially dot-shaped voids evolved into the spindle-shaped voids and the eventually-developed ruptured cracks. The initiation of this three-stage evolution begins with chemical-resting and is exacerbated by further electrochemical cycling. From corrosion science and fracture mechanics, theoretical simulations suggest that the evolution of porous NRIL is driven by the concentrated stress at crack tips. The findings illustrate the importance of preventing electro-chemo-mechanical degradation of Na anodes in practically
rechargeable NaOBs.
The mechanical compression of metal foam flow-field based polymer electrolyte fuel cells (PEFCs) is critical in determining the interfacial contact resistance with gas diffusion layers (GDLs), reactant flow and water management.
The distinct scale between the pore structure of metal foams and the entire flow-field warrant a multilength scale characterization that combines ex-situ tests of compressed metal foam samples and in-operando analysis of operating PEFCs using X-ray computed tomography (CT) and neutron radiography. An optimal ‘medium’ compression was found to deliver a peak power density of 853 mW/cm². The X-ray CT data indicates that the compression process significantly decreases the mean pore size and narrows the pore size distribution of metal foams. Simulation results suggest compressing metal foam increases the pressure drop and gas velocity, improving the convective liquid water removal. This is in agreement with the neutron imaging results that demonstrates an increase in the mass of accumulated liquid water with minimum compression compared to the medium and maximum compression cases. The results show that a balance between Ohmic resistance, water removal capacity and parasitic power is imperative for the optimal performance of metal foam based PEFCs.
A strain-based automated operational modal analysis algorithm is proposed to track the long-term dynamic behavior of a horizontal wind turbine under operational conditions.
This algorithm is firstly validated by a scaled wind turbine model, and then it is applied to the dynamic strain responses recorded from a 5 MW wind turbine system. We observed variations in the fundamental frequency and 1f, 3f excitation frequencies due to the mass imbalance of the blades and aerodynamic excitation by the tower dam or tower wake. Inspection of the Campbell diagram revealed that the adverse resonance phenomenon and Sommerfeld effect causing excessive vibrations of the wind tower.
X-ray computed tomography (CT) and mercury porosimetry were combined to connect density gradients and the distribution of open porosity in a sintered compact. CT clearly showed that open porosity follows the initial distribution of low-density zones. Mercury porosimetry detected three distinct levels of porosity. Microstructural examination correlated the porosity level with the coordination of (i) two to three or (ii) multiple grains around pores. This combination of techniques provides a novel tool for the study of pore and density-gradient evolution during sintering.
Structural health monitoring systems have been widely implemented to provide real-time continuous data support and to ensure structural safety in the context of structural integrity management. However, the quantification of the potential benefits of structural health monitoring systems has not yet attracted widespread attention. At the same time, there is an urgent need to develop strategies, such as optimizing the monitoring period, monitoring variables, and other factors, to maximize the potential benefits of structural health monitoring systems. Considering the continuity of structural health monitoring information, a framework is developed in this article to support decision-making for structural Health monitoring systems arrangement in the context of structural integrity management, which integrates the concepts of value of information and risk-based inspection planning based on an approach which utilizes a conjugate prior probability distribution for updating of the probabilistic models of structural performances based on structural health Monitoring information. An example considering fatigue degradation of steel structures is investigated to illustrate the application of the proposed framework. The considered example shows that the choice of monitoring variables, the Monitoring period, and the monitoring quality may be consistently optimized by the application of the proposed framework and approach. Finally, discussions and conclusions are provided to clarify the potential benefits of the proposed Framework with a special view to practical applications of structural health monitoring systems.
This paper addresses operational modal analysis (OMA) and continuous dynamic monitoring (CDM) of two bridges. One of them is installed with Tuned Mass Dampers (TMDs) while another one is a normal bridge. Two ambient vibration tests were performed on these two bridges respectively. It is observed that not only installation of TMDs but also environmental factors influence the variations of structural frequencies, which may mask the subtle change induced by small structural changes. As a result, continuous dynamic monitoring systems were implemented on these two bridges, in order to evaluate efficiency of the TMD system, remove the environmental effects and build reliable damage indices that are only sensitive to structural changes. The results of CDM of these two bridges during several years are presented. Software systems developed for OMA and CDM are also introduced.
This paper proposes a novel method to estimate the lateral displacement of high-rise structures under wind loads. The coefficient β(x) is firstly derived, reflecting the relation between the structural lateral dynamic displacement and the inclination angle at the height x of a structure. If the angle is small, it is the ratio between the structural fundamental mode shape and its first-order derivative without influence of external loads. Several dynamic experiments of structures are performed based on a laser remote sensing vibrometer and an inclinometer, which shows that the fundamental mode is dominated in the structural displacement response under different types of excitations. Once the coefficient β(x) is curve-fitted by measuring both the structural lateral dynamic displacement and the inclination angle synchronously, the real-time structural lateral displacement under operational conditions is estimated by multiplying the coefficient β(x) with the inclination angle. The advantage of the proposed method is that the coefficient β(x) can be identified by lateral dynamic displacement measured in high resolution by the remote sensing vibrometer, which is useful to reconstruct the displacement accurately by the inclination angle under operational conditions
Well-defined and facetted bimetallic gold–palladium nanoalloys have been synthesized and anchored in spherical polyelectrolyte brushes (SPB) as composite particles (AuPd@SPB). These particles are better catalysts in aqueous phase than the pure metals. The atomistic arrangement of these nanoalloys has been analysed by extended X-ray absorption fine structure (EXAFS) spectroscopy at the Au–L3 and the Pd–K absorption edge. The samples with high amounts of gold appear as almost statistically mixed random alloys. Alloy compositions with less gold show slight enrichment of Pd at the surface of the particle. In addition, signals of non-metallic palladium appear at the Pd–K edge which indicate the presence of the Pd2+ species in addition to metallic palladium. The relation of these structural features to the catalytic activity is discussed.
Here, we present an investigation of the triple-shape properties of star-shaped polyhedral oligomeric silsesquioxane-poly(ε-caprolactone) polyurethanes (SPOSS-PUs), which have three-dimensional network structures. In a typical 'triple-shape functionalization process', mostly consisting of two tensile deformations at different temperatures, chain immobilization of the polymer network component poly(ε-caprolactone) (PCL) was successfully realized first through crystallization and then through vitrification. Subsequently, large parts of the respective strains were released under stress-free recovery conditions. The two-fold fixed ('programmed') specimens responded to heating with two independent length contractions (switching steps); the first shape change was associated with PCL devitrification and the second one with the melting of hitherto crystalline PCL. It was revealed that the triple-shape properties of SPOSS-PU networks considerably depend on PCL network chain length. When applying exactly the same 'triple-shape creation procedure', larger strain releases were detected in the first transition for polymers with a higher PCL network chain length, whereas the second transition was more accentuated for SPOSS-PU networks with a shorter PCL chain length. In the course of thermo-mechanical cycling, the formation of a neck during the second tensile deformation was repeatedly detected for SPOSS-PUs with higher PCL network chain length; in the subsequent recovery process the specimens even exhibited the highest total strain recoverability. Finally, gradual strain release could be achieved at temperatures below the PCL melting transition through the selection of up to four temperature holding steps, at which every time stable shapes were formed.