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For the first time, an international comparison was conducted on the determination of the purity of a high purity element. Participants were free to choose any analytical approach appropriate for their institute’s applications and services. The material tested was a high purity zinc, which had earlier been assessed for homogeneity and previously used in CCQM-K72 for the determination of six defined metallic impurities. Either a direct metal assay of the Zn mass fraction was undertaken by EDTA titrimetry, or an indirect approach was used wherein all impurities, or at least the major ones, were determined and their sum subtracted from ideal purity of 100 %, or 1 kg/kg. Impurity assessment techniques included glow discharge mass spectrometry, inductively coupled plasma mass spectrometry and carrier gas hot extraction/combustion analysis. Up to 91 elemental impurities covering metals, non-metals and semi-metals/metalloids were quantified. Due to the lack of internal experience or experimental capabilities, some participants contracted external laboratories for specific analytical tasks, mainly for the analysis of non-metals. The reported purity, expressed as zinc mass fraction in the high purity zinc material, showed excellent agreement for all participants, with a relative standard deviation of 0.011 %. The calculated reference value, w(Zn) = 0.999 873 kg/kg, was assigned an asymmetric combined uncertainty of + 0.000025 kg/kg and – 0.000028 kg/kg. Comparability amongst participating metrology institutes is thus demonstrated for the purity determination of high purity metals which have no particular difficulties with their decomposition / dissolution process when solution-based analytical methods are used, or which do not have specific difficulties when direct analysis approaches are used. Nevertheless, further development is required in terms of uncertainty assessment, quantification of non-metals and the determination of purity of less pure elements and/or for those elements suffering difficulties with the decomposition process.
One of the unresolved issues of the European Water Framework Directive is the unavailability of realistic water reference materials for the organic priority pollutants at low nanogram-per-liter concentrations. In the present study, three different types of ready-to-use water test materials were developed for polycyclic aromatic hydrocarbons (PAHs), polybrominated diphenyl ethers (PBDEs) and tributyltin (TBT) at nanogram-per-liter levels. The first type simulated the dissolved phase in the water and comprised of a solution of humic acids (HA) at 5 mg L-1 dissolved organic carbon (DOC) and a spike of the target compounds. The second type of water sample incorporated the particulate phase in water. To this end, model suspended particulate matter (SPM) with a realistic particle size was produced by jet milling soil and sediments containing known amounts of PAHs, PBDEs and TBT and added as slurry to mineral water. The most complex test materials mimicked 'whole water' consequently containing both phases, the model SPM and the HA solution with the target analytes strongly bound to the SPM. In this paper, the development of concepts, processing of the starting materials, characterisation of the HA and model SPMs as well as results for homogeneity and stability testing of the ready-to-use test materials are described in detail.
Aroyl-S,N-ketene acetal-based bichromophores are synthesized by a catalytic aryl amination and their photophysics are studied in the solid state, in ethanol–water mixtures inducing aggregation, and after encapsulation in polystyrene nanoparticles. The dye substitution pattern controls aggregation-induced emission and intramolecular energy transfer efficiency, resulting in single-band or dual fluorescence and a strong increase in fluorescence quantum yield upon particle encapsulation.
A multifunctional sensor in line shape was developed and introduced in previous work for measuring of gas concentrations, temperature change, and strain. A current field study focuses on a spatially distributed monitoring of subsurface CO2 gas storage sites in near real time.
Mechanical impacts, e.g., caused by construction work, denudation, and seismic activity, can affect the integrity of underground gas storage sites. Thermal or moisture impacts, e.g., caused by weather conditions, can influence the gas distribution behavior. In this paper, we briefly describe the setup of a CO2 injection soil test field. This setup contains actuating elements for the investigation of mechanical and thermal impacts on distributed subsurface gas monitoring. A concept is given for evaluating these impacts and first experimental results are presented.
A 400 m² soil test field with gas injection system was built up for the purpose of large-scale validation, optimization, and characterization of a novel comprehensive monitoring method for underground gas storage areas. The method combines gas sensing technology with linear form factor for in-situ monitoring of gases in soil with the mapping capabilities of Computed Tomography (CT) to reconstruct time-series of gas distribution maps based on samples of orthogonally-aligned linear gas sensors. Several injection experiments with carbon dioxide (CO2) at different days with varying boundary conditions indicates the potential of the method for, e.g., rapid leakage detection with respect to Carbon Capture and Storage (CCS) issues.
The standardization and calibration of fluorescence microscopy have become increasingly vital due to the wide-spread use of in life and materials sciences. As the demand for reliable and user-friendly methods to assess micro-scope performance grows, universal calibration tools accessible to both researchers and vendors are needed. To support the standardization of characterization methods in microscopy, it is crucial to provide calibration tools together with standardized operating procedures for their effective implementation.
The public-funded project "FluMiKal"* develops calibration tools in the shape of typical microscopic slides to assess key parameters such as spatial resolution, point spread function, spectral sensitivity, linearity and sensitivity of the detection system. The focus is on creating calibration tools that are user-friendly, robust, and versatile in their application.
This work addresses the critical parameter of wavelength-dependent spectral sensitivity, which affects the meas-ured signals from the instrument side, yielding instrument-specific data and instrument aging-induced changes over time. For this purpose, μ-slides from ibidi with six channels are used, allowing them to be filled with different solutions containing molecular or nanoscale fluorophores with well-characterized absorption and fluorescence properties. The certified spectral fluorescence standards BAM-F003, F004, F005, and F007 assessed provided as ethanolic solutions by the Federal Institute for Materials Research and Testing (BAM), cover a broad spectral range from the blue to the near-infrared [1], [2]. Dye-based slide prototypes have been used to determine the spectral sensitivity of confocal microscopes from different vendors with various detector types by acquiring the spectral data of the BAM dyes under standardized measurement conditions, demonstrating the applicability of this concept. Proof-of-concept experiments could demonstrate the proper sealing of the slides. Further experiments will explore long-term stability and their potential as standards for relative intensity calibrations.
* FluMiKal is funded by the Federal Ministry for Economic Affairs and Climate Action, Germany (WIPANO FKZ 03TN0047B)
[1] doi: 10.1007/4243_2008_028.
[2] doi: 10.1007/s00216-024-05723-w.
Concept for investigating mechanical and thermal impacts on distributed subsurface gas monitoring
(2016)
A multifunctional sensor in line shape was developed and introduced in previous work for measuring of gas concentrations, temperature change, and strain. A current field study focuses on a spatially distributed monitoring of subsurface CO 2 gas storage sites in near real time.
Mechanical impacts, e.g., caused by construction work, denudation, and seismic activity, can affect the integrity of underground gas storage sites. Thermal or moisture impacts, e.g., caused by weather conditions, can influence the gas Distribution behavior. In this paper, we briefly describe the setup of a CO 2 injection soil test field. This setup contains actuating elements for the investigation of mechanical and thermal impacts on distributed subsurface gas monitoring. A concept is given for evaluating these impacts and first experimental results are presented.
