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Chapter 5 Analytical techniques for Per- and Polyfluoroalkyl substances (PFAS)
No full textPer- and polyfluoroalkyl substances (PFAS) are a group of various anthropogenic organic products, in which the hydrogen atoms on the carbon skeleton of at least one carbon atom have been completely replaced by fluorine atoms. Because this group contains more than 7 million compounds, they can have very different properties. PFAS analysis in environmental samples is currently mainly utilized by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and related techniques as well as gas chromatography-mass spectrometry (GC-MS) to conduct target analysis. However, to get a better overview of the amount of “total” amount of PFAS, sum parameter methods like total oxidizable precursor assay (TOPA), absorbable organic fluorine (AOF), and extractable organic fluorine (EOF) are in development. Additionally, for research purposes, several spectroscopical methods like X-ray photoelectron spectroscopy (XPS), fluorine K-edge X-ray absorption near-edge structure (XANES) spectroscopy, particular induced gamma-ray emission (PIGE) spectroscopy as well as19 F nuclear magnetic resonance (NMR), infrared, and Raman spectroscopy are available. Therefore, an overview is given on currently available analytical techniques for PFAS in environmental samples and their application possibilities discussed for different kinds of PFAS subgroups
Characteristic Frequencies of Train-Induced Bridge, Track, Ground and Building Vibrations – Excitation and Mitigation
No full textThe characteristic frequencies of train-induced vibrations are discussed in theory and experiment following the propagation of vibrations from the source to the receiver: 1. Out-of-roundness frequencies of the wheels, 2. sleeper-passage frequency, 3. the vehicle-track eigenfrequency, 4. band frequency of the impulses of the passing static axle loads, 5. car-length frequency and multiples, 6. axle-distance frequencies with two characteristic zeros, 7. bridge eigenfrequencies, 8. the cut-on frequency due to the layering, and 9. the cut-off frequency due to the material damping of the soil, 10. the building-soil eigenfrequency, 11. as a rigid building or flexible wall/column mode, 12. floor eigenfrequencies, 13. acoustic room resonances, 14. the „resonance“ frequency or cut-off frequency of a base isolation. Coincidences of some of these characteristic frequencies or frequency ranges can be typically problematic and mitigation measures at the track or at the building can be necessary. The bridge response to the passing static loads is deter¬mined by the axle-sequence spectrum, the eigenfrequency (transfer function) of the bridge, and the modal force or mode shape spectrum. The ground vibration has typically high frequencies for a stiff soil and low frequencies for a soft soil. The high amplitudes between the zeros of the axle-sequence spectrum are often measured in the ground vibrations, and they can be mitigated by soft support elements or a higher bending stiffness of the track
Characteristic Frequencies of Train-Induced Bridge, Track, Ground and Building Vibrations – Excitation and Mitigation
No full textThe characteristic frequencies of train-induced vibrations are discussed in theory and experiment following the propagation of vibrations from the source to the receiver: 1. Out-of-roundness frequencies of the wheels, 2. sleeper-passage frequency, 3. the vehicle-track eigenfrequency, 4. band frequency of the impulses of the passing static axle loads, 5. car-length frequency and multiples, 6. axle-distance frequencies with two characteristic zeros, 7. bridge eigenfrequencies, 8. the cut-on frequency due to the layering, and 9. the cut-off frequency due to the material damping of the soil, 10. the building-soil eigenfrequency, 11. as a rigid building or flexible wall/column mode, 12. floor eigenfrequencies, 13. acoustic room resonances, 14. the „resonance“ frequency or cut-off frequency of a base isolation. Coincidences of some of these characteristic frequencies or frequency ranges can be typically problematic and mitigation measures at the track or at the building can be necessary. The bridge response to the passing static loads is deter¬mined by the axle-sequence spectrum, the eigenfrequency (transfer function) of the bridge, and the modal force or mode shape spectrum. The ground vibration has typically high frequencies for a stiff soil and low frequencies for a soft soil. The high amplitudes between the zeros of the axle-sequence spectrum are often measured in the ground vibrations, and they can be mitigated by soft support elements or a higher bending stiffness of the track
Digital image processing for the advanced characterization and simulation of experimental fire tests
No full textThe fire engulfment of storage tanks of hazardous materials is among the most critical scenarios in hazard assessment of industrial value chains. Laboratory and full-scale experimental trials are used to test the tank performance and integrity in such scenarios. However, strong uncertainties usually affect the actual fire load experienced by the tank, in particular when large-scale experiments are carried out in open test fields. Such uncertainties arise from several factors difficult to control during experimental tests, such as the atmospheric conditions as there is the influence of wind drifts influencing the actual fire engulfment, the flame temperature and the flame dynamic distribution around the target. Consequently, verifying the concordance of an experimental test with standard test criteria and defining accurate boundary conditions in correlated model simulations is challenging. In this study, the development of a novel method for the analysis of fire conditions based on image processing is presented. The approach allows identifying the flame coverage on the target surface during the test and provides an accurate map of the flame distribution on the equipment over time. The approach is tested using experimental data from a full-scale fire test campaign carried out on liquid hydrogen cryogenic tanks. The results prove to be accurate in replicating the experimental temperatures measured on the outer tank shell during the test. The proposed methodology can be used to better understand the results of experimental fire tests and to characterize realistic fire scenarios, also supporting the definition of fire test requirements. Moreover, the approach produces results that can be implemented as advanced space-time-varying boundary conditions in simulation models, improving their accuracy in reproducing real cases
Initial VOC Emissions from Consumer Products Determined in Micro-Scale Test Chambers: Results of a Round Robin Test
No full textEmissions of volatile organic compounds (VOCs) from consumer products may have a negative impact on indoor air quality, potentially also affecting human wellbeing. Since consumers may be exposed to these VOCs immediately after e.g. unwrapping of newly purchased products, reliable analytical methods are needed to determine air concentration profiles in the early phase of VOC emissions. Concerning typical sample sizes of consumer products, micro-scale test chambers (μ-chambers) were considered suitable for this purpose. In addition, compared to medium- or large-scale test chambers, μ-chambers require lower initial investment and operational costs, and offer options for emissions screenings where higher sample throughput is essential. For these reasons, a μ-chamber-based method to determine initial concentrations of VOCs emitting within the first hours of simulated product use was developed. The chamber air was frequently sampled on desorption tubes loaded with Tenax® TA, followed by quantification of emitted VOCs via thermal desorption gas chromatography mass spectrometry (TD-GC-MS). The method was assessed in a round robin test involving eight participating laboratories from 2 countries. Pieces of a rain poncho (sample area A: 2.01·10-4 m2) emitting cyclohexanone, phenol, 2-ethylhexanol, naphthalene and isophorone in significant concentrations were distributed as sample material. Each laboratory conducted triplicate emission tests over a period of 48 h in μ-chambers with volumes of 44 or 114 mL. The loading factors L of 4.57 m2·m-3 (44 mL) or 1.76 m2·m-3 (114 mL) and air flow rates of 24 mL·min-1 resulted in area-specific air flow rates q of 7.17 m3·m-2·h-1 in both chamber types. The temperature was set to 23°C and, if possible, relative humidity was set to approx. 50%. The chamber air was sampled after 0.5, 1, 2, 4, 24 and 48 hours. In addition, to assess the analytical performance, each participating laboratory received two analyte-spiked Tenax® TA-loaded desorption tubes for quality control (QC). Very low relative standard deviations (11–17%) were obtained for the QC test. The results of the emissions tests in the early phase (0.5–4 h) were also adequate, with acceptable z scores (|z|≤2.00) received by six to seven participating laboratories. All eight laboratories obtained acceptable z scores after the longer sampling periods (24 and 48 h). Hence, the inter-laboratory comparability of the results obtained with the developed μ-chamber method was successfully confirmed
Superparamagnetic Bead-Based Microfluidic Fluoroimmunoassay Platform for Rapid Ochratoxin A Detection in Flour
No full textSimplification and reduction of time and costs are the primary goals in the development and use of onsite methods in diagnostics and food safety. To facilitate the transition from laboratory techniques to simple, miniaturized devices, we have developed a modular microfluidic platform. This platform integrates a competitive fluorescence immunoassay on the surface of superparamagnetic beads, serving as a complementary technique to traditional cytometry assays. In the first chip module, a fast competitive reaction (5 min) occurs, after which the particles are retained in the second module. This module consists of a PDMS chip and a permanent magnet, allowing only the fluorescent competitor to reach the detection module. Ochratoxin A (OTA) was chosen as the model analyte for device development, using fluorescein-labeled OTA as a competitor. The system efficiently separates particles, with OTA concentration directly correlated to the amount of fluorescent competitor remaining in solution after the competitive reaction. This innovative setup allows to perform rapid measurements with small sample volumes in a short time (10 min), achieving a limit of detection for OTA of 1.2 μg L–1. The system was successfully applied to the accurate determination of OTA in wheat flour spiked at regulatorily relevant concentrations. Using this device, conventional cytometry immunoassays can be seamlessly transformed into user-friendly, miniaturized analytical methods at reduced cost for applications outside of a laboratory directly at the point of need
Combined passive and active ultrasonic stress wave monitoring of a full‑scale laboratory reinforced concrete bridge column subject to reverse‑cyclic lateral loading
No full textEffective monitoring of reinforced concrete structures requires techniques that detect early-stage material change and active, localized cracking. This study investigates a combined structural health monitoring approach using passive acoustic emission and active ultrasonic methods on a full-scale reinforced concrete bridge column subjected to reverse-cyclic lateral loading.
Active monitoring, based on coda wave interferometry, was used to track changes in wave velocity and waveforms, while passive acoustic emission monitoring was used to detect crack activity. The instrumentation consisted of three embedded ultrasonic transducers and three surface-mounted acoustic emission sensors. The results show that active ultrasonic monitoring is most effective prior to visual damage, successfully detecting the onset of internal cracking via wave velocity decreases exceeding 0.4%, and distinguishing load-induced effects from permanent damage. However, its utility diminished in later stages of damage progression, as strong signal decorrelation hindered further data interpretation. Additionally, active US measurements allowed a comparison of damage severity in different parts of the column. Conversely, passive acoustic emission monitoring effectively tracked the formation of concrete cracks throughout the experiment, with distinct event clusters and high-amplitude signals (> 60 dB) confirming ongoing fracture processes in all damage states. This study confirms that combining these methods results in a more robust structural health monitoring strategy by leveraging their complementary strengths. Active techniques excel at tracking continuous material changes in early damage states, while passive methods are superior for detecting discrete cracking events as damage progresses. Importantly, both methods can utilize the same measurement equipment, enabling a cost-effective approach to continuous damage tracking
Fire Test Stand for Thermal Testing of Large Packages for the Transport of Radioactive Materials
No full textPackages for the transport of high level radioactive materials are designed to withstand severe accidents. These packages must comply with the specific safety requirements SSR 6 [ of the International Atomic Energy Agency (IAEA). To guarantee compliance with these requirements, specific mechanical and thermal tests need to be addressed r egard ing the package type. Typically,
the r egulations prescribe mechanical tests followed by a thermal test as part of a cumulative test scenario. The thermal test is specified by the exposure of a test specimen for a period of 30 minutes to a thermal environment that provides a heat flux equivalent to that of a hydrocarbon fuel air fire with an av erage fire temperature of at least 800 °C fully flame engulfing the test specimen. The Federal Institute for Materials Research and Testing (BAM) operates various test facilities for this purpose at their Test Site for Technical Safety (near Berlin in Germany).
Thermal tests for large packages are conducted in an established fire test stand that may be adapted by the test setup to the geometric boundary conditions of a test specimen. This fire test stand is built for test specimens with masses up to 200,000 kg an d geometric dimensions relating to large transport packages including their impact limiters. The test specimen is usually placed on a water cooled support frame in the middle of the test stand. The fire is realized by burning propane gas which is released in liquid state from an array of gas nozzles arranged in the form of a burner ring surrounding the test specimen. For particularly extra large test specimens, two burner rings are used on top of each other and at different heights to firstly achieve full f ire engulfment with a significantly larger volume of fire and secondly to achieve the required heat output , cf. In advance of a regular thermal test BAM usually performs so called fire reference tests to determine the test conditions for compliance with the IAEA requirements. These tests are performed using a generic package which corresponds to the external geometr ic dimensions of the test specimen used later in the approval test. Then, this reference package is exposed to a fire under defined test parameters whereas the corresponding heat input determined from the temperature changes measured is regarded as main cr iterion for proofing compliance with the IAEA criteria. The paper shows the experimental proof of the suitability of BAM’s fire test stand for thermal testing of extra large packages. The heat input and fire temperatures fully meet the IAEA criteria and can also be set significantly higher for example for extra regulatory testing
Long-term tests on metal seals using continuous force measurement in compressed state
No full textIn Germany, spent fuel and heat generating radioactive waste is stored in casks for transport and storage (DPCs). The storage licenses were granted for up to 40 years. Due to the delay in identifying a final repository site for such radioactive waste, the storage periods are to be extended significantly. The objective of our research work is to collect additional material data for metal seals in order to be able to better assess the long-term safety of the sealing system of the casks for a period of up to 100 years.
A principal safety consideration for the DPCs is the long-term performance of bolted lid sealing systems utilizing metal seals to ensure the safe enclosure of the radioactive inventory during interim storage. To assess the sealing behavior, it is necessary to examine the aging-dependent residual restoring force for the metal seals and the usable resilience. By investigating the change in these values as a function of time and temperature, further insight can be gained into the assessment of long-term safety for extended interim storage.
In the present study, the restoring force of metal seals with an outer aluminum jacket and a torus diameter of 9.9 mm was measured continuously. For this purpose, a specially designed device equipped with a load cell was used under isothermal conditions. As part of the investigation, the level and rate of decrease of the restoring seal force were recorded over test periods of one and two months. The seal temperature was set to 35 °C, 75 °C, 100 °C, 125 °C, and 150 °C, respectively. A direct correlation was observed between the temperature of the seal, the level of the restoring force after compressing and heating the seal, and the drop-off characteristics of the restoring force. It was found that in our test device the force level immediately after reaching the respective temperature is lower for higher seal temperatures, while the drop rate of the restoring force is higher. This paper describes the experimental setting and discusses first results in comparison with our long-term discontinuous measurements
In-service and repair welding of pressurized hydrogen pipelines–a review on current challenges and strategies
No full textHydrogen is the energy carrier for a sustainable future without fossil fuels. As this requires a reliable transportation infrastructure, the conversion of existing natural gas (NG) grids is an essential part of the worldwide individual national hydrogen strategies, in addition to newly erected pipelines. In view of the known effect of hydrogen embrittlement, the compatibility of the materials already in use (typically low-alloy steels in a wide range of strengths and thicknesses) must be investigated. Initial comprehensive studies on the hydrogen compatibility of pipeline materials indicate that these materials can be used to a certain extent. Nevertheless, the material compatibility for hydrogen service is currently of great importance. However, pipelines require frequent maintenance and repair work. In some cases, it is necessary to carry out welding work on pipelines while they are under pressure, e.g., the well-known tapping of NG grids. This in-service welding brings additional challenges for hydrogen operations in terms of additional hydrogen absorption during welding and material compatibility. The challenge can be roughly divided into two parts: (1) the possible austenitization of the inner piping material exposed to hydrogen, which can lead to additional hydrogen absorption, and (2) the welding itself causes an increased temperature range. Both lead to a significantly increased hydrogen solubility in the respective materials compared to room temperature. In that connection, the knowledge on hot tapping on hydrogen pipelines is rare so far due to the missing service experiences. Fundamental experimental investigations are required to investigate the possible transferability of the state-of-the-art concepts from NG to hydrogen pipeline grids. This is necessary to ensure that no critical material degradation occurs due to the potentially increased hydrogen uptake. For this reason, the paper introduces the state of the art in pipeline hot tapping, encompassing current research projects and their individual solution strategies for the problems that may arise for future hydrogen service. Methods of material testing, their limitations, and possible solutions will be presented and discussed