Chemische Charakterisierung und Spurenanalytik
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Since 1997, the Committee for Health-related Evaluation of Building Products (AgBB) has been developing the basis for building regulations for protection against indoor health risks that may arise when building products are used. In 2009, the AgBB decided to include relevant VVOCs in the assessment procedure. The ISO 16000-6 (2021) states that the use of the thermal desorption gas chromatography technique is appropriate for VVOCs, if adaptations are considered. However, a suitable method for the trustworthy quantification of VVOC emissions from building products and in the indoor air is still missing.
This webinar will present the results of a research project on the development of a procedure for VVOC analysis:
• identification of the gaps towards standardization
• investigations on gas standards and the suitability of chromatography columns
• investigations on sorbent combinations and water management
• validation of the method and screening of VVOC emissions from building products.
Das europäische Projekt MefHySto befasst sich mit dem Bedarf an großmaßstäblichen Energiespeichern, die für eine Umstellung der Energieversorgung auf erneuerbare Energien erforderlich sind. Eine solche Speicherung ist entscheidend, um Energie zu Spitzenzeiten zu liefern, wenn die erneuerbaren Energiequellen schwanken. Eine mögliche Lösung für die Energiespeicherung ist der großtechnische Einsatz von Wasserstoff. Die messtechnische Rückführbarkeit in der Energieinfrastruktur für die Wasserstoffspeicherung ist dann von entscheidender Bedeutung und eine bessere Kenntnis der chemischen und physikalischen Eigenschaften von Wasserstoff sowie rückführbare Messungen und validierte Techniken unverzichtbar.
The aim of this study was to identify specific truffle marker substances within the truffle aroma. The aroma profile of different truffle species was analyzed using static headspace sampling with gas chromatography mass spectrometry analysis (SHS/GC-MS). Possible marker substances were identified, taking the additional literature into account. The selected marker substances were tested in an experiment with 19 truffle dogs. The hypothesis “If trained truffle dogs recognize the substances as supposed truffles in the context of an experiment, they can be regarded as specific” was made. As it would be nearly impossible to investigate every other possible emitter of the same compounds to determine their specificity, this hypothesis was a reasonable approximation. We were interested in the question of what it is the dogs actually search for on a chemical level and whether we can link their ability to find truffles to one or more specific marker substances. The results of the dog experiment are not as unambiguous as could have been expected based on the SHS/GC-MS measurements. Presumably, the truffle aroma is mainly characterized and perceived by dogs by dimethyl sulfide and dimethyl disulfide. However, as dogs are living beings and not analytical instruments, it seems unavoidable that one must live with some degree of uncertainty regarding these results.
Nebivolol (NEB), a β-blocker frequently used to treat cardiovascular diseases, has been widely detected in aquatic environments, and can be degraded under exposure to UV radiation, leading to the formation of certain transformation products (UV-TPs). Thus, the toxic effects of NEB and its UV-TPs on aquatic organisms are of great importance for aquatic ecosystems. In the present study, the degradation pathway of NEB under UV radiation was investigated. Subsequently, zebrafish embryos/larvae were used to assess the median lethal concentration (LC50) of NEB, and to clarify the sub-lethal effects of NEB and its UV-TPs for the first time. It was found that UV radiation could reduce the toxic effects of NEB on the early development of zebrafish. Transcriptomic analysis identified the top 20 enriched Kyoto Encyclopedia of Genes and Genomes (KEGG) pathways in zebrafish larvae exposed to NEB, most of which were associated with the antioxidant, nervous, and immune systems. The number of differentially expressed genes (DEGs) in the pathways were reduced after UV radiation. Furthermore, the analysis of protein biomarkers, including CAT and GST (antioxidant response), AChE and ACh (neurotoxicity), CRP and LYS (immune response), revealed that NEB exposure reduced the activity of these biomarkers, whereas UV radiation could alleviate the effects. The present study provides initial insights into the mechanisms underlying toxic effects of NEB and the detoxification effects of UV radiation on the early development of zebrafish. It highlights the necessity of considering the toxicity of UV-TPs when evaluating the toxicity of emerging pollutants in aquatic systems.
Inflammatory bowel diseases (IBD) comprise mainly ulcerative colitis (UC) and Crohn´s disease (CD). Both forms present with a chronic inflammation of the (gastro) intestinal tract, which induces excessive changes in the composition of the associated extracellular matrix (ECM). In UC, the inflammation is limited to the colon, whereas it can occur throughout the entire gastrointestinal tract in CD. Tools for early diagnosis of IBD are still very limited and highly invasive and measures for standardized evaluation of structural changes are scarce. To investigate an efficient non-invasive way of diagnosing intestinal inflammation and early changes of the ECM, very small superparamagnetic iron oxide nanoparticles (VSOPs) in magnetic resonance imaging (MRI) were applied in two mouse models of experimental colitis: the dextran sulfate sodium (DSS)-induced colitis and the transfer model of colitis. For further validation of ECM changes and inflammation, tissue sections were analyzed by immunohistochemistry. For in depth ex-vivo investigation of VSOPs localization within the tissue, Europium-doped VSOPs served to visualize the contrast agent by imaging mass cytometry (IMC). VSOPs accumulation in the inflamed colon wall of DSS-induced colitis mice was visualized in T2* weighted MRI scans. Components of the ECM, especially the hyaluronic acid content, were found to influence VSOPs binding. Using IMC, colocalization of VSOPs with macrophages and endothelial cells in colon tissue was shown. In contrast to the DSS model, colonic inflammation could not be visualized with VSOP-enhanced MRI in transfer colitis. VSOPs present a potential contrast agent for contrast-enhanced MRI to detect intestinal inflammation in mice at an early stage and in a less invasive manner depending on hyaluronic acid content.
Materials are key for our modern communities; current life seems nearly impossible without concrete, plastic and metal. In particular metals play important roles in all areas of our daily life - from building materials to high tech products.
However, due to the increasing consumption of metals and corresponding waste production, an elevated release of metals from buildings and consumer goods into the environment takes place. Furthermore, metals in direct contact with the environment undergo corrosion processes which leads also to a release of metals into the (aquatic) environment. Besides this immediate metal release, the lifespan of products/buildings are substantially reduced – hence unnecessary economic costs arise. Thus, research in this regard is needed within the force field of metal/material environment.
However, to evaluate the environmental impact of materials as well as developing “safe” materials, new analytical methods are highly needed. One promising powerful tool in this regard is single cell-ICP-ToF-MS for multi-elemental analysis on a single cell/organism level.
Within this presentation the concept, strength as well as challenge of single cell-ICP-MS are briefly introduced. Afterwards, two application examples are presented: (i) assessing the environmental impact of metals and (ii) the impact of the environment on metal-based materials and the derivation of potential environmental-friendly material protection strategies. These applications highlight the strength of new analytical approaches to explore the durability and safety of newly developed materials. Thus, analytical chemistry is one corner stone to transformation of modern society into circular economy (CEco).
(i) Diatoms are located at the bottom of the food chain. Thus, toxicological relevant metals taken up by diatoms can possibly accumulate within the food web and cause harmful effects. Diatoms are a common test system in ecotoxicology. To investigate potential metal uptake and harmful effects on a single cell level, we developed an on-line single cell-ICP-ToF-MS approach for multi-elemental diatom analysis. Our approach is a new potential tool in ecotoxicological testing for metal-based materials.
(ii) Next to classical corrosion processes, microorganisms are responsible for so called microbially influenced corrosion (MIC). MIC is a highly unpredictable process relying on the interaction pathways between cells and the metal surface. To shed light on MIC processes and derivate potential metal protection strategies, we applied single cell-ICP-ToF-MS for MIC research on a single bacteria/archaea level. It turned out that microorganism are taking up particular metals from alloys - thus, single bacteria-ICP-ToF-MS will enable the development of environmental friendly corrosion protection strategies.
Rapid, cost-efficient, and eco-friendly methods are desired today for routine analysis of the Fusarium mycotoxin zearalenone (ZEN) in edible vegetable oils. Liquid chromatography with fluorescence detection (HPLC-FLD) is commonly used to reliably control the specified ZEN maximum levels, which requires efficient sample clean-up to avoid matrix interferences. Therefore, a highly selective extraction and clean-up method based on reversible covalent hydrazine chemistry (RCHC) using hydrazine-functionalized silica was developed. This efficient solid-phase extraction (SPE) involves reversible hydrazone formation of ZEN with the hydrazine moiety covalently bound to a solid phase. Optimal conditions were achieved with 1 mL SPE cartridges filled with 400 mg of hydrazine-functionalized silica. The developed RCHC-SPE method was validated in an interlaboratory comparison study (ILC) with twelve participants analyzing six edible vegetable oils with a focus on maize oils. The derived method parameters (ZEN recovery 83%, repeatability 7.0%, and reproducibility 18%) meet the performance criteria of Commission Regulation (EC) No 401/2006. The developed RCHC-SPE-based HPLC-FLD method allows the reliable quantification of ZEN in the range of 47–494 μg/kg for different types of edible vegetable oils, also for matrix-reach native oils. Due to the high efficiency, the significantly reduced matrix load helps to extend the lifetime of analytical equipment. Furthermore, the re-useability of the RCHC-SPE cartridges contributes to an eco-friendly approach and reduced analysis costs. To our knowledge, this is the first report on ZEN quantification in edible vegetable oils based on manual RCHC-SPE cartridges. Due to its high performance, the developed RCHC-SPE method is a promising alternative to the current European standard method EN 16924:2017 (HPLC-FLD part).
Lithium and boron are trace components of magmas, released during exsolution of a gas phase during volcanic activity. In this study, we determine the difusivity and isotopic fractionation of Li and B in hydrous silicate melts. Two glasses were synthesized with the same rhyolitic composition (4.2 wt% water), having diferent Li and B contents; these were studied in difusion-couple experiments that were performed using an internally heated pressure vessel, operated at 300 MPa in the temperature range 700–1250 °C for durations from 0 s to 24 h. From this we determined activation energies for Li and B difusion of 57±4 kJ/mol and 152±15 kJ/mol with pre-exponential factors of 1.53 × 10–7 m2/s and 3.80× 10–8 m2 /s, respectively. Lithium isotopic fractionation during difusion gave β values between 0.15 and 0.20, whereas B showed no clear isotopic fractionation. Our Li difusivities and isotopic fractionation results difer somewhat from earlier published values, but overall confrm that Li difusivity increases with water content. Our results on B difusion show that similarly to Li, B mobility increases in the presence of water. By applying the Eyring relation, we confrm that B difusivity is limited by viscous fow in silicate melts. Our results on Li and B difusion present a new tool for understanding degassing-related processes, ofering a potential geospeedometer to measure volcanic ascent rates.
Im Rahmen des EU-Projekts „CONSENS – Integrated Control and Sensing“ wurde ein vollautomatisiertes, gemäß Atmosphère-Explosibles(ATEX)-Regeln zertifiziertes Analysatormodul auf Basis eines kommerziellen Benchtop-Kernspinresonanzspektrometers (Engl. nuclear magnetic resonance, NMR) entwickelt und im Umfeld einer modularen containerbasierten Produktionsanlage validiert. Auf Basis der gewonnenen Daten konnten sowohl eine iterative Optimierung der Prozessparameter erfolgen als auch Referenzdaten für die Kalibrierung eines Nahinfrarot-Spektrometers gewonnen werden.