1.7 Organische Spuren- und Lebensmittelanalytik
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A sustainable mechanochemical process for the generation of sodium aluminium fluorides by conversion of polyvinylidene fluoride (PVDF) waste on using ball milling in the presence of a Lewis acid was developed. The generated fluorides can be key materials for the aluminium production process. The Lewis acid AlCl3 initiates dehydrofluorination steps at PVDF, releasing HF for further fluorination of both NaCl and AlCl3 to yield chiolite under ball milling conditions. Further calcination of chiolite generates cryolite with an overall yield of 62% with respect to AlCl3. The procedure avoids the use of solvents and minimises energy consumption. The identity and phase purity of the products was confirmed by XRD, NMR, IR, and Raman analyses. It was also demonstrated that powdered PVDF, real-life PVDF membrane waste orPVDFextracted from Li-ion batteries can be upcycled into industrially relevant fluoride materials. The presented method offers a sustainable approach for resource recovery and environmental remediation.
Ergot alkaloids (EAs) are toxic secondary metabolites formed by various fungi, most notably Claviceps purpurea, which infects cereal crops such as rye, wheat, and barley. Due to their toxicity, the European Commission established maximum levels for 12 priority EAs in cereals and related products in 2022. Routine monitoring, typically employing high-performance liquid chromatography coupled to tandem mass spectrometry, is challenged by the unavailability of isotope-labeled internal standards. To address this, we previously synthesized internal standards (ISTDs) for 12 priority EAs and herein we evaluate their performance through an interlaboratory comparison against the standard addition approach prescribed in EN 17425. The ISTDs significantly improved method precision and trueness, with results in good agreement across both laboratories. Furthermore, we developed a reference material for EAs in rye flour, in accordance with ISO 33405 guidelines, using stable isotope dilution mass spectrometry as primary method. This internal RM contributes to safer foodstuffs by supporting reliable method development and validation for EAs.
This talk is for validation of the ISO standard on mass-based microplasic detection methods. Results of an VAMAS ILC on microplastics from BAM (2023/2024) are presented and evaluated after ISO 5725-2. The criteria are also presented, which must be fullfilled that the results can fit for the ISO standard validation. Finally, the summary gives all evaluation data, which are mandatory and relevant. Polymer types were PE and PET.
Ergotalkaloide (EA) sind toxische sekundäre Stoffwechselprodukte, welche von unterschiedlichen Pilzarten gebildet werden. Aufgrund ihrer toxikologischen Relevanz hat die EU 2022 erstmals Grenzwerte für EA in verschiedenen Lebensmitteln festgelegt. Um diese Grenzwerte zuverlässig zu kontrollieren, sind valide Analyseverfahren erforderlich. In diesem Projekt wurden jetzt erstmals EA-Isotopenstandards hergestellt und erfolgreich in die LC-MS/MS Analytik implementiert.
Analysis of nanomaterial (NM) surface chemistry is essential for understanding and controlling NM properties relevant for NM functionality, stability, and safety. In this work, we present a multimethod study of the quantification of the frequently used, biocompatible surface ligand citrate for lanthanide-based upconversion nanoparticles (UCNPs) and iron oxide nanoparticles (IONPs). Methods applied that address different yet correlated measurands with varying chemo-selectivity and rely on different sample preparation workflows include chemo-selective reversed-phase high-performance liquid chromatography (RP-HPLC) with photometric detection measuring liquid samples and dissolved NMs as well as non-selective thermogravimetric analysis (TGA) and chemo-selective pyrolysis-gas chromatography-mass spectrometry (PyGC-MS) analyzing dried NMs. Thereby, we demonstrate the applicability of the RP-HPLC method, recently developed for citrate quantification on IONPs, for UCNPs as another application-relevant NM class. In addition, the feasibility of PyGC-MS, emerging for material characterization at the trace level due to the consumption of very small sample amounts and minimum sample preparation, for NM ligand quantification is assessed. This method, which has not been applied before for NM surface analysis, indirectly quantifies citrate via the amount of acetone formed during citrate decomposition. For UCNPs, PyGC-MS measurements led to a good agreement with the TGA and RP-HPLC results within the respective measurement uncertainties. However, quantifying citrate on IONPs with PyGC-MS resulted in an overestimation of citrate, which is tentatively ascribed to IONP catalytic activity. Overall, our method cross-comparison underlines the importance of multimethod characterization schemes to assure a reliable and precise ligand quantification and to identify method- and NM-specific effects.
Offshore wind structures (OWS) must remain reliable for decades to ensure stable renewable energy production. However, microbiologically influenced corrosion (MIC) poses a significant threat to the long-term integrity of monopiles, particularly at the sediment–water interface. This study investigates how naturally occurring microbial communities contribute to carbon steel corrosion under conditions representative of monopile environments.
An in-house column system was established and inoculated with sediment and seawater from the North Sea. Controlled flow regimes were applied to mimic seabed hydrodynamics. Corrosion progression and biofilm development were characterized using molecular microbiological analyses, metabolomics, and 3D surface profilometry.
Distinct microbial and corrosion responses emerged under different hydrodynamic conditions. High-flow treatments were dominated by sulfur-oxidizing bacteria (SOB), which oxidize hydrogen sulfide to sulfate, reducing the persistence of corrosive sulfur intermediates near the steel surface. In contrast, low-flow conditions favored sulfate-reducing bacteria (Desulfocapsaceae, Desulfolunaceae), associated with localized anoxia and moderate sulfide accumulation. Under static conditions, Desulfovibrionaceae prevailed, reflecting strict anoxia and high H₂S concentrations that promote aggressive corrosion.
Surface analyses revealed treatment-dependent corrosion patterns. High-flow conditions produced the greatest variability and deepest pits, suggesting enhanced localized corrosion driven by turbulence and nutrient exchange. All microorganism-treated samples exhibited higher pitting depths compared to sterile controls, confirming the strong influence of microbial processes on corrosion intensity.
Our findings demonstrate that hydrodynamic conditions shape microbial community structure and biofilm-associated corrosion patterns, providing mechanistic insights into MIC in offshore settings. These results contribute to improving monitoring strategies and informing mitigation approaches for protecting OWS infrastructure.
Microbiologically influenced corrosion (MIC) represents a significant threat to offshore infrastructure (such as monopile) operating in the mud zone. The sediment–water interface creates an aggressive environment, where steel structures are in direct contact with sediment, and oxygen availability is limited, creating conditions favorable for anaerobic microbial activity and MIC. At the same time, near-bed hydrodynamic conditions in offshore environments are inherently heterogeneous, even within nominally laminar regimes. However, despite this variability, a mechanistic understanding of how small changes in near-bed flow modulate biofilm development, mass transport, and dominant MIC mechanisms remain limited. Here, we investigated the role of controlled laminar hydrodynamics under anoxic sediment–water interface conditions relevant to offshore wind monopiles. Carbon steel coupons were exposed in a column system inoculated with the North Sea sediment communities. Corrosion rates and pit morphology were quantified by gravimetry and three-dimensional surface profilometry, while microbial community composition (16S rRNA gene sequencing), dissolved sulfide, and untargeted metabolomics resolved the governing biogeochemical processes. The result indicated that static (no flow) conditions promoted diffusion-limited biofilms dominated by sulfate-reducing bacteria (SRB) and acetogens, resulting in low and relatively uniform corrosion. Low laminar flow conditions enhanced syntrophic interactions and sulfide accumulation, producing moderate corrosion severity. In contrast, higher laminar flow reduced bulk sulfide accumulation and biofilm thickness yet generated the most pronounced pitting rate. These findings demonstrate that MIC cannot be confirmed or excluded based solely on sulfide concentration, microbial presence, etc. Rather, corrosion emerges from the coupled interplay between hydrodynamics, biofilm architecture, mass transport, and electrochemical surface processes.
Oleic acid (OA) is used in the synthesis of upconversion nanoparticles (UCNPs) to control UCNP size and morphology as well as a non-polar surfactant allowing dispersion in apolar media. Widely employed technical grade OA is industrially synthesized from natural fat sources, yielding a complex mixture of various fatty acids. To gain insight into the influence of fatty acid ligands on UCNP size, morphology, and optical properties, we employed OA precursors during the high temperature synthesis of NaYF4 (Yb,Er) UCNPs and tuned the surface ligand concentration with a partial ligand removal approach, using NOBF4. The ligand shell was then analyzed by HPLC-MS/MS.
Per- and polyfluoroalkyl substances (PFAS) are a large group of emerging organic pollutants that contaminate the environment, food, and consumer products. They have a wide range of applications due to their water- and oil-repellent properties, as well as their chemical and thermal stability. However, the use of PFAS has raised concerns due to their persistence in the environment and their adverse health effects, leading to regulations aimed at controlling their use and minimizing exposure. Substances such as PFOS, PFHxS, and PFOA are listed in the Stockholm Convention on Persistent Organic Pollutants (POP Regulation, EU 2019/1021). Maximum levels have been set for PFAS in environmental matrices such as water and soil.
Reliable PFAS analysis leads to an increasing global demand for certified reference materials (CRM). However, CRMs for PFAS in soils are rare or currently not available. To improve the metrological infrastructure and support environmental PFAS measurements, a CRM for PFAS in soil (BAM-U027) based on ISO 17034 and ISO 33405 was developed. This poster provides an overview of the different steps for the preparation and characterization of BAM-U027. The assignment of the certified mass fractions for 13 relevant PFAS targets compounds is based on isotope dilution HPLC-MS/MS at three independent workplaces. The results of the BAM in-house certification study on BAM-U027 were supported by an interlaboratory comparison study (ILC) involving 17 participating laboratories in Germany.
BAM-U027 is intended for analytical quality control and contributes to improving environmental protection.
The increasing demand for alkali-metal batteries, lithium and sodium, highlights the importance of recycling approaches. For batteries which encompass low-value components such as cobalt-free and sodium-ion, a requirement for low-cost and low-energy processes for recovery and reuse. In this respect, direct recycling, is preferred where the functional structure of active materials is preserved. In this study, a direct recycling route for sodium nickel-iron-manganese-copper oxide cathode material for sodium-ion batteries was investigated and preliminary results reveal the challenges in this direct recycling approach. Commercial sodium-ion battery cells were safely disassembled in a Glovebox and the positive electrode material was extracted via ice stripping. The recovered electrode material was structurally and compositionally characterised using scanning electron microscopy (SEM), X-ray diffraction (XRD), and inductive coupled plasma optical emission spectroscopy (ICP-OES) to assess morphology, crystallinity, and elemental stoichiometry.
