Open Access

Like all edible vegetable oils, olive oils can be contaminated with lipophilic organic pollutants such as polycyclic aromatic hydrocarbons (PAH). Olive oils are susceptible to PAH contamination, typically due to combined effects including environmental pollution, oil processing, and migration from food contact materials. Monitoring PAH levels in olive oil is therefore essential to ensure food safety and consumer protection. According to Commission Regulation 2023/915, maximum Levels have been set for certain PAH: 2 µg kg−1 for benzo[a]pyrene (BaP) and 10 µg kg−1 for PAH-4, representing the sum of BaP, benz[a]anthracene (BaA), benzo[b]fluoranthene (BbF), and chrysene (Chr). However, no certified reference material (CRM) is currently available containing PAH-4 at the regulated maximum levels. To address this deficiency, the first CRM for PAH-4 in extra virgin olive oil (BAM-A001) was developed based on the requirements of ISO 33405. BAM-A001 is intended to be used for performance evaluation and validation of analytical methods for the determination of PAH in olive oil and similar vegetable oils. The entire CRM development process including preparation, homogeneity and stability studies, and value assignment is presented. The certified mass fractions of BaP (1.44 µg kg−1 ) and PAH-4 (7.33 µg kg−1 ) were determined upon in-house study at BAM using stable isotope dilution analysis gas chromatography mass spectrometry (SIDA-GC-MS). In addition, BAM-A001 underwent secondary characterization for lead (Pb) and cadmium (Cd) levels, acknowledging an EU regulation allowing a maximum of 0.1 mg kg−1 Pb in oils and fats.

Fluorine-containing phases are closely linked to electrolyte decomposition, interphase formation, and failure processes in Li-ion batteries, yet their spatially resolved analysis in composite cathodes remains difficult. Here, laser-induced XUV spectroscopy (LIXS) was used to map fluorine- and lithium-related emission lines in composite lithium cobalt oxide cathodes (LCO). The study used the fluorine emission line at λ = 12.72 nm and the lithium emission line at λ = 13.42 nm and applied them to pristine, formed, aged, and failed LCO cathodes. A matrix-matched calibration using seven Li metal oxide cathode materials at three fluorine levels showed increasing fluorine-related intensity within each matrix, along with pronounced matrix specificity and dispersion. This indicated that fluorine quantification in composite cathodes is influenced by matrix effects, non-thermal equilibrium plasma behavior, and heterogeneity of polyvinylidene fluoride (PVDF) containing fluorine-bearing phases. In the mapped cathodes, the F/Li intensity ratio provided the most sensitive descriptor of degradation, showing increasing imbalance and greater spatial heterogeneity from pristine to failed electrodes. LIXS is therefore advantageous for comparative mapping of light-element/halogen heterogeneity in battery cathodes, where reliable fluorine quantification across chemically distinct composite materials remains intrinsically difficult.

This repository contains the experimental data underlying the research work “Spatial Heterogeneity of the Fluorine-to-Lithium Intensity Ratio as a Descriptor of Battery Degradation and Failure by Laser-Induced XUV Spectroscopy” and it can be found on Zenodo at https://doi.org/10.5281/zenodo.20929465. Laser-induced XUV spectroscopy (LIXS) was used to investigate fluorine, lithium, and cobalt in composite Li-ion battery cathodes. The dataset supports the matrix-matched calibration of fluorine in different lithium metal oxide materials and the spatially resolved comparison of pristine, formed, aged, and failed lithium cobalt oxide (LCO) cathodes. The archive is organized into two groups: · Calibration This group contains 21 CSV files corresponding to seven cathode chemistries (NMC111, NMC442, NMC532, NMC622, NMC811, LCO, and LMO) prepared at three fluorine levels. Each file contains a wavelength axis and 49 individual LIXS spectra acquired on a 7 × 7 measurement grid. A PDF file with the elemental mass composition of the cathodes is provided. · Cells (maps) This group contains spatially resolved LIXS data (maps) for four LCO cathode states: o pristine: as-prepared cathode not assembled into a cell; o formed: cathode recovered after the initial formation procedure without subsequent cycling; o aged: cathode recovered after 100 cycles at 1C; o failed: cathode recovered after rapid performance loss over 30 cycles. Each CSV file contains the wavelength axis and 289 spectra acquired on a 17 × 17 raster. All spectral files contain 2048 wavelength points covering approximately 3.48-20.67 nm. The intensity columns correspond to individual laser-ablation positions and retain the spatial coordinates in their file headers. The spectra were exported to CSV after averaging the detector image across its non-dispersive dimension. The dataset can be used to reproduce the calibration plots, spatial intensity maps, radial profiles, boxplots, kernel density estimates, and F/Li ratio analysis reported in the associated manuscript. It may also support alternative spectral processing, calibration, chemometric, or multivariate approaches for LIXS data from battery materials.

Zertifizierte Referenzmaterialien (ZRM) sind ein unverzichtbares Werkzeug zur Sicherung der Qualität und Vergleichbarkeit chemischer Analysen in der Eisen- und Stahlindustrie. Der vorliegende Beitrag beleuchtet die historische Entwicklung der europäischen EURONORM-ZRM-Herstellergruppe und die zentrale Rolle von Ringversuchen bei der Herstellung und Zertifizierung von Referenzmaterialien.

The report describes preparation, analysis and certification of the nickel silver reference material BAM-M398, which is available in the form of discs (38 mm diameter and 25 mm height).