TY - CONF A1 - van de Kreeke, Johannes A1 - Melzer, Michael T1 - The Digital RM Document (DRMD) N2 - The Digital Reference Material Document (DRMD) is a machine-readable replacement of the usual PDF Certificate. We have developed a fully functional beta version that is already in use for selected BAM materials and publicly available from the COMAR database, which showcases its feasibility. T2 - Deutsche Marktüberwachungskonferenz 2025 CY - Berlin, Germany DA - 17.09.2025 KW - Reference materials KW - Certified reference materials KW - Digital zertificates KW - QI-Digital PY - 2025 AN - OPUS4-64148 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sommerfeld, Thomas A1 - Riedel, Juliane A1 - Lisec, Jan A1 - Mauch, Tatjana A1 - Richter, Silke A1 - Koch, Matthias T1 - Development of a certified reference material for per- and polyfluoroalkyl substances (PFAS) in textiles N2 - Per- and polyfluoroalkyl substances (PFASs) are a large group of emerging organic pollutants that contaminate the environment, food, and consumer products. Textiles and other outdoor products are a major source of PFAS exposure due to their water-repellent impregnations. Determination of PFASs in textiles is increasingly important for enhancing their contribution to the circular economy. While maximum levels and restrictions exist for certain key compounds under the Stockholm Convention on Persistent Organic Pollutants and the REACH regulation, certified reference materials (CRMs) are not currently available. To address this issue, the first CRM for determining PFASs in outdoor textiles (BAM-B003) was developed. It fully complies with the requirements of ISO 17034 and ISO 33405. This work presents the entire process of CRM development process, including preparation, a homogeneity study, a stability study, and value assignment. Certification was based on an in-house study at BAM using liquid chromatography tandem mass spectrometry (LC–MS/MS) with stable isotope dilution analysis (SIDA). The certified mass fractions of 18 PFASs range widely from 0.46 to 69 µg/kg, with a prevalence of PFOA (69 µg/kg), PFOS (41 µg/kg) and PFHxA (35 µg/kg) exceeding legal limits. BAM-B003 is intended for analytical quality control and contributes to improving the chemical safety of textiles and strengthening the circular economy. KW - Reference Material KW - PFAS KW - Textiles PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641040 DO - https://doi.org/10.1007/s00216-025-06098-2 SN - 1618-2642 SP - 1 EP - 9 PB - Springer Science and Business Media LLC AN - OPUS4-64104 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Melzer, Michael T1 - The Digital Reference Material Document Derived from the DCC N2 - The DCC enables automatization in the metrological traceability of measurements and the dissemination and processing of data from calibration services. Many calibration and measurement procedures, however, rely on certified reference materials (CRMs) to obtain metrological traceability, especially in the broad field of chemical analysis. The metrological information of those reference materials is also provided in the form of certificates, and hence, their digitization bears the same automatization potential for quality assurance and traceability as the DCC itself. Although fairly similar, a reference material certificate contains some different information, and has a variable structure and proprietary requirements compared to a calibration certificate, as it is based on the dedicated ISO 33401 standard (formally known as ISO Guide 31) rather than the ISO/IEC 17025. Accordingly, the established DCC-schema does not fully fit the purpose of machine-readable reference material certificates. At the German Federal Institute for Materials Research and Testing (BAM), we started to adapt the DCC-schema in order to derive a dedicated schema for CRM certificates. For the seamless digital description of its certified values and their uncertainties, the newly developed schema also utilizes the Digital SI and thus provides a direct link to BIPM’s digital reference point for a global harmonization of metrological quantities. Furthermore, the schema will also be suitable for non-certified reference materials in order to form a common data structure for digital reference material documents (DRMD) in general. As a validated XML report, the DRMD is also compatible with established digital security and verification infrastructure, such as electronic seals and the novel digital accreditation symbol. In this presentation we will highlight some of the essential differences between reference material documents and calibration certificates, but also point out their similarities, which well justify the derivation of the DRMD-Schema from the DCC. In addition to the metrological traceability and quality assurance, further automatization use cases by means of DRMDs are presented, ranging from database maintenance to machine learning for automated analytics. This work was supported in part by national QI-Digital initiative funded by the German Federal Ministry for Economic Affairs and Climate Action. T2 - 5th International DCC Conference CY - Online Meeting DA - 25.02.2025 KW - Reference materials KW - Certified reference materials KW - Digital certificates KW - Digitalization KW - QI-Digital PY - 2025 UR - https://www.youtube.com/watch?v=0Mzu-bNNmbM&t=2446s UR - https://www.dcc-conference-2025.ptb.de/5th-international-dcc-conference AN - OPUS4-64178 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Monavari, Mehran A1 - Prellwitz, Matthias A1 - Koch, Claudia A1 - van de Kreeke, Johannes A1 - Melzer, Michael A1 - Richter, Silke T1 - The Digital Reference Material Document: From Paper Certificates to Interoperable Data Objects in Digital Quality Infrastructure N2 - Reference materials (RMs) are essential for traceable and reliable measurements in science and industry, yet their certificate/document remain largely paper-based. The Digital Reference Material Document (DRMD) project at BAM introduces a transformative approach by converting traditional RM certificates/documents into machine-interpretable, XML-based digital assets. Building on the Digital Calibration Certificate framework, DRMDs encode ISO 33401 requirements and integrate semantic standards like D-SI and material identifiers. These digital documents support automated data exchange, integration into laboratory systems, and interoperability e.g. via asset administration shells and data spaces. The paper presents the DRMD schema concept, and outlines the path toward international harmonization and large-scale deployment, positioning DRMDs as a cornerstone of a digital quality infrastructure. T2 - IMEKO TC-6 International Conference on Metrology and Digital Transformation - M4DConf 2025 DA - 03.09.2025 KW - Digital Reference Material Document KW - Quality Infrastructure KW - Reference Material Certificate KW - DRMD PY - 2025 UR - https://www.m4dconf.org/ UR - https://www.sciencedirect.com/journal/measurement-digitalization SP - 1 EP - 6 AN - OPUS4-64269 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Improvement of manufacturing processes of Li-ion batteries by Glow Discharge Optical Emission Spectroscopy N2 - Manufacturing lithium-ion coin cells (LIBs) for scientific research demands reproducibility, precision, and thorough metrology to ensure consistent quality and performance. Glow-discharge optical emission spectroscopy (GD-OES) emerges as a crucial analytical technique in this context, providing detailed insights into elemental composition and material homogeneity [1,2]. This study focuses on using GD-OES to optimize and standardize the manufacturing processes of LIBs, emphasizing metrology and traceability to develop reproducible and high-quality batteries for research purposes. We refined cell production by adjusting key parameters such as cathode doping, electrolyte concentration, and calendar pressing. GD-OES facilitated depth analysis of elemental composition and distribution, which is essential for identifying and maintaining optimal manufacturing conditions. Validation was achieved through electrochemical impedance spectroscopy (EIS), ensuring the quality and consistency of the manufactured batteries. GD-OES analysis revealed critical insights into elemental uniformity and impurities, guiding adjustments significantly improving cell performance and reproducibility. The method proved fast and effective in detecting and correcting variations in the manufacturing process, leading to enhanced battery quality. To understand the aging mechanisms, GD-OES was employed for fluorine depth profiling, which is crucial for studying polymer and electrolyte degradation. We significantly enhanced fluorine detection sensitivity by substituting the argon plasma with a neon/argon mixture, providing a more accurate aging analysis. By demonstrating the versatility and efficacy of GD-OES in optimizing LIB manufacturing processes and gaining deeper insights into aging mechanisms, this research has significant practical implications. It not only advances lab research but also offers tangible industrial benefits, including improved battery quality, extended lifespan, and enhanced performance. By ensuring metrology and traceability, GD-OES contributes to developing a robust method for the reproducible manufacturing of Li-ion coin cells, boosting innovation and sustainability in battery technology. T2 - SciX 2025 CY - Covington, KY, USA DA - 05.10.2025 KW - GD-OES KW - Battery analysis KW - Depth profile KW - Lithium-ion battery PY - 2025 AN - OPUS4-64878 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Morcillo, Dalia A1 - Winckelmann, Alexander A1 - Oelze, Marcus A1 - Leonhardt, Robert A1 - Schmidt, Anita A1 - Richter, Silke A1 - Recknagel, Sebastian A1 - Vogl, Jochen A1 - Panne, Ulrich A1 - Abad Andrade, Carlos Enrique T1 - Exploring Age-Induced Lithium Isotope Fractionation in Lithium-Ion Batteries using Microwave-Induced Cold Nitrogen Plasma Mass Spectrometry N2 - This study explores Microwave-Inductively Coupled Atmospheric-pressure Plasma Mass Spectrometry (MICAP-MS) as a cost-effective alternative to Multi-Collector Inductively Coupled Plasma Mass Spectrometry (MC-ICP-MS) for analyzing lithium isotopic composition in lithium-ion batteries (LIBs). We investigate the performance of MICAP-MS in measuring Li isotope ratios in new and aged commercial lithium cobalt oxide (LCO) batteries. Our results show that MICAP-MS, operating under cold plasma conditions at 800 W with an 8 mm torch position, achieves results metrologically compatible with MC-ICP-MS, with a precision ranging from 0.6‰ to 3.4‰ for δ7Li values. MICAP-MS benefits from a dielectric resonator for uniform plasma, better ion velocity control, and higher energy efficiency. Optimal settings were identified with dwell times of 10 ms for 6Li and 1 ms for 7Li. The study of LIBs revealed that 6Li migrates towards the anode over multiple charge–discharge cycles, causing 7Li to accumulate in the cathode, a fractionation effect that becomes more pronounced with prolonged cycling. MICAP-MS provides a cost-effective, precise alternative to MC-ICP-MS, with lower operational costs and enhanced portability, advancing the study of isotopic fractionation and aging in lithium-ion batteries. KW - MICAP-MS KW - Lithium KW - Battery aging KW - Lithium isotopes KW - Nitrogen plasma KW - Isotope fractionation KW - lithium cobalt oxide KW - LCO PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643777 DO - https://doi.org/10.1039/d4ja00324a SN - 0267-9477 SP - 1 EP - 11 PB - Royal Society of Chemistry (RSC) AN - OPUS4-64377 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Tracking Lithium-Ion Battery Ageing via Lithium Isotope Fractionation N2 - Lithium-ion batteries power portable devices, electric vehicles, and stationary power grids, yet hidden aging reactions still shorten their service life and raise concerns about cost and safety. An analytical proxy is needed to report these reactions and accelerate product development, quality control, and recycling. Here, we demonstrate that subtle shifts in the natural 7Li/6Li ratio accurately record the two decisive stages of cell aging, solid-electrolyte interphase (SEI) formation and field-driven aging, which can be detected using multi-collector ICP-MS. Because Li is easily stripped from digested electrodes or electrolyte in a one-step cation-exchange column, high-purity solutions reach the spectrometer in minutes. A streamlined MC-ICP-MS run yields a δ7LiLSVEC precision of 0.4 ‰, enabling dozens of battery fractions to be analyzed per day. Applying the workflow to LiCoO2 coin cells as models, sampled from pristine to 700 cycles, reveals a clear isotopic narrative. During the first ≈45 cycles, 7Li leaves the LiCoO2 lattice, dissolves into the electrolyte, and is locked in the SEI on graphite, driving cathode δ7Li from +8 to –10 ‰ and raising the anode to +13 ‰ while capacity drops by 10 %. After the interphase matures, the electric field takes over: the lighter 6Li migrates faster to the anode, 7Li accumulates in the contracting Li1-xCoO2 lattice, and the bulk separation factor rises to α≈1.045 by 700 cycles. The δ7Li curve flattens roughly 70 cycles before capacity falls to 80%, providing an early warning of end-of-life. Isotopic gradients scale linearly with impedance growth, SEI thickness, and crack density confirmed by LA-ICP-MS mapping, FIB-SEM, XANES, and EXAFS. Although each data point requires one cell, lithium-isotope fractionation provides direct, element-specific, and structural fatigue insight unavailable from non-destructive tests. The straightforward chemistry and fast MC-ICP-MS routine make the approach practical for targeted aging studies, additive screening, and forensic autopsies, complementing high-throughput electrochemical methods and supporting the design of longer-lived batteries. T2 - SciX 2025 CY - Covington, KY, USA DA - 05.10.2025 KW - Isotope KW - Lithium KW - MC-ICP-MS KW - MICAP-MS KW - Isotope fractionation KW - Battery PY - 2025 AN - OPUS4-64879 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -