TY - CONF A1 - Battistella, Beatrice T1 - Uncovering Li-ion Battery Degradation: Possibilities Offered by GD-MS Analysis N2 - Uncovering Li-ion Battery Degradation: Possibilities Offered by GD-MS Analysis Since their introduction, lithium-ion batteries (LIBs) have revolutionized the energy storage market, which they now dominate thanks to their high energy density, power capability, and efficiency.1, 2 Despite widespread adoption, global demand for LIBs is projected to grow by around 27% per year.3 This raises concerns about the availability of critical minerals essential to LIB production. Meeting future demand will therefore require next-generation LIBs—an ambition that hinges on a deeper understanding of the degradation processes that limit performance and lifetime. Because LIBs are chemically and physically complex systems, capacity fade stems from multiple degradation phenomena that act concurrently as cells age.4 In particular, the formation and growth of interfacial layers at the electrodes during repeated charge–discharge cycling make a substantial contribution to component degradation.5 Glow Discharge Mass Spectrometry (GD-MS) offers depth-resolved elemental and isotopic analysis of battery electrodes and has proven to be a powerful tool for tracking degradation in LIBs. Using a ASTRUM Swift GD-MS spectrometer, we identified degradation pathways in both cathodes and anodes across various cell chemistries, linking electrochemical behavior with changes in structure and elemental distributions. These insights help clarify the mechanisms that accelerate aging and capacity loss. T2 - Nu Instruments Webinar CY - Online meeting DA - 15.10.2025 KW - Li-ion Batteries KW - Isotope KW - LA-ICP-MS KW - GD-MS PY - 2025 AN - OPUS4-64396 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Battistella, Beatrice T1 - Glow discharge techniques applied to lithium ion battery analysis N2 - Glow Discharge Techniques Applied to Lithium-Ion Battery Analysis Beatrice Battistella, V. Hoffmann, A. Revill, S. Richter, S. Recknagel, C. Abad Seit ihrer Einführung haben Lithium-Ionen-Batterie (LIB) Technologien die Welt der tragbaren Elektronik und der nachhaltigen Mobilität revolutioniert [1] und sind dank ihrer langen Lebensdauer und ihrer unübertroffenen Energiedichte in vielen Bereichen nach wie vor unersetzlich. Angesichts des kontinuierlich wachsenden Marktvolumens der LIBs [2,3] und der begrenzten Verfügbarkeit der für ihre Herstellung benötigten Ressourcen ist die Entwicklung verbesserter Batterien der nächsten Generation erforderlich. Eine wesentliche Voraussetzung für diese Entwicklung ist ein tieferes Verständnis der Degradationsmechanismen in LIB-Zellen, das jedoch häufig durch die Komplexität der Systeme und die gleichzeitig ablaufenden Prozesse, die zum Versagen beitragen, erschwert wird. In diesem Zusammenhang zeigt unsere Arbeit, wie Glimmentladungstechniken dazu beitragen können, grundlegende Fragestellungen in der LIB-Analyse zu beantworten. Einerseits hat sich die GD OES als wertvolles Werkzeug zur Qualitätskontrolle bei der Elektrodenherstellung erwiesen und zeigt Potential bei der Analyse von Fluor für diagnostische Zwecke an Zellen. Andererseits wurde die GD MS in Post-Mortem-Analysen eingesetzt, um die Korrelation zwischen Veränderungen in der elementaren und isotopischen Verteilung an den Elektroden und der elektrochemischen Leistung der Zellen zu untersuchen. Insbesondere ermöglichte der Einsatz von GD-MS bei LIBs die Detektion und Lokalisierung einer Lithium-Isotopenfraktionierung innerhalb der Elektroden und setzte damit einen neuen Maßstab für die Untersuchung der Grenzflächen zwischen Elektrode und Elektrolyt. _____________________________ Since their introduction, lithium-ion battery (LIB) technologies have revolutionized the world of portable electronics and sustainable mobility [1], and they remain irreplaceable in several sectors thanks to their long cycle life and unmatched energy density. In view of the continuously growing LIB market [2,3] and the limited availability of the resources required for their manufacture, the development of improved next-generation batteries is needed. This requires a deeper understanding of degradation pathways in LIB cells, which is often hindered by the complexity of these systems and the concurrent processes that contribute to failure. In this context, our work demonstrates how glow discharge techniques can help address fundamental questions in LIB analysis. On one hand, GD-OES has proven to be a valuable tool for quality control in electrode manufacturing, showing potential in the analysis of fluorine for cell diagnostics. On the other hand, GD-MS applied in post-mortem analysis enabled correlation of changes in elemental and isotopic distributions within electrodes and the electrochemical performance of the cells. In particular, GD-MS analysis on LIBs allowed detection and depth localization of lithium isotope fractionation in the electrodes, establishing a new benchmark for the study of electrode-electrolyte interfaces. T2 - 20th GD-Users Meeting, TAZ GmbH CY - Aichach, Germany DA - 01.10.2025 KW - GD-MS KW - GD-OES KW - Lithium-Ion Battery PY - 2025 AN - OPUS4-64392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Juliane T1 - PFAS determination in wastewater – monitoring and quality assurance N2 - Per- and polyfluoroalkyl substances (PFAS) are well-known as “forever chemicals” and persistent pollutants. The potential release of PFAS from different anthropogenic sources has gained increasing attention in the past years. This creates a need for the monitoring of PFAS in environmental matrices. Due to their high polarity and mobility, PFAS determination in surface-, ground- and wastewater is of particular interest for monitoring purposes. The investigation of PFAS contaminations in real wastewater samples is extremely challenging because of their high and varying matrix loads, and the high requirements for PFAS target-analysis regarding sensitivity according to current regulations (e.g., Drinking Water Ordinance, TrinkwV). Since there is hardly any quality-assured measurement data available for PFAS quantified in wastewater, a monitoring project was conducted in 2024/2025 to determine PFAS levels from various wastewater sources in the state of Brandenburg (Germany). The main results will be presented and discussed with emphasis on analytical issues related to the HPLC-MS/MS determination. While investigations were focused on the 20 PFAS targets based on TrinkwV, also several other relevant PFAS compounds, e.g., trifluoroacetic acid (TFA) and HFPO-DA (GenX), were included into the monitoring. T2 - PFAS – Challenges and Scientific Perspectives in Human Health Risk Assessment CY - Berlin, Germany DA - 08.10.2025 KW - Quality assurance KW - PFAS in wastewater KW - Monitoring of PFAS in wastewater KW - GenX in wastewater KW - TFA in wastewater PY - 2025 AN - OPUS4-64389 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Juliane T1 - Interlaboratory comparison study for PFAS analysis in soils and eluates N2 - PFAS (per- and polyfluoroalkyl substances) comprise more than 10,000 compounds that have been used in various industrial and consumer products for decades. However, PFAS represent a growing problem because of their persistence in the environment and their adverse health effects. Therefore, reliable PFAS analysis of environmental compartments is indispensable but poses a complex challenge due to the large number of individual compounds in widely varying concentrations. The investigation and assessment of PFAS contamination in soil, as well as the determination and monitoring of necessary remediation measures, require comparable and high-quality standards in chemical analysis. Interlaboratory comparison studies (ILCs) are suitable tools to ensure these quality standards. Thus, an ILC involving 17 participating laboratories in Germany was organized and conducted by BAM, SenMVKU, and BImA in 2024 to determine PFAS in real soil samples (solid matter and eluates). Essential results of the ILC will be presented focusing on analytical issues related to the HPLC-MS/MS determination of the PFAS target compounds based on current regulations but also alternatives such as GenX and Capstone A/B. Furthermore, unexpectedly observed effects interfering with the quantification of specific PFAS will be discussed. T2 - PFAS – Challenges and Scientific Perspectives in Human Health Risk Assessment CY - Berlin, Germany DA - 08.10.2025 KW - Quality assurance KW - PFAS in soil KW - PFAS in eluate KW - Interlaboratory comparison study PY - 2025 AN - OPUS4-64388 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Obenlüneschloß, Jorit A1 - Boysen, Nils A1 - Rönnby, Karl A1 - Muriqi, Arbresha A1 - Hoffmann, Volker A1 - Abad Andrade, Carlos Enrique A1 - Rogalla, Detlef A1 - Brokmann, Ulrike A1 - Rädlein, Edda A1 - Nolan, Michael A1 - Devi, Anjana T1 - Ein seltener mononuklearer Lithium‐Carben‐Komplex für die Atomlagenabscheidung von lithiumhaltigen Dünnschichten N2 - KurzfassungLithium ist das zentrale Element moderner Batterietechnologien, und die Herstellung von lithiumhaltigen Materialien mittels Atomlagenabscheidung (engl. Atomic Layer Deposition, ALD) bietet erhebliche Vorteile bei der Kontrolle der Schichtdicke und ‐zusammensetzung. In dieser Studie wird ein neuer mononuklearer, durch ein N‐heterocyclisches Carben (NHC) stabilisierter Lithiumkomplex, [Li(tBuNHC)(hmds)], als vielversprechender Präkursor für die ALD von lithiumhaltigen Dünnschichten vorgestellt. Die strukturelle Charakterisierung erfolgt durch den Vergleich von Dichtefunktionaltheorie (DFT) und Einkristall‐Röntgenbeugung (engl. Single‐Crystal X‐ray Diffraction, SC‐XRD), wobei die seltene mononukleare Struktur bestätigt wird. Thermogravimetrische Analysen (TGA) zeigen vorteilhafte thermische Eigenschaften für ALD‐Anwendungen. Die Verbindung weist einen niedrigen Schmelzpunkt, saubere Verdampfung und ermutigende Volatilitätsparameter im Vergleich zu anderen Lithium‐Präkursoren auf. ALD‐Experimente mit [Li(tBuNHC)(hmds)] und Ozon zeigen dessen Effektivität bei der Abscheidung von LiSixOy‐Filmen. Der ALD‐Prozess zeigt ein gesättigtes Wachstum pro Zyklus (engl. Growth per Cycle, GPC) von 0,95 Å. Die Zusammensetzung, analysiert mittels Rutherford‐Rückstreu‐Spektrometrie/Kernreaktionsanalyse (engl. Rutherford Backscattering Spectrometry/Nuclear Reaction Analysis, RBS/NRA), Röntgenphotoelektronenspektroskopie (engl. X‐ray Photoelectron Spectroscopy, XPS) und Glimmentladungsspektroskopie (engl. Glow Discharge Optical Emission Spectrometry, GD‐OES), bestätigt das Vorhandensein von Lithium und Silizium in den erwarteten Verhältnissen. Diese Arbeit stellt nicht nur einen neuen ALD‐Präkursor vor, sondern trägt auch zum Verständnis der Lithiumchemie bei und bietet Einblicke in die faszinierende Koordinationschemie und das thermische Verhalten von durch NHC‐Liganden stabilisierten Lithiumkomplexen. KW - Atomlagenabscheidung KW - N-heterozyklischer-Carben-(NHC)-stabilisierter Lithium-Präkursor KW - Mononuklearer Li–Carben-Komplex KW - Lithiumsilicat-Dünnfilme KW - Filmanalytik/-Charakterisierung PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-644045 DO - https://doi.org/10.1002/ange.202513066 SN - 0044-8249 N1 - Es gibt eine parallele Sprachausgabe (englisch), ein Link befindet sich im Feld zugehöriger Identifikator - There is a parallel language edition (English), a link is in the field related identifier SP - 1 EP - 12 PB - Wiley-VCH CY - Weinheim AN - OPUS4-64404 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - Production of reference materials - not only for batteries N2 - The presentation describes the basic procedure used by BAM to produce certified reference materials. In particular, BAM's reference material activities in the field of lithium batteries are discussed. Following the first NMC 111 reference material, which is already commercially available, further materials are in production, including black masses and lithium carbonate. T2 - Rigaku Battery Forum 2025 CY - Neu-Isenburg, Germany DA - 24.06.2025 KW - Reference material KW - Li-battery KW - Cathode material PY - 2025 AN - OPUS4-64374 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rua-Ibarz, Ana A1 - Nakadi, Flávio V. A1 - Bolea-Fernandez, Eduardo A1 - Bazo, Antonio A1 - Battistella, Beatrice A1 - Matiushkina, Anna A1 - Resch-Genger, Ute A1 - Abad Andrade, Carlos Enrique A1 - Resano, Martín T1 - Discrete entity analysis via microwave-induced nitrogen plasma–mass spectrometry in single-event mode N2 - In this work, single-event microwave-induced nitrogen plasma–mass spectrometry (single-event MINP-MS) was evaluated for the first time for the analysis of discrete entities such as nanoparticles, biological cells, and microplastics. Nitrogen (N2) effectively overcomes Ar-based polyatomic interferences, enabling (ultra)trace element determination of Fe and Se using their most abundant isotopes, 56Fe (91.66%) and 80Se (49.82%). Iron oxide nanoparticles (Fe2O3 NPs) ranging from 20 to 70 nm were accurately characterized, with excellent agreement with established sizing techniques, such as transmission electron microscopy (TEM) and dynamic light scattering (DLS). A limit of detection (LoD) of 8.6 ag for Fe─equivalent to an LoDsize of 19 nm for Fe2O3─was achieved, which is significantly lower than recent values reported for high-end quadrupole-based ICP-MS. Selenium nanoparticles (SeNPs) of 150 and 250 nm were also accurately characterized, without the N2-based plasma experiencing issues handling relatively large metallic NPs (linearity, R2 = 0.9994). Se-enriched yeast cells (SELM-1 certified reference material) were successfully analyzed via single-cell MINP-MS using external calibration based on SeNPs and a transport efficiency-independent approach. In addition, 2–3 μm polystyrene (PS) and polytetrafluoroethylene (PTFE) were accurately sized by monitoring 12C+, confirming the method’s suitability for handling micrometer-sized polymeric materials (microplastics). The average duration of individual events (680 ± 160 μs) suggests that the digestion of individual entities in N2-based plasmas is comparable to that in Ar-based plasmas. These results open new avenues for this instrumentation as an alternative to ICP ionization sources, also in the context of discrete entity analysis. KW - Microwave-Induced Nitrogen Plasma KW - Discrete entity analysis KW - Particle/droplet event counting KW - Comparison to SP-ICP-MS methodologies KW - Nitrogen plasma vs. argon ICP trade-offs KW - Trace elemental quantification at the single-entity level KW - Time-resolved mass spectrometry for discrete entities PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643825 DO - https://doi.org/10.1021/acs.analchem.5c04341 SN - 0003-2700 SP - 1 EP - 8 PB - American Chemical Society (ACS) AN - OPUS4-64382 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Obenlüneschloß, Jorit A1 - Boysen, Nils A1 - Rönnby, Karl A1 - Muriqi, Arbresha A1 - Hoffmann, Volker A1 - Abad Andrade, Carlos Enrique A1 - Rogalla, Detlef A1 - Brokmann, Ulrike A1 - Rädlein, Edda A1 - Nolan, Michael A1 - Devi, Anjana T1 - Rare Mononuclear Lithium-Carbene Complex for Atomic Layer Deposition of Lithium Containing Thin Films N2 - Lithium is the core material of modern battery technologies and fabricating the lithium‐containing materials with atomic layer deposition (ALD) confers significant benefits in control of film composition and thickness. In this work, a new mononuclear N‐heterocyclic carbene (NHC) stabilized lithium complex, [Li(tBuNHC)(hmds)], is introduced as a promising precursor for ALD of lithium‐containing thin films. Structural characterization is performed, comparing density functional theory (DFT) and single‐crystal X‐ray diffraction (SC‐XRD), confirming a rare mononuclear structure. Favorable thermal properties for ALD applications are evidenced by thermogravimetric analysis (TGA). The compound exhibits a low melting point, clean evaporation, and its volatility parameters are encouraging compared to other lithium precursors. ALD trials using [Li(tBuNHC)(hmds)] with ozone demonstrate its effectiveness in depositing LiSixOy films. The ALD process exhibits a saturated growth per cycle (GPC) of 0.95 Å. Compositional analysis using Rutherford backscattering spectrometry/nuclear reaction analysis (RBS/NRA), X‐ray photoelectron spectrometry (XPS), and glow discharge optical emission spectrometry (GD‐OES), confirms the presence of lithium and silicon in the expected ratios. This work not only presents a new ALD precursor but also contributes to the understanding of lithium chemistry, offering insights into the intriguing coordination chemistry and thermal behavior of lithium complexes stabilized by NHC ligands. KW - Atomic layer deposition (ALD) KW - N-heterocyclic carbene (NHC) ligands KW - Lithium ALD precursor chemistry KW - Mononuclear Li–carbene complex [Li(tBuNHC)(hmds)] KW - Li-silicate thin films (LiSixOy) KW - Thermal properties & TGA/volatility KW - Compositional analysis (RBS/NRA, XPS, GD-OES) PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643790 DO - https://doi.org/10.1002/anie.202513066 SN - 1433-7851 N1 - Es gibt eine parallele Sprachausgabe (deutsch), ein Link befindet sich im Feld zugehöriger Identifikator - There is a parallel language edition (German), a link is in the field related identifier SP - 1 EP - 11 PB - Wiley-VCH CY - Weinheim AN - OPUS4-64379 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abad Andrade, Carlos Enrique A1 - Jegielka, Dennis A1 - Aloysius, Allen A1 - Recknagel, Sebastian T1 - SI-traceable total analysis of nitrate and nitrite by isotope dilution optical spectroscopy and its application to Berlin surface waters N2 - Accurate nitrate and nitrite data support water-quality regulation, yet routine methods rely on external calibration and rarely achieve SI traceability. We report a calibration-free determination of nitrate and nitrite by combining isotope dilution with high-resolution continuum-source graphite furnace molecular absorption spectrometry (ID-HR-CS-GF-MAS). A 15N-enriched nitrate spike (its concentration verified by reverse isotope dilution against the standard reference material NIST 3185) provides the SI link, and it is gravimetrically added to samples; nitrate and residual nitrite are converted in situ to nitric oxide (NO), whose 215 nm band is recorded at a pixel resolution of λ/Δλ ≈ 140 000. The 0.2127 nm shift between 14NO and 15NO electronic spectra is resolved, and a three-latent-variable partial least squares regression model yields the 15N/14N ratio with 0.3% precision. Instrumental LoD values of 4.8 ng (14N) and 3.2 ng (15N) translate to a method LoD of 4.8 ng of nitrogen (equivalent to 1.05 mg L−1 NO3− for a 20 μL aliquot). The furnace program allows for successive drying/pyrolysis loops, so additional 20 μL aliquots can be layered onto the graphite platform. Alternatively, a 10 mL anion-exchange solid-phase extraction step concentrates nitrate and nitrite fivefold, allowing for the analysis of even lower sample concentrations. Results for four certified reference materials (2.9 to 1000 mg L−1 NO3−) agreed with certified values, giving relative expanded uncertainties of 2 to 4%. Analysis of twenty Berlin surface-water samples revealed concentrations ranging from 0.10 to 7.3 mg L−1 NO3−, indicating that the Panke River and Teltow Canal are the primary sources of nitrogen. ID-HR-CS-GF-MAS thus delivers ID-MS-level accuracy in a few minutes per run with bench-top optics, and, with optional on-platform or SPE pre-concentration, extends SI-traceable nitrate/nitrite monitoring into the low-ng regime. KW - Isotope dilution KW - Nitrate and nitrite determination KW - SI-traceable quantification KW - Calibration-free analysis KW - Water quality KW - Berlin surface waters KW - NO molecular absorption bands PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643785 DO - https://doi.org/10.1039/D5JA00252D SN - 0267-9477 VL - 40 IS - 10 SP - 2692 EP - 2701 PB - Royal Society of Chemistry (RSC) AN - OPUS4-64378 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 -