TY - JOUR A1 - Kowalewska, Z. A1 - Abad Andrade, Carlos Enrique A1 - Okruss, M. A1 - Recknagel, Sebastian T1 - Feasibility of high-resolution continuum source molecular absorption spectrometry for vanadium determination N2 - This work aimed to evaluate high-resolution continuum source molecular absorption spectrometry (HR-CS MAS), traditionally used to determine non-metals, for the determination of a new element, metal, vanadium. VO was selected as a target molecule because it is relatively stable and was expected to be spontaneously generated in a flame or a graphite furnace (GF). The high-resolution overview spectra of the molecule were obtained in a wide range of 480–630 nm, and absorption due to the X4Σ−–C4Σ− electronic transition was registered. A unique instrumental setup, comprising a prototype Modular Simultaneous Echelle Spectrograph (MOSES) and a commercial HR-CS MAS apparatus, was applied in the research. Finally, the spectral area centered at 550.6230 nm was selected for analysis. A method was developed to determine V in solutions of catalysts of heavy petroleum oil hydroprocessing using a commercial HR-CS spectrometer in a flame version. Although sensitivity was relatively poor (characteristic concentration 380 mg L−1), an extremely low noise enabled reaching a satisfactory detection limit (20 mg L−1 in solution, i.e. 0.1% m:m in the catalyst). For the first time vanadium was determined using ordinary air-acetylene flame. The obtained results were consistent with the results of atomic absorption spectrometry with N2O-C2H2 flame. Unfortunately, only a small population of VO molecules could have been generated in GF measurements. Furthermore, the observed VO molecules appeared only at unfavorably high temperatures. The work shows the potential of HR-CS MAS as a scientific tool for investigating the mechanism of processes occurring in the GF. This work can inspire other research of new analytes for HR-CS MAS. KW - Vanadium KW - HR-CS-MAS KW - VO KW - High-resolution continuum source molecular absorption spectrometry KW - AAS PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569899 DO - https://doi.org/10.1039/D2JA00281G SN - 0267-9477 VL - 38 IS - 2 SP - 472 EP - 483 PB - Royal Society of Chemistry AN - OPUS4-56989 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian A1 - Vogel, Kristin T1 - Berechnung und Nutzung von Unsicherheiten zertifizierter Werte von Referenzmaterialien N2 - Referenzmaterialien sind unter anderem ein wichtiges Werkzeug zur Qualitätskontrolle von Messungen bestimmter Merkmalswerte. Dabei ist zu berücksichtigen, dass zertifizierte Merkmalswerte immer eine gewisse Unsicherheit haben. Die Ermittlung dieser Unsicherheitsbeiträge ist Gegenstand des Vortrags. Referenzmaterialien sind gleichzeitig ein wertvolles Werkzeug zur Ermittlung der Unsicherheit von Messverfahren und -Analysen unbekannter Proben. Die Vorgehensweise bei der Ermittlung der Messunsicherheit mit Hilfe eines Referenzmaterials wird beschrieben. T2 - 11. VDI-Fachtagung Messunsicherheit und Prüfprozesse CY - Erfurt, Germany DA - 14.11.2023 KW - Referenzmaterial KW - Messunsicherheit KW - ISO Guide 35 PY - 2023 AN - OPUS4-58946 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian A1 - Vogel, Kristin T1 - Berechnung und Nutzung von Unsicherheiten zertifizierter Werte von Referenzmaterialien N2 - Referenzmaterialien sind unter anderem ein wichtiges Werkzeug zur Qualitätskontrolle von Messungen bestimmter Merkmalswerte. Dabei ist zu berücksichtigen, dass zertifizierte Merkmalswerte immer eine gewisse Unsicherheit haben. Die Ermittlung dieser Unsicherheitsbeiträge ist Gegenstand des Vortrags. Referenzmaterialien sind gleichzeitig ein wertvolles Werkzeug zur Ermittlung der Unsicherheit von Messverfahren und -Analysen unbekannter Proben. Die Vorgehensweise bei der Ermittlung der Messunsicherheit mit Hilfe eines Referenzmaterials wird beschrieben. T2 - Jahrestagung des GDMB-Chemiker-Ausschusses CY - Kassel, Germany DA - 07.11.2023 KW - Referenzmaterial KW - Messunsicherheit KW - ISO Guide 35 PY - 2023 AN - OPUS4-58929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winckelmann, Alexander A1 - Roik, Janina A1 - Recknagel, Sebastian A1 - Abad Andrade, Carlos Enrique A1 - You, Zengchao T1 - Investigation of matrix effects in nitrogen microwave inductively coupled atmospheric-pressure plasma mass spectrometry (MICAP-MS) for trace element analysis in steels N2 - We investigated the performance of nitrogen microwave inductively coupled atmospheric-pressure plasma mass spectrometry (MICAP-MS) under matrix effects and its applicability to trace element analysis in steels. Influences of different gas flows and ion optics on the matrix tolerance are studied, indicating that nebulizer gas flow has the most significant impact. Optimization of ion optics improves matrix tolerance for light elements due to the reduction of the inelastic collisional scattering effect. With optimized operating conditions, MICAP-MS achieves an internal standard intensity recovery of over 90% at an Fe concentration of 500 mg L−1. Even at an Fe concentration of 1 g L−1, the recovery remains above 80%. Three certified reference materials – non-alloy, low-alloy and high-alloy steel – were analyzed using MICAP-MS. The determined mass concentrations of the trace and minor components show metrological compatibility to the reference values. No significant differences are observed between the results obtained with aqueous and matrix-matched calibration, demonstrating the strong matrix tolerance of MICAP-MS, and its promising applicability to steel analysis. KW - MICAP-MS KW - Trace Analysis KW - Steel PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576323 DO - https://doi.org/10.1039/d3ja00088e SN - 0267-9477 VL - 38 IS - 6 SP - 1253 EP - 1260 PB - Royal Society of Chemistry AN - OPUS4-57632 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - You, Zengchao A1 - Hoffmann, V. A1 - Morcillo, Dalia A1 - Agudo Jácome, Leonardo A1 - Leonhardt, Robert A1 - Winckelmann, Alexander A1 - Richter, Silke A1 - Recknagel, Sebastian A1 - Abad Andrade, Carlos Enrique T1 - Investigation of aluminum current collector degradation in lithium-ion batteries using glow discharge optical emission spectrometry N2 - In this work, we employed glow discharge optical emission spectrometry (GD-OES) depth profiling as a fast and semi-quantitative method to investigate the aluminum (Al) current collector degradation in commercial lithium cobalt oxide (LCO) pouch cells with no Al2O3 pretreatment. After battery aging, a heterogeneous deposit was found on the surface of the cathode. Gray hotspot areas within an extensive pale white region were formed. Consistent with energy dispersive X-ray (EDX) analysis of micro-cross sections milled via targeted focused ion beam (FIB), an Al-containing layer of approximately 3 µm can be observed using GD-OES. We attribute one main cause of this layer is the degradation of the Al current collector. The nonuniform growth of this layer was investigated by performing GD-OES depth profiling at different in-plane positions. We found that the gray area has a higher mass concentration of Al, probably in metallic form, whereas the white area was probably covered more homogeneously with Al2O3, resulting from the inhomogeneous distribution of the pitting positions on the current collector. Compared to FIB-EDX, GD-OES enables a faster and more convenient depth profile analysis, which allows the more productive characterization of lithium-ion batteries (LIBs), and consequently benefits the development of preferable battery materials. KW - GD-OES KW - depth profiles KW - Li-ion battery KW - battery aging mechanism KW - current collector corrosion PY - 2023 DO - https://doi.org/10.1016/j.sab.2023.106681 SN - 0584-8547 VL - 205 SP - 106681 PB - Elsevier B.V. CY - Amsterdam, Netherlands AN - OPUS4-57383 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Andresen, Elina A1 - Islam, Fahima A1 - Prinz, Carsten A1 - Gehrmann, P. A1 - Licha, K. A1 - Roik, Janina A1 - Recknagel, Sebastian A1 - Resch-Genger, Ute T1 - Assessing the reproducibility and up‑scaling of the synthesis of Er,Yb‑doped NaYF4‑based upconverting nanoparticles and control of size, morphology, and optical properties N2 - Lanthanide-based, spectrally shifting, and multi-color luminescent upconverting nanoparticles (UCNPs) have received much attention in the last decades because of their applicability as reporter for bioimaging, super-resolution microscopy, and sensing as well as barcoding and anti-counterfeiting tags. A prerequisite for the broad application of UCNPs in areas such as sensing and encoding are simple, robust, and easily upscalable synthesis protocols that yield large quantities of UCNPs with sizes of 20 nm or more with precisely controlled and tunable physicochemical properties from lowcost reagents with a high reproducibility. In this context, we studied the reproducibility, robustness, and upscalability of the synthesis of β-NaYF4:Yb, Er UCNPs via thermal decomposition. Reaction parameters included solvent, precursor chemical compositions, ratio, and concentration. The resulting UCNPs were then examined regarding their application-relevant physicochemical properties such as size, size distribution, morphology, crystal phase, chemical composition, and photoluminescence. Based on these screening studies, we propose a small volume and high-concentration synthesis approach that can provide UCNPs with different, yet controlled size, an excellent phase purity and tunable morphology in batch sizes of up to at least 5 g which are well suited for the fabrication of sensors, printable barcodes or authentication and recycling tags. KW - Photoluminescence KW - Nano KW - Nanomaterial KW - Synthesis KW - Reproducibility KW - Upconversion nanoparticle KW - Lanthanide PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570170 DO - https://doi.org/10.1038/s41598-023-28875-8 SN - 2045-2322 VL - 13 IS - 1 SP - 1 EP - 13 AN - OPUS4-57017 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lisec, Jan A1 - Recknagel, Sebastian A1 - Prinz, Carsten A1 - Vogel, Kristin A1 - Koch, Matthias A1 - Becker, Roland T1 - eCerto—versatile software for interlaboratory data evaluation and documentation during reference material production N2 - The statistical tool eCerto was developed for the evaluation of measurement data to assign property values and associated uncertainties of reference materials. The analysis is based on collaborative studies of expert laboratories and was implemented using the R software environment. Emphasis was put on comparability of eCerto with SoftCRM, a statistical tool based on the certification strategy of the former Community Bureau of Reference. Additionally, special attention was directed towards easy usability from data collection through processing, archiving, and reporting. While the effects of outlier removal can be flexibly explored, eCerto always retains the original data set and any manipulation such as outlier removal is (graphically and tabularly) documented adequately in the report. As a major reference materials producer, the Bundesanstalt für Materialforschung und -prüfung (BAM) developed and will maintain a tool to meet the needs of modern data processing, documentation requirements, and emerging fields of RM activity. The main features of eCerto are discussed using previously certified reference materials. KW - Reference material KW - Statistics KW - Software KW - Collaborative trial PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-591851 DO - https://doi.org/10.1007/s00216-023-05099-3 SP - 1 EP - 9 PB - Springer Science and Business Media LLC AN - OPUS4-59185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -