TY - JOUR A1 - Vogl, Jochen A1 - Yim, Y.-H. A1 - Lee, K.-S. A1 - Goenaga-Infante, H. A1 - Malinowskiy, D. A1 - Ren, T. A1 - Wang, J. A1 - Vocke Jr., R.D. A1 - Murphy, K. A1 - Nonose, N. A1 - Rienitz, O. A1 - Noordmann, J. A1 - Näykki, T. A1 - Sara-Aho, T. A1 - Ari, B. A1 - Cankur, O. T1 - Final report of the key comparison CCQM-K98: Pb isotope amount ratios in bronze KW - CCQM KW - Metrology KW - Isotope amount ratios KW - Lead PY - 2014 UR - http://www.bipm.org/utils/common/pdf/final_reports/QM/K98/CCQM-K98.pdf DO - https://doi.org/10.1088/0026-1394/51/1A/08017 SN - 0026-1394 SN - 1681-7575 VL - 51 IS - 1A Tech. Suppl. SP - 08017-1 EP - 08017-47 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-31929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Vogl, Jochen A1 - Yim, Y.-H. A1 - Lee, K.-S. A1 - Goenaga-Infante, H. A1 - Malinovskiy, D. A1 - Vocke, R. D. A1 - Murphy, K. A1 - Nonose, N. A1 - Rienitz, O. A1 - Noordmann, J. A1 - Näykki, T. A1 - Sara-Aho, T. A1 - Ari, B. A1 - Cankur, O. T1 - CCQM-P134 Pb isotope amount ratios and delta-values in bronze N2 - Isotope amount ratios (hereafter referred to as simply isotope ratios) are proving useful in an ever increasing array of applications that range from studies unravelling transport processes, to pinpointing the provenance of specific samples as well as trace element quantification by using isotope dilution mass spectrometry (IDMS). These expanding applications encompass fields as diverse as archaeology, food chemistry, forensic science, geochemistry, medicine and metrology. However, to be effective tools, the isotope ratio data must be reliable and traceable to enable the comparability of measurement. The importance of traceability and comparability in isotope ratio analysis has already been recognized by the Inorganic Analysis Working Group (IAWG) within the CCQM. Three pilot studies have focused on the quality of isotope ratio determinations (P48 “U isotope ratios in urine”, P75 “stable isotopes in Methionine”, P105 “87Sr/86Sr in wine”). Moreover, isotope ratio measurements are fundamental to IDMS amount of substance determinations. For example, when Pb quantification using IDMS is undertaken, this requires the measurements of Pb isotope ratios. While the requirements for isotope ratio accuracy and precision in the case of of IDMS are generally quite modest, “absolute” Pb isotope ratio measurements for geochemical age dating and source rock characterization as well as forensic provenance and fingerprinting studies require Pb isotope ratio measurements of the highest quality. To support present and future CMCs on isotope ratio determinations, a Key Comparison was urgently needed. Therefore, it was decided at the IAWG meeting in Paris in April 2011 that a Key Comparison on the determination of Pb isotope ratios in a pure Pb solution and in a bronze sample should be organized and accompanied by a pilot study. Measuring Pb isotope amount ratios in a pure Pb solution, while seemingly straight forward, rigorously tests the ability of analyst to correct for any instrumental effects (such as mass discrimination and blank correction) on the measured ratios. Pb, present in trace amounts in a metal matrix sample (e.g. Pb in bronze), provides a real world test of the whole chemical and instrumental procedure, from chemical separation and sample purification to analysis and subsequent correction of appropriate instrumental effects on the separated samples. A suitable bronze material with a Pb mass fraction between 10 and 100 mg·kg-1 was available at BAM. A high purity solution of Pb with a mass fraction of approximately 100 mg·kg-1 was also available. By comparing the Pb isotope ratio results obtained for the bronze sample with the Pb isotope ratio results from the Pb solution, potential biases arising from the processing of the bronze sample could be effectively identified and separated from the instrumental effects arising from the measurement and data processing protocol. KW - Isotope ratio KW - Delta value KW - Molar mass KW - Measurement uncertainty KW - Traceability PY - 2017 UR - https://www.bipm.org/wg/CCQM/IAWG/Allowed/IAWG_Pilot_Studies/CCQM-P134.pdf SP - 1 EP - 42 PB - BIPM (Bureau International des Poids et Mesures) CY - Paris AN - OPUS4-47709 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - D'Agostino, Giancarlo A1 - Oelze, Marcus A1 - Vogl, Jochen A1 - Ghestem, Jean-Philippe A1 - Lafaurie, Nicolas A1 - Klein, Ole A1 - Pröfrock, Daniel A1 - Di Luzio, Marco A1 - Bergamaschi, Luigi A1 - Jaćimović, Radojko A1 - Oster, Caroline A1 - Irrgeher, Johanna A1 - Lancaster, Shaun T. A1 - Walch, Anna A1 - Röthke, Anita A1 - Michaliszyn, Lena A1 - Pramann, Axel A1 - Rienitz, Olaf A1 - Sara-Aho, Timo A1 - Cankur, Oktay A1 - Kutan, Derya A1 - Noireaux, Johanna T1 - Development and application of reference and routine analytical methods providing SI-traceable results for the determination of technology-critical elements in PCB from WEEE N2 - The recovery and reprocessing of technology-critical elements (TCE) present in printed circuit boards (PCB) from electrical and electronic waste is essential both for recycling valuable materials subject to supply risk and for reducing the environmental impact. Although the quantitative knowledge of TCE amounts in endof- life PCB plays a key role, there are neither matrix certified reference materials nor harmonized analytical methods available to establish the traceability of the results to the International System of Units. To fill these gaps, we developed and applied five reference analytical methods based on ICP-MS standard addition calibrations and INAA k0- and relative calibrations suitable to certify reference materials. In addition, we developed and tested six analytical methods based on more commonly used ICP-MS external standard calibrations to provide industry with routine analysis methods. Twenty TCE (Ag, Au, Co, Cu, Dy, Ga, Gd, Ge, In, La, Li, Nd, Ni, Pd, Pr, Pt, Rh, Sm, Ta and Ti) were selected as target analytes and a batch of powdered PCB was used as measurement material. An overall mutual agreement was observed among data collected by reference methods at a few percent relative uncertainty levels. Moreover, all but one of the methods developed for routine analysis demonstrated their suitability in industrial applications by producing data within ± 20% of the values established with reference methods. KW - Technology critical elements KW - Electronic waste KW - Printed circuit boards KW - Traceability KW - Uncertainty PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612416 DO - https://doi.org/10.1039/d4ja00235k SN - 1364-5544 VL - 39 IS - 11 SP - 2809 EP - 2823 PB - Royal Society of Chemistry (RSC) AN - OPUS4-61241 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lancaster, Shaun T. A1 - Sahlin, Eskil A1 - Oelze, Marcus A1 - Ostermann, Markus A1 - Vogl, Jochen A1 - Laperche, Valérie A1 - Touze, Solène A1 - Ghestem, Jean-Philippe A1 - Dalencourt, Claire A1 - Gendre, Régine A1 - Stammeier, Jessica A1 - Klein, Ole A1 - Pröfrock, Daniel A1 - Košarac, Gala A1 - Jotanovic, Aida A1 - Bergamaschi, Luigi A1 - Di Luzio, Marco A1 - D’Agostino, Giancarlo A1 - Jaćimović, Radojko A1 - Eberhard, Melissa A1 - Feiner, Laura A1 - Trimmel, Simone A1 - Rachetti, Alessandra A1 - Sara-Aho, Timo A1 - Roethke, Anita A1 - Michaliszyn, Lena A1 - Pramann, Axel A1 - Rienitz, Olaf A1 - Irrgeher, Johanna T1 - Evaluation of X-ray fluorescence for analysing critical elements in three electronic waste matrices: A comprehensive comparison of analytical techniques N2 - As the drive towards recycling electronic waste increases, demand for rapid and reliable analytical methodology to analyse the metal content of the waste is increasing, e.g. to assess the value of the waste and to decide the correct recycling routes. Here, we comprehensively assess the suitability of different x-ray fluorescence spectroscopy (XRF)-based techniques as rapid analytical tools for the determination of critical raw materials, such as Al, Ti, Mn, Fe, Co, Ni, Cu, Zn, Nb, Pd and Au, in three electronic waste matrices: printed circuit boards (PCB), light emitting diodes (LED), and lithium (Li)-ion batteries. As validated reference methods and materials to establish metrological traceability are lacking, several laboratories measured test samples of each matrix using XRF as well as other independent complementary techniques (instrumental neutron activation analysis (INAA), inductively coupled plasma mass spectrometry (ICP-MS) and ICP optical emission spectrometry (OES)) as an inter-laboratory comparison (ILC). Results highlighted key aspects of sample preparation, limits of detection, and spectral interferences that affect the reliability of XRF, while additionally highlighting that XRF can provide more reliable data for certain elements compared to digestion-based approaches followed by ICP-MS analysis (e.g. group 4 and 5 metals). A clear distinction was observed in data processing methodologies for wavelength dispersive XRF, highlighting that considering the metals present as elements (rather than oxides) induces overestimations of the mass fractions when compared to other techniques. Eventually, the effect of sample particle size was studied and indicated that smaller particle size (<200 μm) is essential for reliable determinations. KW - XRF KW - WEEE KW - PCB KW - Battery KW - LED KW - Recycling PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-614060 DO - https://doi.org/10.1016/j.wasman.2024.10.015 VL - 190 SP - 496 EP - 505 PB - Elsevier B.V. AN - OPUS4-61406 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -