TY - JOUR A1 - Vogl, Jochen A1 - Rosner, M. A1 - Kasemann, S. A. A1 - Kraft, R. A1 - Meixner, A. A1 - Noordmann, J. A1 - Rabb, S. A1 - Rienitz, O. A1 - Schuessler, J. A. A1 - Tatzel, Michael A1 - Vocke, R. D. T1 - Intercalibration of Mg isotope delta scales and realisation of SI traceability for Mg isotope amount ratios and isotope delta values N2 - The continuous improvement of analytical procedures using multi-collector technologies in ICP-mass spectrometry has led to an increased demand for isotope standards with improved homogeneity and reduced measurement uncertainty. For magnesium, this has led to a variety of available standards with different quality levels ranging from artefact standards to isotope reference materials certified for absolute isotope ratios. This required an intercalibration of all standards and reference materials, which we present in this interlaboratory comparison study. The materials Cambridge1, DSM3, ERMAE143, ERM-AE144, ERM-AE145, IRMM-009 and NIST SRM 980 were cross-calibrated with expanded measurement uncertainties (95% confidence level) of less than 0.030‰ for the δ25/24Mg values and less than 0.037‰ for the δ26/24Mg values. Thus, comparability of all magnesium isotope delta (δ) measurements based on these standards and reference materials is established. Further, ERM-AE143 anchors all magnesium δ-scales to absolute isotope ratios and therefore establishes SI traceability, here traceability to the SI base unit mole. This applies especially to the DSM3 scale, which is proposed to be maintained. With ERM-AE144 and ERM-AE145, which are product and educt of a sublimation-condensation process, for the first time a set of isotope reference materials is available with a published value for the apparent triple isotope fractionation exponent θapp, the fractionation relationship ln α(25/24Mg)/ln α(26/24Mg). KW - Delta scale KW - Traceability KW - Scale anchor KW - Absolute isotope ratio KW - Comparability KW - Triple isotope fractionation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-511557 DO - https://doi.org/10.1111/ggr.12327 SN - 1751-908X VL - 44 IS - 3 SP - 439 EP - 457 PB - Wiley-Blackwell CY - Oxford AN - OPUS4-51155 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rienitz, O. A1 - Jährling, R. A1 - Noordmann, J. A1 - Pape, C. A1 - Röhker, K. A1 - Vogl, Jochen A1 - Manzano, J. V. L. A1 - Kozlowski, W. A1 - Caciano de Siena, R. A1 - Marques Rodrigues, J. A1 - Galli, A. H. A1 - Yim, Y.-H. A1 - Lee, K.-S. A1 - Lee, J. H. A1 - Min, H.-S. A1 - Chingbo, C. A1 - Naijie, S. A1 - Qian, W. A1 - Ren, T. A1 - Jun, W. A1 - Tangpaisarnkul, N. A1 - Suzuki, T. A1 - Nonose, N. A1 - Mester, Z. A1 - Yang, L. A1 - Pagliano, E. A1 - Greenberg, P. A1 - Mariassy, M. A1 - Näykki, T. A1 - Cankur, O. A1 - Coskun, F. G. A1 - Ari, B. A1 - Can, S. Z. T1 - CCQM-K122 "Anionic impurities and lead in salt solutions" N2 - The determination of the mass fractions of bromide, sulfate, and lead as well as the isotopic composition of the lead (expressed as the molar mass and the amount fractions of all four stable lead isotopes) in an aqueous solution of sodium chloride with a mass fraction of 0.15 g/g was the subject of this comparison. Even though the mass fractions ranged from 3 μg/g (bromide) to 50 ng/g (lead), almost all results reported agreed with the according KCRVs. KW - Absolute isotope ratio KW - Lead isotope ratios KW - Metrology KW - Traceability PY - 2020 DO - https://doi.org/10.1088/0026-1394/57/1A/08012 VL - 57 IS - 1A SP - 8012 PB - IOP Science AN - OPUS4-51156 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Molloy, J. L. A1 - Winchester, M. R. A1 - Butler, T. A. A1 - Possolo, A. M. A1 - Rienitz, O. A1 - Roethke, A. A1 - Goerlitz, V. A1 - Caciano de Sena, R. A1 - Dominguez Almeida, M. A1 - Yang, L. A1 - Methven, B. A1 - Nadeau, K. A1 - Romero Arancibia, P. A1 - Bing, W. A1 - Tao, Z. A1 - Snell, J. A1 - Vogl, Jochen A1 - Koenig, Maren A1 - Kotnala, R. K. A1 - Swarupa Tripathy, S. A1 - Elishian, C. A1 - Ketrin, R. A1 - Suzuki, T. A1 - Oduor Okumu, T. A1 - Yim, Y.-H. A1 - Heo, S. W. A1 - Min, H. S. A1 - Sub Han, M. A1 - Lim, Y. A1 - Velina Lara Manzano, J. A1 - Segoviano Regalado, F. A1 - Arvizu Torres, M. A1 - Valle Moya, E. A1 - Buzoianu, M. A1 - Sobina, A. A1 - Zyskin, V. A1 - Sobina, E. A1 - Migal, P. A1 - Linsky, M. A1 - Can, S. Z. A1 - Ari, B. A1 - Goenaga Infante, H. T1 - CCQM-K143 Comparison of Copper Calibration Solutions Prepared by NMIs/DIs N2 - CCQM-K143 is a key comparison that assesses participants’ ability to prepare single element calibration solutions. Preparing calibration solutions properly is the cornerstone of establishing a traceability link to the International System of Units (SI), and therefore should be tested in order to confirm the validity of CCQM comparisons of more complex materials. CCQM-K143 consisted of participants each preparing a single copper calibration solution at 10 g/kg copper mass fraction and shipping 10 bottled aliquots of that solution to the coordinating laboratory, the National Institute of Standards and Technology (NIST). The masses and mass fraction for the prepared solutions were documented with the submitted samples. The solutions prepared by all participants were measured at NIST by high performance inductively coupled plasma optical emission spectroscopy (HP-ICP-OES). The intensity measurements for copper were not mapped onto values of mass fraction via calibration. Instead, ratios were computed between the measurements for copper and simultaneous measurements for manganese, the internal standard, and all subsequent data reductions, including the computation of the KCRV and the degrees of equivalence, were based on these ratios. Other than for two participants whose measurement results appeared to suffer from calculation or preparation errors, all unilateral degrees of equivalence showed that the measured values did not differ significantly from the KCRV. These results were confirmed by a second set of ICP-OES measurements performed by the Physikalisch-Technische Bundesanstalt (PTB). CCQM-K143 showed that participants are capable of preparing calibration solutions starting from high purity, assayed copper metal. Similar steps are involved when preparing solutions for other elements, so it seems safe to infer that similar capabilities should prevail when preparing many different, single-element solutions. KW - Metrology KW - Primary calibration solution KW - Traceability PY - 2020 DO - https://doi.org/10.1088/0026-1394/58/1A/08006 SN - 0026-1394 VL - 58 IS - 1A SP - 08006 PB - IOP Science CY - Cambridge AN - OPUS4-51983 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - New applications and reference materials in isotope analysis N2 - The presentations gives a short introduction into isotope analysis illustrated by examples from archaeology, food provenancing and metrology. In the main part current projects on the provenance determination of cement, the intercalibration of Mg isotope reference materials and the development of a new calibration approach for isotope measurements are presented. T2 - Seminar der Abteilung 1 CY - Online meeting DA - 19.01.2021 KW - Isotope reference material KW - Absolute isotope ratio KW - Metrology KW - Traceability KW - Triple isotope fractionation KW - Archaeometry KW - Cement PY - 2021 AN - OPUS4-52460 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - The triple isotope calibration approach BT - A new calibration approach for obtaining absolute isotope ratios of multi-isotopic elements N2 - The calibration of isotope ratio measurements is an ongoing challenge since instrumental isotope fractionation (IIF) has been detected in mass spectrometry (MS). There is a variety of approaches which either bypass IIF such as delta measurements or refer to reference materials (RMs) and thus shifting the problem of calibration to somebody else: the RM producer. For certifying isotope RMs with absolute isotope ratios only a few approaches are available, namely the isotope mixture approach, the double spike approach, the mass bias regression model and total evaporation in TIMS. All of them require either enriched isotopes, isotope RMs of another element or an RM for correcting residual error. As the enriched isotopes required for the isotope mixture and the double spike approach need to be fully characterized beforehand, all mentioned calibration approaches require a standard. Here, a new and standard-free calibration approach for obtaining absolute isotope ratios of multi-isotopic elements has been developed. The underlying principle is that each MS suffers from IIF and thus yields a specific isotope fractionation line in a three-isotope diagram. When applying a second MS featuring a different ionization mechanism, we obtain a second isotope fractionation line with a different slope in the same three-isotope diagram. In both cases the absolute isotope ratios range somewhere on the isotope fractionation line. Consequentially, the intersect of both lines yield the absolute isotope ratios of the measured sample. This theory has been tested by measuring Cd and Pb isotope ratios of suitable isotope RMs with a TIMS and an ICP-MS, both equipped with multi-collector array. During the measurements the ionization conditions were changed such that different extent of the isotope fractionation has been achieved. With the resulting data set the theory described above could be verified. The obtained absolute isotope ratios were metrologically compatible with the certified isotope ratios. The remaining average bias of -5 ‰ can be reduced with further improvements. The calibration approach is universal and can be applied to any multi-isotopic element and it is not limited by the type of the mass spectrometer. T2 - Virtual Goldschmidt 2021 CY - Online meeting DA - 04.07.2021 KW - Absolute isotope ratio KW - Traceability KW - Metrology KW - Calibration KW - Uncertainty KW - Triple isotope fractionation PY - 2021 AN - OPUS4-53023 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Herausforderungen bei der Analytik von Technologie-kritischen Elementen (TCE) in Abfällen N2 - Technologie-kritische Elemente (TCE) sind unentbehrliche Materialien für High-Tech Produkte wie Smartphones, Notebooks und Monitors. Ihr Bedarf wird voraussichtlich aufgrund des gesellschaftlichen Wandels hin zu einer grünen Ökonomie exponentiell ansteigen. Dieser Wandel wird vor allem auch durch erneuerbare Energien und Elektromobilität geprägt (European Green Deal). Diese Entwicklung in Verbindung mit einer nahezu fehlenden TCE Produktion in Europa setzt den Markt unter Druck und führt zu steigenden Preisen. Die Sicherung des TCE Nachschubs wurde in der gegenwärtigen Gesundheitskrise noch dringender und wurde daher auch zu einem der Hauptthemen des COVID-19 Recovery Plan, der eine Stärkung der europäischen Resilienz und Autonomie zum Ziel hat. Ein nachhaltige Lösung ist das Recycling der Abfall- bzw. Wertstoffe und letztendlich eine Circular Economy. Allerdings ist die Analyse von Abfallströmen schwierig und erfordert geeignete analytische Lösungen, die SI-rückführbare und somit vergleichbare Messergebnisse im gesamten Recyclingprozess ermöglichen. Die dafür erforderlichen, für TCE zertifizierte, Referenzmaterialien und nötige standardisierte Verfahren fehlen bisher nahezu vollständig. In diesem Beitrag werden die analytischen Herausforderungen, wie z.B. die extreme Heterogenität der Materialien, Schwierigkeiten beim Probenaufschluss und das Fehlen von Referenzmaterialien diskutiert. Und es wird das EMPIR-Projekt MetroCycleEU vorgestellt, dessen Ziel es ist Referenz- und Routineverfahren für ausgewählte TCE (Co, Ga, Ge, In, Ta, Nd, Pr, Dy, Gd, La, Au, Pt, Pd, Rh) zu entwickeln und Referenzmaterialien für Platinen, LEDs und Li-Batterien bereitzustellen. T2 - Workshop Nachhaltige Prozesse für eine Circular Economy CY - Berlin, Germany DA - 23.09.2021 KW - TCE KW - Circular economy KW - Metrology KW - Traceability KW - Uncertainty PY - 2021 AN - OPUS4-53371 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kazlagić, Anera A1 - Vogl, Jochen T1 - Investigating the differences in 87Sr/ 86Sr isotope ratio measurements between MC-ICP-MS and MC-TIMS in cement RMs N2 - Thirteen laboratories participated in an international interlaboratory comparison for the determination of 87Sr/86Sr isotope ratios in four cement reference materials (RM) using the conventional method for 87Sr/86Sr isotope ratios analyses. Sample dissolution and Sr isolation via ion exchange chromatography were required since the cement samples were distributed as powders. Analytical preparation included the use of various digestion methods including mixed mineral acids, microwave/acid, bomb/acid digestion or borate fusion, followed by Sr separation using ion exchange chromatography. In this study, we evaluated whether any statistically significant differences were attributable to instrumental differences (i.e., MC-ICP-MS and MC-TIMS), or to laboratory-specific techniques (different sample preparation techniques, Sr isolation and the procedures for correcting the data outputs). To evaluate these effects, consensus values for cement RMs and associated standard uncertainties were estimated by fitting a linear, Gaussian mixed effects model using the R function “lmer” defined in package “lme4”. No statistically significant effects (SSE) attributable to instrumental differences regardless of whether the materials are considered together or separately were evident. There were SSE attributable to differences between laboratories for three cement RMs when the individual cements were considered separately. Since consideration or disregard for such differences does not induce significant changes in the estimate of the consensus values for the 87Sr/86Sr isotope ratios in cement RMs, these effects can safely be neglected when calculating the best estimates for the true values of 87Sr/86Sr isotope ratios in these RMs. T2 - ICP-MS Anwender*innentreffen 2022 CY - Leoben, Austria DA - 05.09.2022 KW - Conventional isotope ratio KW - Reference material KW - Metrology KW - Traceability KW - Uncertainty PY - 2022 AN - OPUS4-55682 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen A1 - Oelze, Marcus T1 - Isotope reference materials N2 - The variation of isotope ratios is increasingly used to unravel natural and technical questions. In the past, the investigation and interpretation of such variations was the field of a limited number of experts. With new upcoming techniques and research topics in the last decades, such as provenance or food authenticity studies, the number of published isotope data strongly increased. Instrumental developments such as the enhancement of inductively coupled plasma mass spectrometers (ICP-MS) from an instrument for simple quantitative analysis to highly sophisticated isotope ratio machines influenced this process significantly. While in former times only experts in mass spectrometry were able to produce reliable isotope data, nowadays many laboratories, never been in touch with mass spectrometry before, produce isotope data with an ICP-MS. Isotope reference materials (iCRM) are indispensable to enable a reliable method validation or in rare cases even SI-traceability. The fast development and the broad availability of ICP-MS also lead to an expansion of the classical research areas and new elements are under investigation. Irrespective of the investigated element or the knowledge of the user all isotope ratio applications require reference materials either for correction of instrumental isotope fractionation, for method validation or to provide a common accepted basis as needed for delta measurements. This presentation will outline the basic principles and illustrate the urgent need for new iCRMs. Consequently, the production and certification of iCRMs will be discussed and illustrated by examples of already completed certification projects. Finally, plans for future iCRMs to be produced at BAM will be presented. T2 - ICP-MS Anwender*innentreffen 2022 CY - Leoben, Austria DA - 05.09.2022 KW - Absolute isotope ratio KW - Traceability KW - Metrology KW - Comparability KW - Uncertainty KW - Isotope reference materials KW - Delta scale PY - 2022 AN - OPUS4-55681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - IRWG strategy update N2 - This talk presents a strategy update of the Isotope Ratio Working Group of CCQM. The focus is on future comparisons and the promotion of international comparability. T2 - IRWG Meeting CY - Online meeting DA - 12.05.2022 KW - Isotope ratio KW - Traceability KW - Metrology PY - 2022 AN - OPUS4-55160 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Plan for comparison on absolute Cu isotope ratios by applying the isotope mixture approach N2 - Based on a previously circulated questionnaire, the plan for a key comparison is presented which focuses on the determination of absolute copper isotope ratios by the means of synthetic isotope mixtures. T2 - IRWG Meeting CY - Online meeting DA - 12.05.2022 KW - Absolute isotope ratio KW - Traceability KW - CCQM PY - 2022 AN - OPUS4-55161 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - CCQM-P213: BAM procedure for obtaining Cu delta values N2 - BAM participated in the CCQM pilot study P213 for obtaining copper isotope delta values. This presentations provides details on the MC-ICP-MS based measruement procedure, which has been applied to obtain such copper delta values. T2 - IRWG Meeting CY - Online meeting DA - 12.05.2022 KW - Isotope delta value KW - Copper KW - Metrology KW - Traceability PY - 2022 AN - OPUS4-55162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - CCQM-P213: BAM procedure for obtaining Cu delta values N2 - BAM participated in the CCQM pilot study P213 for obtaining copper isotope delta values. This presentations provides details on the MC-ICP-MS based measruement procedure, which has been applied to obtain such copper delta values. T2 - IRWG Meeting 2022 CY - Online meeting DA - 20.09.2022 KW - Isotope ratio KW - Copper KW - Metrology KW - Traceability KW - Uncertainty PY - 2022 AN - OPUS4-55864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Can, S. Z. A1 - Engin, B. A. A1 - İşleyen, A. A1 - Jotanovic, A. A1 - Acosta, O. A1 - Prina, P. A1 - Schvartz, M. A1 - Savić, M. A1 - Stojanović, M. A1 - Ahumada, D. A. A1 - Abella, J. P. A1 - Näykki, T. A1 - Saro-Aho, T. A1 - Vogl, Jochen A1 - Koenig, Maren A1 - Rienitz, O. A1 - Noordmann, J. A1 - Pape, C. A1 - Towara, J. A1 - Kakoulides, E. A1 - Alexopoulos, C. A1 - Ketrin, R. A1 - Mardika, E. A1 - Komalasari, I. A1 - Elishian, C. A1 - Naujalis, E. A1 - Knašienė, B. A1 - Uribe, C. A1 - Carrasco, E. A1 - Zoń, A. A1 - Warzywoda, B. A1 - Stakheev, A. A1 - Dobrovolskiy, V. A1 - Stolboushkina, T. A1 - Glinkova, A. A1 - Sobina, E. A1 - Tabatchikova, T. A1 - Gažević, L. A1 - Paunovic, M. A1 - Jaćimović, R. A1 - Zuliani, T. A1 - Zambra, R. P. A1 - Napoli, R. T1 - Determination of elements in river water N2 - The need for quality assessment of anthropogenic impact on environmental pollution is increasing due to discharge from various industries, the use of chemicals in agriculture and the consumption of fossil fuels. Diminishing resources such as natural waters used for the cultivation of agricultural products, plant and animal habitats are under severe pollution pressure and are at constant risk. Several parameters, such as Pb, Cd, Ni, Hg were listed by Water Framework Directive in Directive(2008/105/EC) in the priority substances. Cadmium and Hg were identified as priority hazardous substances whereas As is an important contaminant for its potential toxicological and carcinogenic effects. An inter-comparison study is organised in EURAMET TC-MC in order to demonstrate the capability participants for measuring five elements in river water. The participants carried out measurements for analytes: Pb, Cd, Ni and As as mandatory elements, and Se as an optional one. Participants were asked to perform the measurements with respect to the protocol provided. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA). KW - Metrology KW - Traceability KW - Toxic elements KW - River water PY - 2023 DO - https://doi.org/10.1088/0026-1394/60/1A/08001 VL - 60 IS - 1a SP - 1 EP - 40 PB - BIPM & IOP Publishing Ltd AN - OPUS4-56786 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen A1 - Irrgeher, J. T1 - IUPAC Commission on Isotopic Abundances and Atomic Weights its history, role, and work N2 - This presentation provides a short introduction to the Commission on Isotopic Abundances and Atomic Weights (CIAAW). It describes the role of the Commission and provides an insight into its work and the corresponding principal tasks. Finally, it provides the reader with the latest achievements and with the most recent publications. T2 - IUPAC Virtual General Assembly CY - Online meeting DA - 25.07.2023 KW - Absolute isotope ratio KW - Atomic weights KW - Metrology KW - Traceability KW - Isotope reference material PY - 2023 AN - OPUS4-58013 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yang, L. A1 - Vogl, Jochen A1 - Mann, J. A1 - Kraft, R. A1 - Vocke, R. A1 - Pramann, A. A1 - Eberhardt, J. A1 - Rienitz, O. A1 - Lee, K.-S. A1 - Lim, J. S. A1 - Sobina, E. A1 - Song, P. A1 - Wang, J. A1 - Mester, Z. A1 - Meija, J. T1 - Copper isotope delta measurements in high purity materials: CCQM-P213 pilot study N2 - Accurate and precise isotope ratio measurements of heavy elements are playing an increasinglyimportant role in modern analytical sciences and have numerous applications. Today, isotope ratio measurements are typically performed with two principal techniques: thermal ionization mass spectrometry (TIMS) and multiple collector-inductively coupled plasma mass spectrometry (MC-ICP-MS). To obtain accurate results by mass spectrometry, isotopic certified reference materials (iCRMs) are needed for mass bias correction and for the validation of the method used for analysis.Thus, it is of paramount importance to achieve measurement comparability of all data reported, and to assess measurement capability of each CRM producer/National Metrology Institute (NMI). Therefore, the international comparison (CCQM-P213) was performed to assess the analytical capabilities of NMIs for the accurate determination of copper isotope ratio delta values in high purity materials. The study was proposed by the coordinating laboratories, National Research Council Canada (NRC), National Institute of Standards and Technology (NIST), Bundesanstalt für Materialforschung und -prüfung (BAM) and Physikalisch-Technische Bundesanstalt (PTB), as an activity of the Isotope Ratio Working Group (IRWG) of the Consultative Committee for Amount of Substance - Metrology in Chemistry and Biology (CCQM). Participants included six NMIs and one designated institute (DI) from the six countries. Although no measurement method was prescribed by the coordinating laboratories, MC-ICP-MS with either standard-sample bracketing (SSB) or combined SSB with internal normalization (C-SSBIN) models for mass bias correction were recommended. Results obtained from the six NMIs and one DI were in good agreement. KW - Comparability KW - Traceability KW - Metrology KW - Isotope delta KW - Copper PY - 2023 DO - https://doi.org/10.1088/0026-1394/60/1A/08019 VL - 60 IS - 1A SP - 1 EP - 23 PB - IOP Science AN - OPUS4-58040 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Metrology in Chemistry - Basics and international structure N2 - Basics in Metrology in Chemistry are explained and the international structure of the metrology network is presented. T2 - Workshop & Training "Isotope Ratio Analysis" CY - Pathum Thani, Thailand DA - 06.12.2023 KW - Metrology in Chemistry KW - Traceability KW - Uncertainty PY - 2023 AN - OPUS4-59163 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kazlagić, Anera A1 - Rosner, M. A1 - Vogl, Jochen T1 - Investigating the differences between MC-ICP-MS and MC-TIMS using conventional 87Sr/86Sr isotope ratios in limestone and slate reference materials N2 - The Federal Institute for Materials Research and Testing (BAM) organised an interlaboratory comparison (ILC) for the characterisation of 87Sr/86Sr isotope ratios in limestone (IAG/CGL ML-3) and Penrhyn slate (IAG OU-6) reference materials by applying the conventional method for 87Sr/86Sr isotope ratios. Samples were sent to thirteen analytical laboratories . Since both samples are powdered, rock materials, dissolution of the sample and Sr isolation via ion exchange chromatography were mandatory. This was done using acid, microwave/acid, bomb/acid digestion or borate fusion and subsequent isolation of Sr by means of commercially available ion exchange resins. In this study, we present and discuss the potential effects that differences between laboratories, and between two instrumental measurement techniques (i.e., MC-ICP-MS and MC-TIMS), may have upon the dispersion of measurement results of the 87Sr/86Sr isotope ratio in the two aforementioned reference materials. We used a statistical mixed effects model to assess the potential effects of both the laboratory and the measurement technique. Consensus values for both materials and associated standard uncertainties {(IAG/CGL ML-3 (0.708245±0.000004) mol/mol; IAG OU-6 (0.729769±0.000008) mol/mol} were estimated by fitting a linear, Gaussian mixed effects model (Pinheiro and Bates 2000) using the R function “lmer” defined in package “lme4”. The statistical results showed that there is no significant effect attributable to differences between instrumental techniques when both materials are considered together, or separately. The p-value of the test of significance of the measurement technique effect is greater than 0.54. For both materials there were statistically significant effects attributable to differences between laboratories when the measurement results for both materials were considered together and separately. This effect is less than 0.00004 in absolute value. However, for neither material did consideration or disregard for such differences induce significant changes in the estimate of the consensus value for the 87Sr/86Sr isotope ratio. Therefore, the effects attributable to differences between instrumental techniques or between laboratories can safely be disregarded when computing the best estimate for the true value of 87Sr/86Sr isotope ratio in these materials, by the community of expert laboratories represented in this study. T2 - GeoAnalysis 2022 CY - Freiberg, Germany DA - 06.08.2022 KW - Isotope ratio KW - Conventional isotope ratio KW - ILC KW - Traceability KW - Uncertainty KW - Isotope reference materials PY - 2022 AN - OPUS4-56848 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pramann, A. A1 - Vogl, Jochen A1 - Flierl, L. A1 - Rienitz, O. T1 - Determination of absolute (SI‐traceable) isotope ratios: The use of Gravimetric Isotope Mixtures N2 - The presentation is brief overview on how to use gravimetric isotope mixtures to determine SI traceable isotope ratios. There is no mass spectrometer on earth that directly measures isotope ratios. Mass spectrometers will always measure signal intensity ratios instead. The actual problem is that the measured intensity ratios differ more or less from the isotope ratios. The difference can be up to more than 10 % in case of lithium while it‘s below 1 % in case of the heavier elements like lead or uranium. Consequently, the signal intensity ratios are expressed for example in V/V depending on the type of mass spectrometer you are using, while the isotope ratios are expressed in mol/mol. This phenomenon is called Instrumental Isotopic Fractionation (or short IIF) but the more common name is still mass bias (even though this name is not entirely correct). To convert the measured into the isotope ratio usually a simple multiplication with a so-called correction (or short K) factor is done. Therefore, the problem is to determine the K factor. In absence of isotope reference materials the golden route is via gravimetric isotope mixtures, which will be explained within the presentation. T2 - CCRI-CCQM Workshop on the use of mass spectrometry in radionuclide metrology: Opportunities and challenges - Video Tutorial CY - Online meeting DA - 14.02.2023 KW - Absolute isotope ratio KW - Traceability KW - Uncertainty KW - Isotope mixtures PY - 2023 AN - OPUS4-57172 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Isotope Ratio Measurements and Certification of iCRMs at BAM N2 - A short overview on isotope ratio measurements at BAM and related CRM activities is given. The current isotope CRM range offered by BAM and future iCRM projects are presented. T2 - CCQM IRWG Meeting CY - Sevres, France DA - 24.04.2023 KW - Absolute isotope ratio KW - Reference material KW - Metrology KW - Traceability PY - 2023 AN - OPUS4-57399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - IRWG strategy update N2 - An update of the IRWG strategy for the period 2023-2030 is given. The status and the futuere work of the task group on quantities, symbols and units is discussed. The present status of IRWG comparisons is shown and the need for specific key comparisons is discussed. T2 - CCQM IRWG Meeting CY - Sevres, France DA - 24.04.2023 KW - Isotope ratio KW - Traceability KW - Metrology PY - 2023 AN - OPUS4-57400 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Plan for comparison on absolute Cu isotope ratios by applying the isotope mixture approach N2 - The reference method for obtaining absolute isotope ratios still is the isotope mixture approach. Due the huge efforts required the full isotope mixture approach is applied only by a few institutes worldwide. To enable an IRWG key comparison with a sufficiently large number of participants a proposal for absolute cu isotope ratios is presented where participants will be provided with the enriched isotopes, the isotope mixtures and the samples. In parallel a pilot study will be organized where alternative approaches for obtaining absolute Cu isotope ratios can be applied. T2 - CCQM IRWG Meeting CY - Sevres, France DA - 24.04.2023 KW - Absolute isotope ratio KW - Traceability KW - Metrology PY - 2023 AN - OPUS4-57401 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hill, Sarah A1 - Infante, Heidi Goenaga A1 - Entwisle, John A1 - Strekopytov, Stanislav A1 - Ward-Deitrich, Christian A1 - Cowen, Simon A1 - Rienitz, Olaf A1 - Roethke, Anita A1 - Goerlitz, Volker A1 - Schulz, Ursula A1 - Pape, Carola A1 - Vogl, Jochen A1 - Koenig, Maren A1 - Jacimovic, Radojko A1 - Fisicaro, Paola A1 - Ren, Tongxiang A1 - Wang, Song A1 - Song, Panshu A1 - Li, Haifeng A1 - Linsky, Maré A1 - Sobina, Egor A1 - Lozano, Hernán Ezequiel A1 - Puelles, Mabel A1 - Yamani, Randa A1 - Haraldsson, Conny T1 - CCQM-K160: platinum group elements in automotive catalyst N2 - The platinum group elements (PGEs) play an important role in reducing emissions from automotive vehicles through their use in catalytic convertors but also for catalysis in the pharmaceutical industry. The immense economic value of platinum (Pt), palladium (Pd) and rhodium (Rh) highlights the importance of highly accurate measurements. Therefore, there is a need for National Metrology Institutes (NMIs) and Designated Institutes (DIs) to demonstrate measurement capability in this space. A pilot comparison (CCQM-P63) for precious metals in automotive catalyst took place in 2006, but with a limited number of institutes participating. Furthermore, this study was performed over 17 years ago. Therefore, there was a need to maintain existing capability and demonstrate new capability in a key comparison, in order to claim calibration and measurement capability claims (CMCs). With the core capability matrix, this study falls into the "Difficult to dissolve metals/metal oxides" which will support CMC categories 8 (Metal and metal alloys), 9 (Advanced materials) and 14 (Other materials). Eleven NMIs and DIs participated in the Key Comparison CCQM-K160 Platinum Group Elements in Automotive Catalyst. Participants were requested to evaluate the mass fractions of Pt, Pd and Rh in mg/kg in an unused autocatalyst material (cordierite ceramic base). The Key Comparison Reference Values (KCRVs) and Degrees of Equivalence (DoEs) were calculated utilising the NIST Decision Tree for the measurands. The participants utilised a number of sample preparation and analytical methods including hot plate digestion, microwave digestion and sodium fusion, followed by either atomic absorption spectroscopy (AAS), inductively coupled plasma optical emission spectroscopy (ICP-OES) or inductively coupled plasma mass spectrometry (ICP-MS) detection. Several calibration techniques were used, namely external calibration, standard addition, isotope dilution mass spectrometry (IDMS) and an exact matching procedure. Additionally, one participant employed instrumental neutron activation analysis (INAA) with k0 standardisation which is a direct solid analysis method. The majority of participants claimed traceability to NIST primary calibrants or their own CRMs. Furthermore, several matrix CRMs were included or spiked samples for quality control. All institutes were required to determine the dry mass fraction using the stipulated protocol. The NIST decision tree was implemented for the calculation of the KCRVs and DoEs. The participant results overall showed good agreement with the KCRV, despite the variety of dissolution procedures and measurement techniques for this highly complex matrix and challenging measurands. Successful participation in CCQM-K160 demonstrated measurement capabilities for the determination of mass fraction of Pt, Pd and Rh in the mg/kg range and will support broad scope CMC claims for a wide range of challenging matrices. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA). KW - Metrology in Chemistry KW - Traceability KW - Uncertainty PY - 2024 DO - https://doi.org/10.1088/0026-1394/61/1A/08011 VL - 61 IS - 1A SP - 1 EP - 39 PB - IOP Publishing AN - OPUS4-60524 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 - Phukphatthanachai, P. A1 - Panne, Ulrich A1 - Traub, Heike A1 - Pfeifer, Jens A1 - Vogl, Jochen T1 - Quantification of sulphur in copper and copper alloys by GDMS and LA-ICP-MS, demonstrating metrological traceability to the international system of units N2 - The quantification of the sulphur mass fraction in pure copper and copper alloys by GDMS and LA-ICP-MS revealed a lack of traceability mainly due to a lack of suitable certified reference materials for calibrating the instruments. Within this study GDMS and LA-ICP-MS were applied as routine analytical tools to quantify sulphur in copper samples by applying reference materials as calibrators, which were characterized for their sulphur mass fraction by IDMS beforehand. Different external calibration strategies were applied including a matrix cross type calibration. Both techniques with all calibration strategies were validated by using certified reference materials (others than those used for calibration) and good agreement with the reference values was achieved except for the matrix cross type calibration, for which the agreement was slightly worse. All measurement results were accompanied by an uncertainty statement. For GDMS, the relative expanded (k = 2) measurement uncertainty ranged from 3% to 7%, while for LA-ICP-MS it ranged from 11% to 33% when applying matrix-matched calibration in the sulphur mass fraction range between 25 mg kg-1 and 1300 mg kg-1. For cross-type calibration the relative expanded (k = 2) measurement uncertainty need to be increased to at least 12% for GDMS and to at least 54% for LA-ICP-MS to yield metrological compatibility with the reference values. The so obtained measurement results are traceable to the international system of units (SI) via IDMS reference values, which is clearly illustrated by the unbroken chain of calibrations in the metrological traceability scheme. KW - Sulfur KW - Copper KW - GDMS KW - LA-ICP-MS KW - Uncertainty KW - Traceability KW - SI PY - 2021 DO - https://doi.org/10.1039/d1ja00137j SN - 0267-9477 VL - 36 IS - 11 SP - 2404 EP - 2414 PB - Royal Society of Chemistry AN - OPUS4-53412 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matschat, Ralf A1 - Richter, Silke A1 - Vogl, Jochen A1 - Kipphardt, Heinrich T1 - On the way to SI traceable primary transfer standards for amount of substance measurements in inorganic chemical analysis N2 - During its 25 years of existence, the Inorganic Analysis Working Group of the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM IAWG) has achieved much in establishing comparability of measurement results. Impressive work has been done on comparison exercises related to real-world problems in fields such as ecology, food, or health. In more recent attempts, measurements and comparisons were focused on calibration solutions which are the basis of most inorganic chemical measurements. This contribution deals with the question of how to achieve full and transparent SI traceability for the values carried by such solutions. Within this framework, the use of classical primary methods (CPMs) is compared to the use of a primary difference method (PDM). PDM is a method with a dual character, namely a metrological method with a primary character, based on the bundling of many measurement methods for individual impurities, which lead to materials with certified content of the main component. As in classical methods, where small corrections for interferences are accepted, in PDM, many small corrections are bundled. In contrast to classical methods, the PDM is universally applicable to all elements in principle. Both approaches can be used to certify the purity (expressed as mass fraction of the main element) of a high-purity material. This is where the metrological need of National Metrology Institutes (NMIs) for analytical methods meet the challenges of analytical methods. In terms of methods, glow discharge mass spectrometry (GMDS) with sufficient uncertainties for sufficiently small impurity contents is particularly noteworthy for the certification of primary transfer standards (PTS), and isotope dilution mass spectrometry (IDMS), which particularly benefits from PTS (back-spikes) with small uncertainties, is particularly noteworthy for the application. The corresponding relative uncertainty which can be achieved using the PDM is very low (< 10−4). Acting as PTS, they represent the link between the material aspect of the primary calibration solutions and the immaterial world of the International System of Units (SI). The underlying concepts are discussed, the current status of implementation is summarised, and a roadmap of the necessary future activities in inorganic analytical chemistry is sketched. It has to be noted that smaller measurement uncertainties of the purity of high-purity materials not only have a positive effect on chemical measurements, but also trigger new developments and findings in other disciplines such as thermometry or materials science. KW - Inorganic chemical analysis KW - Primary transfer standards (PTSs) KW - Traceability KW - Classical primary measurement method (CPM) KW - Primary difference measurement method (PDM) KW - Metrology in chemistry PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572743 DO - https://doi.org/10.1007/s00216-023-04660-4 SN - 1618-2642 SN - 1618-2650 VL - 415 SP - 3057 EP - 3071 PB - Springer CY - Berlin AN - OPUS4-57274 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -