TY - CONF A1 - Vogl, Jochen T1 - CCQM-P149 Statistical evaluation of results N2 - The results for CCQM-P149 "Purity Determination of high purity zinc" are displayed and three different statistical approaches for the calculation of the reference value are compared. T2 - CCQM IAWG Meeting CY - Paris, France DA - 24.04.2017 KW - Purity KW - Metrology KW - Comparison KW - Impurities PY - 2017 AN - OPUS4-40033 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Roadmap for the purity determination of pure metallic elements N2 - High purity materials can serve as a realisation of the Système International d’Unitès (SI) unit amount of substance for the specific element. Solutions prepared from such high purity materials using gravimetric preparation and the concept of molar mass are used as calibration solutions in many fields of analytical chemistry. Calibration solutions prepared this way provide the traceability to the SI and are the metrological basis in elemental analysis. The preparation and characterization of such primary pure substances, representing the realisation of the SI unit amount of substance, is undertaken only by a small number of National Metrology Institutes (NMI) and Designated Institutes (DI). Many other NMIs and DIs, however, prepare elemental calibration solutions as calibrants for their measurement services, such as the certification of matrix Reference Materials or the provision of reference values for Proficiency Testing schemes. The elemental calibration solutions used for this purpose are not a direct service to customers, such as preparing secondary calibration solutions, but provide the source of traceability for the other services. Hence, it is necessary for the NMI or DI to obtain data on the purity of the pure metals or other materials used to prepare the solutions with measurement uncertainties meeting the needs of the above described services. This is commonly undertaken as a “fit for purpose” assessment, appropriate for the uncertainty requirement of the service provided to customers. As a consequence, total purity measurements are a long-term strategy of CCQM-IAWG. Several studies were conducted (CCQM-P107, CCQM-K72 and CCQM-P149) on the measurement of the purity of zinc. From these studies, several conclusions can be drawn for the purity assessment of a pure (metallic) element. These conclusions will be put together in this document in order to assist all NMIs/DIs in performing a purity assessment, whenever needed. T2 - CCQM IAWG Meeting CY - Paris, France DA - 24.04.2017 KW - CCQM KW - Metrology KW - Purity assessment PY - 2017 AN - OPUS4-40034 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Vogl, Jochen A1 - Becker, Dorit A1 - Koenig, Maren A1 - Yim, Y.-H. A1 - Lee, K.-S. A1 - Goenaga-Infante, H. A1 - Malinowskiy, D. A1 - Hill, S. A1 - Ren, T. A1 - Wang, J. A1 - Vocke, R. D. A1 - Murphy, K. A1 - Nonose, N. A1 - Rienitz, O. A1 - Noordmann, J. T1 - Certification Report for the Isotopic Reference Materials ERM-AE142 and ERM-EB400 N2 - Lead (Pb) isotope amount ratios are commonly used in applications ranging from archaeology and forensic sciences to terrestrial and extra-terrestrial geochemistry. Despite their utility and frequency of use, only three certified isotope amount ratio reference materials are currently available for Pb: NIST SRMs 981, 982 and 983. Because SRM 981 has a natural Pb isotopic composition, it is mainly used for correcting instrumental mass discrimination or fractionation. This means that, at present, there are no other certified isotope reference materials with natural Pb isotopic composition that could be used for validating or verifying an analytical procedure involving the measurement of Pb isotope amount ratios. To fill this gap, two new reference materials, both certified for their Pb isotopic composition, have been produced together with a complete uncertainty assessment. These new reference materials offer SI traceability and an independent means of validating or verifying analytical procedures used to produce Pb isotope amount ratio measurements. ERM-EB400 is a bronze material containing a nominal Pb mass fraction of 45 mg/kg. ERM-AE142 is a high purity solution of Pb with a nominal mass fraction of 100 mg/kg. Both materials have been specifically produced to assist analysts in verifying or validating their analytical procedures. Note that while one of these reference materials requires the chemical separation of Pb from its matrix (ERM-EB400), the other does not (ERM-AE142). Details on the certification of these isotope reference materials are provided in this report. KW - Lead isotopic composition KW - Isotope ratio KW - Reference material KW - Mass spectrometry PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-392060 SP - 1 EP - 16 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-39206 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tütken, T. A1 - Tatzel, Michael A1 - Vogl, Jochen A1 - Rosner, M. T1 - Assessing δ26Mg in bioapatite as proxy for faunivory N2 - Knowledge about feeding behavior is essential to determine trophic interactions and reconstruct predator-prey relationships in modern and past foodwebs. Traditionally, nitrogen isotopes (δ15N) of collagen are used to quantify the ingestion of animal protein, however collagen usually does not preserve over geological time scales. To infer the diet of extinct vertebrates from fossil material more resistant dietary proxies such as Ca and Mg isotopes are needed, which are major elements in the bioapatite of bones and teeth. Magnesium is a bio-essential element that replaces calcium in the bioapatite lattice and bone and enamel δ26Mg values of extant mammals increase systematically along the foodchain [1, 2]. The existing δ26Mg data, however, is scarce, in particular with respect to carnivores, thus still limiting the capability of this dietary proxy to reliably determine trophic differences between plant- and animal-feeders. To better constrain trophic-level effects recorded in Mg isotopes, we analyzed δ26Mg of bioapatite from modern mammals with a focus on faunivores, both carnivores and as yet unexplored insectivores. The trophic level effect of δ26Mg is influenced by the geological substrate which causes isotope variability in δ26Mg of faunal remains between different ecosystems [1, 2]. Therefore, as first-order proxy for sample provenance and to assess potential influences of the bedrock substrate of the animals´ habitats on δ26Mg of bones and teeth, we measured the 87Sr/86Sr on the same specimens. This information will enable us to refine trophic level effects and determine whether δ26Mg can be used to distinguish different faunivores isotopically. This will be of paramount importance for dietary reconstructions of trophic niches in fossil foodwebs. [1] Martin et al. (2014) Geochmica Cosmochimica Acta 130, 12-20. [2] Martin et al. (2015) Proceedings of the National Academy of Sciences 112, 430-435. T2 - Goldschmidt CY - Paris, France DA - 13.08.2017 KW - Magnesium stable isotopes KW - Isotope fractionation KW - Trophic level KW - 87Sr/86Sr KW - Provenance PY - 2017 AN - OPUS4-41535 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Paz, B. A1 - Meyer, H.-P. A1 - Varychev, A. A1 - Rosner, M. A1 - Vogl, Jochen A1 - Behrendt, S. ED - Treister, M. ED - Yablonsky, L. T1 - Археометрические исследования стеклянных сосудов из погребений ранних кочевников Южного Приуралья T1 - Archäometrische Untersuchungen an achaimenidischen Glasgefäßen aus den Gräbern der frühen Nomaden des südlichen Urals N2 - Die untersuchten Gläser lassen sich in drei Gruppen einteilen. Die beiden Fragmente aus der Nekropole von Pjatimary deuten auf eine frühe Herstellungszeit hin und lassen sich mit eisenzeitlichen Fragmenten iranischer Herkunft vergleichen. Die Glasfunde aus der Nekropole Filippovka bestehen aus völlig unterschiedlichen Glasmaterialien und müssen einer späteren Herstellungszeit zugeordnet werden. Sowohl die unterschiedlichen Rezepturen als auch der definitive Hinweis auf verschiedene Rohstoffquellen zur Herstellung der untersuchten Gläser, lassen ein breitgefächertes Netz von weitreichenden Handelsbeziehungen erkennen. KW - Archäometrie KW - Isotopenverhältnisse Strontium und Blei KW - Elementanalyse KW - Massenspektrometrie KW - Herkunft PY - 2012 SN - 978-5-903011-85-8 VL - 1 SP - 262 EP - 267 PB - TAUS CY - Moskau AN - OPUS4-26899 LA - rus AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völling, E. A1 - Reifarth, N. A1 - Vogl, Jochen ED - Nosch, M.-L. ED - Laffineur, R. T1 - The intercultural context of treasure A in Troy - Jewellery and textiles N2 - At the end of May 1873, Heinrich Schliemann recovered Treasure A in Troy. He brought all the metal artifacts illegally to Athens and published his iscoveries one year later. Then he bequeathed the Trojan finds to Berlin where from 1881 onwards, Treasure A was exhibited in the Museum of Arts and Crafts (later Gropius Bau). Hubert. Schmidt inventoried and catalogued the Trojan remains in 1902 without the so-called “Dubletten” (duplicates). The transfer of the Treasure trove in 1945 to former Leningrad (St. Petersburg) and Moscow is well known, but there was a partial restoration of the looted art from the former Soviet Union back to the former GDR: eight out of eleven silver vessels of Treasure A came via Leipzig in 1979 finally back to Berlin’s Museum für Vor- und Frühgeschichte, Stiftung Preussischer Kulturbesitz in 1994. During its safe keeping in Leningrad and Leipzig, these silver jars remained ignored in the boxes in which they were transported, a Situation, which today permits them to be investigated almost in their condition of discovery. The study of the Originals allowed Information to be gleaned about their manufacture and offered opportunities for various analyses. After the gold jewellery came to light, technical data and an archaeological appraisal of the Trojan gold kept in the Pushkin Museum of Fine Arts in Moscow could be published in 1996. The considerable quantity of the outstanding gold artifacts of Treasure A was deposited inside the great silver vessel Sch 5873 and listed by Heinrich Schliemann. T2 - 13th International Aegean Conference CY - Copenhagen, Denmark DA - 21.04.2010 PY - 2012 SN - 978-90-429-2665-3 SP - 531 EP - 538 PB - Peeters Publishers CY - Liège, Belgium AN - OPUS4-26408 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Calibration of Mg isotope amount ratios and delta values N2 - In the past, δ26/24Mg measurements were referenced to NIST SRM 980, the initial zero of the δ26/24Mg scale. With the development of MC-ICPMS, the detection of small but measurable isotopic differences in different chips of SRM 980 became apparent. To solve this problem a suite of magnesium isotope reference materials, ERM-AE143, -AE144 and -AE145, has been certified in a first study by applying an ab initio calibration for absolute Mg isotope ratios without any a priori assumptions, a procedure which fulfils all requirements of a primary method of measurement. We could achieve for the first time measurement uncertainties for isotope amount ratios close to the typical precision of magnesium delta values, δ26/24Mg, which are at the 0.1 ‰ level (2SD). In addition, it was demonstrated that commonly used fractionation laws are invalid for correcting Mg isotope ratios in multi-collector ICPMS as they result in a bias which is not covered by its associated uncertainty. Depending on their type, fractionation laws create a bias up to several per mil, with the exponential law showing the smallest bias between 0.1 ‰ to 0.7 ‰. With these isotope reference materials, it is possible to establish SI-traceability for magnesium delta measurements. To realize this, we organized a second study within which five expert laboratories participated to cross-calibrate all available magnesium isotope standards, which are NIST SRM 980, IRMM-009, ERM-AE143, ERM-AE144, ERM-AE145 and the standards DSM3 and Cambridge-1. The mean δ26/24Mg values for the individual iRMs, calculated from the laboratory means show 2 SD reproducibilities varying between 0.025 and 0.093 ‰. Propagated measurement uncertainties suggest a standard uncertainty of about 0.1‰ for δ26/24Mg determinations (2SD). Thus, SI traceability for magnesium isotope amount ratios and delta values is demonstrated to be established. T2 - 53rd annual conference of the DGMS including 27th ICP-MS User's Meeting CY - Münster, Germany DA - 01.03.2020 KW - Isotope ratio KW - Delta value KW - Metrology KW - Magnesium KW - Magnesium isotope ratios PY - 2020 N1 - Geburtsname von Mieller, Björn: Brandt, B. - Birth name of Mieller, Björn: Brandt, B. AN - OPUS4-50549 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Cu project on calibration approaches for absolute isotope ratios N2 - This presentations summarizes the difficulties in the purification of enriched copper isotopes by high vacuum subimation. It shows as well thelimitations for a CCQM key comparison on this topic. T2 - CCQM Isotope Ratio Work Group Meeting CY - Bern, Switzerland DA - 09.10.2019 KW - Absolute isotope ratio KW - Isotope purification KW - Metal sublimation KW - Gravimtric isotope mixtures PY - 2019 AN - OPUS4-49518 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Realization of SI traceability for Mg isotope amount ratios & delta values N2 - In isotope ratio applications metrological principles such as measurement uncertainty and SI traceability often are not considered or realized. This is also well-documented by the traceability exception related to delta scale isotope ratio measurements CCQM requested from the CIPM. Generally, delta scale isotope ratio measurements can be performed on a precision level that is significantly lower than the uncertainty level of isotope amount ratio measurements. In the case of magnesium, we demonstrated for the first time that isotope amount ratios can be measured with uncertainties close to the typical precision of magnesium delta values, δ26/24Mg, which are at the 0.1 ‰ level. In the past, δ26/24Mg measurements were referenced to NIST SRM 980, the initial zero of the δ26/24Mg scale. With the development of MC-ICPMS, the detection of small but measurable isotopic differences in different chips of NIST SRM 980 became apparent and NIST SRM 980 was replaced by an intermediate artefact, DSM3. To solve this problem a suite of magnesium isotope reference materials, ERM-AE143, -AE144, and -AE145, has been certified in a first study by applying an ab initio calibration for absolute Mg isotope ratios without any a priori assumptions, a procedure which fulfils all requirements of a primary method of measurement. Thus, these materials qualified to establish SI-traceability for magnesium delta measurements. In a second study five expert laboratories participated to cross-calibrate all available magnesium isotope standards, which are NIST SRM 980, IRMM-009, ERM-AE143, ERM-AE144, ERM-AE145 and the standards DSM3 and Cambridge-1. The mean δ26/24Mg values for the individual iRMs, calculated from the laboratory means show 2 SD reproducibilities varying between 0.025 and 0.093 ‰. Propagated measurement uncertainties suggest a standard uncertainty of about 0.1 ‰ for δ26/24Mg determinations. Thus, SI traceability for magnesium isotope amount ratios and delta values is demonstrated to be established. T2 - CCQM Workshop on "Advances in Metrology in Chemistry and Biology" CY - Sèvres, France DA - 09.04.2019 KW - Delta values KW - SI traceability KW - Isotope amount ratio KW - Magnesium PY - 2019 N1 - Geburtsname von Mieller, Björn: Brandt, B. - Birth name of Mieller, Björn: Brandt, B. AN - OPUS4-47930 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Isotope ratios and delta values with minimal measurement uncertainties -measuring magnesium using MC-ICP-MS N2 - Multi-collector inductively coupled plasma-mass spectrometry (MC-ICP-MS) has evolved significantly since its introduction in 1992. The second and third generation instruments now allow isotope ratio measurements at unprecedented precisions, 0.001 % or better. However, precision alone is not enough for producing accurate and reliable isotope ratio measurements. Metrological considerations such as the selection of suitable calibration strategies, proper assessment of instrumental biases, and the estimation of overall measurement uncertainty remain critical to the measurement process. Properly assessed, measurement uncertainty then provides the interval within which a result can be considered both accurate and precise. All mass spectrometric measurements are affected by instrumental mass discrimination and produce isotope ratios that are biased relative to their “true” ratio. To produce accurate and traceable isotope ratio measurements, it is imperative that certified isotope reference materials (iCRMs) be used for calibration and validation purposes. iCRMs reporting absolute isotope ratios are an analyst’s first choice, particularly when its uncertainty is sufficient for the intended use. However, when smaller uncertainties are required to resolve subtle differences between samples, delta-scale measurements become important. Here, the difference between an isotope ratio measured in a sample and in an internationally accepted isotope reference material (iRM) is determined. This deviation can be positive or negative relative to the iRM, is called a delta value, and is often expressed in per mil units. This presentation will highlight the potential for MC-ICP-MS to produce isotope ratio measurements with minimal uncertainties by examining three applications involving Mg isotopes: 1) the certification of a set of iCRMs for their absolute isotope ratio using a gravimetric isotope mixture approach; 2) the comparison of these iCRMs with currently accepted Mg delta-scale reference materials through intercalibration, and 3) the determination of isotope fractionation exponents for geochemical applications. T2 - 4th International Conference on Frontiers in Mass Spectrometry CY - Kottayam, Kerala, India DA - 04.12.2019 KW - Triple isotope fractionation KW - Absolute isotope ratio KW - Delta value KW - Mangesium PY - 2019 N1 - Geburtsname von Mieller, Björn: Brandt, B. - Birth name of Mieller, Björn: Brandt, B. AN - OPUS4-50004 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -