TY - JOUR A1 - Recknagel, Sebastian T1 - Certified reference material for the determination of hydrolytic resistance of borosilicate glass N2 - The preparation, analysis and certification of a new certified glass reference material (CRM) for the determination of hydrolytic resistance of borosilicate glass with the glass grains test is described. The CRM BAM-S053 is available in the form of glass rods (length: 185 mm, diameter: 9 mm, weight: 27·5 g). Certified properties are the acid consumption determined according to the procedures described in ISO 720, USP<660>, Ph.Eur. 3.2.1, data obtained following the procedure of ISO 719 was scattering too widely. The certified values are based on the results of 15 laboratories which participated in the certification interlaboratory comparison. The CRM is intended for the quality control when applying ISO 720, USP<660>, Ph.Eur. 3.2.1 and with limitations ISO 719. KW - CRM KW - Hydrolytic resistance KW - Borosilicate glass PY - 2021 DO - https://doi.org/10.13036/17533562.62.1.001 VL - 62 IS - 1 SP - 25 EP - 27 AN - OPUS4-52195 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - Certified reference material for the determination of hydrolytic resistance of borosilicate glass N2 - The preparation of certified reference material for the determination of hydrolytic resistance of borosilicate glass is described. Certified properties are the acid consumption according to the relevant standard procedures described in ISO 720, USP<660> and Ph.Eur. 3.2.1. T2 - PharmaGlass Workshop CY - Sheffield, UK DA - 09.10.2019 KW - CRM KW - Hydrolytic resistance KW - Borosilicate glass PY - 2019 AN - OPUS4-49466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian A1 - Scharf, Holger A1 - Lkhagvasuren, B. A1 - Oyuntungalag, U. A1 - Rausch, J. T1 - Certified reference material for determination of total cyanide in soil [BAM-U116/CGL306] N2 - CRM (Certified Reference Material) BAM-U116/CGL306 “Cyanide in soil” was produced within a framework of cooperation between CGL (Central Geological Laboratory) of Mongolia and Federal Institute for Materials Research and Testing (BAM) of Germany in 2013-2017. The CRM BAM-U116/CGL306 represents a mixture of a sandy soil collected from a contaminated former gasworks area in the Berlin region (Germany) and an unpolluted sandy soil from Nalaikh region (Mongolia). The bulk candidate material for this reference material was prepared at CGL CRM Laboratory exclusively destined to the preparation of reference materials and equipped with modern technical equipment. Homogeneity, stability and shelf life were studied in full compliance with ISO Guide 35. The CRM was evaluated as sufficiently homogeneous. Statistical evaluation of certification analysis was software packages SoftCRM and ProLab Plus. Certified value of total cyanide of the CRM is 12.0 mg/kg and expanded uncertainty was assigned as 0.8 mg/kg. The intended purpose of this material is the verification of analytical results obtained for the mass fraction of total cyanide in soils and soil-like materials applying the standardized procedure ISO 11262:2011. As any reference material, it can also be used for routine performance checks (quality control charts) or validation studies. KW - CRM KW - Cyanide in soil KW - Total cyanide PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-469694 DO - https://doi.org/10.17265/2162-5263/2018.04.004 SP - 149 EP - 161 PB - David Publishing AN - OPUS4-46969 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauli, Jutta A1 - Güttler, Arne A1 - Schneider, Thomas A1 - Würth, Christian A1 - Resch-Genger, Ute T1 - Certified Fluorescence Quantum Yield Standards as New Optical Reference Materials N2 - Luminescence techniques are amongst the most commonly used analytical methods in life and material sciences due to their sensitivity and their nondestructive and multiparametric character. Photoluminescence signals are, however, affected by wavelength, polarization and time dependent instrument specific effects, and provide only relative intensities. This hampers the comparability of fluorescence measure-ments and calls for simple tools for instrument characterization and the quantification of measured fluorescence intensities. Well characterized fluorescence standards for instrument calibration and performance validation (IPV) can be used as references for fluorescence signals. Of special importance is the correct determination of photoluminescence quantum yields (QF) (number of emitted per absorbed photons) that provides a direct comparison of the fluorescence efficiency of emitters. Such well characterized standards have been successfully developed by BAM for the relative determination of f values of transparent solutions of molecular and nanoscale emitters in the wavelength range from 350 and 1100 nm and will be soon certified. These standards can also be used to evaluate integrating sphere setups, which are increasingly being used for absolute measurements of QF values. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2091 KW - Fluoreszenz KW - Referenzmaterial PY - 2019 AN - OPUS4-47795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Isleyen, Alper A1 - Can, Suleyman Z. A1 - Cankur, Oktay A1 - Tunc, Murat A1 - Vogl, Jochen A1 - Koenig, Maren A1 - Horvat, Milena A1 - Jacimovic, Radojko A1 - Zuliani, Tea A1 - Fajon, Vesna A1 - Jotanovic, Aida A1 - Gaževic, Luka A1 - Milosevic, Milena A1 - Ochsenkuehn–Petropoulou, Maria A1 - Tsopelas, Fotis A1 - Lymberopoulou, Theopisti A1 - Tsakanika, Lamprini-Areti A1 - Serifi, Olga A1 - Ochsenkuehn, Klaus M. A1 - Bulska, Ewa A1 - Tomiak, Anna A1 - Kurek, Eliza A1 - Cakılbahçe, Zehra A1 - Aktas, Gokhan A1 - Altuntas, Hatice A1 - Basaran, Elif A1 - Kısacık, Barıs A1 - Gumus, Zeynep T1 - Certification of the total element mass fractions in UME EnvCRM 03 soil sample via a joint research project N2 - Soil certified reference material (CRM), UME EnvCRM 03 was produced by a collaborative approach among national metrology institutes, designated institutes and university research laboratories within the scope of the EMPIR project: Matrix Reference Materials for Environmental Analysis. This paper presents the sampling and processing methodology, homogeneity, stability, characterization campaign, the assignment of property values and their associated uncertainties in compliance with ISO 17034:2016. The material processing methodology involves blending a natural soil sample with a contaminated soil sample obtained by spiking elemental solutions for 8 elements (Cd, Co, Cu, Hg, Ni, Pb, Sb and Zn) to reach the level of warning risk monitoring values specified for metals and metalloids of soils in Europe. Comparative homogeneity and stability test data were obtained by two different institutes, ensuring the reliability and back up of the data. The certified values and associated expanded uncertainties for the total mass fractions of thirteen elements (As, Cd, Co, Cr, Cu, Fe, Hg, Mn, Ni, Pb, Sb, V and Zn) are established. The developed CRM can be used for the development and validation of measurement procedures for the determination of the total mass fractions of elements in soil and also for quality control/assurance purposes. The developed CRM is the first example of a soil material originating from Türkiye. KW - Total element content KW - Soil KW - CRM KW - Certification KW - Environmental pollution monitoring PY - 2024 DO - https://doi.org/10.1007/s00769-024-01597-8 SN - 1432-0517 SP - 1 EP - 9 PB - Springer Science and Business Media LLC AN - OPUS4-59954 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Hans-Joachim A1 - Richter, Silke A1 - Recknagel, Sebastian T1 - Certification of the mass fractions of trace elements in a medium purity graphite reference material N2 - The increasing application of graphite materials in various fields of technology and science enhances the demand for strictly controlled properties which are often directly correlated to the contents of trace element impurities. Therefore, the availability of powerful, rapid and reliable analytical methods for the determination of trace impurities is essential for process and quality control. Certified reference materials, indispensable for the development and validation of appropriate trace analytical methods for the characterization of special purity graphite materials are still lacking. Therefore, BAM in co-operation with the working group “Special Materials” of the committee of chemists of GDMB (Gesellschaft der Metallurgen und Bergleute e.V.) certified an industrially sourced graphite material with genuine elemental impurities. The candidate material was a commercial product (NBG 18) taken from the customary production line of the producer SGL CARBON, Chedde (France). The homogeneity of the powdered material was assessed by means of ETV-ICP OES and DC Arc-OES. Certification of the candidate reference material was based on an inter-laboratory comparison involving 17 expert laboratories from Germany, France, Slovenia, USA, South Africa. A variety of different mineralization, digestion, leaching, fusion and combustion techniques prior to ICP OES and photometry, methods without sample preparation (INAA, k0-INAA) as well as typical solid sampling methods (ETV-ICP OES, ETV-ICP-MS, SS-ET AAS, DC Arc-OES, MF-DC Arc-OES) were used to characterise the material. Certified mass fractions and their expanded uncertainties (k = 2) were assigned for 27 elements (Al, B, Ba, Be, Ca, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, S, Si, Sr, Ti, V, W, Y, Zn, Zr), ranging from (0.00050 ± 0.00027) mg/kg for Be to (41 ± 6) mg/kg for Si. Additionally, informative values are given for the: trace element contents of Ag, As, Au, Bi, Cd, Cs, Dy, Eu, Ga, Gd, Hg, In, La, Nb, Rb, Re, Rh, Sb, Sc, Se, Sm, Sn, Ta, Tb, Te, Th, U; method specific values obtained by ETV-ICP OES (BETV and SiETV) and the ash content of the material. The certified material “BAM-S009 Medium Purity Graphite Powder” is available for purchase from BAM. T2 - ESAS & CANAS 2018 CY - Berlin, Germany DA - 20.03.2018 KW - Graphite KW - Certification KW - Trace elements KW - Reference material PY - 2018 AN - OPUS4-44775 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Hans-Joachim A1 - Richter, Silke A1 - Recknagel, Sebastian T1 - Certification of the mass fractions of trace elements in a medium purity graphite reference material N2 - The increasing application of graphite materials in various fields of technology and science enhances the demand for strictly controlled properties which are often directly correlated to the contents of trace element impurities. Therefore, the availability of powerful, rapid and reliable analytical methods for the determination of trace impurities is essential for process and quality control. Certified reference materials, indispensable for the development and validation of appropriate trace analytical methods for the characterization of special purity graphite materials are still lacking. Therefore, BAM in co-operation with the working group “Special Materials” of the committee of chemists of GDMB (Gesellschaft der Metallurgen und Bergleute e.V.) certified an industrially sourced graphite material with genuine elemental impurities. The candidate material was a commercial product (NBG 18) taken from the customary production line of the producer SGL CARBON, Chedde (France). The homogeneity of the powdered material was assessed by means of ETV-ICP OES and DC Arc-OES. Certification of the candidate reference material was based on an inter-laboratory comparison involving 17 expert laboratories from Germany, France, Slovenia, USA, South Africa. A variety of different mineralization, digestion, leaching, fusion and combustion techniques prior to ICP OES and photometry, methods without sample preparation (INAA, k0-INAA) as well as typical solid sampling methods (ETV-ICP OES, ETV-ICP-MS, SS-ET AAS, DC Arc-OES, MF-DC Arc-OES) were used to characterise the material. Certified mass fractions and their expanded uncertainties (k = 2) were assigned for 27 elements (Al, B, Ba, Be, Ca, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, S, Si, Sr, Ti, V, W, Y, Zn, Zr), ranging from (0.00050 ± 0.00027) mg/kg for Be to (41 ± 6) mg/kg for Si. Informative values are given for further parameters: trace element contents of Ag, As, Au, Bi, Cd, Cs, Dy, Eu, Ga, Gd, Hg, In, La, Nb, Rb, Re, Rh, Sb, Sc, Se, Sm, Sn, Ta, Tb, Te, Th, U; method specific values obtained by ETV-ICP OES (BETV and SiETV) and ash content. The new certified material is available as BAM Reference Material BAM-S009 Medium Purity Graphite Powder. T2 - BERM-15 CY - Berlin, Germany DA - 23.09.2018 KW - Certification KW - Graphite KW - Reference material KW - Trace elements PY - 2018 AN - OPUS4-46235 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen A1 - Yim, Y.-H. A1 - Lee, K.-S. A1 - Goenaga-Infante, H A1 - Malinovskiy, D. A1 - Hill, S. A1 - Ren, T. A1 - Wang, J. A1 - Vocke, R. D. A1 - Murphy, K. E. A1 - Nonose, N. A1 - Rienitz, O. A1 - Noordmann, J. T1 - Certification of ERM-EB400, the first matrix reference material for lead isotope amount ratios, and ERM-AE142, a lead solution providing a lead isotopic composition at the edge of natural variation N2 - Lead isotope amount ratios are commonly used in diverse fields such as archaeometry, geochemistry and forensic science. Currently, five reference materials with certified lead isotope amount ratios are available, namely NIST SRM 981, 982 and 983, GBW-04442 and NMIJ 3681-a. Only NIST SRM 981 and NMIJ 3681-a have approximately natural isotopic compositions, and NIST SRM 981 is predominantly used for correcting mass discrimination/mass fractionation in the applied mass spectrometric procedures. Consequently, there is no other certified reference material available to be used for validation and/or quality control of the analytical procedures applied to lead isotope amount ratio measurements. To fill this gap, two new reference materials have been produced and certified for their lead isotope amount ratios. For both certified reference materials, complete uncertainty budgets have been calculated and SI traceability has been established. This provides the users with independent means for validating and verifying their analytical procedures and for conducting quality control measures. ERM-EB400 is a bronze material with a nominal lead mass fraction of 45 mg kg-1 and certified lead isotope amount ratios of n(206Pb)/n(204Pb) = 18.072(17) mol mol-1, n(207Pb)/n(204Pb) = 15.578(18) mol mol-1 and n(208Pb)/n(204Pb) = 38.075(46) mol mol-1 with the associated expanded uncertainties (k = 2) given in brackets. ERM-AE142 is a high-purity solution of lead in 2% nitric acid with a nominal mass fraction of 100 mg kg-1 and certified Pb isotope amount ratios of n(206Pb)/n(204Pb) = 21.114(17) mol mol-1, n(207Pb)/n(204Pb) = 15.944(17) mol mol-1 and n(208Pb)/n(204Pb) = 39.850(44) mol mol-1 with the associated expanded uncertainties (k = 2) given in brackets. Both materials are specifically designed to fall within the natural lead isotopic variation and to assist users with the validation and verification of 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). As additional information, δ208/206PbNIST SRM981 values are provided for both materials. For ERM-AE142, a delta value of δ208/206PbNIST SRM981 = -28.21(30) ‰ was obtained, and for ERM-EB400, a delta value of δ208/206PbNIST SRM981 = -129.47(38) ‰ was obtained, with the associated expanded uncertainties (k = 2) given in brackets. KW - Lead isotope variations KW - Radiogenic isotopes KW - Isotope reference material KW - Metrology in chemistry KW - Measurement uncertainty PY - 2019 DO - https://doi.org/10.1111/ggr.12253 SN - 1751-908X SN - 1639-4488 VL - 43 IS - 1 SP - 23 EP - 37 PB - John Wiley & Sons AN - OPUS4-47383 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blanchard, V. A1 - Traub, Heike A1 - Biskup, K. A1 - Wieczorek, M. A1 - Saatz, Jessica A1 - Pagel, K. T1 - Central project for biochemical analysis of proteoglycans and glycosaminoglycans and for element-specific microscopy N2 - Nearly all disease processes are associated with variations of components of the extracellular matrix (ECM) that are typically observed during the development of inflammation. This concerns for example proteoglycans and their associated glycosaminoglycans (GAG), which have been shown to bind to cationic metal imaging probes due to their strong complexing activity. The complexing activity largely depends on the degree of GAG sulfation and/or carboxylation as well as on the GAG isomericity. In this central project, we investigate GAG structures from inflammatory disorders (namely cardiovascular diseases, inflammatory intestinal diseases and neuroinflammation) provided by researchers of the Collaborative Research Center at the molecular disaccharidic level using chromatographic and mass spectrometric methods. In parallel, the spatial localization and quantification of metal-based imaging probes are evaluated by LA-ICP-MS imaging. T2 - 1st International Symposium In vivo Visualization of Extracellular Matrix Pathology CY - Online Meeting DA - 27.05.2021 KW - Laser ablation KW - ICP-MS KW - MALDI PY - 2021 AN - OPUS4-52716 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kepsutlu, B. A1 - Wycisk, V. A1 - Achazi, K. A1 - Kapishnikov, S. A1 - Perez-Berna, A.J. A1 - Guttmann, P. A1 - Cossmer, Antje A1 - Pereiro, E. A1 - Ewers, H. A1 - Ballauff, M. A1 - Schneider, G. A1 - McNally, J.G. T1 - Cells Undergo Major Changes in the Quantity of Cytoplasmic Organelles after Uptake of Gold Nanoparticles with Biologically Relevant Surface Coatings N2 - Here, we use cryo soft X-ray tomography (cryo-SXT), which delivers 3D ultrastructural volumes of intact cells without chemical fixation or staining, to gain insight about nanoparticle uptake for nanomedicine. We initially used dendritic polyglycerol sulfate (dPGS) with potential diagnostic and therapeutic applications in inflammation. Although dPGS-coated gold nanoparticle (dPGS-AuNP) uptake followed a conventional endocytic/degradative pathway in human lung epithelial cell lines (A549), with cryo-SXT, we detected ∼5% of dPGS-AuNPs in the cytoplasm, a level undetectable by confocal light microscopy. We also observed ∼5% of dPGS-AuNPs in a rarely identified subcellular site, namely, lipid droplets, which are important for cellular energy metabolism. Finally, we also found substantial changes in the quantity of cytoplasmic organelles upon dPGS-AuNP uptake over the 1–6 h incubation period; the number of small vesicles and mitochondria significantly increased, and the number of multivesicular bodies and the number and volume of lipid droplets significantly decreased. Although nearly all organelle numbers at 6 h were still significantly different from controls, most appeared to be returning to normal levels. To test for generality, we also examined cells after uptake of gold nanoparticles coated with a different agent, polyethylenimine (PEI), used for nucleic acid delivery. PEI nanoparticles did not enter lipid droplets, but they induced similar, albeit less pronounced, changes in the quantity of cytoplasmic organelles. We confirmed these changes in organelle quantities for both nanoparticle coatings by confocal fluorescence microscopy. We suggest this cytoplasmic remodeling could reflect a more common cellular response to coated gold nanoparticle uptake. KW - Cellular trafficking KW - Confocal laser scanning microscopy KW - Cytoplasmic remodeling KW - Dendritic polyglycerol sulfate KW - Polyethylenimine KW - 3D ultrastructural analysis KW - Cryo-soft X-ray tomography PY - 2020 DO - https://doi.org/10.1021/acsnano.9b09264 VL - 14 IS - 2 SP - 2248 EP - 2264 AN - OPUS4-50464 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 - Duewer, D. L. A1 - Murray, J. A. A1 - Wood, L. J. A1 - Wise, S. A. A1 - Hein, Sebastian A1 - Koch, Matthias A1 - Philipp, Rosemarie A1 - Werneburg, Martina A1 - Hackenberg, R. A1 - Polzer, J. A1 - Avila, M. A. A1 - Serrano, V. A1 - Kakoulides, E. A1 - Alexopoulos, C. A1 - Giannikopoulou, P. A1 - Gui, E. M. A1 - Lu, T. A1 - Teo, T. L. A1 - Hua, T. A1 - Dazhou, C. A1 - Chunxin, L. A1 - Changjun, Y. A1 - Hongmei, L. A1 - Nammoonnoy, J. A1 - Sander, L. C. A1 - Lippa, K. A1 - Quinn, L. A1 - Swiegelaar, C. A1 - Fernandes-Whaley, M. A1 - Gören, A. C. A1 - Gökcen, T. T1 - CCQM-K95.1 Low-polarity analytes in a botanical matrix: Polycyclic aromatic hydrocarbons (PAHs) in tea N2 - Extraction, chromatographic separation, and quantification of low-concentration organic compounds in complex matrices are core challenges for reference material producers and providers of calibration services. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims made by national metrology institutes (NMIs) and designated institutes (DIs). To enable NMIs and DIs to update or establish their claims, in 2014 the Organic Analysis Working Group (OAWG) initiated CCQM-K95.1 "Low-Polarity Analytes in a Botanical Matrix: Polycyclic Aromatic Hydrocarbons (PAHs) in Tea". This was a follow-on comparison from CCQM-K95 which was completed in 2014. The polycyclic aromatic hydrocarbons (PAHs) benz[a]anthracene (BaA) and benzo[a]pyrene (BaP) are considered priority pollutants by U.S. Environmental Protection Agency and are regulated contaminants in food, pose chromatographic separation challenges, and for which exist well-characterized measurement procedures and standard materials. BaA and BaP in a smoked tea were therefore selected as representative target measurands for CCQM-K95.1. Ten NMIs participated in CCQM-K95.1. The consensus summary mass fractions for the two PAHs are in the range of (50 to 70) ng/g with relative standard deviations of (6 to 10) %. Successful participation in CCQM K95.1 demonstrates the following measurement capabilities in determining mass fraction of organic compounds, with molar mass of 100 g/mol to 500 g/mol and having polarity pKow −2, in a botanical matrix ranging in mass fraction from 10 ng/g to 1000 ng/g: (1) value assignment of primary reference standards (if in-house purity assessment carried out), (2) value assignment of single and/or multi-component organic solutions, (3) extraction of analytes of interest from the matrix, (4) cleanup and separation of analytes of interest from interfering matrix or extract components, and (5) separation and quantification using gas chromatography or liquid chromatography. KW - Benz[a]anthracene (BaA) KW - Benzo[a]pyrene (BaP) KW - Gas chromatography (GC) KW - Isotope dilution (ID) KW - Liquid chromatography (LC) KW - Mass spectrometry (MS) KW - Polycyclic aromatic hydrocarbon (PAH) KW - Yerba mate tea PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-471430 DO - https://doi.org/10.1088/0026-1394/56/1A/08002 SN - 0026-1394 SN - 1681-7575 VL - 56 IS - 1 A SP - 08002, 1 EP - 89 PB - IOP Science AN - OPUS4-47143 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 - Li, X.M. A1 - Li, H.M. A1 - Zhang, Q.H. A1 - Lu, X.H. A1 - Li, S.Q. A1 - Koch, Matthias A1 - Polzer, J. A1 - Hackenber, R. A1 - Moniruzzaman, M. A1 - Khan, M. A1 - Kakoulides, E. A1 - Pak-Wing, K. A1 - Richy, A1 - Chi-Shing, N. A1 - Lu, T. A1 - Gui, E.M. A1 - Cheow, P.S. A1 - Teo, T.L. A1 - Rego, E. A1 - Garrido, B. A1 - Carvalho, L. A1 - Leal, R. A1 - Violante, F. A1 - Baek, S.Y. A1 - Lee, S. A1 - Choi, K. A1 - Kim, B. A1 - Bucar-Miklavcic, M. A1 - Hopley, C. A1 - Nammoonnoy, J. A1 - Murray, J. A1 - Wilson, W. A1 - Toman, B. A1 - Itoh, N. A1 - Gokcen, T. A1 - Krylov, A. A1 - Mikheeva, A. T1 - CCQM-K146 low-polarity analyte in high fat food: benzo a pyrene in olive oil N2 - The demonstration of competency and equivalence for the assessment of levels of contaminants and nutrients in primary foodstuffs is a priority within the 10-year strategy for the OAWG Track A core comparisons. The measurements are core challenges for reference material producers and providers of calibration Services. This key comparison related to low polarity analytes in a high fat, low protein, low carbohydrate food matrix and Benzo[a]pyrene in edible oil was the model System selected to align with this class within the OAWG strategy. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims (CMCs) made by national metrology institutes (NMIs) and designated institutes (Dis). 16 National Metrology Institutions participated in the Track A Key Comparison CCQM-K146 Low-Polarity Analyte in high fat food: Benzo[a]pyrene in Olive Oil. Participants were requested to evaluate the mass fractions, expressed in µg/kg, of Benzo[a]pyrene in the olive oil material. The KCRV was determined from the results of all NMIs/DIs participating in the key comparison that used appropriately validated methods with demonstrated metrological traceability. Different methods such as liquid-liquid extraction, GPC and SPE were applied in the sample pretreatment and HPLC-FLD, HPLC-MS/MS, and GC-MS or GC-MS/MS were applied for detection by the participants. The mass fractions for BaP were in the range of (1.78 to 3.09) µg/kg with Standard uncertainties of (0.026 to 0.54) µg/kg, with corresponding relative Standard uncertainties from 0.9% to 21%. Five labs withdrew their result from the Statistical evaluation of the KCRV for technical reasons. One lab was excluded from the KCRV evaluation, as they did not meet the CIPM metrological traceability requirements. A Hierarchical Bayes option was selected for the KCRV value, which was determined as 2.74 µg/kg with a Standard uncertainty of 0.03 µg/kg. The 10 institutes those were included in the calculation of the consensus KCRV all agreed within their Standard uncertainties. Successful participation in CCQM-K146 demonstrates the measurement capabilities in determining mass fraction of organic compounds, with molecular mass of 100 g/mol to 500 g/mol, having low polarity pKow < -2, in mass fraction range from 0.1 µg/kg to 1000 µg/kg in a high fat, low protein, low carbohydrate food matrix. KW - Metrology KW - CCQM KW - Food KW - PAH PY - 2020 DO - https://doi.org/10.1088/0026-1394/57/1a/08017 VL - 57 IS - 1a SP - 08017 AN - OPUS4-52435 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 - JOUR A1 - Duewer, D. L. A1 - Sander, L. C. A1 - Wise, S. A. A1 - Philipp, Rosemarie A1 - Hein, Sebastian A1 - Hackenberg, R. A1 - Polzer, J. A1 - Avila, M. A. A1 - Serrano, V. A1 - Kakoulides, E. A1 - Alexopoulos, C. A1 - Giannikopoulou, P. A1 - Chan, P. A1 - Lee, H. A1 - Tang, H. A1 - Tang, P. A1 - Yip, Y. A1 - Lu, T. A1 - Cheow, P. S. A1 - Teo, T. L. A1 - Sega, M. A1 - Rolle, F. A1 - Baek, S. A1 - Kim, B. A1 - Lee, S. A1 - Cabillic, J. A1 - Fallot, C. A1 - Hua, T. A1 - Dazhou, C. A1 - Changjun, Y. A1 - Chunxin, L. A1 - Hongmei, L. A1 - Lippa, K. A1 - Itoh, N. A1 - Quinn, L. A1 - Prevoo-Franzsen, D. A1 - Fernandes-Whaley, M. A1 - Gören, A. C. A1 - Gökcen, T. A1 - Gündüz, S. A1 - Krylov, A. A1 - Mikheeva, A. A1 - Baldan, A. A1 - van der Hout, J. W. A1 - van der Veen, A. M. H. T1 - CCQM-K131 Low-polarity analytes in a multicomponent organic solution: Polycyclic aromatic hydrocarbons (PAHs) in acetonitrile N2 - Solutions of organic analytes of known mass fraction are typically used to calibrate the measurement processes used to determine these compounds in matrix samples. Appropriate value assignments and uncertainty calculations for calibration solutions are critical for accurate measurements. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims (CMCs) made by national metrology institutes (NMIs) and designated institutes (DIs). To enable NMIs and DIs to update or establish their claims, in 2015 the Organic Analysis Working Group (OAWG) sponsored CCQM-K131 "Low-Polarity Analytes in a Multicomponent Organic Solution: Polycyclic Aromatic Hydrocarbons (PAHs) in Acetonitrile". Polycyclic aromatic hydrocarbons (PAHs) result from combustion sources and are ubiquitous in environmental samples. The PAH congeners, benz[a]anthracene (BaA), benzo[a]pyrene (BaP), and naphthalene (Nap) were selected as the target analytes for CCQM-K131. These targets span the volatility range of PAHs found in environmental samples and include potentially problematic chromatographic separations. Nineteen NMIs participated in CCQM-K131. The consensus summary mass fractions for the three PAHs are in the range of (5 to 25) μg/g with relative standard deviations of (2.5 to 3.5) %. Successful participation in CCQM-K131 demonstrates the following measurement capabilities in determining mass fraction of organic compounds of moderate to insignificant volatility, molar mass of 100 g/mol up to 500 g/mol, and polarity pKow < −2 in a multicomponent organic solution ranging in mass fraction from 100 ng/g to 100 μg/g: (1) value assignment of primary reference standards (if in-house purity assessment carried out), (2) value assignment of single and/or multi-component organic solutions, and (3) separation and quantification using gas chromatography or liquid chromatography. KW - Benz[a]anthracene (BaA) KW - Benzo[a]pyrene (BaP) KW - Gas chromatography (GC) KW - Isotope dilution (ID) KW - Liquid chromatography (LC) KW - Mass spectrometry (MS) KW - Naphthalene (Nap) KW - Organic calibration solution KW - Polycyclic aromatic hydrocarbon (PAH) PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-471442 DO - https://doi.org/10.1088/0026-1394/56/1A/08003 SN - 0026-1394 SN - 1681-7575 VL - 56 IS - 1A SP - 08003, 1 EP - 102 PB - IOP Science AN - OPUS4-47144 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 - Li, X.Q. A1 - Li, H.M. A1 - Jiao, H. A1 - Guo, Z.H. A1 - Zhang, Q.H. A1 - Kneeteman, L.E. A1 - Lewin, M. A1 - Pires do Rego, E.C. A1 - Leal, R.V. A1 - Violante, F.G.M. A1 - Riedel, Juliane A1 - Koch, Matthias T1 - CCQM Key Comparison track A CCQM-K168: Non-polar analytes in high carbohydrate food matrix: trans-zearalenone in maize powder N2 - Demonstrating competency and equivalence for the measurement capacity of contaminants and nutrients in primary foodstuffs is a priority of the OAWG 10-year strategy for Track A core comparisons. Such measurements have posed significant challenges for reference material producers and calibration service providers. This key comparison (KC), under the topic of “non- polar analyte in high carbohydrate food matrix: trans-Zearalenone (trans-ZEN) in maize powder” , was a sector of the model system selected to align with this class within the OAWG strategy. Evidence of successful participation in formal, relevant international comparisons is needed to demonstrate the Calibration and Measurement Capabilities (CMCs) of national metrology institutes (NMIs) and designated institutes (DIs). 17 NMIs and DIs participated in the Track A KC CCQM- 168 “non-polar analyte in high carbohydrate food matrix: trans-ZEN in maize powder” . Participants were requested to evaluate the mass fraction (μg/kg) of trans-ZEN in maize powder material. Methods like liquid-liquid extraction and SPE were applied in the pre-treatment, and HPLC-MS/MS and HPLC-FLD were used for detection by the participants. The mass fractions for trans-ZEN were in the range of (91.8 to 169) μg/kg with standard uncertainties of (1.5 to 24.7) μg/kg, and corresponding relative standard uncertainties from 1.5% to 14.6%. Two labs, INTI and BAM were excluded from the KCRV evaluation. INTI result was identified as an outlier and confirmed their method had insufficient specificity. For BAM the calibration approach they used does not meet the CIPM traceability requirements. The other 15 labs included in the calculation of the consensus KCRV all agreed within their standard uncertainties. Hierarchical Bayes was used as estimators in calculating KCRV and standard uncertainty. Successful participation in CCQM-K168 demonstrates the measurement capabilities in determining mass fraction of organic compounds, with molecular mass of 100 g/mol to 500 g/mol, having low polarity pKow < -2, in mass fraction range from 1 μg/kg to 1000 μg/kg in a high carbohydrate food matrix. KW - Metrology KW - Quality Assurance KW - Mycotoxin Analysis KW - Sustainable Food Safety PY - 2023 DO - https://doi.org/10.1088/0026-1394/60/1A/08021 VL - 60 IS - 1a SP - 08021 AN - OPUS4-59059 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - CCQM IRWG draft strategy for all elements except for noble gases and H, C, N, O N2 - The presentation describes the draft strategy for metalloids and semi-metals within the IRWG at CCQM. This includes the definition of the measurements space, a suitable set of key comparisons and pilot studies and a proposal for a harmonized CMC application. T2 - EURAMET TC-MC Workshop on Isotope Ratio Analysis CY - Bern, Switzerland DA - 05.02.2020 KW - CMC KW - Measurement space KW - Metrology KW - Isotope ratio PY - 2020 AN - OPUS4-50345 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -