TY - JOUR A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Metrology in chemistry - a rocky road N2 - The application of metrology in chemical analysis is today hampered by psychological and practical barriers. The argumentation is based on the differences in physical and chemical metrology, which arises mainly from the objects of the measurements. The term “measurement” is discussed in the realm of analytical chemistry with a special focus on the inherent relation between chemical identification and determination as well as the consequent use of the concept of traceability and uncertainty. KW - Metrology in chemistry KW - Chemical analysis KW - Traceability KW - Uncertainty PY - 2008 DO - https://doi.org/10.1007/s00604-007-0909-6 SN - 0026-3672 SN - 1436-5073 VL - 162 IS - 1-2 SP - 35 EP - 41 PB - Springer CY - Wien AN - OPUS4-17727 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bremser, Wolfram A1 - Becker, Roland A1 - Kipphardt, Heinrich A1 - Lehnik-Habrink, Petra A1 - Panne, Ulrich A1 - Töpfer, Antje T1 - Stability testing in an integrated scheme N2 - ISO Guide 35 deals with RM stability issues and scrutinizes the evaluation of stability testing results under the assumption that either there is no trend at all (a rather rare situation), or any observed deterministic change is insignificant and thus can be neglected. However, market demands for reliable reference materials are obviously not limited to stable or at least seemingly stable materials. In many analytical applications, analytes and measurands under consideration are known, or at least suspected, to be unstable on time scales that may vary widely from measurand to measurand. The Federal Institute for Materials Research and Testing (BAM) has developed (and successfully uses) an integrated approach in its certification practice. The approach is based on an initial stability study and subsequent post-certification monitoring. Data evaluation is model-based and takes advantage of all information collected in the stability testing scheme(s). It thus allows one to deal with any kind of instability observed, to assess limiting time intervals at any stress condition in the range tested, to estimate a final expiry date for materials with detected instabilities or the maximum admissible re-testing interval for seemingly stable materials, and to assess maximum admissible stress loads during delivery of the material to the customer. The article describes (and exemplifies) typical study layout, the model selection, and the integrated data assessment. KW - Certified reference materials KW - Stability KW - Shelf life KW - Arrhenius model KW - ERM PY - 2006 DO - https://doi.org/10.1007/s00769-006-0152-6 SN - 0949-1775 SN - 1432-0517 VL - 11 IS - 10 SP - 489 EP - 495 PB - Springer CY - Berlin AN - OPUS4-14063 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gusarova, Tamara A1 - Hofmann, T. A1 - Kipphardt, Heinrich A1 - Venzago, C. A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Comparison of different calibration strategies for the analysis of zinc and other pure metals by using the GD-MS instruments VG 9000 and element GD N2 - Synthetic pressed metal powder standards doped with standard solutions were used for the calibration of both commercially available high resolution GD-MS instruments Element GD and VG 9000 for zinc matrix. Different quantification procedures (IBR, Standard RSF, matrix matched RSF from the calibration with CRMs and use of doped synthetic standards) are compared using zinc matrix as an example, whereas the calibration with doped pellets turned out to be the best quantification technique for high-purity materials. The applicability of the Standard RSF concept is scrutinised. In this context, RSF values for several Matrices (Co, Cu, Fe, In and Zn) are reported additionally. PY - 2010 DO - https://doi.org/10.1039/b921649a SN - 0267-9477 SN - 1364-5544 VL - 25 SP - 314 EP - 321 PB - Royal Society of Chemistry CY - London AN - OPUS4-22376 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Development of SI traceable standards for element determination N2 - In Germany a system of primary amount of substance standards for elemental analysis is being developed, which forms the material´s basis for the National Standards for element determination. The metrological concept and technical approach is briefly described. The objective of traceability in chemistry, in this case for elemental determination, is illustrated on the example of copper. KW - Copper KW - Element determination KW - Metrology KW - Primary standards KW - Traceability PY - 2009 DO - https://doi.org/10.2533/chimia.2009.637 SN - 0009-4293 VL - 63 IS - 10 SP - 637 EP - 639 PB - Schweizerische Chemische Gesellschaft CY - Basel AN - OPUS4-20727 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gopala, Anil A1 - Mahn, S. A1 - Panne, Ulrich A1 - Kipphardt, Heinrich T1 - In situ vacuum thermal mass spectroscopy for the selection of an environmentally friendly, energy saving catalytic additive and optimization of the process by a novel ignition mechanism N2 - We report herein the utilization of vacuum thermal mass spectrometry (VTMS) for the selection of an environmentally friendly, energy saving catalytic additive and a novel ignition mechanism, which is complementary to catalysis for the reduction of zinc oxide with carbon. PY - 2013 DO - https://doi.org/10.1039/c3ra40223a SN - 2046-2069 VL - 3 IS - 25 SP - 9677 EP - 9680 PB - RSC Publishing CY - London AN - OPUS4-28659 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gusarova, Tamara A1 - Methven, B. A1 - Kipphardt, Heinrich A1 - Sturgeon, R. A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Calibration of double focusing glow discharge mass spectrometry instruments with pin-shaped synthetic standards N2 - Calibration of two commercially available glow discharge double focusing mass spectrometers, the VG 9000 and Element GD, is described using synthetic pin standards pressed from solution doped copper and zinc matrices. A special pressing die was developed for this purpose and optimal results were obtained with the highest possible pressures, i.e., 95 kN·cm- 2. This calibration approach permits the determination of trace element mass fractions down to µg·kg- 1 with small uncertainties and additionally provides traceability of the GD-MS results in the most direct manner to the SI (International System of Units). Results were validated by concurrent measurements of a number of compact copper and zinc certified reference materials. The impact of the sample pin cross-section (circular or square) was investigated with the use of a new pin-sample holder system for the Element GD. The pin-sample holder was designed by the manufacturer for pin-samples having circular cross-section; however, samples with square pin cross-section were also shown to provide acceptable results. Relative Sensitivity Factors for some 50 analytes in copper (VG 9000, Element GD) and zinc matrices (VG 9000) are presented. The field of applicability of GD-MS may be considerably extended via analysis of pin geometry samples based on their ease of preparation, especially with respect to the accuracy and traceability of the results and the enhanced number of analytes which can be reliably calibrated using such samples. KW - Glow discharge KW - Pin sample KW - Calibration PY - 2011 DO - https://doi.org/10.1016/j.sab.2011.12.001 SN - 0584-8547 SN - 0038-6987 VL - 66 IS - 11-12 SP - 847 EP - 854 PB - Elsevier CY - Amsterdam AN - OPUS4-25346 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rudtsch, S. A1 - Gusarova, Tamara A1 - Aulich, A. A1 - Fahr, M. A1 - Fischer, J. A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Procedure for the impurity-related correction at the indium fixed-point N2 - Determining the influence of impurities on the fixed-point emperatures of the ITS-90 requires the completion of several tasks. In this paper, the Progress made at Physikalisch-Technische Bundesanstalt (PTB) and BAMFederal Institute for Materials Research and Testing is presented and remaining questions are discussed. The projected characterization procedure at PTB, which is based on the established SIE method (sum of the individual estimates), using a new indium fixed-point cell is described as an example. This procedure includes an SI-traceable chemical Analysis of the material in the fixed-point cell with sufficiently low uncertainties, the individual experimental determination of the influence of the quantified impurities on the fixed-point temperature, and the establishment of direct links to the phase-transition temperatures of the national standard and of an assumed material of ideal purity. A characteristic difference to the common practice is the chemical analysis of the fixed-point metal being done after determining the cell’s freezing temperature. This allows for the detection and consideration of contamination and purification effects due to the filling process, or due to the contact with the carbon crucible and other parts of the fixed-point cell. A chemical analysis of an indium fixed-point was carried out by BAM with relative measurement uncertainties below 30 % which have not been previously achieved. The results provide evidence for the precipitation of some impurities, which is apparently inconsistent with the corresponding binary phase diagrams, but was explained in a recent publication. Implications for the use of the SIE method shall be described briefly at the end. KW - Chemical analysis KW - Fixed-points KW - Impurities KW - ITS-90 PY - 2011 DO - https://doi.org/10.1007/s10765-011-0915-0 SN - 0195-928X SN - 1572-9567 VL - 32 IS - 1-2 SP - 293 EP - 302 PB - Springer CY - Dordrecht AN - OPUS4-23373 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Traub, Heike A1 - Czerwensky, Michael A1 - Matschat, Ralf A1 - Kipphardt, Heinrich A1 - Panne, Ulrich T1 - Different calibration strategies for the analysis of pure copper metal by nanosecond laser ablation inductively coupled plasma mass spectrometry N2 - In this work, different calibration strategies for the determination of trace elements in pure copper metal by nanosecond laser ablation ICP-MS were investigated. In addition to certified reference materials (CRMs), pellets of doped copper powder were used for calibration. The micro homogeneity of the CRMs as well as the solution-doped pellets was sufficient to use them as calibration samples in combination with a laser spot size of 200 µm. In contrast, pellets doped with analytes in solid form showed a significant heterogeneity. For most of the investigated analytes and copper CRMs the measured mass fractions were within ± 20% of their certified values when other copper CRMs were used as calibration samples. When solution-doped powder pellets were used as calibration samples a systematic trend towards mass fractions below the certified values was observed for nearly all elements determined in the analysed CRMs. Thermal fractionation effects during the ablation of the solution-doped pellets were suspected as the extent of the fractionation depends on the irradiance, whereas fractionation is reduced at higher irradiance. PY - 2010 DO - https://doi.org/10.1039/b915564c SN - 0267-9477 SN - 1364-5544 VL - 25 IS - 5 SP - 690 EP - 696 PB - Royal Society of Chemistry CY - London AN - OPUS4-21195 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -