Dokument-ID Dokumenttyp Autoren/innen Persönliche Herausgeber/innen Haupttitel Abstract Auflage Verlagsort Verlag Herausgeber (Institution) Erscheinungsjahr Titel des übergeordneten Werkes Jahrgang/Band ISBN Veranstaltung Veranstaltungsort Beginndatum der Veranstaltung Enddatum der Veranstaltung Ausgabe/Heft Erste Seite Letzte Seite URN DOI Lizenz Datum der Freischaltung OPUS4-25346 Zeitschriftenartikel Gusarova, Tamara; Methven, B.; Kipphardt, Heinrich; Sturgeon, R.; Matschat, Ralf; Panne, Ulrich Calibration of double focusing glow discharge mass spectrometry instruments with pin-shaped synthetic standards 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. Amsterdam Elsevier 2011 Spectrochimica acta B 66 11-12 847 854 10.1016/j.sab.2011.12.001 2016-02-19 OPUS4-13483 Posterpräsentation Gusarova, Tamara Improvement of signal sensitivity using hollow cathode effect in glow discharge optical emission spectroscopy 2006 13. GDS-Anwendertreffen 13. GDS-Anwendertreffen Hanau, Germany 2006-09-04 2006-09-04 2016-02-19 OPUS4-13485 Vortrag Gusarova, Tamara Analysis of high purity zinc by glow discharge mass spectrometry for use in thermometry 2006 13th International Conference on ultra high-purity base metals 13th International Conference on ultra high-purity base metals Berlin, Germany 2006-09-11 2006-09-14 2016-02-19 OPUS4-13497 Vortrag Gusarova, Tamara Analysis of high purity zinc by glow discharge mass spectrometry for use in thermometry 2006 Euromet Workshop -732 / LNE - INM Euromet Workshop -732 / LNE - INM Paris, France 2006-11-23 2006-11-24 2016-02-19 OPUS4-14799 Vortrag Gusarova, Tamara New way to overcome the drawbacks of RSF- and Standard-RSF quantification concepts for VG 9000 and Element GD 2007 Joint GLADNET - EW-GDS - German GDS Users' Group meeting Joint GLADNET - EW-GDS - German GDS Users' Group meeting Brussels, Belgium 2007-09-14 2016-02-19 OPUS4-14800 Posterpräsentation Gusarova, Tamara GD-MS: calibration for VG9000 and Element GD - Do RSF- and StRSF-concepts always work? 2007 EuroAnalysis XIV EuroAnalysis XIV Antwerp, Belgium 2007-09-09 2007-09-14 2016-02-19 OPUS4-13680 Posterpräsentation Gusarova, Tamara Comparison of different quantification procedures in glow discharge mass spectrometry applied to high-purity metals 2007 2007 European Winter Conference on Plasma Spectrochemistry 2007 European Winter Conference on Plasma Spectrochemistry Taormina, Italy 2007-02-18 2007-02-23 2016-02-19 OPUS4-13776 Posterpräsentation Gusarova, Tamara Improvement of signal sensitivity using hollow cathode effect in glow discharge optical emission spectroscopy 2006 Interessengemeinschaft Atomspektroskopie IGAS 2006 Interessengemeinschaft Atomspektroskopie IGAS 2006 Berlin, Germany 2006-11-08 2006-11-08 2016-02-19 OPUS4-14639 Posterpräsentation Gusarova, Tamara Enhancement of signal sensitivity in glow discharge optical emission spectroscopy by use of the hollow cathode effect for the analysis of pure metals 2007 2007 European Winter Conference on Plasma Spectrochemistry 2007 European Winter Conference on Plasma Spectrochemistry Taormina, Italy 2007-02-18 2007-02-23 2016-02-19 OPUS4-14640 Posterpräsentation Gusarova, Tamara Enhancement of signal sensitivity in optical emission spectroscopy by coupling a grimm type glow discharge with hollow cathode 2007 ANAKON 2007 ANAKON 2007 Jena, Germany 2007-03-27 2007-03-30 2016-02-19 OPUS4-14631 Vortrag Gusarova, Tamara Glimmentladungsmassenspektrometrie im Einsatz für die Thermometrie 2007 CANAS '07, Colloquium Analytische Atomspektroskopie CANAS '07, Colloquium Analytische Atomspektroskopie Konstanz, Germany 2007-03-18 2007-03-21 2016-02-19 OPUS4-17539 Vortrag Gusarova, Tamara Hohlkathode in Kombination mit einer Grimmschen Glimmentladung zur Spurenanalyse von Reinstmetallen 2008 14. Deutsche GDS-Anwendertreffen 14. Deutsche GDS-Anwendertreffen Berlin, Germany 2008-04-17 2008-04-18 2016-02-19 OPUS4-17455 Zeitschriftenartikel Rudtsch, S.; Fahr, M.; Fischer, J.; Gusarova, Tamara; Kipphardt, Heinrich; Matschat, Ralf High-Purity Fixed Points of the ITS-90 with Traceable Analysis of Impurity Contents The International Temperature Scale of 1990 (ITS-90) is based on thermodynamic equilibrium states of ideally pure substances. The largest contribution to the uncertainty budgets of most metallic fixed points is the influence of impurities on the fixed-point temperature. Therefore, a traceable chemical analysis of the remaining impurities with small uncertainty is the basis of further progress. Further requirements are better knowledge of the phase diagrams at very low impurity contents, impurity segregation, and the quantification and correction of thermal effects during a fixed-point realization. In this article, current and future activities at PTB and BAM in order to develop improved metallic fixed-point cells of the ITS-90 are reviewed. Dordrecht Springer 2008 International Journal of Thermophysics 29 1 139 150 10.1007/s10765-007-0358-9 2016-02-19 OPUS4-18989 Posterpräsentation Gusarova, Tamara Calibration of DC GD-MS with synthetic standards 2009 ANAKON 2009 ANAKON 2009 Berlin, Germany 2009-03-17 2009-03-20 2016-02-19 OPUS4-19600 Zeitschriftenartikel Gusarova, Tamara; Hodoroaba, Vasile-Dan; Matschat, Ralf; Kipphardt, Heinrich; Panne, Ulrich Exploitation of the hollow cathode effect for sensitivity enhancement of Grimm-type DC glow discharge optical emission spectroscopy The hollow cathode (HC) effect was investigated in non-cooled 15 mm deep drilled flat metallic analytical samples that were easy to prepare. The deep cavity used ("complete HC" in contrast to "recessed HC" with 2-3 mm deep cavity) intensified the HC effect notably and therefore distinctly improved the detection power of the common GD-OES with planar cathodes. A signal enhancement of up to a factor of 150, not reported earlier, in comparison with flat conventional samples was achieved. A better separation of the analytical lines from spectral interferences was observed when the HC assembly was applied. Additionally, an effect of strongly enhanced intensities of atomic lines and somewhat decreased intensities of ionic lines was detected in the case of HC in comparison to usual planar cathodes. The investigations were carried out with samples of copper, steel and zinc matrices using both the same and individually optimised glow discharge (GD) electrical parameters. London Royal Society of Chemistry 2009 Journal of analytical atomic spectrometry 24 680 684 10.1039/b814977a 2016-02-19 OPUS4-23373 Zeitschriftenartikel Rudtsch, S.; Gusarova, Tamara; Aulich, A.; Fahr, M.; Fischer, J.; Kipphardt, Heinrich; Matschat, Ralf; Panne, Ulrich Procedure for the impurity-related correction at the indium fixed-point 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. Dordrecht Springer 2011 International Journal of Thermophysics 32 1-2 293 302 10.1007/s10765-011-0915-0 2016-02-19 OPUS4-103 Dissertation Gusarova, Tamara Wege zur genauen Charakterisierung hochreiner Materialien mit der Glimmentladungs-Massenspektrometrie (GD-MS) Die vorliegende Arbeit befasst sich mit der Analyse hochreiner Metalle mittels GD-MS (Glimmentladungs-Massenspektrometrie). Der Schwerpunkt war dabei die Verbesserung der genauen Bestimmung von Elementspuren, insbesondere im μg kg-1-Bereich, für den Kalibrierproben bekannter Zusammensetzung praktisch nicht existieren. Zur Überwindung des Problems wurden flüssigdotiere Pulverpresslinge als synthetische Kalibrierproben für die Matrices Zn, In, Cu, Fe sowie Co und das System Co/C hergestellt. Durch umfassende Untersuchungen der Praparationsschritte und eine eingehende Charakterisierung der Presslinge konnte deren Herstellungsprozess optimiert und deren Verhalten in der Glimmentladung besser verstanden werden. Das erarbeitete Quantifizierungskonzept wurde durch die Messung zertifizierter Matrixreferenzmaterialien mit Gehalten im mg kg-1-Bereich validiert, und seine Eignung auf hohem metrologischen Niveau bei der sehr erfolgreichen Teilnahme an einem weltweiten Ringversuch der internationalen Metrologieinstitute nachgewiesen. Gegenüber den bislang mangels tragfähiger Alternative verwendeten kalibrierprobenfreien Quantifizierungskonzepten ist der Einsatz der Presslinge bezüglich Richtigkeit, Unsicherheit und Rückführung auf das internationale Einheitensystem deutlich überlegen. Die GD-MS mit ihren Vorteilen als schnelle direkte Feststoffmethode erreicht so erstmalig die Analysenqualität der etablierten losungsbasierten Analysenmethoden, und erhöht damit ihren Anwendungsbereich deutlich, so dass sie schließlich auch für die Analyse von realen Proben für wichtige metrologische Fragestellungen angewendet werden konnte, wie für die Analyse von Zn-Fixpunktzellen, die für die Definition der internationalen Temperaturskala ITS 90 benötigt werden, oder für Primarnormale der chemischen Analytik. Darüber hinaus wurde grundlegend die Übertragbarkeit der klassischen kalibrierprobenfreien Quantifizierungskonzepte auf das neu auf dem Markt befindliche hochauflösenden GD-MS Gerat (Element GD) untersucht. Dabei wurden insbesondere die Einschränkungen herausgearbeitet, die für das völlig anders konstruierte Vorgängermodell VG 9000 nicht gelten. Ergänzende Untersuchungen zum Hohlkathodeneffekt führten zwar nicht bei der GD-MS, wohl aber bei der GD OES (Glimmentladung mit optischer Emissionsspektrometrie), zu einer enormen Steigerung des Nachweisvermögens für Elementspuren. Berlin Bundesanstalt für Materialforschung und -prüfung (BAM) 2010 55 978-3-9813346-1-6 1 225 urn:nbn:de:kobv:b43-1035 http://www.gesetze-im-internet.de/urhg/index.html 2015-01-23 OPUS4-20767 Zeitschriftenartikel Kipphardt, Heinrich; Matschat, Ralf; Vogl, Jochen; Gusarova, Tamara; Czerwensky, Michael; Heinrich, Hans-Joachim; Hioki, A.; Konopelko, L.A.; Methven, B.; Miura, T.; Petersen, O.; Riebe, Gundel; Sturgeon, R.; Turk, G.C.; Yu, L. L. Purity determination as needed for the realisation of primary standards for elemental determination: status of international comparability Within the National Metrology Institutes (NMIs) and designated laboratories, an interlaboratory comparison, CCQM-P107, was conducted to verify the degree of international comparability concerning the results of purity analysis. The mass fractions of Ag, Bi, Cd, Cr, Ni, Tl at the lower mg/kg-level in a high purity zinc material were determined, but the real measurand in metrological sense was the sum of the six mass fractions. Homogeneity was investigated by glow discharge mass spectrometry, reference values were obtained using isotope dilution mass spectrometry. Six NMIs participated, contributing eight independent data sets. The agreement amongst the results of the participants, their median and the agreement with the reference values were usually excellent and in almost all cases below the target uncertainty of 30% relative. In this manner, the accuracy of results and the comparability between the participants was demonstrated to be established. Berlin Springer 2010 Accreditation and quality assurance 15 1 29 37 10.1007/s00769-009-0557-0 2016-02-19 OPUS4-22376 Zeitschriftenartikel Gusarova, Tamara; Hofmann, T.; Kipphardt, Heinrich; Venzago, C.; Matschat, Ralf; Panne, Ulrich 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 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. London Royal Society of Chemistry 2010 Journal of analytical atomic spectrometry 25 314 321 10.1039/b921649a 2016-02-19