TY - JOUR A1 - Kipphardt, Heinrich A1 - Czerwensky, Michael A1 - Matschat, Ralf T1 - Use of microwave induced plasma spectrometry as detector for the determination of O, N and H traces after carrier gas hot extraction N2 - The determination of O, N and H using a microwave induced plasma coupled to carrier gas hot extraction was exploratory investigated. The signal intensities versus time of blanks and calibration materials were recorded. To check for interferences the signal intensities versus wavelength were recorded at the times just before increase and at the maximum of the time dependent analytical signal. O, N and H were investigated at their prominent wavelengths of 777 nm, 174 nm and 486 nm, respectively. Calibration was performed for O, N and H in the ranges of 0–27 µg, 35–1000 µg and 3–43 µg respectively. For concentration values in the middle of the linear part of the investigated calibration interval, a relative precision of 5% at 13 µg, 2% at 74 µg and 0.6% at 23 µg for O, N and H respectively was found. The maximum matrix load to the plasma used was found to be 150 µg min-1. From the signal to noise ratio and the sensitivity obtained, instrumental limits of detection (3s) of 0.01 µg for O, 1 µg for N and 0.1 µg for H were found. Assuming a typical sample mass of 1 g this corresponds to relative LODs of 0.01 µg g-1, 1 µg g-1 and 0.1 µg g-1 for O, N and H respectively. KW - Non-metal determination KW - Microwave induced plasma spectrometry KW - Carrier gas hot extraction PY - 2008 U6 - https://doi.org/10.1039/B714734a SN - 0267-9477 SN - 1364-5544 VL - 23 IS - 4 SP - 588 EP - 591 PB - Royal Society of Chemistry CY - London AN - OPUS4-17359 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 U6 - 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 - TY - JOUR A1 - Lange, Britta A1 - Recknagel, Sebastian A1 - Czerwensky, Michael A1 - Matschat, Ralf A1 - Michaelis, Matthias A1 - Peplinski, Burkhard A1 - Panne, Ulrich T1 - Analysis of pure copper - a comparison of analytical mehods KW - Pure copper KW - Elemental analytical mehtods KW - Reference material KW - Sample dissolution PY - 2008 U6 - https://doi.org/10.1007/s00604-007-0849-1 SN - 0026-3672 SN - 1436-5073 VL - 160 SP - 97 EP - 107 PB - Springer CY - Wien AN - OPUS4-17565 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Vogl, Jochen A1 - Gusarova, Tamara A1 - Czerwensky, Michael A1 - Heinrich, Hans-Joachim A1 - Hioki, A. A1 - Konopelko, L.A. A1 - Methven, B. A1 - Miura, T. A1 - Petersen, O. A1 - Riebe, Gundel A1 - Sturgeon, R. A1 - Turk, G.C. A1 - Yu, L. L. T1 - Purity determination as needed for the realisation of primary standards for elemental determination: status of international comparability N2 - 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. KW - Interlaboratory comparison KW - Purity analysis KW - High purity metals KW - CCQM-P107 KW - Zinc PY - 2010 U6 - https://doi.org/10.1007/s00769-009-0557-0 SN - 0949-1775 SN - 1432-0517 VL - 15 IS - 1 SP - 29 EP - 37 PB - Springer CY - Berlin AN - OPUS4-20767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -