TY - JOUR A1 - Gopala, Anil A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Process methodology for the small scale production of m6N5 purity zinc using a resistance heated vacuum distillation system JF - Materials chemistry and physics N2 - Ultra high purity Zn (m6N5) was obtained through triple vacuum distillation using an m4N5 Zn as input material. High-volatile impurities were removed from the zinc matrix by vacuum evaporation, while traces having lower volatility than the matrix remained in the residual material after finishing of the entire purification process. The time required for the removal of the main high-volatile impurity (Cd) was monitored using a connected gas source mass spectrometer. During distillation the Zn vapor of the distillate was condensed on the cap of a glassy carbon crucible which was water cooled by a movable copper block. The temperatures were optimized for the removal of the volatiles and for the distillation process using vapor pressure data. High resolution glow discharge mass spectrometry was applied for the analysis and purity evaluation of the distilled and input zinc. The analysis confirmed the reduction of the metallic impurities from 43 mg kg-1 to 0.5 mg kg-1 (m6N5) after three consecutive vacuum distillations. An increase in the grain size and a decrease in the micro-hardness were observed for the purified Zn material. KW - Ultra high purity KW - Vacuum distillation KW - High resolution glow discharge mass KW - Spectrometry KW - Micro-hardness KW - Zinc KW - Purification PY - 2010 DO - https://doi.org/10.1016/j.matchemphys.2010.02.080 SN - 0254-0584 VL - 122 IS - 1 SP - 151 EP - 155 PB - Elsevier CY - Amsterdam AN - OPUS4-21127 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Traub, Heike A1 - Wälle, M. A1 - Koch, J. A1 - Panne, Ulrich A1 - Matschat, Ralf A1 - Kipphardt, Heinrich A1 - Günther, D. T1 - Evaluation of different calibration strategies for the analysis of pure copper and zinc samples using femtosecond laser ablation ICP-MS JF - Analytical and bioanalytical chemistry N2 - Solution-doped metal powder pellets as well as aspirated liquids were used as calibration samples to analyze pure copper and zinc certified reference materials (CRMs) by femtosecond laser ablation ICP-MS. It was demonstrated that calibration by copper pellets resulted in relative deviations up to 20%, whereas fs-LA-ICP-MS among copper-based CRMs led to inaccuracies in the same range unless nominal mass fractions were chosen to be <3 mg/kg. Calibration by zinc pellets generally provided better accuracy. Depending on the analyte considered, deviations below 10% were obtained even for mass fractions close to the limit of quantification. Our data, therefore, indicate solution-doped metal powder pellets to be suitable as calibration samples for fs-LA-ICP-MS of metals. Furthermore, the utilization of liquid standards for calibration was found to result in stronger deviations of up to 50% for both copper and zinc samples which, in addition, turned out to be dependent on the plasma conditions. KW - Laser ablation KW - ICP-MS KW - Calibration KW - Copper KW - Zinc KW - Metal PY - 2009 DO - https://doi.org/10.1007/s00216-009-3061-9 SN - 1618-2642 SN - 1618-2650 VL - 395 IS - 5 SP - 1471 EP - 1480 PB - Springer CY - Berlin AN - OPUS4-20402 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -