7 research outputs found

    Development of SI Traceable Standards for Element Determination

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    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

    Evaluation of different calibration strategies for the analysis of pure copper and zinc samples using femtosecond laser ablation ICP-MS

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    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 <3mg/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. Figure Different calibration strategies for fs-LA-ICP-M

    Special new techniques of atomic spectrometric methods for trace analysis of high purity metals

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    How spectral interferences of analyte ions with polyatomic ions containing matrix atoms can be identified, reduced or eliminated was demonstrated for different pure metals using a double focussing ICP mass spectrometer in higher mass resolution. An in-situ coating procedure of the nickel inlet cones of the ICP mass spectrometer with a thin quartz glass film was developed in our laboratory. It leads to a drastic decrease of memory effects and blanks, especially for the analytes Na, Ni and Li. The limits of determination (LODs) of these analytes were decreased for more than one order of magnitude. The analytical performance of two atomic spectrometric techniques combined with electrothermal vaporization (ETV) of metallic microsamples was investigated using tungsten as an example. An ICP optical emission spectrometer equipped with ETV (ETV ICP OES) as well as a solid sampling atomic absorption spectrometer (SS-ET AAS) were used. Benefits and drawbacks of both method combinations were summarized and compared. The multielement capability of ETV ICP OES was much higher than the of SS-ET AAS. LODs of the less refractory analytes were lower with SS-ET AAS than with ETV ICP OES
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