Summary
A method for the determination of chlorine in high-purity molybdenum and tungsten with isotope dilution mass spectrometry (IDMS) has been developed using a 37Cl enriched spike solution. After dissolution of the sample in H2O2, chlorine is separated by AgCl precipitation. Negative Cl- thermal ions are produced in a double-filament ion source using an easy-to-handle and cost-efficient quadrupole thermal ionization mass spectrometer. The detection limit, which is mainly influenced by contaminations from the laboratory air, lies between 0.006 and 0.1 μg/g depending on the variation of the blank values. Chlorine concentrations between 0.07 and 10.5 μg/g are analysed in different tungsten and molybdenum samples. A comparison with other sensitive analytical methods shows the urgent necessity of developing alternative methods for the determination of chlorine traces in refractory metals.
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Dedicated to Professor Dr. V. Krivan on the occasion of his 60th birthday
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Gäbler, HE., Heumann, K.G. Trace analysis of chlorine in high-purity refractory metals with isotope dilution mass spectrometry. Fresenius J Anal Chem 346, 426–428 (1993). https://doi.org/10.1007/BF00325855
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DOI: https://doi.org/10.1007/BF00325855