Quantitative Spectrographic Determination of Impurities in Tantalum and its Compounds by d.c. Arc Method

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  • タンタル中の不純金属元素の直流アークによる定量分光分析法
  • タンタル チュウ ノ フジュン キンゾク ゲンソ ノ チョクリュウ アーク ニ ヨル テイリョウ ブンコウ ブンセキホウ

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Abstract

Recent development of the tantalum refining industry made it necessary to determine the trace impurities in the high purity tantalum products. To meet the requirement of increasing sensitivity for the author’s previous intermittent a.c. arc method, a spectrographic d.c. arc method was studied with a medium quartz spectrograph Qu-24. Experiments were carried out to establish the optimum conditions regard to the various factors, such as carrier, arc current, exposure time, internal standard, analytical line pairs etc, yielding a sensitive, simple and rapid method, suited for the practical uses. The method includes converting sample to oxide, mixing with carbon powder which contains two internal standard materials (GeO2, BeO), arcing in a d.c. arc, and photographing spectra with a medium quartz spectrograph. The method can be applied to the analysis of the high purity tantalum products of various forms which could be brought into tantalum oxide, and used to determine the fourteen elements in them at the concentrations greater than 0.01% of Nb, W, 0.003% of Mo, 0.001% of Ti, 0.0005% of Fe, Ca, 0.0003% of Si, Cr, V, Ni, Al, 0.0001% of Mn, Cu, and 0.00003% of Mg, with the precision of about 10%, in terms of the variation coefficient.

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