スパークソース質量分析法による高純度タンタル粉末中の不純物の定量
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概要
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The spark source mass spectrometric conditions were studied for the determination of impurities in high purity tantalum powder by using JMS-01 BM-2 mass spectrometer. The sample electrodes were molded with tantalum powder and compressed at a pressure of 10 t. The electrodes molded with added graphite powder were unsatisfactory with respect to the electric conductivity and the mechanical strength under load. The increase of the spark source voltage from (2〜4.5) kV caused the increase of ion intensity for the elements, F, Si, Cl, Ca, Ti, Cr, Mn, Fe, Ni, Nb, and Sn; no increase was observed for B, Na, Al, K, and Ta. The pulse width variation from (20〜40) *s did not affect the ion intensity, but at 80 *s pulse width, ion intensities increased for the elements, B, F, Si, Cl, Ti, and Sn. Ion intensities stayed constant for the change in pulse frequency from (100〜1000) Hz. The relative sensitivity coefficient of trace elements in standard tantalum was determined by comparing with the analyzed data by JIS methods; the values ranged from 0.75 to 2.9. The optimal conditions for the r-f spark source mass spectrography were settled: pulse width, 20 *s; pulse repetition frequency, 1000 Hz; accelerating voltage, 25 kV; spark voltage, 3.0 kv; magnetic field current, 3.6 A; main slit, 60 *m, α-slit, 1.0 mm; β-slit, 2.0 mm; photoplate, Ilford Q_2. The analytical values by mass spectrography were consistent with those obtained by graphite furnace atomic absorption spectrometry.
- 社団法人日本分析化学会の論文
- 1982-10-05
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