Measuring method of trace impurities in high-purity tantalum

Abstract

The invention relates to a measuring method of multiple trace impurities in high-purity tantalum. The measuring method comprises the steps of: (1) preparing a tantalum specimen solution, wherein tantalum specimen content is 1-5g / L, HF is 1-5vol%, and nitric acid is 0.3-0.8vol%; and (2) connecting an ion chromatograph, a film desolventing device and an ICP-MS (inductively coupled plasma-mass spectrometry) device, pumping the prepared specimen solution to a cation exchange column of the ion chromatograph by a concentrating pump for 5 minutes, adsorbing cations formed by impurity elements to theexchange column, flowing TaF7<2-> or TaOF5<2-> formed by substrate tantalum through the column without adsorption, leaching the exchange column with hydrofluoric acid to leach the residual substrate on the column, starting an on-line working procedure, eluting impurities adsorbed to the cation exchange column (sulfonic acid type cation exchange column) with nitric acid, and carrying out a blank test along with a specimen. The method is low in interference and good in precision, can simultaneously detect multiple trace impurities, and avoids the error introduced by multiple operations.

Description

technical field [0001] The invention relates to a method for determining trace impurity elements in metallurgical products, in particular to a method for determining trace impurities in high-purity tantalum. Background technique [0002] At present, the determination methods of trace impurities in high-purity tantalum include electrothermal atomic absorption method, inductively coupled plasma atomic emission spectrometry, inductively coupled plasma mass spectrometry, and glow discharge mass spectrometry. The electrothermal atomic absorption method itself has poor stability and high sensitivity, so the reproducibility of the obtained results is not ideal; the lower limit of determination of direct detection by inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry is relatively high It cannot meet the detection requirements of 4N-5N high-purity tantalum; in addition, there is glow discharge mass spectrometry, which is simple, ...

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Problems solved by technology

The electrothermal atomic absorption method itself has poor stability and high sensitivity, so the reproducibility of the obtained results is not ideal; the lower limit of determination of direct detection by inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry is relatively high It cannot meet the detection requirements of 4N~5N high-purity tantalum; in addition, there is glow discharge mass spectrometry, which is simple, fast, and has a low lower limit of determination, but it needs to be equipped with a very expensive glow discharge mass spectrometer

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