Method for determining content of silicon in potassium fluotantalate

Abstract

The invention relates to a method for determining the content of silicon in potassium fluotantalate. The method adopts an ICP (Inductively Coupled Plasma) spectrometer and a hydrofluoric acid resistant sampling system; purified electronic-grade nitric acid and hydrofluoric acid are adopted, and the heights of a center pipe of an ICP spectrometer quarter bend and an inner pipe are adjusted to enable a distance between the bottom of a flame and an outer quartz pipe of the ICP spectrometer quarter bend to be increased by about 50% compared with a standard distance; solution prepared by a surfactant (Triton-X100) is used as washing liquid for washing the sampling system of the ICP spectrometer before each time of determination. The method overcomes the technological barrier existing in the industry, and realize the determination of the content of silicon in potassium fluotantalate through ICP spectrum analysis through comprehensive technical schemes of introducing the hydrofluoric acid (HF) resistant sampling system, adjusting the positions of the center pipe of the ICP spectrometer quarter bend and the inner pipe, setting special parameters, developing the washing liquid, preparing a standard sample, purifying and selecting reagents and the like, and the determination limit can reach 0.0005%; therefore, the method is initiative in domestic peers.

Description

Technical field: [0001] The invention relates to the technical field of methods for determining the content of impurity elements in potassium fluorotantalate, in particular to a method for determining the content of silicon in potassium fluorotantalate. Background technique: [0002] Potassium fluorotantalate is the main raw material for producing tantalum powder, and its purity directly affects the quality of tantalum powder. Therefore, enterprises have higher and higher requirements for the purity of potassium fluorotantalate. Potassium fluorotantalate contains more than a dozen impurity elements such as Al, B, Ca, Cr, Mn, Cu, Fe, Mg, Mo, Nb, Ni, Ti, Si, W, etc. For impurities other than Si, currently There is an ICP spectrometer measuring method (inductively coupled plasma emission spectrometry) to measure, and the lower limit of determination can reach 0.0005%, which can meet the requirements of enterprises. [0003] As for Si element, because the quartz outer tube and ...

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Problems solved by technology

[0003] As for Si element, because the quartz outer tube and inner tube of the rectangular tube in the ICP spectrometer contain a large amount of Si element, the background concentration is too high, which makes the sample easy to contaminate, and the reagent blank is too high, so it is still impossible to use the above method to determine tantalum fluoride Si element content in potassium acid potassium

At present, domestic manufacturers use chemical method or arc spectrometry to analyze silicon in potassium fluorotantalate. The silicon blank is high, the stability is poor, and the blank value changes greatly during the analysis process, resulting in no reproducibility of the analyzed samples.

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