Method for determining content of silicon and zirconium in silicozirconium alloy

Abstract

The invention relates to a method for determining content of silicon and zirconium in silicozirconium alloy, and belongs to the technical field of material chemical analysis. The method comprises the following steps: decomposing a sample with nitric acid and hydrofluoric acid to convert the silicon into fluosilicic acid; adding potassium fluoride to generate potassium fluosilicate precipitation; filtering, washing and adding hot water to decompose the potassium fluosilicate precipitation to release hydrofluoric acid; using bromothymol blue or phenolphthalein as indicator to carry out titration with a sodium hydroxide standard solution until the solution turns to blue or light red as an end point; calculating the content of silicon; dissolving the sample with nitric acid and hydrofluoric acid, carrying out perchloric acid smoking, reacting zirconium with mandelic acid in a hot hydrochloric acid medium to generate an insoluble mandelic acid white precipitation; calcining the precipitation at 850-900 DEG C; weighing in the form of oxide; and conducting conversion to obtain the content of zirconium. The method for determining silicon and zirconium content in silicozirconium alloy has not been reported so far, and the method provided by the invention solves the problem, has the advanategs of simpleness, fastness, high accuracy and good repeatability, and is favorable for popularization and application.

Description

technical field [0001] The invention relates to a method for chemically analyzing materials, in particular to a method for measuring the content of silicon and zirconium in silicon-zirconium alloys, and belongs to the technical field of material chemical analysis. Background technique [0002] Silicon-zirconium alloy is added to steel as an additive, which can deoxidize and reduce the influence of harmful components such as oxygen, nitrogen, and sulfur. The compound formed by zirconium is evenly distributed in the structure, which can refine the grain, improve the toughness and hardenability of the material, improve the high temperature creep performance of the steel grade, and improve the deep drawing performance of the low carbon thin steel plate. Adding silicon-zirconium alloys to cast iron can promote the formation of graphite, facilitate the graphitization process, and improve the mechanical properties and processing properties of cast iron. It has been widely used in ...

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Problems solved by technology

[0003] There is no known measurement method for silicon-zirconium alloys. Usually, gravimetric methods are used for the analysis of higher silicon content, such as the analysis of various ferroalloys such as silicomanganese, ferrosilicon, and silicon-calcium. However, in silicon-zirconium alloys, the silicon volatilization step cannot carried out, so it does not apply

Directly referring to the industry standard SN / T1014.1-2001 "Determination of silicon content in ferrosilicon for export by potassium fluorosilicate capacity method" for measurement, it is found that for silicon-zirconium alloys with high zirconium content, it is difficult to completely react, and the measurement results are low; The determination method of zirconium includes the determination of zirconium in aluminum-zirconium alloy, magnesium-zirconium alloy, etc., usually using EDTA complexometric titration method, but the titration interference is serious, the end point is not easy to observe, and the effect is not ideal

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