Preparation method for specimen used for measuring silicon contents in ferrosilicon by X-ray fluorometric analysis method

Abstract

The invention relates to a preparation method for a specimen used for measuring silicon contents in ferrosilicon by an X-ray fluorometric analysis method. The preparation method comprises the following steps of primary burdening, pre-oxidation, secondary burdening and fusion. In primary burdening, filter paper and mixed oxidizing agent are used for coating a ferrosilicon specimen, and the specimenis coated into a sphere; in pre-oxidation, a crucible is full of graphite, the spherical specimen is put into a graphite pit, and then, the spherical specimen is oxidized in a high-temperature mufflefurnace to obtain an elliptical specimen; in secondary burdening, ammonium iodide release agent is laid in a platinum vessel, the cooled elliptical specimen is placed and is covered with lithium borate and metaboric acid mixed fusing agent; and in fusion, the platinum vessel is put in a piece fusion machine and is subjected to fusion at the temperature of 900-1050DEG C for 19min to obtain the fused piece, i.e., the specimen, and the specimen can be directly used for an X-ray spectrum analyzer for analysis. By use of the method, various specimens can be simultaneously manufactured, in addition, process controllability is simple, time consumed for experiments is short, manufacture cost is low, and an X-ray fluorometric analysis result is high in accuracy.

Description

technical field [0001] The invention relates to a method for measuring silicon content in ferrosilicon by X-ray fluorescence analysis, in particular to a method for preparing a sample used for measuring silicon content in ferrosilicon by X-ray fluorescence analysis. Background technique [0002] Ferrosilicon is an important raw material for steelmaking, and its chemical composition detection is one of the important links to ensure steelmaking process control and quality control. At present, the national standard method for determining the silicon content in ferrosilicon is the perchloric acid dehydration gravimetric method, but this method is cumbersome to operate, is greatly affected by other interfering elements, and the analysis time is about 1 day. Therefore, technicians in the industry are looking for an efficient and fast method to analyze the silicon content in ferrosilicon. [0003] Zhou Honghong and Cao Zhonglie's "Determination of Silicon in Ferrosilicon" proposed...

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Problems solved by technology

[0005] Glass dissolution method, lithium tetraborate wall pre-oxidation method, centrifugal casting method, and melting method after mixed acid treatment: these can eliminate the influence of particle size effect and matrix effect, and improve the accuracy of analysis results, but these methods are in the process of implementation There is a reaction between metal and other reducing substances in the material and platinum at high temperature, corroding the platinum crucible, and repeated high-life use of the experimental utensils cannot be achieved. Even if there is a protection step of using lithium tetraborate on the wall in these methods, the platinum crucible still exists once. In addition, the price of platinum crucible is relatively expensive. Serious corrosion of platinum crucible causes interruption of experimental operation, re-preparation of materials used in samples, and increased repetitive process, which virtually increases the cost of testing and testing.

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