Method of determining major elements in ferrotitanium through X-fluorescence fuse piece method

Abstract

The invention discloses a method of determining major elements in ferrotitanium through an X-fluorescence fuse piece method. The method comprises the steps that (1) multiple standard samples with granularity being 200 meshes are selected; (2) the standard samples are weighed, and a composite oxidant and a viscosity reducer are added for uniform stirring; (3) a fusing agent is weighed into a platinum crucible, a standard sample obtained after uniform mixing is poured into the platinum crucible and covered with the fusing agent, and the platinum crucible is placed in a muffle furnace to completealloy sample pre-oxidation; (4) the platinum crucible subject to pre-oxidation is placed in a melting furnace for melting, a release agent is added for rotary shaking before release, and then coolingrelease is performed to prepare a glass sheet for analysis; (5) an X-ray fluorescence spectrometer is adopted to test the strength of the major elements in the standard sample, and tested strength values and standard values are made into a primary work curve; and (6) a to-be-detected sample of the blocky ferrotitanium is ground to have the same granularity as the standard sample and is melted into a glass sheet according to the steps (2) to (5), and the X-ray fluorescence spectrometer is used to analyze component values of the to-be-detected sample. The method can be used for determining theelements in the ferrotitanium with high titanium content, the life of the platinum crucible is prolonged, and result accuracy and precision are guaranteed.

Description

technical field [0001] The invention relates to a method for measuring major elements in ferro-titanium alloys by an X-fluorescence fusion chip method, which belongs to the technical field of physical and chemical detection. Background technique [0002] In order to meet the industrial requirements for steel properties, it is necessary to add alloying elements such as titanium and iron for microalloying treatment in the steelmaking process to improve the crystal structure of steel and improve the mechanical and physical properties of materials. On the one hand, or to guide the operation of the steelmaking process, the chemical composition of the ferro-titanium alloy needs to be tested and analyzed. Using traditional wet chemical analysis and the current national standard method to determine the content of titanium, silicon, manganese, aluminum, phosphorus, copper and other related elements in ferro-titanium alloy, the operation is complicated and cumbersome, the steps are lo...

AI Technical Summary

Problems solved by technology

This technical solution has the following deficiencies: 1. The final product after the strong alkali sodium hydroxide or potassium hydroxide is melted is potassium oxide or sodium oxide, because sodium hydroxide or potassium hydroxide has strong water absorption and carbon dioxide absorption , so that the amount of the final product after accurate weighing cannot be accurately controlled; 2. The release agent added is ammonium iodide solution. Because ammonium iodide decomposes and volatilizes extremely fast at high temperature, the residual ammonium iodide after long-term melting 3. After a long-term test, the oxidizing agent listed in the patent has insufficient oxidation ability, and when the titanium content in the ferro-titanium alloy reaches about 70% (70 ferro-titanium alloy) The alloy cannot be completely oxidized, and the platinum crucible will corrode after the fusing is completed, and a layer of white mist appears on the surface, losing its metallic luster

This method has the following deficiencies: 1, Lithium Nitrate is a pure oxidant in its composite oxidant (called flux in this application) formula, sodium carbonate and lithium carbonate are all strongly alkaline substances in nature, and the effects of sodium carbonate and lithium carbonate overlap Lithium nitrate infiltrates and disperses in the flux in the molten state, which cannot guarantee the concentration of oxidant around the alloy particles, resulting in alloys, especially titanium-iron alloys with high titanium content, such as 70 titanium-iron alloys, which are easily oxidized incompletely, and eventually corrode the platinum crucible; 2. If the mold agent is added too early, the remaining amount of release agent is insufficient when the sample is melted, and the sample is easy to adhere to the platinum crucible wall during the cooling and demoulding process, causing the sample to break. In order to obtain a complete high-quality sample, the control of the melting condition is extremely demanding Strict, and the platinum crucible wall is likely to have sample component microbeads remaining, which will affect the production of the next sample

[0005] At present, there are many reports on the analysis of ferroalloys by X-ray fluorescence pellet method, but because the pellet method is greatly affected by the sample particle size effect and matrix effect, the accuracy of the analysis data is poor, and the attempts to analyze ferroalloys by X-ray fluorescence pellet method are often unable to find Suitable oxidizers cannot completely oxidize iron alloy samples, causing corrosion of platinum crucibles, so the X-ray fluorescence fusion method is not widely used in iron alloy testing

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