Molten sample preparation method of molybdenum, manganese, vanadium or chromium iron alloy sample for X-ray fluorescence spectroscopy

Abstract

The invention discloses a simple, quick and more reliable molten sample preparation method capable of avoiding corroding a platinum-gold crucible. The method comprises the following steps: a. weighing right amounts of lithium tetraborate, lithium carbonate, oxidizer and sample material, and evenly mixing to obtain balls, wherein the sample material is a silicon-iron, silicon-calcium-barium, silicon-manganese, aluminum-iron or titanium-iron alloy sample material; b. putting the balls obtained in the step a into a crucible with graphite powder on the bottom, and carrying out melting preoxidation in a high-temperature furnace; taking out the crucible, and cooling to obtain the preoxidated molten balls; c. weighing a certain amount of fluxing agent, adding the fluxing agent into the platinum gold crucible, and adding releasing agent and molten balls; melting for 12-20 minutes, taking out, shaking up, and removing bubbles; and melting for 12-20 minutes, taking out, shaking up, and cooling by standing to obtain the molten sheet. The invention does not need to carry out wall built-up treatment on the platinum gold crucible, simplifies the operation, and basically avoids corroding the platinum gold crucible in the preoxidation process; and the prepared molten sheet is uniform and flawless, and satisfies the requirements of X-ray fluorescence spectroscopy.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, and in particular relates to a melting sample preparation method for analyzing molybdenum, manganese, vanadium or chromium-iron alloy samples by X-ray fluorescence spectrometry. Background technique [0002] Metal ferroalloys such as ferromolybdenum, ferromanganese, ferrochrome and ferrovanadium are mainly used as additives in steelmaking to improve the process and performance of steel. The country has strict standards for their content, but the qualified range of each element is relatively narrow, and The content of each element is the direct and main factor affecting its performance. Therefore, it is very important to quickly and accurately analyze the chemical composition of metallic iron alloys. At present, the domestic metallurgical industry generally adopts traditional chemical analysis for the determination of single elements in the analysis of primary and secondary trace e...

AI Technical Summary

Problems solved by technology

This method has two disadvantages: one is that it requires a platinum gold crucible (referred to as a platinum yellow crucible) to hang on the wall and the sample pre-oxidation process, and the operation of the wall hanging is strict and cumbersome, and a slight mistake will cause corrosion of the precious platinum yellow crucible; It is because the pre-oxidant is not selected according to the characteristics of the analyzed sample. Commonly used are lithium carbonate, sodium carbonate and lithium nitrate, which affect the sufficiency of oxidation

[0005] CN102207475A discloses a metal alloy X-ray fluorescence spectroscopic detection method using a new sample preparation technology. The steps are as follows: 1) acid dissolution, dissolving the metal alloy sample with inorganic acid; 2) precipitation, dissolving the above-mentioned dissolved sample solution Adjust the sample solution with alkaline solution until the sample solution is alkaline, so that the element to be measured is precipitated in the form of precipitation, and filter the precipitate with ashless filter paper; 3) Ignition, put the filter residue after the above filtration together with the filter paper In a porcelain crucible with constant weight, the filter residue is converted into metal oxide through drying, carbonization, ashing, burning and other steps, and the weight of the filter residue after burning is calculated; The glass melting sample preparation method is used to make test pieces for X-ray fluorescence spectrometer detection. This method needs to be dissolved in acid, precipitated, burned and then melted. The operation process is cumbersome and is not suitable for mass production inspection and analysis.

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