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Determination method of gallium and scandium content in blast furnace dust

A measurement method, the technology of smoke and dust, applied in the field of analysis and testing, can solve the problems of difficult measurement and difficult to popularize and apply, and achieve the effect of reliable method, convenient operation and high accuracy

Active Publication Date: 2015-09-09
WUKUN STEEL
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For most of the content of gallium and scandium in blast furnace dust is 0.01%~0.1%, there is no suitable analytical method for accurate determination
However, with inductively coupled plasma atomic emission spectrometry, this method only needs to dissolve the sample to measure gallium and scandium in the sample, which saves time and effort, and does not need to consume a large amount of chemical reagents, which can reduce the impact on the environment. Pollution, to protect the health of operators, but it is difficult to popularize and apply due to the difficulty of measurement

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment １

[0014] Prepare gallium and scandium standard solutions routinely

[0015] 1. Preparation of gallium standard solution:

[0016] 1A. According to the amount of 300-400mL / g sample, add dilute hydrochloric acid solution to 0.1000g of commercially available pure gallium. The volume ratio of commercially available analytical pure hydrochloric acid to water in the dilute hydrochloric acid solution is 1:1, and then add 10-15 drops of commercially available analytical pure nitric acid, heated on a water bath until the gallium is dissolved, cooled to room temperature, diluted with water to form a 1 mg / mL gallium solution to obtain a gallium standard solution;

[0017] 1B. Pipette the gallium standard solution in step 1A, and dilute it with the dilute hydrochloric acid solution in step 1A to form a 10 μg / mL gallium standard solution.

[0018] 2. Preparation of scandium standard solution:

[0019] 2A. Burn commercially available reference pure scandium trioxide (above 99.99%) at 800°C ...

Embodiment 2

[0032] Determination of Gallium and Scandium in Blast Furnace Dust

[0033] 1. Preparation of sample solution of blast furnace dust to be tested

[0034] 1A. Put 1.0000g of blast furnace dust sample in a nickel crucible, add 4g of commercially available analytically pure solid sodium hydroxide at an amount of 4g / g of sample, heat and melt the sample at 800°C for 10min to obtain molten Sample;

[0035] 1B. Take the melted sample from step 1A and cool it slightly, put 30mL of hot water at 70°C into the melted sample according to the amount of 30mL / g sample, stir until the melted sample dissolves, and wash it with hot water Crucible, merge eluent in dissolving solution, obtain dissolving solution;

[0036] 1C. In the solution obtained in step 1B, slowly neutralize with a hydrochloric acid solution with a volume ratio of hydrochloric acid to water of 1:1 until the sodium hydroxide precipitate in the solution is just dissolved, and then add 5 mL of hydrochloric acid solution of t...

Embodiment 3

[0041] Determination of Gallium and Scandium in Blast Furnace Dust

[0042] 1. Preparation of sample solution of blast furnace dust to be tested

[0043] 1A. Put 1.0000g of blast furnace dust sample in a nickel crucible, add 6g of commercially available analytically pure solid sodium hydroxide at an amount of 6g / g sample, and heat and melt the sample at 700°C for 20min to obtain molten Sample;

[0044] 1B. Take the melted sample from step 1A and cool it slightly, put 40mL / g sample into 40mL of hot water at a temperature of 80°C for leaching, stir until the melted sample dissolves, and elute the crucible with hot water, combine and remove The washing liquid is in the dissolving solution to obtain the dissolving solution;

[0045] 1C. In the solution obtained in step 1B, slowly neutralize with a hydrochloric acid solution with a volume ratio of hydrochloric acid to water of 1:1 until the sodium hydroxide precipitate in the solution is just dissolved, and then add 10 mL of hydr...

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Abstract

The invention provides a method for measuring gallium and scandium contents in blast furnace smoke dust. The method comprises the following step: measuring the spectral line intensity of a sample solution by using the conventional inductively coupled plasma atomic emission spectrometry, so as to obtain the corresponding gallium and scandium content values from a standard working curve of gallium and scandium according to the spectral line intensity; the method is characterized in that a sample solution is prepared by the following steps: adding sodium hydroxide into the sample for melting the sample at high temperature, leaching the molten sample to obtain a dissolution solution by using hot water, dissolving a sodium hydroxide precipitate in the dissolution solution by using hydrochloric acid, acidifying the test solution by using hydrochloric acid, and obtaining the sample solution to be tested. According to the method, after the sample is dissolved, the gallium and scandium contents in the blast furnace smoke dust can be directly measured, and the operation is convenient to operate; moreover, the measured gallium and scandium contents are high in accuracy rate, the measurement results have high stability, reproducibility and accuracy, and the daily requirements of measuring the gallium and scandium contents in the blast furnace smoke dust can be completely met.

Description

technical field [0001] The invention relates to a method for measuring the contents of gallium and scandium, in particular to a method for measuring the contents of gallium and scandium in blast furnace dust, and belongs to the technical field of analysis and testing. Background technique [0002] There is no national standard analytical method for the determination of gallium and scandium content in blast furnace dust. The determination of gallium content in other samples such as steel is by spectrophotometry. A large number of chemical reagents not only pollute the environment, but also endanger the health of operators, and increase the cost, and are only suitable for the determination of trace gallium content, and the determination range is 0.0005%~0.010%. Although the determination of scandium content in steel is also by inductively coupled plasma atomic emission spectrometry, the sample is dissolved in acid, which is not suitable for the determination of gallium and sca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/73G01N1/28G01N1/38G01N1/44
Inventor 陶俊李玉清陈涛高玲林辉
Owner WUKUN STEEL
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