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Method for measuring total iron content in directly-reduced iron

A method of determination, the technology of reducing iron, applied in the field of analysis and testing, can solve the problems of difficult determination, cumbersome sample dissolving operation, and difficult calculation of titer, and achieve the effect of reliable method, convenient operation and high accuracy

Inactive Publication Date: 2012-01-18
WUKUN STEEL
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  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problems of cumbersome sample dissolving operation, difficult measurement, and difficult calculation of titer, the purpose of the present invention is to provide a method that can accurately measure total iron once a sample is dissolved, and is realized by the following technical scheme

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1. Preparation and calibration of potassium dichromate standard solution:

[0023] 1A, according to the amount of 25mL / g potassium dichromate, add commercially available potassium dichromate into water until potassium dichromate is completely dissolved, dilute with water to a concentration of 0.080 mol / L, and obtain potassium dichromate standard solution;

[0024] 1B. Dry commercially available reference ferric oxide at 105°C to constant weight, and cool to room temperature in a desiccator;

[0025] 1C. Add three parts of 0.2000 g of ferric oxide dried in step 1B to three parts of 30 mL of hydrochloric acid solution in an amount of 150 mL / g of ferric oxide. The hydrochloric acid solution has the following volume ratio: hydrochloric acid: water = 1:1, heated at 150°C until completely dissolved to obtain three parts of yellow solution; while hot, respectively add stannous chloride solution with a concentration of 100g / L to the three parts of yellow solution to reduce unt...

Embodiment 2

[0038] 1. The preparation and calibration of potassium dichromate standard solution are the same as in Example 1:

[0039] 2. Preparation of sample solution to be tested:

[0040]2A. Add 7 mL of potassium fluoride solution with a concentration of 250 g / L to 0.2000 g of direct reduced iron sample in an amount of 35 mL / g sample, and then add a mixed acid of sulfuric acid and phosphoric acid in an amount of 100 mL / g sample. 20mL, the mixed acid has the following volume ratio: sulfuric acid: phosphoric acid = 1:1, at 150°C, heat until the sample dissolves, and at 350°C, heat sulfuric acid and phosphoric acid to the bottle mouth, and then continue to smoke Sulfuric acid and phosphoric acid fume for 3 minutes, and the test solution was cooled to 70° C. to obtain 1 mL of a solution, wherein the preparation of the potassium fluoride solution was the same as in Step 2A of Example 1;

[0041] 2B. Add 22mL of hydrochloric acid solution to the 1mL solution in step 2A according to the amo...

Embodiment 3

[0045] 1. The preparation and calibration of potassium dichromate standard solution are the same as in Example 1:

[0046] 2. Preparation of sample solution to be tested:

[0047] 2A. Add 6 mL of potassium fluoride solution with a concentration of 250 g / L to 0.2000 g of direct reduced iron sample at an amount of 30 mL / g sample, and then add a mixed acid of sulfuric acid and phosphoric acid at an amount of 85 mL / g sample. 17mL, the mixed acid has the following volume ratio: sulfuric acid: phosphoric acid = 1:1, at 120°C, heat until the sample dissolves, and at 320°C, heat sulfuric acid and phosphoric acid to the bottle mouth, and then continue to smoke Sulfuric acid and phosphoric acid fume for 2 minutes, and the test solution was cooled to 65°C to obtain 1 mL of solution, wherein the preparation of potassium fluoride solution was the same as Step 2A of Example 1;

[0048] 2B. Add 21mL of hydrochloric acid solution to the 1mL solution in step 2A according to the amount of 21mL...

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Abstract

The invention provides a method for measuring the total iron content in directly-reduced iron. The method comprises the following steps of: adding potassium fluoride solution and mixed acid of sulfuric acid and phosphoric acid into a directly-reduced iron test sample, heating to dissolve the test sample, and thus obtaining dissolving solution; adding hydrochloric acid solution and stannous chloride solution into the dissolving solution, heating until the dissolving solution is boiled, cooling to room temperature, and thus obtaining sample solution to be measured; and directly measuring the total iron content in the directly-reduced iron by a titration method in the prior art. The method is convenient to operate and is high in accuracy rate of the measured total iron content and high in stability, repeatability and accuracy of a measured result. Experiments prove that: the method is reliable and practical and can meet the requirement of the total iron content in the directly-reduced iron during daily measurement.

Description

[0001] technical field [0002] The invention relates to a determination method, in particular to a determination method of total iron content in direct reduced iron, which belongs to the technical field of analysis and testing. Background technique [0003] There is no quantitative analysis and determination method for the determination of total iron content in direct reduced iron. The content of total iron in other materials such as iron ore is mostly determined by titration. Potassium dichromate titration method is used to measure the total iron content in direct reduced iron. After the sample is completely dissolved, the total iron can be measured. However, due to the large difference in the total iron content in direct reduced iron, the sample is dissolved by the conventional sample dissolution method. Incomplete, and there is a large error in the determination of the conventional titration method. Therefore, there is no effective method to measure the total iron conte...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N21/79
Inventor 陶俊郑玲高丽萍高玲李宏萍
Owner WUKUN STEEL
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