Method for measuring contents of manganese, copper and oxides in directly reduced iron

A technology for reducing iron and oxides, applied in the field of analysis and testing, can solve problems such as difficult determination, and achieve the effects of reliable method, convenient operation and high accuracy.

Active Publication Date: 2011-11-16
WUKUN STEEL +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Flame atomic absorption spectrometry is used for determination. Although multiple elements can be determined once a sample is dissolved, it saves time and effort, and does not need to consume a large amount of chemical reagents, which can reduce environmental pollution and protect the health of operators. However, due to the difficulty of determination Therefore, there is no effective method to determine the content of calcium oxide, magnesium oxide, potassium oxide, sodium oxide, manganese and copper in direct reduced iron

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment １

[0019] Prepare each of the following standard solutions:

[0020] 1. Preparation of manganese standard solution:

[0021] 1A. Wash commercially available electrolytic manganese (with a content of more than 99.9%) with sulfuric acid solution with a mass concentration of 4.9% until there is no manganese oxide on the surface, then repeatedly wash with water, dip in absolute ethanol for 4 to 5 times, and dry ;

[0022] 1B. According to the amount of 40mL / g electrolytic manganese, put the above dried electrolytic manganese into dilute nitric acid, wherein the volume ratio of dilute nitric acid is: HNO 3 : H 2 O=1: 3; heat and dissolve until boiling to drive away nitrogen oxides, cool, add water and dilute to 500 μg / mL to obtain manganese standard solution;

[0023] 1C. Pipette 20.00 mL of manganese standard solution prepared in step 1B into a 100 mL volumetric flask, dilute to the mark with water, and shake well. This solution contains 100 μg / mL manganese;

[0024] 2. Preparat...

Embodiment 2

[0058] Determination of calcium oxide, magnesium oxide, potassium oxide, sodium oxide, manganese and copper in direct reduced iron samples to be tested:

[0059] 1. Preparation of direct reduced iron sample solution to be tested:

[0060] 1A. Add 15mL of hydrochloric acid to 0.1000 g of the direct reduced iron sample to be tested at an amount of 150mL / g of the sample, and heat at 100°C until the sample is dissolved to obtain 5mL of the solution;

[0061] 1B. Add 2mL of the mixed acid of nitric acid and hydrofluoric acid to the dissolving solution in step 1A in an amount of 0.4mL / 1mL, heat and dissolve at 100°C for 10min to obtain 1mL of dissolving solution, in which the mixed acid is as follows Volume ratio: HNO 3 : HF=1:1;

[0062] 1C. Add 5mL of perchloric acid to the dissolving solution in step 1B according to the amount of 5mL / mL dissolving solution, and heat at 300°C to blow perchloric acid fumes to the mouth of the bottle, and then continue to blow perchloric acid fum...

Embodiment 3

[0068] Determination of calcium oxide, magnesium oxide, potassium oxide, sodium oxide, manganese and copper in direct reduced iron samples to be tested:

[0069] 1. Preparation of direct reduced iron sample solution to be tested:

[0070] 1A. Add 20 mL of hydrochloric acid to 0.1000 g of the direct reduced iron sample to be tested at an amount of 200 mL / g of the sample, and heat at 100°C until the sample is dissolved to obtain 10 mL of the solution;

[0071] 1B. Add 6mL of the mixed acid of nitric acid and hydrofluoric acid to the dissolving solution in step 1A in an amount of 0.6mL / 1mL, heat and dissolve at 150°C for 15min to obtain 2mL of dissolving solution, in which the mixed acid is as follows Volume ratio: HNO 3 : HF=1:1;

[0072] 1C. Add 20mL of perchloric acid to the solution in step 1B at an amount of 10mL / mL, and heat at 350°C to blow perchloric acid fumes to the mouth of the bottle, and then continue to blow perchloric acid fumes for 15 minutes. Cool to obtain 2...

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PUM

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Abstract

The invention provides a method for measuring contents of calcium oxide, magnesium oxide, potassium oxide, sodium oxide, manganese and copper in directly reduced iron. An absorbance value of a sample solution is measured by using a conventional flame atomic absorption spectrometry method, and corresponding contents of calcium oxide, magnesium oxide, potassium oxide, sodium oxide, manganese and copper are obtained according to the absorbance value in a standard working curve of calcium oxide, magnesium oxide, potassium oxide, sodium oxide, manganese and copper. The method is characterized by comprising the steps of: adding hydrochloric acid in a sample, adding mixed acid of nitric acid and hydrofluoric acid, adding perchloric acid for dissolving, adding diluted hydrochloric acid for dissolving salts, and filtering a dissolution solution to prepare the sample solution. The method is convenient for operation, and has high accuracy rate of measured contents of calcium oxide, magnesium oxide, potassium oxide, sodium oxide, manganese and copper; and measurement results in the method have better stability, repeatability and accuracy. Experiments prove that the method is reliable and practical, and can meet demands of daily measuring the contents of calcium oxide, magnesium oxide, potassium oxide, sodium oxide, manganese and copper in the directly reduced iron.

Description

[0001] technical field [0002] The invention relates to a method for determining the content of calcium oxide, magnesium oxide, potassium oxide, sodium oxide, manganese and copper in direct reduced iron, belonging to the technical field of analysis and testing. Background technique [0003] There is no quantitative analysis and determination method for the determination of calcium oxide, magnesium oxide, potassium oxide, sodium oxide, manganese and copper content in direct reduced iron. The contents of other materials such as calcium oxide, magnesium oxide, potassium oxide, sodium oxide, manganese and copper in steel are mostly determined by titration or spectrophotometry. Since different elements need different methods to complete the determination, the operation is cumbersome. The analysis and measurement process is long. Flame atomic absorption spectrometry is used for determination. Although multiple elements can be determined once a sample is dissolved, it saves time ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28
Inventor 陶俊许涯平李文生高丽萍李玉清曾海梅陈涛郑玲王磊高玲李宏萍
Owner WUKUN STEEL
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