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Determination method of phosphorus content in direct reduced iron

A determination method and technology for reducing iron, applied in the field of analysis and testing, can solve problems such as the difficulty of direct reduction iron, and achieve the effects of reliable method, high accuracy and good stability

Active Publication Date: 2011-11-30
WUKUN STEEL +1
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Problems solved by technology

[0004] In order to solve the problems such as the difficulty of determining the content of phosphorus in direct-reduced iron, the purpose of the invention is to provide a method capable of accurately measuring the content of phosphorus in direct-reduced iron, which is achieved through the following technical solutions

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0019] Preparation of phosphorus standard solution:

[0020] 1A. Dry commercially available potassium dihydrogen phosphate (with a content of more than 99.99%) at 105°C to constant weight and cool to room temperature in a desiccator;

[0021] 1B. Put the potassium dihydrogen phosphate dried in step 1A at 10 mL / g potassium dihydrogen phosphate into water until completely dissolved, and dilute with water to 500 μg / mL to obtain a phosphorus standard solution;

[0022] 1C. Pipette 10.00mL of phosphorus standard solution prepared in step 1B into a 500mL volumetric flask, dilute to the mark with water, and shake well. This solution contains 10μg / mL phosphorus;

[0023] 2. Preparation of iron solution:

[0024] 2A. Add commercially available analytically pure hydrochloric acid to the high-purity iron sample at a rate of 3.2 mL / g, and heat at 150°C until the sample dissolves to obtain a solution;

[0025] 2B. Add commercially available analytically pure nitric acid dropwise to the s...

Embodiment 2

[0033] A. Add 20mL of analytically pure hydrochloric acid to 0.2000g direct reduced iron sample at an amount of 100mL / g sample, and heat at 100°C until the sample dissolves to obtain 5mL of solution;

[0034] B. Add 5 mL of a mixed acid of analytically pure nitric acid and analytically pure hydrofluoric acid to the solution obtained in step A at an amount of 1.0 mL / mL, and then heat and dissolve at 100°C for 5 minutes to obtain 1 mL of the solution, of which The volume ratio of analytically pure nitric acid to analytically pure hydrofluoric acid is 4:1;

[0035] C. Add 5 mL of analytically pure perchloric acid to 1 ml of the solution obtained in step B at an amount of 5 mL / mL, and heat at 300°C until perchloric acid fumes come out of the bottle mouth, continue heating for 5 minutes, and cool to dissolve Liquid 1mL;

[0036] D. Add 20mL of water to the solution obtained in step C according to the amount of 20mL / mL solution, and heat to 100°C to dissolve the salt, cool the solu...

Embodiment 3

[0041] A. Add 30mL of analytically pure hydrochloric acid to 0.2000g direct reduced iron sample at an amount of 150mL / g sample, and heat at 150°C until the sample dissolves to obtain 10mL of solution;

[0042] B. Add 15mL of the mixed acid of analytically pure nitric acid and analytically pure hydrofluoric acid to the solution obtained in step A at an amount of 1.5mL / mL, and then heat and dissolve at 150°C for 10min to obtain 2ml of the solution, of which The volume ratio of analytically pure nitric acid to analytically pure hydrofluoric acid is 4:1;

[0043] C. Add 20mL of analytically pure perchloric acid to the 2ml solution obtained in step B at an amount of 10mL / mL, and heat at 350°C until the smoke of perchloric acid rises from the bottle mouth, continue heating for 10min, cool, and dissolve Liquid 2mL;

[0044] D. Add 50mL of water to the 2ml solution obtained in step C according to the amount of 25mL / mL solution, and heat to 150°C to dissolve the salt, cool the solutio...

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Abstract

The invention provides a method for measuring phosphorus content of directly reduced iron. A reagent is added into a directly reduced iron test sample for certain treatment so as to prepare test sample solution to be measured; and after color development, the phosphorus content of the directly reduced iron can be measured directly by spectrophotometry in the prior art. The method is convenient tooperate; furthermore, the accuracy rate of the measured phosphorus content is high, so a measurement result of the phosphorus content has high stability, reproducibility and accuracy. The experiment shows that the method is reliable and practical, and can meet the daily requirement of measuring the phosphorus content of the directly reduced iron.

Description

[0001] technical field [0002] The invention relates to a determination method, in particular to a determination method of phosphorus 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 phosphorus content in direct reduced iron. The phosphorus content in other materials, such as steel, is mostly measured by spectrophotometry, which is cumbersome to operate, and the analysis and measurement process is long. The content of phosphorus in direct reduced iron was determined by bismuth phosphomolybdenum blue photometry. After the sample was dissolved in acid, the phosphorus was oxidized with perchloric acid to be orthophosphoric acid. Reduction of phosphorus bismuth molybdenum heteropolyacid is phosphorus bismuth molybdenum blue, measuring its absorbance can calculate the phosphorus content in direct reduced iron, but because...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N21/31
Inventor 陶俊李玉清郑玲王磊高玲高丽萍李宏萍
Owner WUKUN STEEL
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