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
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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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