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A kind of determination method of total iron content in vanadium slag

A determination method and technology for iron content, applied in the field of chemical detection, can solve the problems of incomplete dissolution of the sample, interference with the total iron content, large measurement error, etc., and achieve the effect of good promotion and application prospects, fast analysis speed, and reduction of test errors.

Active Publication Date: 2016-06-01
WUKUN STEEL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The titration method is used to measure the total iron content in the vanadium slag, and the total iron can be measured after the sample is completely dissolved, but due to the high content of vanadium pentoxide in the vanadium slag, the sample is not completely dissolved by the conventional sample dissolution method, and due to The high content of vanadium pentoxide interferes with the determination of the total iron content, and the conventional titration method has a large error. Therefore, there is currently no effective method for the determination of the total iron content in vanadium slag.

Method used

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  • A kind of determination method of total iron content in vanadium slag
  • A kind of determination method of total iron content in vanadium slag
  • A kind of determination method of total iron content in vanadium slag

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] ——Determination of total iron content in vanadium slag samples

[0042] Reagents for detection:

[0043] Sodium Hydroxide: (solid).

[0044] Sulfuric acid: the concentration is (ρ1.84g / mL).

[0045]Phosphoric acid: the concentration is (ρ1.69g / mL).

[0046] Hydrochloric acid: the concentration is (ρ1.19g / mL).

[0047] Titanium trichloride: the concentration is (150g / L-200g / L).

[0048] Sodium hydroxide solution: the concentration is 50g / L.

[0049] Hydrochloric acid: (1+1).

[0050] Hydrochloric acid: (5+95).

[0051] Ammonium thiocyanate solution: the concentration is 50g / L.

[0052] Stannous chloride solution 100g / L: Weigh 10g of stannous chloride and dissolve it in 20mL of hot hydrochloric acid (ρ1.19g / mL), dilute to 100mL with water, and shake well.

[0053] Sodium tungstate solution 250g / L: Weigh 25g of sodium tungstate and dissolve it in 95mL of water (if it is cloudy, filter it), add 5mL of phosphoric acid (4.2), and shake well.

[0054] Titanium trichlo...

Embodiment 2

[0076] ——Determination of total iron content in vanadium slag samples

[0077] Detection reagent: same as embodiment 1

[0078] Sample testing:

[0079] A. Sample pretreatment: crush the sample to a particle size of ≤0.125mm, dry it at 105-110°C for 1.5-2.5h, seal it in a desiccator, and cool it to 20-25°C.

[0080] B, C, D, E, F steps are the same as embodiment 1.

[0081] G. Calculation of content: The calculation of iron content in the sample is as follows:

[0082] c - the concentration of potassium dichromate standard titration solution is 0.0400 (mol / L);

[0083] m - the mass of the sample in step B is 0.2000g;

[0084] V 0 - The volume of the standard titration solution of potassium dichromate consumed by the blank test solution for titration is 0.00ml;

[0085] V——The titration sample solution consumes a volume of potassium dichromate standard titration solution of 34.50ml;

[0086] 55.85 - the mass per mole of iron, in grams per mole (g / mol).

[0087]

[00...

Embodiment 3

[0091] ——Determination of total iron content in vanadium slag samples

[0092] Detection reagent: same as embodiment 1

[0093] Sample testing:

[0094] A. Sample pretreatment: crush the sample to a particle size of ≤0.125mm, dry it at 105-110°C for 1.5-2.5h, seal it in a desiccator, and cool it to 20-25°C.

[0095] B, C, D, E, F steps are the same as embodiment 1.

[0096] G. Calculation of content: The calculation of iron content in the sample is as follows:

[0097] c - the concentration of potassium dichromate standard titration solution is 0.0400 (mol / L);

[0098] m - the mass of the sample in step B is 0.2000g;

[0099] V 0 - The volume of the standard titration solution of potassium dichromate consumed by the blank test solution for titration is 0.00ml;

[0100] V - titration sample solution consumes potassium dichromate standard titration solution volume is 6.95ml;

[0101] 55.85 - the mass per mole of iron, in grams per mole (g / mol).

[0102]

[0103]

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Abstract

The invention discloses a method for testing total iron content in vanadium slag. A sample is smashed and dried, the smashed sample and sodium hydroxide are mixed uniformly in a corundum crucible, then sodium hydroxide is added, melting is carried out, melt is dissolved in hot water in a beaker, boils slightly for 2-3 minutes and then is cooled to be at the room temperature through water cooling, filtering is carried out through medium-speed filter paper, the beaker and sediment are washed for five to six times through sodium hydroxide solutions, the sediment on the filer paper is washed in the original beaker through hot water and hot hydrochloric acid and boils slightly for 5 minutes, stannous chloride is dripped into the solution and is faint yellow, and the solution is cooled to be at the room temperature through water cooling. Sodium tungstate solutions are dripped for ten times, tungsten blue is produced through titanium trichloride solutions in a reduction mode, potassium dichromate solutions are dripped until the blue color disappears, sulphur and phosphorus mixed acid solutions of 15 millimeters are added, aniline sulfonic acid sodium indicators are dripped for three to five times, potassium dichromate standard titration solutions are dripped until the solutions are purple stably, and the total iron content in the sample is calculated according to the formula shown in the instruction. The method is good in accuracy, reproducibility and stability and is especially suitable for detecting the total iron content in the vanadium slag.

Description

technical field [0001] The invention belongs to the technical field of chemical detection, and in particular relates to a method for measuring total iron content in vanadium slag. Background technique [0002] Vanadium slag is a general term for vanadium oxide-containing slag obtained by oxidation blowing of vanadium-containing molten iron or vanadium-containing iron concentrate by wet extraction of vanadium. It is used for smelting and producing vanadium alloys and metals. Raw material of vanadium. The main component of vanadium slag is V 2 0 5 , P, CaO and SiO 2 And Fe content. Among them, the content of total iron has an important influence on the performance of the product, so the accurate determination of its content has very important practical significance for smelting production. Determination of total iron content in vanadium slag, there is no quantitative analysis and determination method. The content of total iron in other materials such as iron ore is mostl...

Claims

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Application Information

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IPC IPC(8): G01N31/16G01N31/22
Inventor 郑玲陶俊孙肖媛李文生王宁
Owner WUKUN STEEL
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