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Detecting method for phosphorus content in vanadium slag

A detection method and technology for phosphorus content, applied in the field of chemical detection, can solve problems such as difficult to master, cumbersome operation, interference of phosphorus, etc., and achieve the effects of saving detection time, high analysis efficiency, and reducing experimental errors.

Active Publication Date: 2016-02-03
WUKUN STEEL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Oxygen is blown to vanadium-containing molten iron during the smelting process, while vanadium is oxidized to vanadium pentoxide, phosphorus is also oxidized to phosphorus pentoxide and enters the vanadium slag, and the phosphorus content of molten iron is also high, resulting in vanadium The phosphorus content in the slag is higher, wherein the higher vanadium content interferes with the determination of phosphorus, and the determination of phosphorus content in the existing metallurgical industry standard YB / T547.4-1995 vanadium slag "acid-base volumetric method and bismuth phosphorus molybdenum blue light Determination of Phosphorus Amount by Bismuth Phosphorus Molybdenum Blue Photometry Method is 0.05-0.5%, and the acid-base capacity method is 0.3-0.8%. The acid-base volumetric determination of high content of phosphorus is cumbersome, time-consuming and difficult to master

Method used

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  • Detecting method for phosphorus content in vanadium slag
  • Detecting method for phosphorus content in vanadium slag
  • Detecting method for phosphorus content in vanadium slag

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0076] ——Determination of phosphorus content in vanadium slag samples

[0077] Reagents for detection:

[0078] Sodium carbonate-boric acid mixed flux: It is made by mixing sodium carbonate and boric acid with a mass ratio of 2:1 and grinding them finely.

[0079] Hydrochloric acid solution: It is formed by mixing 37% hydrochloric acid and water with a volume ratio of 1:2, and 37% hydrochloric acid and water with a volume ratio of 4:96.

[0080] p-nitrophenol solution: ethanol solution with a concentration of 10g / L.

[0081] Sodium hydroxide solution: the concentration is 200g / L.

[0082] Mixed solution of ascorbic acid-hydroxylamine hydrochloride-bismuth nitrate: dissolve 2g of bismuth nitrate in 20ml of 1+1 hydrochloric acid, and dissolve 25g of ascorbic acid and 25g of hydroxylamine hydrochloride in 480ml of 1+47 of hydrochloric acid, combine the above two solutions, and mix well.

[0083] Ammonium molybdate-potassium antimony tartrate mixed liquid: Dissolve 10g ammonium...

Embodiment 2

[0100] ——Determination of phosphorus content in vanadium slag samples

[0101] Detection reagent: same as embodiment 1

[0102] Sample testing:

[0103] 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 room temperature;

[0104] B, C, D, E, F steps are the same as embodiment 1.

[0105] G. Content calculation: The phosphorus content in the vanadium slag sample is calculated as follows:

[0106] m 1 ——Based on the vanadium slag sample absorbance value of 0.401, the phosphorus quality found on the working curve is 67.33ug;

[0107] m - the mass of the sample in step B is 0.2000g;

[0108] V 1 - The volume of the test solution pipetted in step C is 20.00ml;

[0109] V—the total volume of the test solution in step B is 250ml.

[0110]

Embodiment 3

[0112] ——Determination of phosphorus content in vanadium slag samples

[0113] Detection reagent: same as embodiment 1

[0114] Sample testing:

[0115] 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 room temperature;

[0116] B, C, D, E, F steps are the same as embodiment 1.

[0117] G. Calculation of content: the calculation of vanadium slag content in the sample is as follows:

[0118] m 1 ——Based on the vanadium slag sample absorbance value 0.690, the phosphorus quality found from the working curve is 125.36ug;

[0119] m - the mass of the sample in step B is 0.2000g;

[0120] V 1 - The volume of the test solution pipetted in step C is 20.00ml;

[0121] V—the total volume of the test solution in step B is 250ml.

[0122]

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Abstract

The invention discloses a detecting method for the phosphorus content in vanadium slag. According to the method, a sample is smashed and dried; the sample and sodium carbonate-boric acid mixed flux are mixed uniformly, the mixture is fused for 20-25 min at the temperature of 900 DEG C+ / -10 DEG C, frit is dissolved with 75 ml of hydrochloric acid, and the volume is metered to 250 ml; filtering is carried out, 20.00 ml of filter liquor is taken, three drops of paranitrophenol solution are added, a sodium hydroxide solution is dripped until the solution is yellow, hydrochloric acid is dripped until yellow fades, 5 ml of hydrochloric acid is added, 5 ml of ascorbic acid-hydroxylamine hydrochloride-bismuth nitrate mixed liquor is added, the mixed liquor is placed for 3-5 min, 5 ml of mecaammonium heptamolybdate tetrahydrate-antimony potassium tartrate mixed liquor is added, and the volume is metered to 100 ml; the mixed liquor is placed for 20 min, and with a blank as a reference, a spectrophotometer is used for measuring absorbance of developing liquid at the portion with the wavelength of 700 nm; a phosphorus standard sample with the concentration of 20 micrograms / ml is prepared, transferred and placed into volumetric flasks, water is added, hydrochloric acid is added, after developing, under the same condition, the absorbance is measured, and a working curve is drawn; the phosphorus content in the sample is calculated according to the following formula (see the formula in the description). The method is fast, efficient and particularly suitable for detecting the sample with the phosphorus content of 0.05-1.5%, and has high accuracy, repeatability and stability.

Description

technical field [0001] The invention belongs to the technical field of chemical detection, and in particular relates to a method for detecting phosphorus 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 components of vanadium slag are V205, P205, Al203, CaO, SiO2 and Fe. Oxygen is blown to vanadium-containing molten iron during the smelting process, while vanadium is oxidized to vanadium pentoxide, phosphorus is also oxidized to phosphorus pentoxide and enters the vanadium slag, and the phosphorus content of molten iron is also high, resulting in vanadium The phosphorus content in the slag is higher, wherein the higher vanadium content interferes with the determinatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/78G01N21/31
Inventor 郑玲陶俊欧阳光洪建波杨跃华
Owner WUKUN STEEL
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