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Method for direct determination of trivalent vanadium content in vanadium slag

A technology for trivalent vanadium and vanadium slag, applied in the field of chemical analysis, can solve the problems of complex measurement process and low accuracy, and achieve the effects of high measurement accuracy, good precision and reduction of measurement errors.

Active Publication Date: 2016-11-02
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This patented method is also an indirect method for the determination of trivalent vanadium, the determination process is complicated and the accuracy is not high

Method used

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  • Method for direct determination of trivalent vanadium content in vanadium slag
  • Method for direct determination of trivalent vanadium content in vanadium slag
  • Method for direct determination of trivalent vanadium content in vanadium slag

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] The mensuration of trivalent vanadium in the vanadium slag of embodiment 1

[0057] Weigh 5 samples, 0.15g each in a conical flask, weigh 0.1-0.2g of the sample to be tested in a conical flask, add 1g sodium fluoride, 1g sodium bicarbonate, 30mL hydrochloric acid, 1.0mL trichloride Titanium, pour a small amount of water, cover the porcelain crucible lid, place the sample in a high-temperature furnace to boil quickly, then move the sample to a low-temperature heating plate to keep the sample slightly boiling. After the sample is completely decomposed, add 2.0 mL of sodium sulfite and 0.5 g of sodium bicarbonate, cover the porcelain crucible and continue to boil for 5 minutes to decompose the remaining sodium sulfite. Take it off, cool to 60-70°C, add 50mL of water, 40mL of sulfuric acid, add 5mL of ammonium thiocyanate indicator, titrate with ferric ammonium sulfate standard titration solution until the solution is dark red as the end point, the preparation and calibrati...

Embodiment 2

[0071] The determination rate of recovery of trivalent vanadium in the vanadium slag of embodiment 2

[0072] Weigh 4 samples, each 0.15g in a conical flask, weigh 0.1-0.2g of the sample to be tested in a conical flask, add 1g sodium fluoride, 1g sodium bicarbonate, 30mL hydrochloric acid, 1.0mL trichloride Titanium, into a small amount of water, add trivalent vanadium standard solution (concentration of trivalent vanadium standard solution 4.48mg / mL) 3.0mL, 4.0mL, 5.0mL cover porcelain crucible lid, put the sample in a high-temperature furnace to boil quickly, and immediately The sample is moved into a low temperature heating plate to keep the sample slightly boiling. After the sample is completely decomposed, add 2.0 mL of sodium sulfite and 0.5 g of sodium bicarbonate, cover the porcelain crucible and keep boiling for 5 minutes to decompose the remaining sodium sulfite. Take it off, cool it to 60-70°C, add 50mL of water, add 40mL of sulfuric acid, add 5mL of ammonium thioc...

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Abstract

The invention belongs to chemical analysis methods, in particular to an analysis method for directly measuring the content of trivalent vanadium in vanadium slag. The method for directly measuring the content of trivalent vanadium in vanadium slag of the present invention comprises the following steps: A, taking X / g of the sample to be tested in a reaction vessel; B, adding hydrochloric acid and fluoride salt to dissolve the sample, and adding titanium trichloride as a mask agent, using carbon dioxide gas as a protective gas, heat until the solution is slightly boiling; C. After the sample is completely dissolved, add sodium sulfite, continue the reaction for 5-10 minutes, stop heating, and cool to 60-70°C; D. Add to the cooled solution Add sulfuric acid to adjust the acidity, add ammonium thiocyanate dropwise as the indicator, and use ferric ammonium sulfate standard solution as the titration solution, carry out titration until the reaction solution turns dark red, stop the titration, and calculate the vanadium slag with the consumed ferric ammonium sulfate solution The content of trivalent vanadium in the The method for determining the trivalent vanadium in the vanadium slag is simple and has high accuracy.

Description

technical field [0001] The invention belongs to chemical analysis methods, in particular to an analysis method for directly measuring the content of trivalent vanadium in vanadium slag. Background technique [0002] Vanadium slag is a process ore that is fully enriched in vanadium after smelting vanadium-containing raw materials. 2 o 5 ), the main raw material has great economic value. Understanding the valence state and content of vanadium slag is of great significance to determine the production process conditions of vanadium in the vanadium extraction process and improve the production conversion rate. Aiming at the research on the valence state of vanadium in vanadium slag, there have been many domestic studies, among which "X-ray photoelectric spectroscopy analysis of the valence state of vanadium in vanadium slag clinker" and "Valence state analysis of vanadium in vanadium slag" are qualitative analysis "Valence State Analysis of Vanadium in Sodium Vanadium Slag" is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N31/16
Inventor 苏洋汪雪梅郑小敏
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP