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Method for measuring content of vanadium by potassium permanganate oxidation-ferrous ammonium sulphate titrating method

A technology of ferrous ammonium sulfate and potassium permanganate is applied in the direction of chemical analysis by titration, and can solve the problems of low measurement results and the like

Inactive Publication Date: 2011-04-13
PANGANG GROUP VANADIUM TITANIUM & RESOURCES +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Chromium (VI) has a strong oxidizing property, and common reducing agents such as sodium sulfite, ascorbic acid, and hydroxylammonium hydrochloride can reduce it, but it must be used in the determination of potassium permanganate oxidation-ferrous ammonium sulfate titration. To ensure that vanadium (V) is not reduced, experiments have found that sodium sulfite, ascorbic acid, and hydroxylammonium hydrochloride have strong reducing properties, which not only reduce chromium (VI) to chromium (III), but also reduce vanadium (V) to vanadium ( IV), resulting in low measurement results
At present, there is no report on a new method to eliminate the interference of chromium on the determination of vanadium in the potassium permanganate oxidation-ferrous ammonium sulfate titration method

Method used

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  • Method for measuring content of vanadium by potassium permanganate oxidation-ferrous ammonium sulphate titrating method
  • Method for measuring content of vanadium by potassium permanganate oxidation-ferrous ammonium sulphate titrating method

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Experimental program
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Embodiment 1

[0018] Example 1: Determination of Vanadium Content in Panzhihua Hongge Iron Mine

[0019] Take 8 parts of samples, four of which are operated according to the national standard GB / T 6730.32-1986 "Iron Ore Chemical Analysis Method - Ferrous Sulfate Volumetric Method for Determination of Vanadium Content" (except 4.5.2), and the Panzhihua Hongge Iron Mine The amount of vanadium in the sample was measured; the other four were also determined according to the national standard GB / T 6730.32-1986 "Methods for Chemical Analysis of Iron Ore-Ferrous Sulfate Volumetric Method for Determination of Vanadium Amount" (except 4.5.2), but after adding indicator Afterwards, 10 mL of selective reducing agent was added. The determination results of the two methods were compared, and the results are shown in Table 2.

[0020] Table 2

[0021]

[0022] Since Panzhihua Hongge iron ore contains about 2% Cr 2 o 3 , if no selective reducing agent is added, V 2 o 5 The measurement results wil...

Embodiment 2

[0023] Embodiment 2: the mensuration of vanadium content in chromium-containing wastewater

[0024] Pipette an appropriate amount of wastewater sample (the amount of vanadium is 1mg~20mg) into a 500mL Erlenmeyer flask, add 2mL~5mL nitric acid (if the sample contains organic matter, more nitric acid can be added), 50mL sulfuric acid (1+1), and place on an electric heating plate Heat until sulfuric acid fumes are emitted, remove, cool to room temperature, add 5mL phosphoric acid (1+1), boil for 1min, remove and cool to room temperature, add ferrous ammonium sulfate (50g / L) until the solution turns blue-green, cool to After room temperature, add potassium permanganate solution (25g / L) dropwise to a stable purple-red color, let it stand for 5 minutes, add 10mL urea solution (100g / L), add sodium nitrite solution (20g / L) dropwise until the red color disappears and overdose 1-2 drops, stand for about 1min, add 20mL selective reducing agent, stand for 2min, add 3-5 drops of diphenylam...

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Abstract

The invention provides a method for measuring content of vanadium by a potassium permanganate oxidation-ferrous ammonium sulphate titrating method. The method is characterized by comprising the following steps: dissolving a sample to be measured; adding ferrous ammonium sulphate into the sample to be measured, reducing the sample to be measured to solution in bluish green, and cooling the solution to room temperature; adding potassium permanganate into the sample to be measured, oxidizing the sample to be measured to solution in stable purple; adding urea into the sample to be measured; adding sodium nitrite into the sample to measured, reducing the sample to be measured until purple of the potassium permanganate fades away, and standing the sample to be measured until the vanadium is oxidized completely; adding a selective reducing agent and an indicator into the sample to be measured; and titrating the sample to be measured to a termination by ferrous ammonium sulphate standard solution. The selective reducing agent is mixed solution of absolute ethanol, hydrogen peroxide and water.

Description

technical field [0001] The invention relates to a method for measuring vanadium content, in particular to the determination of vanadium content by potassium permanganate oxidation-ferrous ammonium sulfate titration method. Background technique [0002] Vanadium is one of the important alloying elements in steel. Vanadium in steel can improve the strength, toughness, hardness and wear resistance of steel. According to the level of vanadium, the usual determination methods are divided into titration method and photometric method. The titration method is used for the determination of vanadium content (mass fraction) ≥ 0.10%. It is divided into oxidation-reduction titration and complexometric titration. Because the complexation reaction is very slow, it has not been widely used in actual analysis and is currently more common. And applicable is ferrous ammonium sulfate titration method, this method is mainly based on the characteristics of easy oxidation and reduction of vanadiu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N31/16
Inventor 郑小敏汪雪梅杨平刘红英
Owner PANGANG GROUP VANADIUM TITANIUM & RESOURCES
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