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Method for rapidly determining content of total iron in vanadium titano-magnetite

A vanadium-titanium magnetite, rapid determination technology, applied in chemical analysis by titration, material analysis by observing the influence of chemical indicators, analysis by making materials undergo chemical reactions, etc., can solve the problem of total iron analysis Accuracy is greatly affected, does not meet the requirements of rapid analysis, and increases the cost of analysis, etc., to achieve the effect of rapid on-site analysis, reduction of uncertain conditions and system errors, and rapid determination of methods

Inactive Publication Date: 2014-12-03
武汉钢铁有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the determination method of total iron in vanadium-titanium magnetite is to use the sample to separate vanadium after alkali fusion. This method has a long process and increases the analysis cost, which does not meet the requirements of the production site for rapid analysis.
In addition, Zhang Yubin, Du Chunping, etc. published the article "Rapid Analysis of Total Iron in Vanadium-Titanite" in "Jiangxi Metallurgy", 2007, 27(6): 39-40, 43, introducing the addition of fluoride Ammonium, use ammonium fluoride to eliminate the interference of vanadium and titanium. In this process, vanadium is not all reduced to trivalent vanadium and fluorine complex, and some of it may be reduced to tetravalent vanadium, which will also consume potassium dichromate standard titration solution, so that The analysis result is too high, it is often accumulated with the negative error in the analysis method, and a false accurate result is formed for the sample with low vanadium content, and some iron ions will also be complexed by fluorine ions, and will not be reduced, forming a negative error , so for vanadium-titanium magnetite samples with high vanadium content, it has a great influence on the accuracy of total iron analysis

Method used

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  • Method for rapidly determining content of total iron in vanadium titano-magnetite
  • Method for rapidly determining content of total iron in vanadium titano-magnetite
  • Method for rapidly determining content of total iron in vanadium titano-magnetite

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Embodiment 1

[0032] Get the vanadium-titanium magnetite of a certain mine, wherein the total iron content is quickly measured, and the measuring method comprises the following steps in turn:

[0033] 1) take by weighing the vanadium-titanium magnetite sample to be measured that is 0.1018g, place in the 250mL Erlenmeyer flask;

[0034] 2) Add a sufficient amount of ore dissolving solution to the Erlenmeyer flask. The composition of the ore dissolving solution is 5 mL of sodium fluoride solution with a volume mass fraction concentration of 50 g / L, and 12.0 mL of sulfur-phosphorus mixed acid solution with a volume ratio of 1:1. and 2mL concentrated nitric acid, shake the bottle gently to disperse the sample, heat it on a high-temperature electric furnace until sulfuric acid fumes come out of the bottle to the mouth of the bottle, remove it, and cool slightly;

[0035] 3) Add 10 mL of hydrochloric acid solution with a volume ratio of 1:3;

[0036] 4) Add dropwise a stannous chloride solution ...

Embodiment 2

[0059] Get the vanadium-titanium magnetite of a certain mine, wherein the total iron content is quickly measured, and the measuring method comprises the following steps in turn:

[0060] 1) Weigh 0.2005g of the vanadium-titanium magnetite standard sample GBW07226 to be measured, and place it in a 250mL conical flask;

[0061] 2) Add a sufficient amount of ore dissolving solution to the Erlenmeyer flask, the composition of the ore dissolving solution is: 8mL potassium fluoride solution with a volume mass fraction of 50g / L, 20mL sulfur-phosphorus mixed acid solution with a volume ratio of 1:1, 3mL Concentrated nitric acid, gently shake the bottle to disperse the sample, heat it on a high-temperature electric furnace until sulfuric acid fumes come out of the bottle to the mouth of the bottle, remove it, and cool slightly;

[0062] 3) Add 15mL of hydrochloric acid solution with a volume ratio of 1:2;

[0063] 4) Add dropwise a stannous chloride solution with a volume mass fractio...

Embodiment 3

[0081] Get the vanadium-titanium magnetite of a certain mine, wherein the total iron content is quickly measured, and the measuring method comprises the following steps in turn:

[0082] 1) Weigh 0.4997g vanadium-titanium magnetite standard sample GBW07224, and place it in a 1000mL conical flask;

[0083] 2) Add a sufficient amount of ore dissolving solution to the Erlenmeyer flask, the composition of the ore dissolving solution is: 30mL volume mass fraction 50g / L sodium fluoride solution, add 90mL sulfur phosphorus mixed acid solution with a volume ratio of 1:1, add 10mL of concentrated nitric acid, gently shake the bottle to disperse the sample, heat it on a high-temperature electric furnace until sulfuric acid fumes come from the bottle to the mouth of the bottle, remove it, and cool slightly;

[0084] 3) Add 30mL of hydrochloric acid solution with a volume ratio of 1:2;

[0085] 4) Add dropwise a stannous chloride solution with a volume mass fraction of 60g / L (dissolve 6g...

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Abstract

The invention provides a method for rapidly determining the content of total iron in vanadium titano-magnetite. The method comprises the following steps: (1) weighing a to-be-determined vanadium titano-magnetite sample with the weight of M; (2) adding sufficient mineral dissolving solution to dissolve the to-be-determined vanadium titano-magnetite sample in a heating manner; (3) adding dilute hydrochloride acid into a reaction vessel; (4) dropwise adding stannous chloride solution to the reaction vessel until the mixed solution turns pale yellow, reheating the mixed solution to be boiled slightly, and cooling the mixed solution to the room temperature; (5) adding sodium tungstate solution into the reaction vessel, dropwise adding titanium trichloride solution until the mixed solution turns blue, and dropwise adding titanium trichloride solution to be slightly excessive in volume; (6) dropwise adding potassium dichromate solution into the reaction vessel until the mixed solution is colorless, and dropwise adding sodium diphenylaminesulfonate indicator; (7) titrating the mixed solution in the reaction vessel to be purple by adopting potassium dichromate standard titration solution; (8) sampling the solution after being titrated to be purple, and determining the weight percentage of vanadium in the sample; and (9) calculating. The method is easy to operate, high in determination speed, capable of enabling the detection result to be equivalent to that of a national standard method and capable of better meeting the in-situ rapid analysis requirement.

Description

technical field [0001] The invention belongs to the technical field of iron ore component analysis, and in particular relates to a rapid determination method for total iron content in vanadium-titanium magnetite. Background technique [0002] Vanadium-titanium magnetite is not only an important source of iron, but also associated with various components such as vanadium, titanium, chromium, cobalt, nickel, platinum group and scandium, which have important comprehensive utilization value. Total iron is an important indicator of the grade and quality of vanadium-titanium magnetite, so the content of total iron is one of the items that must be inspected in the trade and process application research of vanadium-titanium magnetite. [0003] At present, the determination method of total iron in vanadium-titanium magnetite is to separate the vanadium after alkali melting of the sample. This method has a long process and increases the analysis cost, which does not meet the requireme...

Claims

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Application Information

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IPC IPC(8): G01N31/16G01N21/79
Inventor 闻向东邵梅周郑赖碧波陈士华张穗忠吴立新杨艳朱缨
Owner 武汉钢铁有限公司
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