Method for rapidly determining content of total iron in nitrided ferrovanadium

A rapid determination technology for ferrovanadium nitride, applied in the preparation of test samples, chemical analysis by titration, etc., can solve the problems of difficult to obtain accurate results, provide quality data, cumbersome operation, etc., and prevent molten samples from splashing , to ensure accuracy, and to simplify the operation steps

Inactive Publication Date: 2013-05-08
HEBEI IRON AND STEEL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method needs to measure multiple elements, the operation is cumbersome, time-consuming and labor-intensive, it is difficult to obtain accurate results, let alone provide quality data for production in a tim

Method used

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  • Method for rapidly determining content of total iron in nitrided ferrovanadium
  • Method for rapidly determining content of total iron in nitrided ferrovanadium

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Effect test

Embodiment 1

[0025] Embodiment 1: The processing steps of the method for the rapid determination of total iron content in ferrovanadium nitride are as follows.

[0026] (1) Decomposition of the sample: Weigh 0.2000g of sample A into a high-alumina crucible filled with 3g of sodium peroxide in advance. Heat and melt in an electric furnace at 250°C. After all the solids in the crucible are melted, transfer to a muffle furnace at 700°C for melting for 10 minutes, take it out and cool slightly, and obtain an alkali fusion sample;

[0027] (2) Eliminate the interference of high vanadium on the determination of total iron: put the slightly cooled crucible above into a 400mL beaker filled with 20mL analytically pure concentrated hydrochloric acid (mass fraction 36-38%) in advance to extract the sample, wash out the crucible, Obtain leaching solution; Add 20mL, 50wt% sodium hydroxide in leaching solution, after solution precipitation is complete, filter with medium-speed quantitative filter paper,...

Embodiment 2

[0040] Embodiment 2: The process steps of the method for the rapid determination of total iron content in ferrovanadium nitride are as follows.

[0041] (1) Decomposition of the sample: Weigh 0.1500g of sample B into a high-alumina crucible containing 2g of sodium carbonate and sodium hydroxide (mass ratio 1:1) mixed flux in advance, mix well, and then cover with 1g of the above-mentioned Mix the flux, place it on a 300°C electric furnace and heat it to melt. After all the solids in the crucible have melted, transfer it to a 750°C muffle furnace to melt for 15 minutes, and take it out to cool slightly;

[0042](2) Eliminate the interference of high vanadium on the determination of total iron: put the slightly cooled crucible above into a 400mL beaker filled with 22.5mL analytically pure concentrated hydrochloric acid in advance to extract the sample, wash out the crucible, and add 18mL, 80wt% sodium hydroxide, after the solution precipitates completely, filter with medium-spee...

Embodiment 3

[0047] Embodiment 3: The processing steps of the method for the rapid determination of total iron content in ferrovanadium nitride are as follows.

[0048] (1) Decomposition of the sample: Weigh 0.2500g of sample C into a high-alumina crucible containing 7g of sodium carbonate and sodium peroxide (mass ratio 1:1) mixed flux in advance, mix well, and then cover with 3g of mixed flux For fluxing agent, place it on a 200°C electric furnace to heat and melt it. After all the solids in the crucible have melted, transfer it to an 800°C muffle furnace to melt for 12 minutes, and take it out to cool slightly;

[0049] (2) Eliminate the interference of high vanadium on the determination of total iron: put the slightly cooled crucible above into a 400mL beaker filled with 30mL of analytically pure concentrated hydrochloric acid in advance to extract the sample, wash out the crucible, and add 37.5mL, 20% sodium hydroxide, after the solution is completely precipitated, filter it with medi...

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Abstract

The invention discloses a method for rapidly determining the content of total iron in nitrided ferrovanadium. The method comprises the steps of: 1, decomposing a nitrided ferrovanadium sample by an alkali fusion method to obtain an alkali fusion sample; 2, leaching the alkali fusion sample by hydrochloric acid, adding sodium hydroxide to a leaching solution for precipitation, and filtering and separating the solution to obtain a ferric hydroxide precipitate; 3, acidifying the ferric hydroxide participate by hydrochloric acid, heating the acidified precipitate to a boiling point, dropwise adding stannous chloride to the heated precipitate to reduce ferric iron into ferrous until the stannous chloride is excessive; and 4, oxidizing the excessive stannous chloride by mercuric chloride, titrating the oxidized stannous chloride by a potassium dichromate standard solution with sodium diphenylaminesulfonate being an indicator, thus calculating the content of the total iron of the nitrided ferrovanadium sample. The method is capable of separating vanadium and ferrum and eliminating interference of high vanadium to determination of the total iron, thereby ensuring the accuracy of a determination result. The method is used for directly determining the content of the total iron in the nitrided ferrovanadium, the detection time is shortened from original 10h to 1h, and the detection speed is greatly enhanced. The method has the characteristics of being direct, simple, convenient and feasible.

Description

technical field [0001] The invention relates to a method for measuring iron content in alloys, in particular to a method for quickly measuring total iron content in ferrovanadium nitride. Background technique [0002] With the development of vanadium-containing steel grades, the full composition of ferrovanadium nitride as an additive for iron and steel smelting has attracted much attention. In recent years, in the inspection of the full composition of vanadium nitride, there have been relatively mature methods for the detection of vanadium composition content, such as a method for the determination of vanadium in vanadium nitrogen alloy provided by patent application number 200810015607.1, and provided by patent application number 201110193060.6 A method for the determination of vanadium in vanadium-nitrogen alloys, but the detection method for total iron (TFe) content is rarely reported. After checking the relevant information, it was found that the research on the determ...

Claims

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Application Information

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IPC IPC(8): G01N31/16G01N1/34
Inventor 高树峰李彩云张玉平宋晓军武挺张海岩
Owner HEBEI IRON AND STEEL
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