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Method for determining vanadium element in vanadium iron alloy

A technology for vanadium ferroalloy and element, applied in the field of vanadium ferroalloy determination of vanadium element, can solve problems such as affecting the accuracy of measurement results, affecting work efficiency, narrow measuring range, etc., achieving accurate and reliable analysis methods, saving manpower and material resources, and accelerating dissolution. the effect of speed

Inactive Publication Date: 2015-01-07
AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the domestic detection method for determining the content of vanadium in vanadium-iron alloy is GB / T8704.5-2007. The sample weight of this method is 0.2g-0.3g, which is large, and it is dissolved with phosphoric acid, nitric acid and sulfuric acid. It is difficult to dissolve the sample with hydrochloric acid. In the actual operation process, if the sample is weighed and dissolved according to this standard, the sample is often incompletely dissolved, which affects the accuracy of the measurement result.
[0003] The standard solution of ferrous ammonium sulfate in GB / T8704.5‐2007 needs to be calibrated by potassium dichromate standard solution. First, prepare potassium dichromate standard solution, then pipette a certain amount of potassium dichromate standard solution, and indicator, and then titrated with ferrous ammonium sulfate standard solution, the process is tedious, the workload is heavy, and the work efficiency is affected
[0004] GB / T8704.5‐2007 has a narrow measurement range of 35%-85%. If the customer requests that the vanadium content in the test sample be lower than 35% or higher than 85%, the test report will not be provided to the customer, which will affect the customer’s The test report is issued according to the product certificate and subsequent production and delivery for use

Method used

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  • Method for determining vanadium element in vanadium iron alloy
  • Method for determining vanadium element in vanadium iron alloy
  • Method for determining vanadium element in vanadium iron alloy

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Determination of the content of vanadium element in vanadium-iron alloy adopts ferrous ammonium sulfate volumetric method, and the reagent used in the determination process of this method is as follows:

[0046] Hydrochloric acid, ρ1.19g / mL; superior grade;

[0047] Nitric acid, ρ1.42g / mL; superior grade;

[0048] Sulfuric acid, ρ1.84g / mL; superior grade;

[0049] Sulfuric acid, 1+1;

[0050] Sulfuric acid, 5+95;

[0051] Phosphoric acid, ρ1.69g / mL; superior grade;

[0052]Potassium permanganate solution: the mass-volume concentration is 5.00mg / mL, weigh 5g of potassium permanganate, add appropriate amount of water to dissolve, and set the volume in a 1000mL volumetric flask;

[0053] Urea solution: mass-volume concentration is 0.20g / mL, ready-to-use and ready-to-use, weigh 40g of urea, add appropriate amount of water to dissolve, and set the volume in a 200mL volumetric flask;

[0054] Sodium nitrite solution: the mass-volume concentration is 5.00mg / mL, weigh 0.5g...

Embodiment 2

[0073] Determination of the content of vanadium in the V-Fe alloy adopts the ferrous ammonium sulfate volumetric method, and the reagents used in the determination process of this method are as follows:

[0074] Hydrochloric acid, ρ1.19g / mL; high purity;

[0075] Nitric acid, ρ1.42g / mL; high purity;

[0076] Sulfuric acid, ρ1.84g / mL; high purity;

[0077] Sulfuric acid, 1+1;

[0078] Sulfuric acid, 5+95;

[0079] Phosphoric acid, ρ1.69g / mL; high purity;

[0080] Potassium permanganate solution: the mass-volume concentration is 5.00mg / mL, weigh 5g of potassium permanganate, add appropriate amount of water to dissolve, and set the volume in a 1000mL volumetric flask;

[0081] Urea solution: mass-volume concentration is 0.20g / mL, ready-to-use and ready-to-use, weigh 40g of urea, add appropriate amount of water to dissolve, and set the volume in a 200mL volumetric flask;

[0082] Sodium nitrite solution: the mass-volume concentration is 5.00mg / mL, weigh 0.5g of sodium nitrite...

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Abstract

The invention relates to a method for determining vanadium element in vanadium iron alloy. The method is characterized by comprising the steps of oxidizing the vanadium into pentavalence by utilizing potassium permanganate in the existence of a sulfur phosphorus mixed acid medium, reducing the excessive potassium permanganate by utilizing sodium nitrite in the existence of urea, titrating the mixture by utilizing an ammonium ferrous sulfate standard solution and adopting N-phenyl o-aminobenzoic acid as an indicator agent, wherein the determination range is more than 0.5 percent. According to the method, the sample amount is reduced to 0.1g, and the process of dissolving the test sample is changed to comprise the following steps: dissolving a test sample by adding 20mL to 50mL of hydrochloric acid, 5 to 15mL of nitric acid, 10mL of phosphoric acid in a slightly heating manner, adding 30mL of 1+1 sulfuric acid, and heating and evaporating the mixed solution to produce sulfuric acid smoke for 2 to 3 minutes; slightly cooling the mixture, adding 50mL of water, and dissolving salt in a heating manner. Through the improvement, the test sample can be completely dissolved, the sample dissolving time is greatly shortened, and the working efficiency is improved on the premise of not influencing the accuracy of a detection result.

Description

technical field [0001] The invention relates to a method for determining vanadium elements in vanadium-iron alloys, belonging to the technical field of alloy element analysis. Background technique [0002] At present, the domestic detection method for determining the content of vanadium in vanadium-iron alloy is GB / T8704.5-2007. The sample weight of this method is 0.2g-0.3g, which is large, and it is dissolved with phosphoric acid, nitric acid and sulfuric acid. It is difficult to dissolve the sample with hydrochloric acid. In the actual operation process, if the sample is weighed and dissolved according to this standard, the phenomenon of incomplete sample dissolution often occurs, which affects the accuracy of the measurement result. [0003] The standard solution of ferrous ammonium sulfate in GB / T8704.5‐2007 needs to be calibrated by potassium dichromate standard solution. First, prepare potassium dichromate standard solution, then pipette a certain amount of potassium d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16G01N21/79
Inventor 任慧叶晓英杨春晟
Owner AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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