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Method for determining zirconium content in silicon-zirconium alloy

A silicon-zirconium alloy and determination method technology, applied in the field of chemical analysis and test, can solve the problems of many reagent consumption, complicated operation, long time required, etc., and achieve the effects of reducing the amount of reagents, reducing the degree of pollution, and improving the accuracy

Inactive Publication Date: 2015-05-06
INST OF RES OF IRON & STEEL JIANGSU PROVINCE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The gravimetric method takes too long; the titration method usually adopts the EDTA complexometric titration method, the reaction rate is slow at room temperature, heating is required, the titration interference is serious, the end point will appear repeatedly, and it is difficult to observe; the photometric method and polarographic method can only measure trace or Trace zirconium requires adding a large amount of masking agent, which is cumbersome to operate, consumes a lot of reagents, and pollutes the environment

Method used

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  • Method for determining zirconium content in silicon-zirconium alloy
  • Method for determining zirconium content in silicon-zirconium alloy
  • Method for determining zirconium content in silicon-zirconium alloy

Examples

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specific example 1

[0024] Drawing of calibration curve with pure iron base:

[0025] Weigh 0.2500g of high-purity iron into a 250mL polytetrafluoroethylene beaker, add 40mL of nitric acid (1+1), drop about 10mL of hydrofluoric acid, heat slightly until completely dissolved, transfer to a 250mL plastic volumetric flask after cooling, and dilute with water To the mark, mix well, the solution is 1.000mg / mL; when in use, pipette 25.00mL into six 250mL plastic volumetric flasks as a base, and add different volumes of zirconium standard solutions, see Table 1.

[0026] The drawing of the calibration curve based on ferrosilicon:

[0027] Select a ferrosilicon standard substance with a similar iron content to silicon-zirconium alloy, weigh 6 parts of 0.1000g and place them in a 250mL polytetrafluoroethylene beaker, add 20mL nitric acid (1+1), and drop about 5mL hydrofluoric acid, After adding 5mL of perchloric acid to fume, add an appropriate amount of hydrochloric acid, heat to dissolve the salts, tra...

specific example 2

[0036] Drawing of calibration curve with pure iron base:

[0037] Weigh 0.2500g of high-purity iron into a 250mL polytetrafluoroethylene beaker, add 40mL of nitric acid (1+1), drop about 10mL of HF, slightly heat until completely dissolved, transfer to a 250mL plastic volumetric flask after cooling, and dilute to the mark with water. Mix well, the solution is 1.000mg / mL; when in use, pipette 25.00mL into six 250mL plastic volumetric flasks as a base, and add different volumes of zirconium standard solutions, see Table 1.

[0038] The drawing of the calibration curve based on ferrosilicon:

[0039] Select a ferrosilicon standard substance with a similar iron content to silicon-zirconium alloy, weigh 6 parts of 0.1000g and place them in a 250mL polytetrafluoroethylene beaker, add 20mL nitric acid (1+1), and drop about 5mL hydrofluoric acid, After adding 5mL of perchloric acid to fume, add an appropriate amount of hydrochloric acid, heat to dissolve the salts, transfer to a 250m...

specific example 3

[0045] Drawing of calibration curve with pure iron base:

[0046] Weigh 0.2500g of high-purity iron into a 250mL polytetrafluoroethylene beaker, add 40mL of nitric acid (1+1), drop about 10mL of HF, slightly heat until completely dissolved, transfer to a 250mL plastic volumetric flask after cooling, and dilute to the mark with water. Mix well, the solution is 1.000mg / mL; when in use, pipette 25.00mL into six 250mL plastic volumetric flasks as a base, and add different volumes of zirconium standard solutions, see Table 1.

[0047] The drawing of the calibration curve based on ferrosilicon:

[0048] Select a ferrosilicon standard substance with a similar iron content to silicon-zirconium alloy, weigh 6 parts of 0.1000g and place them in a 250mL polytetrafluoroethylene beaker, add 20mL nitric acid (1+1), and drop about 5mL hydrofluoric acid, After adding 5mL of perchloric acid to fume, add an appropriate amount of hydrochloric acid, heat to dissolve the salts, transfer to a 250m...

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Abstract

The invention relates to a method for rapidly determining zirconium content in silicon-zirconium alloy, belonging to the technical field of chemical analysis tests. The method comprises the following steps: dissolving pure iron or silicon iron as matrix, adding standard solutions with different amounts of zirconium to prepare a standard solution; determining the standard solution by virtue of an ICP-OES to prepare a standard curve; dissolving a sample with one or more of nitric acid, hydrochloric acid, hydrofluoric acid and perchloric acid, and diluting with water to achieve a certain volume; introducing the solution into the ICP-OES to determine to-be-determined spectral line intensity; determining the concentration of a to-be-determined element on a calibration curve. The zirconium content range in the silicon-zirconium alloy can be determined to be 0-30%; the standard solution prepared by the method is similar to sample solution matrix; the matrix effect is removed; the problems of fussy chemical analysis operation and slow analysis speed are solved by virtue of a high-precision analysis instrument; and the method has the advantages of being simple, fast, high in accuracy and precision and the like.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis tests, and relates to a method for determining the content of zirconium in silicon-zirconium alloys, in particular to a method for rapidly determining the content of zirconium in silicon-zirconium alloys as metallurgical raw materials is 0-30%. Background technique [0002] Silicon-zirconium alloys are widely used in metallurgy, casting and other industries. First of all, it is a high-quality composite deoxidizer for steelmaking, which has the functions of grain refinement, deoxidation, desulfurization, dephosphorization, etc. In addition, zirconium has the tendency to reduce inclusion segregation, which can improve the strength and toughness of steel, especially for deep-drawing steel plates. Improve its elongation; adding a small amount of zirconium alloy in the production of cast iron can promote graphitization, shorten the annealing time of ductile cast iron, and at the same time imp...

Claims

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Application Information

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IPC IPC(8): G01N21/71
Inventor 年季强朱春要顾峰张良芬
Owner INST OF RES OF IRON & STEEL JIANGSU PROVINCE
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