Method for simultaneously determining Zr, Cu and Ni contents in Zr-Cu-Ni-Al amorphous alloy

A zr-cu-ni-al, amorphous alloy technology, applied in the field of chemical analysis, can solve the problems of no joint determination technology patents and reports, not suitable for nickel-containing material determination, long measurement period, etc.

Active Publication Date: 2014-12-17
AECC AVIATION POWER CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the above method, the copper separation process is complicated, and special electrolysis equipment is required, and it is not suitable for the determination of nickel-containing materials.
In common analysis, high content zirconium and nickel are separated by precipitation, the result is accurate and reliable, but the measurement cycle is long and the operation is cumbersome. In general work, titration method is often used, and direct titration method or back titration method is commonly used
It is very easy to generate polynuclear hydroxyl compounds in direct titration. Before titration, it must be heated and boiled. Titration while hot, and the end point is repeated, and the result is low
For the back titration to determine zirconium, in the existing literature, due to insufficient operational control requirements, the error of the measurement results is also large; the complexation stability constants of Cu, Ni, Al and EDTA are similar, and they interfere with each other in the titration process under the coexistence situation, so they cannot be directly measured.
[0003] No patents and reports were found for the combined determination of Zr, Cu, and Ni in Zr-Cu-Ni-Al amorphous alloys after a novelty search

Method used

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  • Method for simultaneously determining Zr, Cu and Ni contents in Zr-Cu-Ni-Al amorphous alloy
  • Method for simultaneously determining Zr, Cu and Ni contents in Zr-Cu-Ni-Al amorphous alloy
  • Method for simultaneously determining Zr, Cu and Ni contents in Zr-Cu-Ni-Al amorphous alloy

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Embodiment 1

[0038] This embodiment is a method for jointly determining the contents of Zr, Cu, and Ni in Zr55Cu30Al10Ni5.

[0039] Step 1: Zr-Cu-Ni-Al amorphous alloy sample weighing: Weigh 0.2994g of Zr-Cu-Ni-Al amorphous alloy sample, accurate to 0.0001g, and place it in a 250mL beaker. An accurately weighed Zr-Cu-Ni-Al amorphous alloy sample is obtained.

[0040] Step 2: Zr-Cu-Ni-Al amorphous alloy sample dissolves and smokes: Add 10mL of Zr-Cu-Ni-Al amorphous alloy sample with a density of 1.84g / mL in turn to a beaker containing accurately weighed sulfuric acid and 2g of solid ammonium sulfate, place the beaker on an electric stove and heat until the solution in the beaker is clear, continue heating until the solution emits white smoke, then add 2mL of nitric acid with a density of 1.42g / mL, continue heating the beaker until the solution emits white smoke, The beaker was removed from the electric furnace, and cooled naturally to room temperature to obtain a Zr-Cu-Ni-Al amorphous allo...

Embodiment 2

[0058] This embodiment is a method for jointly determining the contents of Zr, Cu and Ni in Zr67Cu26Al4Ni3.

[0059] Step 1: Zr-Cu-Ni-Al amorphous alloy sample weighing: Weigh 0.3002g Zr-Cu-Ni-Al amorphous alloy sample, accurate to 0.0001g, and place it in a 250mL beaker. An accurately weighed Zr-Cu-Ni-Al amorphous alloy sample is obtained.

[0060] Step 2: Zr-Cu-Ni-Al amorphous alloy sample dissolves and smokes: Add 10mL of Zr-Cu-Ni-Al amorphous alloy sample with a density of 1.84g / mL in turn to a beaker containing accurately weighed sulfuric acid and 2g of solid ammonium sulfate, place the beaker on an electric stove and heat until the solution in the beaker is clear, continue heating until the solution emits white smoke, then add 2mL of nitric acid with a density of 1.42g / mL, continue heating the beaker until the solution emits white smoke, The beaker was removed from the electric furnace, and cooled naturally to room temperature to obtain a Zr-Cu-Ni-Al amorphous alloy sam...

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Abstract

The invention provides a method for simultaneously determining Zr, Cu and Ni contents in Zr-Cu-Ni-Al amorphous alloy. The Zr, Cu and Ni are determined by using EDTA complexing back titration, the Zr, Cu, Ni and Al can be directly determined by using back titration in an acidic medium without interference according to a complexing stability constant; the Cu content and Ni content are determined by using the F- to shelter the Zr and Al under the acidity of pH 5-6, and the Ni content is determined by using thiorea to shelter the Cu, and the content of the Cu is obtained according to a computational formula. The contents of the Zr, Cu and Ni are determined in parallel through once sample preparation. The operation is free from electrolysis equipment, according to acidity ranges for EDTA complexing titration of different elements, the F- is used for sheltering the Zr and Al, and the thiorea is used for sheltering the Cu, so that the interference among the elements is eliminated, the titration end point sensitivity and the result accuracy are improved by using the back titration, and the content values of Zr, Cu and Ni can be fast and stably obtained.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis and relates to a method for jointly measuring the contents of Zr, Cu and Ni in a Zr-Cu-Ni-Al amorphous alloy. Background technique [0002] At present, there is no joint determination method for the content of Zr, Cu and Ni in Zr-Cu-Ni-Al amorphous alloy in the national standard and navigation standard. In "Chemical Analysis and Metrology" 1999 04, you can find "Combined Determination of Copper and Zirconium Content in Copper-Zirconium Master Alloy". Copper is separated by electrolysis and then measured by gravimetric method. The solution after separation of copper is directly titrated by EDTA volumetric method. In the above method, the copper separation process is complicated, and special electrolytic equipment is required, and it is not suitable for the determination of nickel-containing materials. In common analysis, high-content zirconium and nickel are separated by precipitation, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16G01N31/22G01N21/79
Inventor 马静刘朝岳航赵勇郭子静
Owner AECC AVIATION POWER CO LTD
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