Method for measuring contents of zinc, cadmium, tin and copper in silver-based brazing filler metal

A technology for silver-based solder and copper content, applied in the field of chemical analysis, can solve the problems of inconsistent sample processing methods, complicated copper separation process, experimental errors, etc., to meet the needs of fast and accurate detection, the determination method is fast and simple, and the analysis is shortened. effect of cycles

Pending Publication Date: 2022-07-12
AECC AVIATION POWER CO LTD
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AI Technical Summary

Problems solved by technology

The above methods are all wet chemical methods, in which the copper separation process is complicated and requires special electrolysis equipment
Tin is measured by the volumetric method, the test process is tedious and the cycle is long
The interfering elements are separated by precipitation method in the determination of zinc and cadmium. The test needs to undergo secondary separation. Experimental error, and the joint determination of zinc and cadmium will affect the accuracy of the results, which is greatly interfered by human factors
In summary, the pretreatment process of the above method is complicated, time-consuming, labor-intensive and material-consuming
[0003] There is no specific instrumental analysis method for silver-based solder in the current standard. The instrumental analysis methods that can be used for reference include GB / T10046-2018 "Silver Solder", GB / T11067-2006 "Silver Chemical Analysis Method for Copper by Flame Atomic Absorption Spectrometry" 》, the methods involved include electrolysis, volumetric method, atomic absorption method, and inductively coupled plasma atomic emission spectrometry, but the electrolytic method, volumetric method, and atomic absorption method are single-element analysis, the sample processing methods are inconsistent, and the test period is long. Part of the composition is affected by the accuracy of the elemental analysis results of the relevant joint determination
GB / T10046-2018 "Silver Solder" For tin-containing samples, it is necessary to measure copper by step-by-step electrolysis, and use inductively coupled plasma atomic emission spectrometry to measure the remaining components of the electrolyte after copper removal. The method test process is cumbersome and the cycle is long
The allowable difference of the method (the content range is 20% to 30%, and the allowable difference is 0.4%) cannot meet the accuracy requirements of the material, and cannot be directly applied to the analysis of silver-based solder

Method used

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  • Method for measuring contents of zinc, cadmium, tin and copper in silver-based brazing filler metal
  • Method for measuring contents of zinc, cadmium, tin and copper in silver-based brazing filler metal
  • Method for measuring contents of zinc, cadmium, tin and copper in silver-based brazing filler metal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] This embodiment is a method for jointly measuring the contents of Zn, Cd, Cu and Sn in BAg40CuZnCdSn.

[0043] Content range: Zn: 10.0% to 11.5%, Cd: 23.0% to 25.0%, Cu: 23.5% to 25.5%, Sn: 0.8% to 1.2%

[0044] Weighing of BAg40CuZnCdSn samples. Weigh 0.1017g sample and place it in a 250mL polytetrafluoroethylene beaker. Accurately weighed samples of BAg40CuZnCdSn were obtained.

[0045] Dissolution of BAg40CuZnCdSn sample. Add 10 mL of nitric acid to the 250 mL polytetrafluoroethylene beaker of the accurately weighed sample, put the beaker on an electric furnace and heat it up to 50°C for heating and dissolving. During the dissolving process, add 3 drops of hydrofluoric acid dropwise. After the solution is clear, add 10mL of hydrochloric acid and 50mL of distilled water were heated and boiled on an electric stove, removed after the silver chloride was coagulated, and cooled to room temperature naturally. The dissolved BAg40CuZnCdSn sample solution was obtained.

...

Embodiment 2

[0058] This embodiment is a method for jointly measuring the contents of Zn, Cd and Cu in BAg40CdZnCu(Ni)-S.

[0059] Content range: Zn: 17.3% to 18.8%, Cd: 25.1% to 26.5%, Cu: 15.5% to 16.5%

[0060] Weighing of BAg40CdZnCu(Ni)-S alloy samples. Weigh 0.1024g sample and place it in a 250mL polytetrafluoroethylene beaker. Accurately weighed samples of BAG40CDZNCU(NI)-S alloy were obtained.

[0061] Dissolution of BAg40CdZnCu(Ni)-S alloy samples. Add 10 mL of nitric acid to the 250 mL polytetrafluoroethylene beaker of the accurately weighed sample, put the beaker on an electric furnace and heat it up to 50 °C to heat and dissolve, when the solution is clear, add 10 mL of hydrochloric acid and 50 mL of distilled water, and heat and boil on the electric furnace , remove the silver chloride after condensation, and cool to room temperature naturally. The dissolved BAg40CdZnCu(Ni)-S alloy sample solution was obtained.

[0062] Constant volume of BAg40CdZnCu(Ni)-S alloy sample so...

Embodiment 3

[0074]This embodiment is a method for jointly measuring the contents of Zn, Cd and Cu in HBAg42CdCuZn.

[0075] Content range: Zn: 15.0% to 17.0%, Cd: 24.0% to 26.0%, Cu: 16.0% to 18.0%

[0076] Weighing of HBAg42CdCuZn sample. Weigh 0.1005g sample and place it in a 250mL polytetrafluoroethylene beaker. Accurately weighed samples of HBAg42CdCuZn were obtained.

[0077] Dissolution of HBAg42CdCuZn sample. Add 10 mL of nitric acid to the 250 mL polytetrafluoroethylene beaker of the accurately weighed sample, put the beaker on an electric furnace and heat it up to 50 °C to heat and dissolve, when the solution is clear, add 10 mL of hydrochloric acid and 50 mL of distilled water, and heat and boil on the electric furnace , remove the silver chloride after condensation, and cool to room temperature naturally. The dissolved HBAg42CdCuZn sample solution was obtained.

[0078] The constant volume of the HBAg42CdCuZn sample solution. Rinse the bottle wall of the dissolved sample ...

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Abstract

The invention discloses a method for measuring the content of zinc, cadmium, tin and copper in silver-based brazing filler metal, which comprises the following steps: weighing a sample, and preparing a sample solution; weighing pure silver, and preparing a bottoming solution; taking 4 parts of the priming solution to prepare a working curve series solution; measuring the spectral line intensity of each major element, and drawing a working curve of the method; and placing the sample solution in an inductively coupled plasma atomic emission spectrometer, and automatically calculating the mass percentage of each element to obtain the content of each element in the sample solution. The inductively coupled plasma atomic emission spectrometry is adopted, a sample solution is injected at a time, main elements of zinc, cadmium, tin and copper can be analyzed at the same time, the analysis period is shortened, the analysis and detection accuracy is improved, the purpose of synchronously and accurately analyzing multiple components is achieved, the operation time is short, the process is simple, the accuracy is high, and the precision is good; the rapid and accurate detection requirement of the silver-based brazing filler metal can be met.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis, and relates to a method for determining the contents of zinc, cadmium, tin and copper in silver-based solder. Background technique [0002] The main components of silver-based solder are silver, zinc, cadmium, tin, and copper. At present, EDTA volumetric method is used for zinc and cadmium, potassium iodate volumetric method is used for tin, and electrolysis-spectrophotometry is used for copper. The above methods are all wet chemical methods, in which the copper separation process is complicated and requires special electrolysis equipment. Tin is measured by volumetric method, and the test process is cumbersome and the cycle is long. When zinc and cadmium are measured, the interfering elements are separated by precipitation method, and the test needs to be separated twice. The measurement cycle is long, the operation is cumbersome, the use of reagents is large, and the pollution is la...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73
CPCG01N21/73Y02P10/20
Inventor 许丽刘朝马静王益芳张喆昱周雪
Owner AECC AVIATION POWER CO LTD
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