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Method for measuring indissolvable nickel-base superalloy multielement content with microwave digestion ICP method

A nickel-based superalloy, microwave digestion technology, applied in material excitation analysis, thermal excitation analysis and other directions, can solve the problems of affecting the measurement results, instrument pollution, inconsistent acidity of the solution, etc., to achieve high detection accuracy, good precision, reduce The effect of the matrix effect

Inactive Publication Date: 2016-02-10
GUIZHOU AEROSPACE PRECISION PRODS
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Problems solved by technology

However, hydrofluoric acid has a corrosive effect on the quartz sampling system of the inductively coupled high-frequency plasma atomic emission spectrometer, which is easy to pollute the instrument and affect the accuracy and repeatability of the measurement.
Moreover, the acidity of nitric acid sample solution and standard solution is used alone, which will easily lead to inconsistent acidity of the solution and affect the measurement results.

Method used

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  • Method for measuring indissolvable nickel-base superalloy multielement content with microwave digestion ICP method

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Embodiment

[0019] A kind of microwave digestion ICP method of the present invention measures the multielement content method of refractory nickel base superalloy, comprises the following steps:

[0020] a. Weigh 0.1g of insoluble nickel-based superalloy sample and place it in a microwave digestion tank, then add 6mL~7mL of hydrochloric acid with a concentration of 1.19g / mL, cover and tighten the lid, and then digest the sample Put the jar into the microwave digestion apparatus;

[0021] b. Start the microwave digestion instrument, and perform intermittent microwave digestion according to the following microwave digestion procedures:

[0022]

[0023] That is, the power is 800W, the heating program is 10 minutes, the temperature is raised to 200°C, and then the heat is kept for 30 minutes, and then the same power is used, the temperature is raised to 100°C, and the temperature is held for 10 minutes. Repeat the above process once, and finally at 50°C. Keep warm for 10 minutes to compl...

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Abstract

The invention discloses a method for measuring the indissolvable nickel-base superalloy multielement content with the microwave digestion ICP method. According to the method, a sample is digested in a microwave digestion instrument with hydrochloric acid, the acidity of a sample solution and the acidity of a standard solution are stabilized with a sulfuric acid and phosphoric acid mixture, then citric acid is added to prevent high-valent metal ion hydrolysis, the content of a matrix is adjusted for the matching purpose, a standard solution curve is made finally, and a proper analytical line is selected for measurement on an inductive coupling high-frequency plasma atomic emission spectrometer. Due to the fact that the sample is digested by means of hydrochloric acid, pollution to a hydrofluoric acid eroding instrument by a quartz feeding system of the instrument is avoided, and then measurement accuracy can not be affected. Meanwhile, the acidity of the sample solution and the acidity of the standard solution are stabilized with the sulfuric acid and phosphoric acid mixture, then citric acid is added to prevent high-valent metal ion hydrolysis, the content of the matrix is adjusted for the matching purpose, and therefore matrix effect is reduced.

Description

technical field [0001] The invention relates to a method for measuring the multi-element content of an insoluble nickel-based superalloy, in particular to a method for measuring the multi-element content of an insoluble nickel-based superalloy by a microwave digestion ICP method. Background technique [0002] At present, in terms of the means of detecting superalloy elements, inductively coupled plasma (ICP) emission spectrometer has been used since its introduction in 1975 because of its low detection limit, high precision, wide linear range of concentration determination, and small mutual interference between sample components. It has become an analytical method unmatched by other analytical techniques in the simultaneous determination of trace elements. [0003] The traditional sample pretreatment method for insoluble nickel-based superalloy analysis is: use hydrofluoric acid to dissolve the sample, and use nitric acid to adjust the acidity of the sample solution and stan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/71
Inventor 李正权先世兵蒋忠伦
Owner GUIZHOU AEROSPACE PRECISION PRODS
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