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Method for determining arsenic, antimony and bismuth content of pure chromium by using atomic fluorescence spectrometry

A technique of atomic fluorescence spectroscopy and pure chromium, which is applied in the field of alloy trace element analysis, can solve the problems of high maintenance cost, expensive equipment, strict requirements on the environment and reagents, etc., to save manpower and material resources, low maintenance cost, and wide range of measurement wide effect

Inactive Publication Date: 2013-01-16
AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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Problems solved by technology

[0004] Inductively coupled plasma mass spectrometer (ICP-MS) is expensive, with high cost of use and maintenance, strict requirements on the environment and reagents, and the measurement of element As is greatly disturbed, resulting in a high detection limit; atomic absorption spectrometry (AAS ) processing process is complicated, and the sensitivity is relatively low; atomic fluorescence technology is highly sensitive in determining As, Sb, Bi, the instrument is cheap, and the processing process is simple, but atomic fluorescence technology is mostly used in food, biology, etc., but not in raw materials Field metal chemical analysis

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  • Method for determining arsenic, antimony and bismuth content of pure chromium by using atomic fluorescence spectrometry
  • Method for determining arsenic, antimony and bismuth content of pure chromium by using atomic fluorescence spectrometry
  • Method for determining arsenic, antimony and bismuth content of pure chromium by using atomic fluorescence spectrometry

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Embodiment

[0055] Determination of arsenic, antimony and bismuth content in pure chromium (mass fraction not less than 99.99%) for refining superalloys, the technical specifications stipulate that As≤0.0005%, Sb≤0.0005%, Bi≤0.0005%. It is characterized in that: the steps of the assay method are:

[0056] (1) The reagents used in the determination process of this method are:

[0057] 1.1 Hydrochloric acid, ρ1.19g / mL; superior grade or MOS grade;

[0058] 1.2 Nitric acid, ρ1.42g / mL; superior grade or MOS grade;

[0059] 1.3 Sulfuric acid 1+1, superior grade;

[0060] 1.4 Sulfuric acid 1+4, superior grade;

[0061] 1.5 Citric acid solution, 400g / L, the preparation method is to weigh 400g of high-grade pure citric acid and place it in a 500mL beaker. After the solution is completely dissolved, transfer it into a 1000mL volumetric flask, dilute with water to the mark, and mix well;

[0062] 1.6 The mixed solution of thiourea-ascorbic acid is prepared by weighing 10g of superior pure thiou...

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Abstract

The invention discloses a method for determining the arsenic, antimony and bismuth content of pure chromium by using atomic fluorescence spectrometry. The method comprises the following steps of: weighing a specimen; preparing a sample solution; preparing a calibration solution; drawing a working curve; measuring the concentrations of arsenic, antimony and bismuth in the sample solution; and calculating measurement results to obtain the arsenic, antimony and bismuth content. The method for determining the arsenic, antimony and bismuth content of the pure chromium is a hydride generation atomic fluorescence method, is high in analysis sensitivity, convenient to operate, short in analysis cycle and high in efficiency, has broad application prospect, and can be used for measuring the impurities arsenic, antimony and bismuth in the pure chromium which is a widely used raw material. Brazing performance can be greatly influenced by low-melting point impurity elements such as the arsenic, the antimony and the bismuth, and the like, and once the content of the elements exceeds a standard, the mechanical performance of materials can be greatly degraded, so that an accurate and reliable method is required by the measurement of the content of the elements. The requirements of scientific researches and production on control over the quality of raw materials are met, the rejection rate of the product is lowered, and development and production cost is saved.

Description

technical field [0001] The invention belongs to alloy trace element analysis technology and belongs to the technical field of alloy element analysis and measurement. Background technique [0002] With the development of the national defense industry, new materials are constantly introduced, and the requirements for various materials with excellent performance are becoming more and more stringent. The content of impurity elements in the alloy is very important to the performance of the material. The existence of will seriously affect the performance of the material, once its content exceeds the allowable limit, it will bring great harm to the alloy. Purification of alloy components must first control the impurity components of raw materials. Only high-purity raw materials can smelt high-purity alloys. As an important raw material of superalloys, pure chromium needs to strictly control the above-mentioned low melting point elements. However, after checking domestic and forei...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/64
Inventor 庞晓辉高颂高帅白雪峰张艳
Owner AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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