Analysis method for determining gallium element in high aluminium

An analytical method and high-purity technology, applied in the field of high-purity metal trace element analysis, can solve the problems of unfavorable rapid determination, many operation steps, high labor intensity, etc., and achieve fast measurement, good method repeatability, saving manpower and material resources. Effect

Inactive Publication Date: 2018-08-03
AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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Problems solved by technology

At present, there is no standard method for the analysis of gallium in high-purity aluminum at home and abroad. Most of the available methods for gallium are extraction and separation rhodamine B spectrophotometry, butyl rhodamine B spectrophotometry, and graphite furnace atomic absorption method. etc. These methods have many operation steps, high labor intensity and long time, which is not conducive to rapid determination; the found inductively coupled plasma mass spectrometry and inductively coupled plasma mass spectrometry are respectively aimed at the detection of gallium in steel and alloys and precious metal alloys , which is very different from high-purity aluminum materials. If the above method is used, a large number of experimental verifications are required. Therefore, the existing method is not suitable for the analysis of gallium in high-purity aluminum from two aspects.

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  • Analysis method for determining gallium element in high aluminium

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Determination of gallium content in high-purity aluminum, using inductively coupled plasma atomic emission spectrometer, the working conditions and analysis lines of the instrument are as follows: high-frequency frequency: 40.68MHz; incident power: 0.95~1.5kW; reflected power: <15W; argon gas flow : Cooling air flow: 13-20L / min; auxiliary air flow: 0.2-1.0L / min; pump speed: flushing pump speed 110-190rpm; analysis pump speed 110-190rpm; visible integration time: 2-10s;

[0062] (1.1) Hydrochloric acid, ρ1.19g / mL; MOS grade or sub-boiling distillation reagent;

[0063] (1.2) Nitric acid, ρ1.42g / mL; MOS grade or sub-boiling distillation reagent;

[0064] (1.3) Sulfuric acid, ρ1.84g / mL; high-purity reagent or superior grade;

[0065] (1.4) hydrochloric acid, 1+1;

[0066] (1.5) Sulfuric acid, 1+1;

[0067] (1.6) Sodium hydroxide solution, 100g / L;

[0068] (1.7) Gallium standard solution: 0.50 mg / mL; Weigh 0.5000 g of pure gallium with a purity >99.99%, put it in a 200 ...

Embodiment 2

[0105] To measure the content of gallium in high-purity aluminum, an inductively coupled plasma emission spectrometer is used. The working conditions and analysis lines of the instrument are as follows: high-frequency frequency: 40.68MHz; incident power: 0.95~1.5kW; reflected power: <15W; argon flow: Cooling air flow: 13-20L / min; auxiliary air flow: 0.2-1.0L / min; pump speed: flushing pump speed 110-190rpm; analysis pump speed 110-190rpm; visible integration time: 2-10s;

[0106] (1.1) Hydrochloric acid, ρ1.19g / mL; MOS grade or sub-boiling distillation reagent;

[0107] (1.2) Nitric acid, ρ1.42g / mL; MOS grade or sub-boiling distillation reagent;

[0108] (1.3) Sulfuric acid, ρ1.84g / mL; high-purity reagent or superior grade;

[0109] (1.4) hydrochloric acid, 1+1;

[0110] (1.5) Sulfuric acid, 1+1;

[0111] (1.6) Sodium hydroxide solution, 100g / L;

[0112] (1.7) Gallium standard solution: 0.50 mg / mL; Weigh 0.5000 g of pure gallium with a purity >99.99%, put it in a 200 mL bea...

Embodiment 3

[0149] To measure the content of gallium in high-purity aluminum, an inductively coupled plasma emission spectrometer is used. The working conditions and analysis lines of the instrument are as follows: high-frequency frequency: 40.68MHz; incident power: 0.95~1.5kW; reflected power: <15W; argon flow: Cooling air flow: 13-20L / min; auxiliary air flow: 0.2-1.0L / min; pump speed: flushing pump speed 110-190rpm; analysis pump speed 110-190rpm; visible integration time: 2-10s;

[0150] (1.1) Hydrochloric acid, ρ1.19g / mL; MOS grade or sub-boiling distillation reagent;

[0151] (1.2) Nitric acid, ρ1.42g / mL; MOS grade or sub-boiling distillation reagent;

[0152] (1.3) Sulfuric acid, ρ1.84g / mL; high-purity reagent or superior grade;

[0153] (1.4) hydrochloric acid, 1+1;

[0154] (1.5) Sulfuric acid, 1+1;

[0155] (1.6) Sodium hydroxide solution, 100g / L;

[0156] (1.7) Gallium standard solution: 0.50 mg / mL; Weigh 0.5000 g of pure gallium with a purity >99.99%, put it in a 200 mL bea...

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Abstract

The invention belongs to the technical field of high-purity trace element analysis, and relates to an analysis method for determining a gallium element in high aluminium. According to the invention, 10 mL-20 mL of hydrochloric acid (1+1) and 3-8 mL of nitric acid are added, and heating is carried out for dissolving a sample. The method takes dilute hydrochloric acid and nitric acid for dissolvingthe sample to obtain a clarified sample solution; an optimum analysis spectral line is determined through interference experiments, and the measurement accuracy is increased; a determination scope ofthe method is wide, the measurement lower limit is 0.005%, and the measurement upper limit is 0.005%. The synchronous processing of a sample and preparation of a calibration solution are employed formeasuring the gallium element, the analysis error is minimum, and the method repeatability is good; the recovery rate and the precision are good; through standard sample analysis and method reinspection, the analysis method has the advantages of good accuracy and stable method, and completely accords with the requirement of trace element analysis. The method has the advantages of fast measurement,simple operation, and saves a lot of manpower and material resources.

Description

technical field [0001] The invention belongs to high-purity metal trace element analysis technology, and relates to an analysis method for measuring gallium in high-purity aluminum. Background technique [0002] High-purity aluminum is silver-white, with a smooth surface, clear crystal lines, and no inclusions. High-purity aluminum has low deformation resistance, high electrical conductivity and good plasticity, etc. It is mainly used in scientific research, electronics industry, chemical industry and manufacturing high-purity alloys, laser materials and some other special purposes. With the further understanding and development of the properties of high-purity aluminum, the application prospects of high-purity aluminum are becoming more and more broad. At present, there is no standard method for the analysis of gallium in high-purity aluminum at home and abroad. Most of the available methods for gallium are extraction and separation rhodamine B spectrophotometry, butyl rho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73
CPCG01N21/73
Inventor 刘喜山李刚张琮杨春晟叶晓英
Owner AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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