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An analytical method for determining silicon in high-purity aluminum

An analysis method, silicon element technology, applied in the direction of thermal excitation analysis, material excitation analysis, etc., can solve the problems of incomplete dissolution of samples, long analysis period, uncertain selection of analysis lines, etc.

Active Publication Date: 2020-10-20
AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Corresponding analysis methods can be found for different alloy grades. Regarding the analysis of silicon in high-purity aluminum, there is currently no method for accurately analyzing this element at home and abroad. Disadvantages such as long analysis period

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0105] To measure silicon content 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: 1.0kW; reflected power: <10W; incident slit: 20μm; Exit slit: 15μm; argon gas flow: cooling gas flow: 13~20L / min; sheath gas flow: 0.5L / min; integration method: one point, maximum value; analysis line: 251.61nm;

[0106] (1), the reagents used in the determination process are as follows:

[0107] (1.1), hydrochloric acid, ρ1.19g / mL; high-purity or sub-boiling distillation reagent;

[0108] (1.2), nitric acid, ρ1.42g / mL; high-purity or sub-boiling distillation reagent;

[0109] (1.3), hydrochloric acid (1+1);

[0110] (1.4), sodium hydroxide solution, 100g / L;

[0111] (1.5), sodium hydroxide solution, 400g / L;

[0112] (1.6), silicon standard solution: 1.00 mg / mL; weigh 12.12 g of sodium silicate (Na2SiO3 9H2O) into a 500 mL beaker...

Embodiment 2

[0158] To measure silicon content 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: 1.2kW; reflected power: <10W; incident slit: 20μm; Exit slit: 15μm; argon gas flow: cooling gas flow: 15L / min; sheath gas flow: 0.2L / min; integration method: one point, maximum value; analysis line: 252.41nm;

[0159] (1), the reagents used in the determination process are as follows:

[0160] (1.1), hydrochloric acid, ρ1.19g / mL; high-purity or sub-boiling distillation reagent;

[0161] (1.2), nitric acid, ρ1.42g / mL; high-purity or sub-boiling distillation reagent;

[0162] (1.3), hydrochloric acid (1+1);

[0163] (1.4), sodium hydroxide solution, 100g / L;

[0164] (1.5), sodium hydroxide solution, 400g / L;

[0165] (1.6), silicon standard solution: 1.00 mg / mL; weigh 12.12 g of sodium silicate (Na2SiO3 9H2O) into a 500 mL beaker, a...

Embodiment 3

[0210] To measure silicon content 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: 1.5kW; reflected power: <10W; incident slit: 20μm; Exit slit: 15μm; argon gas flow: cooling gas flow: 20L / min; sheath gas flow: 0.4L / min; integration method: one point, maximum value; analysis line: 288.15nm;

[0211] (1), the reagents used in the determination process are as follows:

[0212] (1.1), hydrochloric acid, ρ1.19g / mL; high-purity or sub-boiling distillation reagent;

[0213] (1.2), nitric acid, ρ1.42g / mL; high-purity or sub-boiling distillation reagent;

[0214] (1.3), hydrochloric acid (1+1);

[0215] (1.4), sodium hydroxide solution, 100g / L;

[0216] (1.5), sodium hydroxide solution, 400g / L;

[0217] (1.6), silicon standard solution: 1.00 mg / mL; weigh 12.12 g of sodium silicate (Na2SiO3 9H2O) into a 500 mL beaker, a...

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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 silicon element in high aluminium. According to the invention, 5mL-15 mL of sodium hydroxide (100g / L) is added, an electric hot plate is controlled at about 120-150 V, heating is carried out for about 40-70 min, then the electric hot plate is taken out, cooling is carried out to room temperature, 2-5 mL of nitric acid is added, and the material is placed on the electric hot plate for reheating to dissolve salts. The method takes sodium hydroxide, hydrochloricacid, nitric acid, and hydrofluoric acid for dissolving a 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 of the method is wide, the measurement lower limit is 0.001%, and the measurement upper limit is 0.02%. The synchronous processing of a sample and preparation of a calibration solution are employed for measuring the silicon 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.

Description

technical field [0001] The invention belongs to high-purity metal trace element analysis technology, and relates to an analysis method for measuring silicon in high-purity aluminum. Background technique [0002] High-purity aluminum has many excellent properties and is widely used in electronics industry, aerospace, atomic energy industry, automobile manufacturing, transportation and other fields. 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 silicon in high-purity aluminum at home and abroad. Most of the silicon-related methods that can be found are molybdenum blue extraction photometry, n-butanol extraction photometry, and flame atomic absorption method (applicable to constants). etc., although there are also reports on the determination of silicon in metal materials by ICP-AES, but usua...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/73
CPCG01N21/73
Inventor 刘喜山张琮李刚叶晓英杨春晟
Owner AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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