Method for detecting content of trace impurity content in metal by glow-discharge mass spectrometry

A technology of glow discharge mass spectrometry and trace impurities, which is used in measurement devices, material analysis by electromagnetic means, instruments, etc., can solve the problems of low sensitivity and resolution, and achieve a wide range of analysis, low detection limit, and less interference. Effect

Inactive Publication Date: 2016-12-07
锦州市国家光伏材料质量监督检验中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of this, the object of the present invention is to provide a method for detecting the content of trace impurity elements in metals by glow discharge mass spectrometry, which solves the problems of low sensitivity and resolution

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  • Method for detecting content of trace impurity content in metal by glow-discharge mass spectrometry

Examples

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Embodiment 1

[0029] The method for detecting the content of trace impurity elements in high-purity copper (equivalent concentration ≥ 5N) by glow discharge mass spectrometry in the present embodiment includes the following steps:

[0030] The high-purity copper sample is processed into a tetrahedron with a thickness of 3.5mm, a length of 21mm and a width of 18mm, and the sample is placed in a nitric acid solution with a volume concentration of 28%. Ultrasonic cleaning, washing with pure water, repeated ultrasonic cleaning and pure water washing, then washing with absolute ethanol, drying for use;

[0031] Vacuum the sample chamber of the glow discharge mass spectrometer, open the ball valve, push the dried sample into the ion source cavity, turn on the high voltage and glow, pass in argon, adjust the discharge voltage to 2.6KV, and the discharge current to 2.4 mA, perform ion source tuning, adjust the Beam Centering parameters to obtain the signal peak with the highest sensitivity; adjust ...

Embodiment 2

[0034] The method for detecting the content of trace impurity elements in high-purity copper (equivalent concentration ≥ 5N) by glow discharge mass spectrometry in the present embodiment includes the following steps:

[0035] The high-purity copper sample is processed into a tetrahedron with a thickness of 3mm, a length of 22mm and a width of 20mm. The sample is placed in a nitric acid solution with a volume concentration of 25%, and hydrofluoric acid accounting for 1wt% of the nitric acid solution can be added to perform ultrasonic waves. Cleaning, wash with pure water, repeat ultrasonic cleaning and pure water washing, then wash with absolute ethanol, dry for use;

[0036] Evacuate the sample chamber of the glow discharge mass spectrometer, open the ball valve, push the dried sample into the ion source cavity, turn on the high voltage and glow, pass in argon, adjust the discharge voltage to 2.6KV, and the discharge current to 2.6mA , perform ion source tuning, adjust the Bea...

Embodiment 3

[0039] The method for detecting the content of trace impurity elements in high-purity copper (equivalent concentration ≥ 5N) by glow discharge mass spectrometry in the present embodiment includes the following steps:

[0040] The high-purity copper sample is processed into a tetrahedron with a thickness of 2.6 mm, a length of 18 mm and a width of 16 mm, and the sample is placed in a nitric acid solution with a volume concentration of 30%. Ultrasonic cleaning, rinse with pure water, repeat ultrasonic cleaning and pure water cleaning, then rinse with absolute ethanol, and dry for use;

[0041] Vacuum the sample chamber of the glow discharge mass spectrometer, open the ball valve, push the dried sample into the ion source cavity, turn on the high voltage and glow, pass in argon, adjust the discharge voltage to 2.2KV, and the discharge current to 2.1mA , perform ion source tuning, adjust the Beam Centering parameters to obtain the signal peak with the highest sensitivity; adjust t...

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Abstract

The invention provides a method for detecting content of trace impurity content in metal by a glow-discharge mass spectrometry. The method comprises the following steps: 1) processing a metal sample to a sheet shape or a needle shape, putting the metal sample in a nitric acid solution for performing ultrasonic cleaning, and drying the material; 2)performing vacuum-pumping on a sample warehouse of a glow-discharge mass spectrometer, opening a ball valve, pushing the metal sample into an ion source chamber, opening high pressure and glow, introducing work gas, adjusting discharge voltage and discharge current, adjusting resolution to 3000-4800 through ion source tuning, wherein the matrix peak intensity is 0.05-0.25 V, and pre-sputtering for 30-80 min; and 3) selecting a metal matrix and the impurity element required to be determined, and performing a direct current glow discharge mass spectrometry to obtain the concentration of metal trace impurity. According to the invention, grinding and polishing are not required for a cut sample according to the specification, the sample is only required for being cleaned, pollution can be effectively avoided; sampling is directly carried out, operation is simple and easy; effective tuning is carried out on the ion source, sensitivity is high, detection limit is low, resolution is high, and one-time analysis of the main content elements to ppt-grade element can be carried out.

Description

technical field [0001] The invention relates to the field of detection of trace impurity elements in metals, in particular to a method for detecting the content of trace impurity elements in metals by glow discharge mass spectrometry. Background technique [0002] At present, the determination methods for the analysis of trace impurities in metals include inductively coupled plasma optical emission spectroscopy (ICP-OES), inductively coupled plasma mass spectrometry (ICP-MS), X-ray fluorescence spectroscopy (XRF) and secondary ion mass spectrometry. (SIMS) method, etc., these methods are cumbersome and difficult to master, the process is long, and they are easy to be polluted. [0003] Glow discharge mass spectrometry (GD-MS) allows direct analysis of solid samples, and metal matrices with good electrical conductivity are an advantage for GD-MS analytical applications, such as metals copper, iron, zinc, lead, aluminum, gallium, tantalum , cobalt, titanium, cadmium, antimony...

Claims

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Application Information

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IPC IPC(8): G01N27/68
CPCG01N27/68
Inventor 白杉王爽徐平朱雷朱哲周渊名刘波赫涛
Owner 锦州市国家光伏材料质量监督检验中心
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