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Method for detecting gallium in glow discharge mass spectrometry

A glow discharge mass spectrometry and detection method technology, applied in the field of mass spectrometry detection, can solve the problems of poor reproducibility, unstable GDMS discharge, and low signal intensity of the matrix, so as to ensure accuracy, avoid the introduction of impurities, and shorten the analysis time Effect

Pending Publication Date: 2020-09-08
KONFOONG MATERIALS INTERNATIONAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] CN110186997A discloses a method for detecting the content of impurity elements in aluminum hydroxide by glow discharge mass spectrometry, which relates to the technical field of trace element analysis of inorganic materials, and solves the problem that aluminum hydroxide samples contain crystal water, resulting in unstable discharge of GDMS and matrix Problems such as low signal strength and poor reproducibility

Method used

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Embodiment 1

[0055] This embodiment provides a detection method of gallium in glow discharge mass spectrometry, the detection method of the sample: sequentially cooling and sputtering the gallium samples to be detected after sample preparation and testing;

[0056] Wherein, the cooling time is 12min; the voltage in the sputtering is 0.9kV; the current in the sputtering is 1.2mA; the argon flow rate is adjusted in the sputtering so that the signal strength reaches 2×10 -10 A;

[0057] The sample preparation process includes:

[0058] (1) The solid gallium sample is subjected to acid soaking, rinsing and heat treatment in sequence to obtain liquid gallium; wherein, the acid solution in the acid bubble is a nitric acid solution; the nitric acid mass concentration in the nitric acid solution is 30%; the acid bubble The time of the rinsing is 16min; the medium of the rinsing is water; the time of the rinsing is 0.5min; the rinsing is carried out 3 times; The temperature is 60°C; the heating t...

Embodiment 2

[0063] This embodiment provides a detection method of gallium in glow discharge mass spectrometry, the detection method of the sample: sequentially cooling and sputtering the gallium samples to be detected after sample preparation and testing;

[0064] Wherein, the cooling time is 15min; the voltage in the sputtering is 1kV; the current in the sputtering is 1.5mA; the argon flow rate is adjusted in the sputtering so that the signal strength reaches 4×10 -10 A;

[0065] The sample preparation process includes:

[0066] (1) The solid gallium sample is subjected to acid soaking, rinsing and heat treatment in sequence to obtain liquid gallium; wherein, the acid solution in the acid bubble is a nitric acid solution; the nitric acid mass concentration in the nitric acid solution is 35%; the acid bubble The time of the rinsing is 20min; the medium of the rinsing is water; the time of the rinsing is 1min; the rinsing is carried out 4 times; The temperature is 60°C; the heating time ...

Embodiment 3

[0071] This embodiment provides a detection method of gallium in glow discharge mass spectrometry, the detection method of the sample: the sample to be detected after the sample preparation process is subjected to refrigeration and sputtering in sequence and tested;

[0072] Wherein, the cooling time is 10min; the voltage in the sputtering is 0.8kV; the current in the sputtering is 1.4mA; the argon flow rate is adjusted in the sputtering so that the signal intensity reaches 3×10 -10 A;

[0073] The sample preparation process includes:

[0074] (1) The solid gallium sample is subjected to acid soaking, rinsing and heat treatment in sequence to obtain liquid gallium; wherein, the acid solution in the acid bubble is a nitric acid solution; the nitric acid mass concentration in the nitric acid solution is 40%; the acid bubble The time of the rinsing is 18min; the medium of the rinsing is water; the time of the rinsing is 0.7min; the rinsing is carried out 3 times; The temperatur...

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Abstract

The invention relates to a method for detecting gallium in glow discharge mass spectrometry. The method comprises the following steps of sequentially refrigerating and sputtering a gallium sample to be detected, which is subjected to sample preparation treatment, and then testing. According to the detection method provided by the invention, introduction of impurities can be avoided, the analysis time is shortened, accuracy of data is ensured, meanwhile, a relatively strong signal can be obtained through the detection method provided by the invention, and detection sensitivity is high.

Description

technical field [0001] The invention relates to the field of mass spectrometry detection, in particular to a method for detecting gallium in glow discharge mass spectrometry. Background technique [0002] Glow discharge mass spectrometry (GDMS) is currently the most effective method for the analysis of trace and trace impurities in high-purity solid materials. Glow discharge mass spectrometer has the advantages of high sensitivity, low detection limit, and wide range of elemental analysis. The glow discharge mass spectrometer consists of two parts: the tantalum part of the glow discharge ion source and the mass spectrometer. The tantalum part of the glow discharge ion source uses an inert gas (usually argon) to ionize at a voltage of thousands of volts. The ions produced by the ionization hit the surface of the sample to cause sputtering (that is, atomization), and the sputtered atoms diffuse into the plasma for further ions Through the magnetic field and the electric fiel...

Claims

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Application Information

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IPC IPC(8): G01N27/68G01N1/34
CPCG01N27/68G01N1/34
Inventor 姚力军潘杰边逸军王学泽周童
Owner KONFOONG MATERIALS INTERNATIONAL CO LTD
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