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Method for analyzing small-size conductive and non-conductive materials by applying glow discharge mass spectrometry

A technique of glow discharge mass spectrometry and non-conductive materials, which is applied to the analysis of materials, material analysis by electromagnetic means, and preparation of test samples. It can solve problems such as poor discharge stability, complicated pretreatment, and easy pollution, and achieve Good discharge stability, simple pre-treatment, and the effect of avoiding pollution

Pending Publication Date: 2021-10-19
国合通用测试评价认证股份公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a brand-new method of applying glow discharge mass spectrometry to analyze small-sized conductive materials and non-conductive materials, so as to solve the problems in the prior art of "complicated pre-treatment, easy pollution, poor discharge stability, and limited application range." Narrow" and other defects

Method used

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  • Method for analyzing small-size conductive and non-conductive materials by applying glow discharge mass spectrometry
  • Method for analyzing small-size conductive and non-conductive materials by applying glow discharge mass spectrometry
  • Method for analyzing small-size conductive and non-conductive materials by applying glow discharge mass spectrometry

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Experimental program
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Effect test

Embodiment 1

[0045] Nitric acid (HNO 3 ) and ultrapure water, ultrasonically cleaned, then ultrasonically twice in ultrapure water, and finally washed with ethanol and dried in the air. Put the graphite powder in an aluminum cup with a height of about 5mm and a diameter of 25mm. The thickness of the graphite powder is about 3-4mm. Gently shake the aluminum cup to make the surface of the graphite powder smooth. Use tweezers to pick up several pieces of scrap metal ytterbium and place them on the graphite powder. The diameter covered by scrap metal ytterbium is ≥ 10mm, and the thickness is the thickness of a layer of scrap metal ytterbium. Compress under ~10MPa. Put the pressed sample into the dc-GDMS chip sample cell for analysis, the discharge voltage is 1.2kV, the discharge current is 1.5mA, the argon gas flow rate is 350mL / min, the content of typical elements in different time periods is detected, and the inductively coupled plasma Method comparison by mass spectrometry (ICP-MS).

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Embodiment 2

[0054] Put the graphite powder in an aluminum cup with a height of about 5mm and a diameter of 25mm. The thickness of the graphite powder is 3-4mm. Gently shake the aluminum cup to make the surface of the graphite powder smooth. Take an appropriate amount of ytterbium oxide powder and place it on the graphite powder. The diameter covered by the ytterbium oxide powder is 5mm, and the thickness is 0.5mm. The surface is covered with several layers of sulfuric acid paper, and pressed into a sheet under a pressure of 5-10MPa in a tablet press. The samples were put into the dc-GDMS flake sample cell for analysis, the discharge voltage was 1.3kV, the discharge current was 1.5mA, and the flow rate of argon gas was 400mL / min. ICP-MS) for method comparison.

[0055] The discharge stability of the method of the present invention is characterized by the contents of typical elements detected in different time periods. The relative standard deviation (RSD%) of the typical element content d...

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Abstract

The invention relates to a method for analyzing small-size conductive and non-conductive materials by applying glow discharge mass spectrometry, and belongs to the field of material analysis. The method comprises the following steps: placing graphite powder in an aluminum cup, and slightly vibrating the aluminum cup to flatten the surface of the graphite powder; placing a small-size conductive material or a non-conductive material on the graphite powder; covering with a plurality of layers of parchment paper; pressing by using a tablet press to prepare a test sample; and carrying out direct current glow discharge mass spectrometry. According to the analysis method, grinding, sintering and heating are not needed, the pretreatment is simple, and the pollution is avoided; the problem that the metal element cannot be measured when the metal is used as a conducting medium and the mass spectrum interference formed by the metal element are avoided; the analysis time is shortened, and the analysis efficiency is improved; the method can be suitable for analysis of small-size conductive materials such as crumb-shaped, granular and powdery conductive materials and fine-granular and powdery non-conductive materials, and is high in universality and wide in application range; the method has good discharge stability, analysis repeatability and analysis accuracy.

Description

technical field [0001] The invention relates to a method for analyzing small-sized conductive and non-conductive materials by using glow discharge mass spectrometry, in particular to a new method for analyzing small-sized conductive and non-conductive materials by using direct current glow discharge mass spectrometry (dc-GDMS), belonging to field of material analysis. Background technique [0002] Glow discharge mass spectrometry (GDMS) is an analytical method for direct sampling of solids. It has high sensitivity, high resolution and low detection limit. It is an ideal technical method for purity analysis of high-purity solid materials. [0003] Direct current glow discharge mass spectrometry (dc-GDMS) has its specific discharge battery and ion source, and has certain requirements on the size and conductivity of the material to be analyzed. The sputtering spot diameters of existing glow discharge mass spectrometers are generally 8 mm and 10 mm, so the size of the material ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/68G01N1/28
CPCG01N27/68G01N1/28G01N1/286
Inventor 胡芳菲刘红李爱嫦刘鹏宇杨复光赵景鑫夏雯
Owner 国合通用测试评价认证股份公司
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