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Testing method for detecting low-melting-point material by glow discharge mass spectrometry

A technology of glow discharge mass spectrometry and testing method, which is applied in the field of glow discharge mass spectrometry to detect low melting point materials, which can solve problems such as solid samples are easy to melt, drip into the instrument, damage the instrument and pollute, and reduce the pre-sputtering time , Small matrix effect, good environmental protection effect

Pending Publication Date: 2022-02-11
江西省钨与稀土产品质量监督检验中心(江西省钨与稀土研究院)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the analysis of low melting point material components by glow discharge mass spectrometry, the existing two sample preparation methods have the following deficiencies: such as figure 1 As shown, no matter it is needle-shaped or block-shaped, when the cooled solid sample is directly injected, when a large operating voltage and operating current are used, one is that the temperature of the front surface of the sample is higher during the ionization process of the sample, so that The solid sample with low melting point is easy to melt, thus dripping into the inside of the instrument, thereby damaging the instrument and contaminating it; second, the temperature of the electrode 1 on the back of the sample is relatively high during the sputtering process, and direct contact with electrode 1 is more likely to melt the sample, resulting in The test fails, and the molten sample flows directly into the contacted electrode, causing damage and contamination of the electrode

Method used

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  • Testing method for detecting low-melting-point material by glow discharge mass spectrometry
  • Testing method for detecting low-melting-point material by glow discharge mass spectrometry
  • Testing method for detecting low-melting-point material by glow discharge mass spectrometry

Examples

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Embodiment 1

[0036] A test method for detecting low melting point materials by glow discharge mass spectrometry, comprising the steps of:

[0037] Step 1. Using high-purity tantalum to make a tantalum carrier with a circular groove in the middle;

[0038] Step 2. Put the tantalum carrier into the mixture of concentrated nitric acid, hydrogen fluoride and water for pickling, then soak for 30s, then wash it with ultrapure water once, and then put it into the mixture of concentrated sulfuric acid, hydrogen peroxide and water to acid again Wash, then ultrasonicate three times with deionized water and absolute ethanol successively, each time for 1min, and then blow dry with compressed air to obtain the treated tantalum carrier;

[0039] Step 3. Put the gallium indium tin alloy in a clean beaker, put it into an oil bath in hot oil or a water bath in hot water, and make it fully melt to obtain a liquid gallium indium tin alloy, and then take an appropriate amount of liquid gallium indium tin allo...

Embodiment 2

[0048] A test method for detecting low melting point materials by glow discharge mass spectrometry, comprising the steps of:

[0049] Step 1. Using high-purity metal to make a metal carrier with a circular groove in the middle;

[0050] Step 2: Put the metal carrier into the mixture of concentrated nitric acid, hydrogen fluoride and water for pickling, then soak for 30s, then wash it with ultrapure water once, and then put it into the mixture of concentrated sulfuric acid, hydrogen peroxide and water to pickle again Wash, then ultrasonicate three times with deionized water and absolute ethanol successively, each time for 1min, and then blow dry with compressed air to obtain the treated metal carrier;

[0051] Step 3. Put the low melting point material in a clean beaker, put it into an oil bath in hot oil or a water bath in hot water, make it fully melt, and obtain a liquid low melting point material, and then take an appropriate amount of liquid low melting point material and ...

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Abstract

The invention discloses a testing method for detecting a low-melting-point material by glow discharge mass spectrometry. The testing method comprises the following steps of 1, manufacturing a metal carrier; 2, obtaining a treated metal carrier; 3, a liquid low-melting-point material being obtained, and then a proper amount of the liquid low-melting-point material being taken and poured into the circular groove; 4, sequentially rinsing the surface of the solidified to-be-detected sample with deionized water ethanol for three times, and then naturally airing and putting into a sample cup; and 5, cooling the ion source chamber, connecting the sample cup with an electrode, pushing the sample cup into the ion source chamber, and detecting impurity components. According to the method, complex pretreatment is avoided, so analysis efficiency is improved, impurity interference caused by pretreatment is avoided for component analysis of the high-purity low-melting-point material, accuracy of an analysis result is ensured, and the method can be used for simultaneously analyzing multiple elements, has advantages of high analysis speed, small matrix effect, good environmental friendliness and the like, and has wide application prospects.

Description

technical field [0001] The invention relates to a test method for detecting low-melting point materials by glow discharge mass spectrometry. Background technique [0002] Glow discharge mass spectrometry is to put the sample to be analyzed into the ion source chamber as a cathode, and then apply a voltage through the electrode to ionize the inert gas to generate positively charged positive ions and negatively charged electrons, which are combined with a large number of metastable states. Neutral particles make up the plasma. Under the action of an electric field, positive ions rapidly bombard the surface of the sample and sputter out the cathode material. After the atoms sputtered from the cathode diffuse into the negative glow area, they collide with the metastable inert gas atoms and electrons, and ionize to form positively charged ions to be measured. After the ions are generated, they enter the dual mass analyzer of electric field and magnetic field, the matrix is ​​de...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/68
CPCG01N27/68
Inventor 孙娜李平蒋威徐娜陈文宋旭东
Owner 江西省钨与稀土产品质量监督检验中心(江西省钨与稀土研究院)
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