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A cage-shaped sampling device and sample testing method for glow discharge mass spectrometry analysis

A technology of glow discharge mass spectrometer and sampling device, which is applied in the direction of material analysis, measuring device, and material analysis through electromagnetic means, and can solve problems such as test failure, easy melting, and increased testing costs

Active Publication Date: 2021-10-01
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the metal indium used in the sample preparation process has a low melting point and needs to be discharged after cooling down. It is easy to melt during the long-term discharge process, which leads to the failure of the test.
And because it cannot be reused, it increases the detection cost
Using the tantalum groove method can avoid the cumbersome pretreatment of small-sized samples, but the tantalum groove reduces the measurable area of ​​the sample, resulting in a decrease in signal intensity and a poor detection limit, which cannot take advantage of the GD-MS method
At the same time, the sample is easy to fall off from the opening of the tantalum slot during the push and pull process of the injection rod, which seriously affects the detection speed

Method used

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  • A cage-shaped sampling device and sample testing method for glow discharge mass spectrometry analysis
  • A cage-shaped sampling device and sample testing method for glow discharge mass spectrometry analysis
  • A cage-shaped sampling device and sample testing method for glow discharge mass spectrometry analysis

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Experimental program
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Effect test

Embodiment 1

[0047] Cage tantalum slots (a, b, c), tantalum slots (d), granular Al 2 o 3 Dilute nitric acid (preferably 1:1 nitric acid (HNO 3 ) and ultrapure water), ultrasonically cleaned twice in ultrapure water, and finally washed with absolute ethanol and dried. Put the cleaned sample into the cage sampling device, and put the combination into the GD-MS needle sample cell for analysis after vacuuming. The optimized discharge voltage: 2.5 kV, discharge current: 3.0 mA, discharge gas (Ar) Flow rate: 1.0 cc / min. Then, the signal intensity of the elements in the sample was measured over time to further characterize the stability of the method. At the same time, the GD-MS signal intensity test was performed on the same sample by using the tantalum bath method as the data of the control group. Test results such as image 3 As shown, the results show that when the cage sample injection device with the size of 15 mm×5 mm×5 mm is used for analysis, good signal strength and discharge stabi...

Embodiment 2

[0049] The caged tantalum groove, tantalum groove, granular SiO 2 Dilute nitric acid (preferably 1:1 nitric acid (HNO 3 ) and ultrapure water), ultrasonically cleaned in ultrapure water twice, and finally washed with absolute ethanol and dried. Put the cleaned sample into the cage sampling device, and put the combination into the GD-MS needle sample cell for analysis after vacuuming. The optimized discharge voltage: 2.5 kV, discharge current: 3.0 mA, discharge gas (Ar) Flow rate: 1.0 cc / min. Then, the signal intensity of the elements in the sample was measured over time to further characterize the stability of the method. At the same time, the GD-MS signal intensity test was performed on the same sample by using the tantalum bath method as the data of the control group. Test results such as Figure 4 As shown, the results show that when the cage sample injection device with the size of 15 mm×5 mm×5 mm is used for analysis, good signal strength and discharge stability can b...

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Abstract

The present invention provides a cage-shaped sampling device and a sample testing method for glow discharge mass spectrometry analysis, so as to solve the problem of analyzing samples of different types and sizes by glow discharge mass spectrometry (GD-MS). The cage-like sampling device comprises a cage-like metal tank and a metal handle arranged at one end of the cage-like metal tank, and the metal handle is used to fix the cage-like sampling device relative to the glow discharge mass spectrometer, and the cage The other end of the cage-shaped metal tank has a sample loading port to load and take out samples. The cage-shaped metal tank is prepared by punching holes on a metal sheet with a purity greater than 99.995%. The size of the cage-shaped metal tank is smaller than the The size of the glow discharge cell of the glow discharge mass spectrometer cannot be placed in the glow discharge cell, and the volume of the cage-like metal tank is smaller than that of the glow discharge cell.

Description

technical field [0001] The present invention relates to the field of glow discharge mass spectrometer, more specifically, the present invention relates to a kind of cage sample introduction device that is used for glow discharge mass spectrometry analysis and uses the glow discharge mass spectrometer that has this cage sample introduction device to carry out sample analysis. method of testing. Background technique [0002] Glow discharge mass spectrometry (GD-MS) method is a direct analysis method of solid materials, which has the advantages of simple sample preparation process, high analysis sensitivity, low detection limit, wide concentration response range, small matrix effect, and can analyze more than 70 kinds at one time. Elements and other advantages make GD-MS widely used in the analysis of inorganic solid materials, especially in the field of high-purity material analysis. In glow discharge, a large number of particles with representative composition can be obtaine...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/68
CPCG01N27/68
Inventor 董疆丽卓尚军钱荣盛成
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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