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Cage-like sampling device for glow discharge mass spectrometry and sample test method

A technology of glow discharge mass spectrometry and sample injection device, which is applied in the direction of material analysis, measurement device, and material analysis by electromagnetic means, which can solve the problems of affecting the detection speed, increasing the detection cost, and test failure, etc., to improve the signal strength of the sample , widen the size range and reduce the cost of testing

Active Publication Date: 2020-02-04
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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  • Cage-like sampling device for glow discharge mass spectrometry and sample test method
  • Cage-like sampling device for glow discharge mass spectrometry and sample test method
  • Cage-like sampling device for glow discharge mass spectrometry and sample test method

Examples

Experimental program
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Effect test

Embodiment 1

[0048] 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

[0050] 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, then ultrasonicated 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 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 signa...

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Abstract

The invention provides a cage-like sampling device for glow discharge mass spectrometry and a sample test method, and aims at solving the difficulty of the glow discharge mass spectrometry (GD-MS) foranalyzing different types of samples with different sizes. The cage-like sampling device comprises a cage-like metal groove and a metal handle which is arranged at one end of the cage-like metal groove; the metal handle is used for fixing the cage-like sampling device relative to a glow discharge mass spectrometer; a sample loading port is formed in the other end of the cage-like metal groove toload and unload samples; the cage-like metal groove is prepared by carrying out punching and machining on a metal sheet with the purity greater than 99.995%; the size of the cage-like metal groove issmaller than the size of a glow discharge battery of the glow discharge mass spectrometer and the cage-like metal groove can be put in the glow discharge battery; and the volume of the cage-like metalgroove is smaller than the volume of the glow discharge battery.

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 Applications(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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