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Device for purifying and enriching inert gases and use method

An inert gas, enrichment technology, applied in measurement devices, sample preparation for testing, instruments, etc., can solve problems such as inability to use inert gas content analysis, lack, lack of quadrupole mass spectrometers, etc.

Active Publication Date: 2011-04-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] (1) Due to the lack of a quadrupole mass spectrometer, it cannot be used to analyze the content of each component of the inert gas;
[0009] (2) Due to the lack of a 15K low-temperature cold trap, it is impossible to enrich the separated and purified inert gas, and gradually release the components of the inert gas through staged heating;
[0010] (3) The traditional active gas purification components use Zr-Al alloy furnace, and its working temperature is 650°C, which is not conducive to the safety of experimental operation and the maintenance of system vacuum

Method used

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  • Device for purifying and enriching inert gases and use method
  • Device for purifying and enriching inert gases and use method
  • Device for purifying and enriching inert gases and use method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Embodiment 1 - the embodiment of the device of the present invention

[0050] See figure 1 : figure 1 Middle: V1~V3 DN40 all-metal ultra-high vacuum angle valve; V4~V13 DN16 all-metal ultra-high vacuum angle valve; V14~V17 DN16 high vacuum angle valve; V18~V20 electromagnetic isolation valve; V21 1 / 4 inch vacuum pressure valve ;V22 sapphire fine-tuning valve; G1, G2, G4 compound vacuum gauge; G3 CDG film vacuum gauge; C1~C3 liquid nitrogen activated carbon cold trap; C4 ultra-low temperature cold trap; P1 cryopump; P2 zirconium aluminum suction; P3 ion pump; P4 Molecular pumps, P5~P6 mechanical pumps; F1~F3 flange blind plates are connected by stainless steel pipelines with an outer diameter of 14mm and an inner diameter of 10mm. The equipment flow and connection relationship are as follows: figure 1 shown. The interface is hard-sealed with flange and oxygen-free copper gasket to ensure no air leakage.

Embodiment 2

[0051] Embodiment 2 - the embodiment of the inventive method

[0052] First, the inert gas purification and enrichment device is evacuated to a high vacuum (5.0×10 -8 Pa), and then open the valve (V21) to send sample gas (natural gas, rock desorption gas) into the system. Control the injection volume by adjusting the fine-tuning valve (V22), observe the G3 membrane vacuum gauge and record the injection pressure. Open the valve V13 and the sample gas enters the high-vacuum purification section to purify active gas successively in the activated carbon cold trap (C2) under liquid nitrogen medium, zirconium-based getter furnace (L2) at room temperature, and titanium sponge furnace (L1) at 800 °C.

[0053] After the active gas is removed from the sample gas, the inert gas is extracted. Open the valve V8 and the purified inert gas diffuses into the high vacuum analysis section, close V8 and open the zirconium aluminum getter pump to further inert gas. After the pressure gauge G1 ...

Embodiment 3

[0059] Embodiment 3——Comparative example

[0060] Compared with the all-metal rare gas purification and mass spectrometry system in Document 1, the inert gas in the gas in the volcanic area was analyzed, and the results are shown in Table 4.

[0061] Table 4 Comparison of noble gas results in a volcanic area in file 1

[0062] sample number

[0063] It can be seen from Table 4 that this analysis method can only obtain the isotope ratio of some inert gases, but cannot obtain the content of each component.

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Abstract

The invention relates to a device for purifying and enriching inert gases and a use method. On the basis of an inert gas isotopic analysis technique, a Zr-based getter material capable of working at a room temperature is used in the invention, and meanwhile, a sample quantitative control system and a 15K low temperature cold trap are additionally arranged. All function parts are reasonably arranged and matched in the device so as to make a system have dynamic high vacuum (5.0*10-8Pa) and low leakage rate. A trace of inert gases in a single gas sample can be purified and enriched in 10 minutes. The quantitative analysis of the contents of inert gases He, Ne, Ar, Kr and Xe in the gas sample is conducted by a four-pole mass spectrometer. Meanwhile, one-step sample purification is realized, all components of the inert gases are chilled and enriched by the low temperature activated carbon cold trap (15K), and the inert gases He, Ne, Ar, Kr and Xe are gradually released in a gradual heating way. The invention lays a foundation for conducting isotopic analysis on all components of the inert gases.

Description

technical field [0001] The invention belongs to the field of instrument analysis and detection. In particular, it relates to an inert gas purification and enrichment device and a use method. Background technique [0002] Inert gas isotope, as an important auxiliary means to understand the source of oil and gas, has its unique features. Its development and application make inert gas isotope a branch of geochemistry. It is widely used in source research. In the field of inert gas analysis technology, many advanced laboratories at home and abroad mainly focus their technical strength on isotope analysis, and mainly use it to solve the research of mineral petrochronology and natural gas tracer research. The Lanzhou Institute of Geology, Chinese Academy of Sciences, which has long been engaged in the analysis of inert gas He and Ar isotopes in natural gas, mainly uses the method of segmented equilibrium transfer, that is, through liquid nitrogen cold traps, Zr-Al alloy furnaces...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N1/34G01N1/42G01N27/62
Inventor 刘文汇孙明良陶成秦建中陈伟钧
Owner CHINA PETROLEUM & CHEM CORP
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