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Separating method of hydrogen isotope mixed gas

A technology of mixed gas and hydrogen isotope, which is applied in the field of hydrogen isotope chromatographic separation, can solve the problems of reduced success rate, increased production cost, and uneven distribution of coating materials, so as to reduce emissions, post-processing pressure, and sample demand. Effect

Inactive Publication Date: 2017-10-20
INST OF NUCLEAR PHYSICS & CHEM CHINA ACADEMY OF
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ortho-secondary separation can be eliminated by using transition metal modification, but the process of directly coating transition metal modified aluminum oxide on the inner wall of fused silica tube has the disadvantage of uneven distribution of coating material on the inner wall of the tube
Uneven coating will lead to capillary column clogging, which will lead to the failure of the preparation of the chromatographic column, reduce the success rate, and increase the production cost
Another shortcoming of uneven coating is that the insufficient coating amount causes a decrease in column efficiency and weakens the separation effect of the column.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A 30-meter commercially available aluminum oxide porous layer open-tube chromatographic column is used, and the thickness of the inner surface of aluminum oxide is 10 microns. Nitrogen is used as the booster gas, and the nitrogen pressure is 1.5 bar. MnCl 2 Mix with deionized water to obtain metal salt solution; will contain 2mL MnCl 2 The 5mL glass bottle of the solution is placed in an airtight container; the airtight container is pressurized with a positive pressure inert gas to make the MnCl 2 Pressed into the porous layer open tube column; MnCl 2 After flowing out of the porous layer open tube chromatographic column, the positive pressure inert gas continued to purge for 12 hours. In this example, MnCl 2 During the flow of the solution in the column, there is no clogging phenomenon.

[0019] The porous layer open-tube chromatographic column is loaded into the chromatograph and baked at 180° C. for 2 hours. After cooling, the desired porous layer open-tube chro...

Embodiment 2

[0021] A commercially available aluminum oxide porous layer open-tube chromatographic column of 15 meters is used, and the thickness of the inner surface of aluminum oxide is 30 microns. Argon is used as the booster gas, and the composition of the transition metal salt solution is CoCl 2 . In this embodiment, no clogging occurs during the flow of the metal salt solution in the column. In the hydrogen isotope separation experiment, CoCl 2 The magnetic effect of the protium combined the positive and secondary states to obtain a single H 2 peak, avoiding the o-H 2 Overlap with HD, obtained H 2 , HD, D 2 The separation of each component is greater than 1.5, and the separation time is 5 minutes.

Embodiment 3

[0023] A 20-meter commercially available Al2O3 capillary open-tube chromatographic column is used, and the thickness of Al2O3 on the inner surface is 20 microns. Helium is used as the booster gas, and the composition of the transition metal salt solution is CuSO 4 . In this embodiment, no clogging occurs during the flow of the metal salt solution in the column. In the hydrogen isotope separation experiment, CuSO 4 The magnetic effect of the protium combined the positive and secondary states to obtain a single H 2 peak, avoiding the o-H 2 Overlap with HD, obtained H 2 , HD, D 2 The separation of each component is greater than 1.5, and the separation time is 5 minutes.

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Abstract

The invention discloses a method for separating a hydrogen isotope mixed gas, which comprises the following steps in sequence: using a positive pressure inert gas to press a transition metal salt solution from one end of a porous layer open-tube chromatographic column; After the other end of the column flows out, the inert gas is purged the porous layer open-tube chromatographic column at room temperature for 12 hours; the porous layer open-tube chromatographic column is put into the chromatographic oven, heated and dehydrated, and cooled to obtain the required porous layer open-tube chromatographic column. The above-mentioned porous layer open-tube chromatographic column is placed in a liquid nitrogen Dewar, neon gas is used as a carrier gas, and the hydrogen isotope mixture gas passes through the porous layer open-tube chromatographic column to realize the separation of hydrogen isotopes. The separation method of the invention has the characteristics of simple method, good separation effect, short separation time and the like.

Description

technical field [0001] The invention belongs to the technical field of hydrogen isotope chromatographic separation, and in particular relates to a method for separating hydrogen isotope mixed gas. Background technique [0002] Hydrogen isotopes protium (H), deuterium (D), and tritium (T) combine with each other to form homonuclear hydrogen H 2 、D 2 , T 2 And heteronuclear hydrogen HD, HT, DT. In homonuclear hydrogen, due to the different nuclear spin states, there are positive (ortho-) and secondary (para-) hydrogen isotopes. Therefore, a mixed gas containing three hydrogen isotopes not only has H 2 、D 2 , T 2 The ortho-secondary components of , as well as HD, HT, and DT components, are a complex gas mixture of small molecules, and its quantitative analysis is quite difficult. The analysis of hydrogen isotopes by gas chromatography has the advantages of simple operation and wide application range. It is difficult for the traditional aluminum oxide packed column to ef...

Claims

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Application Information

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IPC IPC(8): B01D59/26
CPCB01D59/26
Inventor 王伟伟任兴碧夏立东陈晓华余铭铭李海容陈绍华张伟光
Owner INST OF NUCLEAR PHYSICS & CHEM CHINA ACADEMY OF
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