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Temperature programming control method for gas chromatography separation

A technology of gas chromatography and temperature programming, which is applied in the direction of material separation, material analysis, and measuring devices, can solve problems such as temperature unevenness, temperature uneven temperature difference stress, etc., achieve stable heating temperature field, no temperature difference stress, and increase temperature Effect

Active Publication Date: 2017-06-13
MATERIAL INST OF CHINA ACADEMY OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The purpose of the present invention is to overcome the deficiencies such as temperature unevenness and temperature difference stress in the programmed temperature control process in the gas chromatography separation method in the prior art, and provide a programmed temperature control system for gas chromatography separation
[0012] In order to overcome the problem of uneven temperature in the process of adjusting the temperature of the heating rod, the method of the present invention uses an intermediate frequency coil for heating, and installs an intermediate frequency induction coil on the upper part of the container of the raw material column / separation column, when the spiral tube lifts out of the liquid nitrogen level Finally, use intermediate frequency coils to manufacture eddy current electric heating to achieve uniform heating of the raw material column / separation column

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Prepare the hydrogen isotope separation device

[0039] Using a container with a diameter of 1.7 meters, a liquid nitrogen tank is arranged in the container, which is filled with liquid nitrogen. Arrange the intermediate frequency coil and connect to the intermediate frequency power supply for subsequent separate heating.

[0040] Intermediate frequency heating rod-shaped separation column (1.2m)

[0041] First, prepare a device for separating hydrogen isotopes by gas chromatography, using Pd / Al containing 30wt% metal palladium 2 O 3 The packing material is filled in the steel pipe to prepare a 1.2-meter packed column. The packed column is made of 316 stainless steel, with a design inner diameter of 12mm, and absorbs 1 bar of hydrogen containing natural abundance of deuterium (deuterium abundance: 150ppm). Under the cooling effect of liquid nitrogen, the adsorption of hydrogen is completed. After the adsorption is completed, transfer the above-mentioned stainless steel sepa...

Embodiment 2

[0046] The influence of the power and frequency of the intermediate frequency coil on the separation

[0047] Pd / Al with 30wt% metal palladium prepared in Example 1 2 O 3 Filling material, 45 meters long 12mm stainless steel pipe, made of 1.5 meters diameter spiral separation column. Adjust the power supply connected to the intermediate frequency coil to control the excitation power and frequency of the intermediate frequency coil, change the intensity of the heating effect of the intermediate frequency coil on the separation column, and analyze the heating efficiency of the different intermediate frequency coils.

[0048] Firstly, the separation column is immersed in a liquid nitrogen tank, and the separation column is cooled with liquid nitrogen to reduce its temperature to the temperature of liquid nitrogen. Then, natural hydrogen gas (deuterium content: 150 ppm) is introduced into the separation column, so that the natural hydrogen is absorbed into the separation column. Afte...

Embodiment 3

[0052] The effect of IF coil with pulling speed on separation

[0053] It can be seen from the results of Example 2 that the separation effect is best when an intermediate frequency power supply with a frequency of 1500 W and a frequency of 200 Hz is used to drive the intermediate frequency coil for heating. In order to further optimize the separation efficiency, control the different pulling speeds and the heating conditions of the intermediate frequency coil to cooperate with each other to optimize and improve the separation efficiency. The specific control pulling speed is continuously changed in the range of 0.5-10cm / min, and the hydrogen discharged from the separation column is sampled by a hydrogen-oxygen recombiner, oxidized into water, and then detected and analyzed by a mass spectrometer.

[0054] By controlling different pulling speeds to match the application of intermediate frequency heating, the effect of different control parameters on the separation efficiency of ga...

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Abstract

The invention discloses a temperature programming control method for gas chromatography separation. An intermediate frequency coil is utilized to heat a raw material column and / or a separating column. A gas chromatography separation heating temperature program provided by the invention utilizes the intermediate frequency coil to perform non-contact heating; a heating temperature field is stable and average; basically, no differential temperature stress exists; and the temperature programming is combined for realizing the direct heating for the palladium in the separating column. The method has an excellent accelerating effect for promoting the gas chromatography separation.

Description

Technical field [0001] The invention relates to a temperature control method, in particular to a temperature-programmed control method for gas chromatographic separation, belonging to the technical field of chromatographic separation, in particular to a temperature control method in a hydrogen isotope separation process. Background technique [0002] In the prior art, there are many research and analysis on the raw materials deuterium and tritium used in thermonuclear fusion research and application, but they mainly involve theoretical and scientific research and analysis, especially the preparation and purification of the raw materials used in thermonuclear fusion reactions. . It is known that some adsorption chromatography methods can be used to separate and purify hydrogen isotopes. Among them, cryogenic adsorption chromatography has the most potential. [0003] Among them, the application of palladium displacement chromatography has the most potential, which can realize the se...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/30
CPCG01N30/30G01N2030/3007
Inventor 杨莞黄国强钱晓静邓立宋江锋文明冯兴文丁海成陈克琳殷雪峰
Owner MATERIAL INST OF CHINA ACADEMY OF ENG PHYSICS
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