Packed chromatographic column for analysis of trace oxygen and argon in gas and preparation method thereof, and analysis method for trace oxygen and argon in high-purity gas

Abstract

The invention relates to a packed chromatographic column for analysis of trace oxygen and argon in gas and a preparation method thereof, and an analysis method for trace oxygen and argon in high-purity gas, belonging to the field of application of gas chromatography. The packed chromatographic column for analysis of trace oxygen and argon in gas comprises a chromatographic column pipe and a 5A molecular sieve, a Pd catalyst and a porous polymer bead successively packed in the chromatographic column pipe, wherein the Pd catalyst is one selected from a group consisting of Pd / C, Pd / Al2O3 and Pd / zeolite, and the porous polymer bead is one selected from a group consisting of Porapak Q, Porapak N and GDX-502. The packed chromatographic column provided by the invention can realize simple and rapid analysis of oxygen and argon at a high temperature (70 to 120 DEG C); and the packed chromatographic column is repeatable in analysis results and high in accuracy and sensitivity and can meet requirements of rapid analysis and detection.

Description

technical field [0001] The invention relates to a packed chromatographic column for analyzing trace oxygen and argon in gas and a preparation method thereof, and a method for analyzing trace oxygen and argon in high-purity gas, belonging to the application field of gas chromatography analysis technology. Background technique [0002] The separation of oxygen and argon gas is a major technical problem in gas analysis. When gas chromatography is used to analyze high-purity gases, oxygen and argon components interfere with each other. However, the relevant national standards for high-purity gas detection require the detection of oxygen, argon The content of argon trace components. [0003] In the prior art, when using packed chromatographic columns to analyze oxygen and argon, 5A or 13X molecular sieves are often used to fill the chromatographic columns, and cold traps (dry ice + acetone) need to be used for low-temperature cooling in order to meet the separation necessary for ...

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Problems solved by technology

[0003] In the prior art, when using packed chromatographic columns to analyze oxygen and argon, 5A or 13X molecular sieves are often used to fill the chromatographic columns, and cold traps (dry ice + acetone) need to be used for low-temperature cooling in order to meet the separation necessary for high-purity gas analysis. The method has high requirements on cold trap equipment and instruments, and the actual analysis is not easy to realize, and the stainless steel chromatographic column tube is easily corroded by acetone and dry ice; in addition, when oxygen and argon are analyzed at lower temperatures, 5A molecular sieve The fixed phase has a certain adsorption effect on oxygen and argon, which will have a certain impact on the accuracy of component concentration detection.

The 5A PLOT quartz capillary column can also achieve the separation of oxygen and argon at room temperature (35°C), but the capacity of the capillary column is small, and the analytical sensitivity is affected to a certain extent; if the heart-cutting technique is used, the detection sensitivity can be improved. , but the operation is complicated, the equipment is expensive, and it is not suitable for the actual analysis and detection of high-purity gases

[0004] GB / T3634.2-2011 (Hydrogen Part 2: Pure Hydrogen, High-Purity Hydrogen and Ultra-Pure Hydrogen) also provides an analysis method. This method uses deoxygenation technology. After two injections, oxygen and argon are respectively measured. The total content of the components and the content of the argon components are calculated to obtain the content of each component; the method is cumbersome to operate, and the error of the analysis result due to the error of the two injections is more obvious

[0005] In addition, the authorized patent CN203688513U discloses a micro-filled chromatographic column for the determination of trace and trace amounts of oxygen and argon in gases. The chromatographic column adopts 5A molecular sieve chromatographic packing to prepare a micro-filled chromatographic column with an inner diameter of 1 mm, which can realize oxygen at 50°C. Separation of argon components, but suffers from the same low column capacity as capillary columns and a longer analysis time (4 minutes)

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