Gas chromatography detection system for analyzing trace impurity sulfides in carbon dioxide gas

Abstract

The utility model relates to a gas chromatography detection system for analyzing trace impurity sulfides in carbon dioxide gas. Comprising a switching valve arranged in the anti-adsorption temperature control device and a flame photometric detector for detecting trace impurity gas phases, a combustion-supporting gas pipeline and a combustible gas pipeline are arranged on the flame photometric detector; a capillary column special for total sulfur and a capillary column special for sulfide are respectively arranged between the switching valve and the flame photometric detector; the switching valve is provided with a sample gas inlet pipeline, a sample gas outlet pipeline, a carrier gas path unit for pushing gas and a gas quantitative segmentation unit for segmenting the sample gas; the system has the advantages that the structure is simple, the design is reasonable, the operation is simple, the detection sensitivity of the system is high, all components are ensured not to interfere with each other and generate peaks, main components are prevented from polluting a chromatographic column, and a carbon dioxide gas pipeline unit is prevented from adsorbing trace impurity sulfides.

Description

TECHNICAL FIELD

[0001] The utility model relates to carbon dioxide gas impurity detection technical field especially relates to a carbon dioxide gas trace impurity sulfide analysis's gas chromatography detection system. BACKGROUND

[0002] Pure gas has important position in modern industry, along with the rapid development of our country industrial economy, gas has "blood" in industry, photovoltaic and semiconductor production, carbon dioxide is an important chemical material, is widely used in industry, electronics, semiconductor industry, and it is mainly used in industry and semiconductor field. Based on the above reason carbon dioxide gas's preparation and for trace impurity sulfide analysis then is particularly important, further, the gas chromatography for carbon dioxide gas analysis in prior art usually adopts traditional TCD and FPD, matches filling column, realizes total sulfur and sulfide separation and detection in carbon dioxide gas, the sensitivity of this configuration is optimal and can only reach 100ppb detection limit, through above-mentioned detection only can satisfy the demand of product quality detection in industrial chemical raw material and welding industry, but for photovoltaic and semiconductor industry, the sensitivity of instrument configuration is required to reach 10ppb at least even higher detection level, the above configuration cannot realize high sensitivity detection demand because of the influence of sulfide adsorption and desorption and poor separation degree of filling column. UTILITY MODEL CONTENT

[0003] The utility model discloses a carbon dioxide gas trace impurity sulfide analysis's gas chromatography detection system can realize the high sensitivity detection demand of carbon dioxide gas trace impurity sulfide analysis.

[0004] In order to realize above-mentioned purpose, the utility model provides the following technical scheme:

[0005] A carbon dioxide gas trace impurity sulfide analysis's gas chromatography detection system, the gas chromatography analysis system includes the switching valve that sets up in the anti-adsorption temperature control device, and the flame photometric detector that carries out detection to trace impurity gas phase, the flame photometric detector is equipped with combustion-supporting gas pipeline and combustible gas pipeline, and the total sulfur special capillary column and sulfide special capillary column are respectively equipped between switching valve and flame photometric detector, the switching valve is equipped with sample gas import pipeline, sample gas export pipeline, the carrier gas gas path unit for pushing gas and the gas quantitative segmentation unit for dividing sample gas.

[0006] The utility model discloses the beneficial effect is: the utility model discloses through setting up the anti-adsorption temperature control device, and the switching valve and the subsidiary pipeline are set up in the anti-adsorption temperature control device, can realize the temperature control of switching valve, and its subsidiary pipeline and carbon dioxide gas, to reach the solution carbon dioxide gas in sulfide adsorption analysis problem, lays the foundation for the subsequent process and improves the detection sensitivity, further, the utility model discloses the total sulfur special capillary column and sulfide special capillary column are used to reach the improvement column efficiency, improve the separation degree of sulfide, realize the higher sensitivity of instrument, to satisfy the higher requirement of instrument sensitivity in fine chemical industry.

[0007] Preferably, the switching valve is a ten-way pneumatic switching valve.

[0008] Preferably, the sample gas inlet pipeline is connected with the No. 10 interface in the switching valve, the sample gas outlet pipeline is connected with the No. 9 interface in the switching valve, the No. 3 interface in the switching valve is connected with the gas inlet end of the total sulfur special capillary column, and the No. 6 interface in the switching valve is connected with the gas inlet end of the sulfide special capillary column.

[0009] Preferably, the gas quantitative division unit comprises a first quantitative ring matched with the total sulfur special capillary column and a second quantitative ring matched with the sulfide special capillary column; the two ends of the first quantitative ring are connected with the No. 1 interface and the No. 4 interface of the switching valve respectively, and the two ends of the second quantitative ring are connected with the No. 5 interface and the No. 7 interface of the switching valve respectively.

[0010] Preferably, the carrier gas pipeline unit comprises a first carrier gas pipeline matched with the first quantitative ring and a second carrier gas pipeline matched with the second quantitative ring; the first carrier gas pipeline is connected with the No. 2 interface in the switching valve, and the second carrier gas pipeline is connected with the No. 6 interface in the switching valve.

[0011] Preferably, the anti-adsorption temperature control device is a temperature control box.

[0012] Preferably, the combustion-supporting gas pipeline is provided with a first adjusting valve, and the combustible gas pipeline is provided with a second adjusting valve.

[0013] The gas chromatography detection system for analyzing trace sulfide in carbon dioxide gas prepared according to the above scheme has the advantages of simple structure, reasonable design, simple operation, high detection sensitivity of the system, prevention of mutual interference between peaks of components, prevention of pollution of the main component to the chromatographic column, and prevention of adsorption of trace sulfide by the carbon dioxide gas pipeline unit. Specifically, the temperature of the switching valve, the auxiliary pipeline and the carbon dioxide gas is controlled to avoid adsorption and desorption, the total sulfur special capillary column and the sulfide special capillary column are arranged to improve the column efficiency and the separation degree of sulfide, and conditions for improving the sensitivity of the instrument are created. Further, the above arrangement and the flame photometric detector can improve the detection level to more than 10 ppb for analyzing trace sulfide in carbon dioxide gas, so as to meet the requirements of the fine chemical industry. BRIEF DESCRIPTION OF DRAWINGS

[0014] Figure 1 It is a detection system flow diagram of the utility model.

[0015] Figure 2 It is a switching valve flow diagram of the utility model.

[0016] Figure 3 It is a detection flow diagram of the utility model.

[0017] In the drawings:

[0018] 1, switching valve; 2, sample gas inlet pipeline; 3, sample gas outlet pipeline; 4, first carrier gas pipeline; 5, second carrier gas pipeline; 6, first constant ring; 7, second constant ring; 8, anti-adsorption temperature control device; 9, total sulfur special capillary column; 10, sulfide special capillary column; 11, combustion-supporting gas pipeline; 12, combustible gas pipeline; 13, flame photometric detector; 14, first regulating valve; 15, second regulating valve. DETAILED DESCRIPTION

[0019] The technical solutions in the embodiments of the utility model will be clearly and completely described below with reference to the drawings in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, rather than all the embodiments.

[0020] In the description of the utility model, it should be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer" and the like indicate the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the utility model and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as a limitation on the utility model.

[0021] ReferenceFigures 1-3 The utility model discloses a kind of carbon dioxide gas trace impurity sulfide analysis gas chromatography detection systems, the gas chromatography analysis system includes switching valve 1 being arranged in anti-adsorption temperature control device 8, and flame photometric detector 13 for detecting trace impurity gas phase;The flame photometric detector 13 is equipped with combustion-supporting gas pipeline 11 and combustible gas pipeline 12, switching valve 1 and flame photometric detector 13 between respectively be equipped with total sulfur special capillary column 9 and sulfide special capillary column 10;Switching valve 1 is equipped with sample gas inlet pipeline 2, sample gas outlet pipeline 3, carrier gas gas path unit for pushing gas and gas quantitative segmentation unit for dividing sample gas.The utility model discloses by sample gas inlet pipeline 2 and sample gas outlet pipeline 3 form passage to realize the sampling of sample gas, the process of sampling is carried out in switching valve 1, and above-mentioned entire sampling environment is carried out in anti-adsorption temperature control device 8, prevent sulfide component adsorption;The utility model discloses still including total sulfur special capillary column 9 and sulfide special capillary column 10, to reach the improvement column efficiency, improve the separation degree of sulfide, create conditions for improving the sensitivity of instrument.It needs to be noted that: the anti-adsorption temperature control device 8 in the utility model is mainly used for controlling temperature, and it can use existing temperature control device.

[0022] Further, the switching valve 1 is a ten-way pneumatic switching valve. By providing the ten-way pneumatic switching valve, the sample gas can be introduced and sampled.

[0023] Further, the sample gas inlet pipeline 2 is connected to the No. 10 interface of the switching valve 1, the sample gas outlet pipeline 3 is connected to the No. 9 interface of the switching valve 1, the No. 3 interface of the switching valve 1 is connected to the gas inlet end of the total sulfur special capillary column 9, and the No. 6 interface of the switching valve 1 is connected to the gas inlet end of the sulfide special capillary column 10.

[0024] Further, the gas quantitative segmentation unit includes a first quantitative ring 6 matched with the total sulfur special capillary column 9 and a second quantitative ring 7 matched with the sulfide special capillary column 10; the two ends of the first quantitative ring 6 are connected to the No. 1 interface and the No. 4 interface of the switching valve 1, respectively, and the two ends of the second quantitative ring 7 are connected to the No. 5 interface and the No. 7 interface of the switching valve 1, respectively.

[0025] Further, the carrier gas gas path unit includes a first carrier gas pipeline 4 matched with the first quantitative ring 6 and a second carrier gas pipeline 5 matched with the second quantitative ring 7; the first carrier gas pipeline 4 is connected to the No. 2 interface of the switching valve 1, and the second carrier gas pipeline 5 is connected to the No. 6 interface of the switching valve 1.

[0026] Further, the anti-adsorption temperature control device 8 is a temperature control box.

[0027] Further, the combustion-supporting gas pipeline 11 is provided with a first regulating valve 14, and the combustible gas pipeline 12 is provided with a second regulating valve 15.

[0028] The working principle of the utility model is: the sample gas inlet pipeline 2 and the sample gas outlet pipeline 3 constitute a passage to realize sampling of sample gas, the sampling process is carried out in the switching valve 1, and the sampling is carried out through the corresponding first quantitative ring 6 and second quantitative ring 7, the whole sampling process is carried out in the temperature control box to prevent adsorption of sulfide components; specifically speaking: the utility model is used for detecting the gas phase of trace impurity sulfide in carbon dioxide gas, the detection mode is a one-time sample gas feeding mode, as shown in Figure 1 、 2 As shown, the sample gas production equipment and / or storage equipment is connected with the sample gas outlet pipeline 3 through the sample gas inlet pipeline 2, the No. 10 interface of the switching valve 1, the No. 1 interface of the switching valve 1, the first quantitative ring 6, the No. 4 interface of the switching valve 1, the No. 5 interface of the switching valve 1, the second quantitative ring 7, the No. 8 interface of the switching valve 1 and the No. 9 interface of the switching valve 1, and constitutes a passage; then as shown in Figure 3 The switching valve 1 is switched to make the sample gas remain in the first quantitative ring 6 and the second quantitative ring 7, the carrier gas in the first carrier gas pipeline 4 is sent into the total sulfur special capillary column 9 through the No. 2 interface of the switching valve 1, the No. 1 interface of the switching valve 1, the first quantitative ring 6, the No. 4 interface of the switching valve 1 and the No. 3 interface of the switching valve 1; the carrier gas in the second carrier gas pipeline 5 is sent into the sulfide special capillary column 10 through the No. 6 interface of the switching valve 1, the No. 5 interface of the switching valve 1, the second quantitative ring 7, the No. 8 interface of the switching valve 1 and the No. 10 interface of the switching valve 1; the total sulfur special capillary column 9 realizes separation of H2S, COS, C2S and thiophene components; the air in the combustion-supporting gas pipeline 11 and the hydrogen in the combustible gas pipeline 12 enter the flame photometric detector 13 through the respective pipelines to provide working conditions for the flame photometric detector 13, the carrier gas in the first carrier gas pipeline 4 carries the total sulfur components to the flame photometric detector 13 to respond to peaks, and simultaneously the carrier gas in the second carrier gas pipeline 5 carries H2S, COS, C2S and thiophene components into the flame photometric detector 13 to respond to peaks.

[0029] The above is only the preferred specific implementation of the utility model, but the protection scope of the utility model is not limited to this, any skilled person in the art can make equivalent replacement or change according to the technical scheme and the utility model concept of the utility model within the technical range disclosed by the utility model, which should be covered in the protection scope of the utility model.

Claims

1. A gas chromatography detection system for analyzing trace amounts of sulfide impurities in carbon dioxide gas, characterized by, The gas chromatography detection system comprises a switching valve (1) arranged in an anti-adsorption temperature control device (8), and a flame photometric detector (13) for detecting trace impurity gas phase; The flame photometric detector (13) is provided with a combustion-supporting gas pipeline (11) and a combustible gas pipeline (12), and the switching valve (1) and the flame photometric detector (13) are respectively provided with a total sulfur special capillary column (9) and a sulfide special capillary column (10). The switching valve (1) is provided with a sample gas inlet pipeline (2), a sample gas outlet pipeline (3), a carrier gas pipeline unit for pushing gas, and a gas quantitative division unit for dividing sample gas.

2. The gas chromatographic detection system for analyzing trace amounts of sulfide impurities in carbon dioxide gas according to claim 1, characterized by, The switching valve (1) is a ten-way pneumatic switching valve.

3. The gas chromatographic system for detecting trace amounts of sulfur compounds in carbon dioxide gas according to claim 2, wherein The sample gas inlet pipeline (2) is connected with the No. 10 interface in the switching valve (1), the sample gas outlet pipeline (3) is connected with the No. 9 interface in the switching valve (1), the No. 3 interface in the switching valve (1) is connected with the gas inlet end of the total sulfur special capillary column (9), and the No. 6 interface in the switching valve (1) is connected with the gas inlet end of the sulfide special capillary column (10).

4. The gas chromatographic system for detecting trace amounts of sulfur compounds in carbon dioxide gas according to claim 3, wherein The gas quantitative division unit comprises a first quantitative ring (6) matched with the total sulfur special capillary column (9) and a second quantitative ring (7) matched with the sulfide special capillary column (10). The two ends of the first quantitative ring (6) are respectively connected with the No. 1 interface and the No. 4 interface of the switching valve (1), and the two ends of the second quantitative ring (7) are respectively connected with the No. 5 interface and the No. 7 interface of the switching valve (1).

5. The gas chromatographic system for detecting trace amounts of sulfur compounds in carbon dioxide gas according to claim 4, wherein The carrier gas pipeline unit comprises a first carrier gas pipeline (4) matched with the first quantitative ring (6) and a second carrier gas pipeline (5) matched with the second quantitative ring (7). The first carrier gas pipeline (4) is connected with the No. 2 interface in the switching valve (1), and the second carrier gas pipeline (5) is connected with the No. 6 interface in the switching valve (1).

6. The system for detecting trace sulfide impurities in carbon dioxide gas according to claim 1, wherein The anti-adsorption temperature control device (8) is a temperature control box.

7. The system for detecting trace sulfide impurities in carbon dioxide gas according to claim 1, wherein The combustion-supporting gas pipeline (11) is provided with a first adjusting valve (14), and the combustible gas pipeline (12) is provided with a second adjusting valve (15).

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