Valve path system for analyzing trace or trace impurities in various high-purity gases

Abstract

The utility model discloses a valve path system for analyzing trace or trace impurities in various high-purity gases. The valve path system is a four-valve six-column system; comprising a pulse discharge helium ionization detector, a detection gas inlet assembly, a first detection branch and a second detection branch. A four-valve six-column system is adopted, and four valves are switched, and six columns are separated; the method comprises the following steps: firstly, dividing trace or trace impurities in single-type high-purity gas into two types for independent detection; and secondly, high-purity gas and impurities which are not detected in the branch are discharged through switching of the states of the valves, and the impurities to be detected are conveyed to a pulse discharge helium ionization detector after being subjected to repeated center cutting for multiple times. Therefore, trace or trace impurities in five high-purity gases, namely hydrogen, argon, oxygen, nitrogen and helium, are simultaneously detected by using the valve path system, the purposes of simplifying the operation process and reducing the analysis cost are achieved, the peak area reproducibility (n is equal to 6) is less than or equal to 1%, and the lowest detection limit of each impurity is less than 20ppb.

Description

Technical Field

[0001] The utility model relates to the field of gas analysis, in particular to a valve circuit system for analyzing micro or trace impurities in a variety of high-purity gases. Background Art

[0002] With the continuous expansion of industrial production capacity, high-purity gas is being used as feed gas, shielding gas, and fuel gas in various fields, including industrial manufacturing, coal chemical industry, energy chemical industry, organic chemical synthesis, electronics, and aerospace. The relationship between its purity and product quality has become increasingly prominent. Because the main components of high-purity gas have large tailing peaks, and some impurity peaks appear on the tail of the main peak, separation is difficult, and the minimum detection limit cannot be guaranteed.

[0003] Existing methods for analyzing trace or trace impurities in high-purity helium, high-purity hydrogen, high-purity argon, high-purity oxygen, and high-purity nitrogen primarily utilize gas chromatography combined with a pulsed discharge helium ionization detector (PDHID). Existing equipment can only detect trace or trace impurities in a single high-purity gas. For example, a valve-path analysis system suitable for trace or trace impurities in high-purity hydrogen cannot simultaneously detect trace or trace impurities in high-purity oxygen and high-purity nitrogen. Furthermore, a valve-path analysis system suitable for trace or trace impurities in high-purity oxygen and nitrogen cannot simultaneously detect trace or trace impurities in high-purity hydrogen. Using a single analysis system to separate these five high-purity gases and obtain accurate analysis and detection is extremely difficult.

[0004] For example, Baidu Wenku discloses a technical solution for using DID gas chromatography to detect impurities in high-purity oxygen in the optical fiber industry. To simultaneously detect trace or trace impurities in five high-purity gases, namely high-purity helium, high-purity hydrogen, high-purity argon, high-purity oxygen, and high-purity nitrogen, multiple instruments are required or the system flow path, valve replacement, and chromatographic column replacement are required for multiple injections and analyses. This results in low analysis efficiency, cumbersome operation, and high analysis costs. Utility Model Content

[0005] In response to the above-mentioned defects in the existing technology, a valve circuit system is provided for analyzing trace or trace impurities in a variety of high-purity gases, which can efficiently complete the detection of trace or trace impurities in 5 high-purity gases, simplify the operation process and reduce the analysis cost.

[0006] The technical solution adopted by the present invention to solve the above technical problems is:

[0007] A valve circuit system for analyzing trace or micro-impurities in a variety of high-purity gases, including a pulse discharge helium ionization detector; characterized in that: the valve circuit system is a four-valve six-column system; including

[0008] Detection gas inlet assembly, the detection system inlet assembly is set with a measuring loop, a sample inlet, a sample exhaust port, and two carrier gas outlets. The external gas source to be tested is stored in the quantitative loop, and the corresponding carrier gas outlet is selected according to the analysis requirements;

[0009] A first detection branch is connected between a carrier gas outlet of the detection gas inlet assembly and a pulse discharge helium ionization detector; the first detection branch is used to separate the mixed gas A and CH4 in the high-purity gas to be detected and transport them to the pulse discharge helium ionization detector for detection;

[0010] The second detection branch is connected between another carrier gas outlet of the detection gas inlet assembly and the pulse discharge helium ionization detector; the second detection branch is used to separate CO2, C2H4, C2H6, and C2H2 in the high-purity gas to be detected and transport them to the pulse discharge helium ionization detector for detection.

[0011] According to the above technical solution, a protective atmosphere component is also included. The detection gas inlet component, the first detection branch, and the second detection branch are all located in the protective atmosphere component, and the protective atmosphere component is filled with carrier gas.

[0012] According to the above technical solution, the test gas inlet assembly includes a ten-way valve A, two carrier gas inlet branches, two quantitative loops, and a test gas inlet branch and a test gas outlet branch; the ten-way valve A has ten connection points, marked A1-A10 in clockwise direction;

[0013] The gas inlet branch to be tested is connected to A10, and the gas outlet branch to be tested is connected to A5; a quantitative loop is connected between A1 and A4, and between A6 and A9 through pipelines respectively; a carrier gas inlet branch is connected to A2 and A8 respectively; A3 serves as the carrier gas outlet and is connected to the first detection branch, and A7 serves as another carrier gas outlet and is connected to the second detection branch.

[0014] According to the above technical solution, the gas intake branch to be measured includes an intake pipe and a first pressure balancing valve. The intake pipe is connected between A10 and the external gas source to be measured, and the first pressure balancing valve is located on the intake pipe.

[0015] The outlet branch of the gas to be measured includes an outlet pipe and a second pressure balancing valve. The outlet pipe is connected between A5 and an external gas collection device to be measured, or between A5 and the atmosphere. The second pressure balancing valve is located on the outlet pipe.

[0016] According to the above technical solution, the first detection branch includes a pre-separation unit, a pipeline with a first main separation column, a main separation unit and a pipeline with a second main separation column. The end of the pipeline with the second main separation column is connected to a pulse discharge helium ionization detector; the first main separation column and the second main separation column separate the gas passing through into multiple gas segments according to the components.

[0017] The pre-separation unit is equipped with a ten-way valve B, a first pre-separation column and a second pre-separation column, a carrier gas inlet branch, an exhaust branch, and a carrier gas outlet connected to the pipeline equipped with the first main separation column. Depending on the main component of the gas to be tested, the gas to be tested is passed into the first pre-separation column or the second pre-separation column, and the first pre-separation column or the second pre-separation column separates the gas to be tested into multiple gas segments according to the components. Based on the required detection components of the gas to be tested, the gas segments containing the detection components in the multiple gas segments are transported to the carrier gas outlet of the pre-separation unit, and the remaining gas segments are transported to the exhaust branch.

[0018] The main separation unit is equipped with a six-way valve a, a carrier gas outlet connected to the pipeline with the second main separation column, an exhaust branch, and a carrier gas inlet branch. The six-way valve a transports the components to be detected in the gas segment transported by the first main separation column to the carrier gas outlet of the main separation unit, and the remaining gas segments are transported to the exhaust branch.

[0019] Among them, the first pre-separation column for analyzing impurities in high-purity hydrogen adopts a high specific surface area carbon molecular sieve column; the second pre-separation column, the first main separation column, and the second main separation column for analyzing high-purity oxygen, high-purity argon, and high-purity nitrogen all adopt 13X molecular sieve analysis columns; for analyzing impurities in high-purity helium, either the first pre-separation column or the second pre-separation column can be selected.

[0020] According to the above technical solution, the ten-way valve B is provided with ten connection points, which are marked as B1-B10 in clockwise direction. The carrier gas outlet of the detection gas inlet assembly is connected to B10, and the pipeline with the first main separation column is connected to B5; the first pre-separation column is connected between B1 and B6, and the second pre-separation column is connected between B4 and B9; the carrier gas inlet branch is connected to B2; B3 and B8 are directly connected by a pipeline; and the exhaust branch is connected to B7.

[0021] The six-way valve a is provided with 6 connection points, which are marked as a1-a6 in clockwise direction; the pipeline with the first main separation column is connected to a6, the exhaust branch is connected to a1, the pipeline with the second main separation column is connected to a5, a2 and a4 are directly connected by a pipeline, and the carrier gas inlet branch is connected to a3.

[0022] According to the above technical solution, the second detection branch includes, in sequence, a pipeline provided with a third pre-separation column, a second separation unit, and a pipeline provided with a third main separation column. The end of the pipeline provided with the third main separation column is connected to a pulsed discharge helium ionization detector. The third pre-separation column and the third main separation column separate the passing gas into multiple gas segments according to their components.

[0023] The second separation unit is provided with a six-way valve b, a carrier gas outlet connected to the pipeline provided with the third main separation column, an exhaust branch, and a carrier gas inlet branch. The six-way valve b transports the components to be detected in the gas segment transported by the first main separation column to the carrier gas outlet of the main separation unit, and transports the remaining gas segment to the exhaust branch.

[0024] The third pre-separation column and the third main separation column adopt polymer porous microsphere analysis columns.

[0025] According to the above technical solution, the six-way valve b is provided with 6 connection points, which are marked as b1-b6 in clockwise direction; the pipeline with the first main separation column is connected to b6, the exhaust branch is connected to b1, the pipeline with the second main separation column is connected to b5, b2 and b4 are directly connected through the pipeline, and the carrier gas inlet branch is connected to b3.

[0026] According to the above technical solution, a carrier gas inlet branch is provided on the pulse discharge helium ionization detector for purging the air inside the pulse discharge helium ionization detector; the carrier gas inlet branch is also connected to the protective atmosphere component, and passes through the cavity including the six-way valve b, the ten-way valve A, the ten-way valve B, and the six-way valve a in sequence, and is connected to the outside world after a damping column is provided at the end.

[0027] According to the above technical solution, a plurality of exhaust branches and carrier gas inlet branches are provided in the valve circuit system. The exhaust branch includes an exhaust pipe and a damping column provided on the exhaust pipe, and the end of the exhaust pipe is directly connected to the outside world; the carrier gas inlet branch includes a carrier gas pipe, a pressure controller and a purifier provided in the carrier gas pipe, and the head end of the carrier gas pipe is connected to the carrier gas source;

[0028] A carrier gas inlet branch is provided in the six-way valve a, and a damping column is also provided on the carrier gas inlet branch of the six-way valve a for balancing the pressure.

[0029] Principle of this utility model:

[0030] The ten-way valve and six-way valve used in the present invention both include two states, a single-line state and a double-line state; in the single-line state, the connection points 10 and 1, 2 and 3, 4 and 5, 6 and 7, 8 and 9 in the ten-way valve are connected, and the connection points 6 and 1, 2 and 3, 4 and 5 in the six-way valve are connected; in the double-line state, the connection points 1 and 2, 3 and 4, 5 and 6, 7 and 8, 9 and 10 in the ten-way valve are connected, and the connection points 1 and 2, 3 and 4, 5 and 6 in the six-way valve are connected.

[0031] A first detection branch and a second detection branch are set up in the same valve circuit system. They are used to separate trace or trace impurities in the high-purity gas to be tested into two major categories: CO2, C2H4, C2H6, C2H2 and CH4, and mixed gas A. The two types of impurities are further separated in the first detection branch and the second detection branch, respectively, and transported to the pulsed discharge helium ionization detector for detection and analysis.

[0032] In the detection gas inlet component, a ten-way valve A is used to construct two test gas inlet branches, and the switching of the ten-way valve A is used to respectively deliver a fixed amount of test gas to the two detection branches and purge the detection branches with carrier gas.

[0033] Two parallel separation branches are formed in the first detection branch using a ten-way valve B. A first pre-separation column and a second pre-separation column are respectively provided on the two separation branches, corresponding to the separation pretreatment of high-purity hydrogen and the separation treatment of high-purity argon, oxygen and nitrogen.

[0034] For high-purity hydrogen testing, after the high-purity gas to be tested passes through the first pre-separation column, the primary components in the front section, along with CO2, C2H4, C2H6, and C2H2, are discharged from the first detection branch through repeated switching of ten-way valve B. The remaining high-purity gas to be tested is then delivered to the first main separation column. Six-way valve a is then switched to discharge the remaining primary components from the first detection branch. The remaining mixed gas A and CH4 are then delivered to the second main separation column, where they are separated into multiple fractions and sequentially delivered to the pulsed discharge helium ionization detector.

[0035] When testing high-purity argon, oxygen, or nitrogen, the high-purity gas to be tested is passed through the second pre-separation column and then to the first main separation column through repeated switching of the ten-port valve B. The main components, along with CO2, C2H4, C2H6, and C2H2, are then discharged from the first detection branch through repeated switching of the six-port valve a. The remaining mixed gas A and CH4 is then fed to the second main separation column. Finally, the mixed gas A and CH4 is separated into multiple fractions by the second main separation column and sequentially fed to the pulsed discharge helium ionization detector.

[0036] In the second detection branch, the high-purity gas to be tested is first separated into two segments by the third pre-separation column: the front segment (main component, mixed gas A, and CH4), and the back segment (CO2, C2H4, C2H6, and C2H2). Six-way valve b is switched to discharge the front segment (main component, mixed gas A, and CH4) out of the second detection branch. The back segment (CO2, C2H4, C2H6, and C2H2) is then separated into multiple segments by the third main separation column and sequentially delivered to the pulsed discharge helium ionization detector.

[0037] The utility model has the following beneficial effects:

[0038] The four-valve, six-column system employs a four-valve, six-column system. By switching four valves and separating six columns, it firstly separates trace impurities in a single high-purity gas into two separate categories for independent detection. Secondly, by switching valve states, the high-purity gas and impurities undetectable by this branch are discharged. The impurities to be detected are then transferred to a pulsed discharge helium ionization detector after repeated heart cutting. This valve-based system enables simultaneous detection of trace impurities in five high-purity gases: hydrogen, argon, oxygen, nitrogen, and helium. This simplifies the operational process and reduces analytical costs. Peak area reproducibility (n=6) is ≤1%, and the minimum detection limit for each impurity is less than 20 ppb.

[0039] The above description is only an overview of the technical solution of the present invention. In order to more clearly understand the technical means of the present invention and to implement it according to the contents of the description, the following is a detailed description of the preferred embodiments of the present invention with the accompanying drawings. The specific implementation methods of the present invention are given in detail in the following embodiments and drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0040] The drawings described herein are used to provide a further understanding of the present invention and constitute a part of this application. The illustrative embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation on the present invention.

[0041] Figure 1 This is a schematic diagram of an embodiment of the present invention;

[0042] Figures 2 to 5 This is a path diagram of the embodiment of the present invention using the first detection branch to detect the mixed gas A and CH4;

[0043] Figures 6 and 7 This is a path diagram of the embodiment of the present invention using the second detection branch to detect CO2, C2H4, C2H6, and C2H2;

[0044] In the figure, 1. Pulse discharge helium ionization detector; 2. Ten-way valve A; 3. Carrier gas inlet branch; 3-1. Carrier gas pipeline; 3-2. Pressure controller; 3-3. Purifier; 4. Quantitative loop; 5. Inlet branch of the gas to be measured; 5-1. Inlet pipeline; 5-2. First pressure balancing valve; 6. Outlet branch of the gas to be measured; 6-1. Outlet pipeline; 6-2. Second pressure balancing valve; 7. First main separation column; 8. Six-way valve a; 9. Second main separation column; 10. Ten-way valve B; 11. First pre-separation column; 12. Second pre-separation column; 13. Exhaust branch; 13-1. Exhaust pipeline; 13-2. Damping column; 14. Third pre-separation column; 15. Third main separation column; 16. Six-way valve b; 17. Protective atmosphere assembly. DETAILED DESCRIPTION

[0045] The following is combined with Figures 1 to 7 The principles and features of the present invention are described, and the examples provided are intended only to illustrate the present invention and are not intended to limit the scope of the present invention. The following paragraphs describe the present invention in more detail by way of example with reference to the accompanying drawings. The advantages and features of the present invention will become more apparent from the following description and claims. It should be noted that the drawings are greatly simplified and not to exact scale, and are intended solely to facilitate and clearly illustrate the embodiments of the present invention.

[0046] It should be noted that when a component is referred to as being "fixed to" another component, it may be directly on the other component or there may also be a central component. When a component is considered to be "connected to" another component, it may be directly connected to the other component or there may also be a central component. When a component is considered to be "set on" another component, it may be directly set on the other component or there may also be a central component. The terms "vertical", "horizontal", "left", "right" and similar expressions used herein are for illustrative purposes only.

[0047] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the art to which this invention pertains. The terms used herein in the specification of this invention are intended only to describe specific embodiments and are not intended to limit the invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0048] Reference Figures 1 to 7 As shown, the utility model provides a valve circuit system for analyzing micro or trace impurities in various high-purity gases.

[0049] Example 1

[0050] It includes a pulse discharge helium ionization detector 1; the valve circuit system is a four-valve six-column system. It also includes

[0051] Detection gas inlet assembly, the detection system inlet assembly is set with a measuring loop, a sample inlet, a sample exhaust port, and two carrier gas outlets. The external gas source to be tested is stored in the quantitative loop, and the corresponding carrier gas outlet is selected according to the analysis requirements;

[0052] A first detection branch is connected between a carrier gas outlet of the detection gas inlet assembly and a pulse discharge helium ionization detector; the first detection branch is used to separate the mixed gas A and CH4 in the high-purity gas to be detected and transport them to the pulse discharge helium ionization detector for detection;

[0053] The second detection branch is connected between another carrier gas outlet of the detection gas inlet assembly and the pulse discharge helium ionization detector; the second detection branch is used to separate CO2, C2H4, C2H6, and C2H2 in the high-purity gas to be detected and transport them to the pulse discharge helium ionization detector for detection.

[0054] In this embodiment, a first detection branch and a second detection branch are provided within the same valve circuit system. These branches separate trace impurities in the high-purity gas to be tested into two main categories: CO₂, C₂H₄, C₂H₆, and C₂H₂, and mixed gases A and CH₄. These two types of impurities are further separated within the first and second detection branches and transported to a pulsed discharge helium ionization detector for detection and analysis.

[0055] In high-purity hydrogen, mixed gas A is O2, N2, and CO. In high-purity argon and oxygen, mixed gas A is H2, N2, and CO. In high-purity nitrogen, mixed gas A is O2, H2, and CO. In high-purity helium, mixed gas A is H2, O2, N2, and CO.

[0056] In Example 1, the test gas inlet assembly includes a ten-way valve A2, two carrier gas inlet branches 3, two quantitative loops 4, a test gas inlet branch 5, and a test gas outlet branch 6; the ten-way valve A has ten connection points, which are marked as A1-A10 in clockwise direction;

[0057] The gas inlet branch to be tested is connected to A10, and the gas outlet branch to be tested is connected to A5; a quantitative loop is connected between A1 and A4, and between A6 and A9 through pipelines respectively; a carrier gas inlet branch is connected to A2 and A8 respectively; A3 serves as the carrier gas outlet and is connected to the first detection branch, and A7 serves as another carrier gas outlet and is connected to the second detection branch.

[0058] The gas inlet branch to be tested includes an inlet pipe 5-1 and a first pressure balancing valve 5-2. The inlet pipe is connected between A10 and the external gas source to be tested. The first pressure balancing valve is located on the inlet pipe.

[0059] The outlet branch of the gas to be measured includes an outlet pipe 6-1 and a second pressure balancing valve 6-2. The outlet pipe is connected between A5 and an external gas collection device to be measured, or between A5 and the atmosphere. The second pressure balancing valve is located on the outlet pipe.

[0060] In Example 1, the first detection branch includes a pre-separation unit, a pipeline with a first main separation column 7, a main separation unit, and a pipeline with a second main separation column 9. The end of the pipeline with the second main separation column is connected to a pulse discharge helium ionization detector; the first main separation column and the second main separation column separate the gas passing through into multiple gas segments according to the components.

[0061] The pre-separation unit is equipped with a ten-way valve B10, a first pre-separation column 11 and a second pre-separation column 12, a carrier gas inlet branch 3, an exhaust branch 13, and a carrier gas outlet connected to the pipeline provided with the first main separation column. Depending on the main component of the gas to be measured, the gas to be measured is passed into the first pre-separation column or the second pre-separation column, and the first pre-separation column or the second pre-separation column separates the gas to be measured into multiple gas segments according to the components. Depending on the required detection components of the gas to be measured, the gas segments containing the detection components in the multiple gas segments are transported to the carrier gas outlet of the pre-separation unit, and the remaining gas segments are transported to the exhaust branch.

[0062] The main separation unit is equipped with a six-way valve a8, a carrier gas outlet connected to the pipeline with the second main separation column, an exhaust branch, and a carrier gas inlet branch. The six-way valve a transports the components to be detected in the gas segment transported by the first main separation column to the carrier gas outlet of the main separation unit, and the remaining gas segments are transported to the exhaust branch.

[0063] In Example 1, the second detection branch sequentially includes a pipeline provided with a third pre-separation column 14, a second separation unit, and a pipeline provided with a third main separation column 15. The end of the pipeline provided with the third main separation column is connected to a pulsed discharge helium ionization detector. The third pre-separation column and the third main separation column separate the passing gas into multiple gas segments according to their components.

[0064] The second separation unit is equipped with a six-way valve b16, a carrier gas outlet connected to the pipeline with the third main separation column, an exhaust branch, and a carrier gas inlet branch. The six-way valve b transports the components to be detected in the gas segment transported by the first main separation column to the carrier gas outlet of the main separation unit, and the remaining gas segments are transported to the exhaust branch.

[0065] The first pre-separation column for analyzing impurities in high-purity hydrogen utilizes a high-surface-area carbon molecular sieve column. For analyzing high-purity oxygen, high-purity argon, and high-purity nitrogen, the second pre-separation column, the first main separation column, and the second main separation column all utilize 13X molecular sieve analytical columns. For analyzing impurities in high-purity helium, either the first or second pre-separation column can be used. The third pre-separation column and the third main separation column utilize polymer porous microsphere analytical columns (e.g., Porapak Q). The preferred outer diameter of these six columns is 2.1 mm, and the length varies depending on the method, potentially ranging from 1 m, 2 m, or 3 m. Other dimensions are also possible.

[0066] In the detection gas inlet assembly, a ten-way valve A is used to construct two gas inlet branches for the carrier gas to be tested and the sample to be carried. The ten-way valve A is switched to deliver a fixed amount of the gas to be tested to the two detection branches and to purge the detection branches with the carrier gas.

[0067] Within the first detection branch, a ten-way valve B is used to form two parallel separation branches. A first pre-separation column and a second pre-separation column are provided in each separation branch, corresponding to the separation and pretreatment of high-purity hydrogen and the separation and treatment of high-purity argon, oxygen, and nitrogen, respectively. By switching the ten-way valve B, CO2, C2H4, C2H6, and C2H2 in the input high-purity gas to be tested are discharged from the first detection branch. If high-purity hydrogen is being tested, a portion of the high-purity hydrogen is also discharged from the first detection branch. Within the first detection branch, the high-purity gas in the pre-treated gas is vented by switching the six-way valve a. If high-purity hydrogen is being tested, the remaining high-purity hydrogen is vented during this process. For high-purity oxygen, nitrogen, and argon, all other gases are vented during this process. Finally, the second main separation column separates the mixed gas A and CH4 into multiple segments, which are then sequentially delivered to the pulsed discharge helium ionization detector.

[0068] In the second detection branch, the high-purity gas, mixed gas A, and CH4 in the high-purity gas to be tested are first separated by the third pre-separation column and then discharged through the switching of six-way valve b. The remaining gases (CO2, C2H4, C2H6, and C2H2) are again divided into multiple sections by the second main separation column and sequentially delivered to the pulsed discharge helium ionization detector.

[0069] The four-valve, six-column system employs four valve switching and six column separation. Firstly, trace impurities in a single high-purity gas are separated into two separate categories for independent testing. Secondly, by switching valve states, the high-purity gas and impurities not detected by this branch are discharged, and the impurities to be tested are delivered to the pulsed discharge helium ionization detector after repeated heart cutting. This valve-based system enables simultaneous detection of trace impurities in five high-purity gases: hydrogen, argon, oxygen, nitrogen, and helium, simplifying the operational process and reducing analytical costs.

[0070] Example 2

[0071] The structure and principle of Example 2 are similar to those of Example 1, except that it also includes a protective atmosphere component 17, the detection gas intake component, the first detection branch, and the second detection branch are all located in the protective atmosphere component, and the protective atmosphere component is filled with carrier gas to avoid the influence of constant O2 and N2 in the air on the detection results.

[0072] Among them, a carrier gas inlet branch is provided on the pulse discharge helium ionization detector, which is used to purge the air in the pulse discharge helium ionization detector; the carrier gas inlet branch is also connected to the protective atmosphere component, and passes through the cavity including the six-way valve b, the ten-way valve A, the ten-way valve B, and the six-way valve a in sequence, and is connected to the outside world after a damping column is provided at the end.

[0073] Example 3

[0074] The structure and principle of embodiment 3 are similar to those of embodiment 1 or 2, except that a preferred connection method of the ten-way valve B and the six-way valve A is provided.

[0075] Ten-way valve B has ten connection points, marked B1-B10 in clockwise order. The carrier gas outlet of the detection gas inlet assembly is connected to B10 (i.e., B10 is connected to A10), the pipeline with the first main separation column is connected to B5; the first pre-separation column is connected between B1 and B6, and the second pre-separation column is connected between B4 and B9; the carrier gas inlet branch is connected to B2; B3 and B8 are directly connected by a pipeline; and the exhaust branch is connected to B7.

[0076] The six-way valve a is provided with 6 connection points, which are marked as a1-a6 in clockwise direction; the pipeline with the first main separation column is connected to a6, the exhaust branch is connected to a1, the pipeline with the second main separation column is connected to a5, a2 and a4 are directly connected by a pipeline, and the carrier gas inlet branch is connected to a3.

[0077] In addition to the connection method of Example 3, the ten-way valve B and the six-way valve a may also be connected in other point-to-point ways, as long as the functions described in Example 1 are achieved.

[0078] Example 4

[0079] The structure and principle of Example 4 are similar to those of Example 1 or 2, except that: a preferred connection method of the six-way valve b is provided; the six-way valve b is provided with 6 connection points, which are marked as b1-b6 in a clockwise direction; the pipeline with the first main separation column is connected to b6, the exhaust branch is connected to b1, the pipeline with the second main separation column is connected to b5, b2 and b4 are directly connected by a pipeline, and the carrier gas inlet branch is connected to b3.

[0080] In addition to the connection method of Example 4, the six-way valve b can also adopt other point connection methods, as long as the functions described in Example 1 are realized.

[0081] In Examples 1-4, a plurality of exhaust branches and carrier gas inlet branches are provided in the valve circuit system. The exhaust branch includes an exhaust pipe 13-1 and a damping column 13-2 provided on the exhaust pipe. The end of the exhaust pipe is directly connected to the outside world. The carrier gas inlet branch includes a carrier gas pipe 3-1, a pressure controller 3-2 provided in the carrier gas pipe, and a purifier 3-3. The head end of the carrier gas pipe is connected to the carrier gas source.

[0082] In order to avoid excessive pressure fluctuation in the valve when the six-way valve a switches the valve to a connected state, a carrier gas inlet branch is provided in the six-way valve a, and a damping column is also provided on the carrier gas inlet branch of the six-way valve a to balance the pressure.

[0083] The detection process of this utility model:

[0084] The ten-way valve and six-way valve used in the present invention both include two states, a single-line state and a double-line state; in the single-line state, the connection points 10 and 1, 2 and 3, 4 and 5, 6 and 7, 8 and 9 in the ten-way valve are connected, and the connection points 6 and 1, 2 and 3, 4 and 5 in the six-way valve are connected; in the double-line state, the connection points 1 and 2, 3 and 4, 5 and 6, 7 and 8, 9 and 10 in the ten-way valve are connected, and the connection points 1 and 2, 3 and 4, 5 and 6 in the six-way valve are connected.

[0085] First, use the first detection branch to measure high-purity gas, such as Figures 2 to 5 As shown:

[0086] S1: Ten-way valve A is initially in a single-line state. Open the pressure balance valve to completely displace and fill the quantitative loop, and then close the pressure balance valve.

[0087] S2: Switch the ten-way valve A to the dual-line state, so that the gas to be tested in the quantitative loop enters the first detection branch.

[0088] S3: When measuring high-purity hydrogen, the ten-way valve B is initially in a single-line state, and the six-way valve a is initially in a single-line state; the high-purity hydrogen gas to be measured enters the first pre-separation column; when the high-purity hydrogen gas to be measured passes through the first pre-separation column and is divided into three gas sections (the main component in the first section, a small amount of main components, O2, N2, CH4, CO in the middle section, and CO2, C2H4, C2H6, and C2H2 in the tail section), by switching the state of the ten-way valve B (from a single-line state to a double-line state), the small amount of main components, O2, N2, CH4, and CO in the middle section are transported to the pipeline provided with the first main separation column, and the remaining gas is discharged through the exhaust branch. After separation in the first main separation column, the small amount of main components is discharged by repeatedly switching the six-way valve a, and O2, N2, CH4, and CO are transported to the second main separation column for further separation and then transported to the pulse discharge helium ionization detector for detection. Then switch the ten-way valve B to the single-line state again to discharge the CO2, C2H4, C2H6, and C2H2 in the tail section into the exhaust branch.

[0089] When measuring high-purity argon, oxygen, or nitrogen, ten-way valve B initially switches to a dual-line state, delivering the high-purity test gas to the pipeline containing the second pre-separation column, while six-way valve a initially switches to a single-line state. The high-purity argon, oxygen, or nitrogen test gas enters the second pre-separation column, where it undergoes preliminary separation. After the entire high-purity test gas has entered the pipeline containing the second pre-separation column, ten-way valve B switches to a single-line state, delivering the initially separated high-purity test gas to the pipeline containing the second pre-separation column for further separation. Subsequently, through repeated switching of six-way valve a, the main components of the high-purity test gas and CO2, C2H4, C2H6, and C2H2 are discharged from the first test branch. The remaining gas is delivered to the pipeline containing the second main separation column for further separation before being sent to a pulsed discharge helium ionization detector for detection.

[0090] If high-purity helium is to be detected, both of the above methods are acceptable.

[0091] Then use the second detection branch to detect high purity gas, such as Figures 6 and 7 As shown:

[0092] S1: Ten-way valve A is initially in a dual-line state. The pressure balance valve is opened to completely displace and fill the other quantitative loop, and then the pressure balance valve is closed.

[0093] S2: Switch the ten-way valve A to the single-line state, so that the gas to be tested in the quantitative loop enters the second detection branch.

[0094] S3: After the gas to be tested passes through the third pre-separation column, it is separated into two gas streams. After the pre-CO2 mixed gas A and CH4 are vented through six-way valve b, CO2, C2H4, C2H6, and C2H2 are delivered to the third main separation column by repeatedly switching six-way valve b to the dual-line position. The remaining gas is discharged through the exhaust branch. The third main separation column separates CO2, C2H4, C2H6, and C2H2 into multiple streams, which are then delivered sequentially to the pulsed discharge helium ionization detector for detection.

[0095] The above description is only a preferred embodiment of the present invention and does not constitute any form of limitation to the present invention. Any ordinary technician in this industry can smoothly implement the present invention as shown in the drawings and described above. However, any equivalent changes, modifications and evolutions made by technicians familiar with this profession without departing from the scope of the technical solution of the present invention using the technical content disclosed above are all equivalent embodiments of the present invention. At the same time, any equivalent changes, modifications and evolutions made to the above embodiments based on the essential technology of the present invention are still within the scope of protection of the technical solution of the present invention.

Claims

1. A valve circuit system for analyzing trace or minor impurities in various high-purity gases, including a pulsed discharge helium ionization detector; characterized by: The valve circuit system is a four-valve six-column system; including Detection gas inlet assembly, the detection system inlet assembly is set with a measuring loop, a sample inlet, a sample exhaust port, and two carrier gas outlets. The external gas source to be tested is stored in the quantitative loop, and the corresponding carrier gas outlet is selected according to the analysis requirements; A first detection branch is connected between a carrier gas outlet of the detection gas inlet assembly and a pulse discharge helium ionization detector; the first detection branch is used to separate the mixed gas A and CH4 in the high-purity gas to be detected and transport them to the pulse discharge helium ionization detector for detection; The second detection branch is connected between another carrier gas outlet of the detection gas inlet assembly and the pulse discharge helium ionization detector; the second detection branch is used to separate CO2, C2H4, C2H6, and C2H2 in the high-purity gas to be detected and transport them to the pulse discharge helium ionization detector for detection.

2. The valve circuit system for analyzing trace or micro-impurities in a plurality of high-purity gases according to claim 1, characterized in that: It also includes a protective atmosphere component. The detection gas inlet component, the first detection branch, and the second detection branch are all located in the protective atmosphere component, and the protective atmosphere component is filled with carrier gas.

3. The valve circuit system for analyzing trace or micro-impurities in a plurality of high-purity gases according to claim 1 or 2, characterized in that: The test gas inlet assembly includes a ten-way valve A, two carrier gas inlet branches, two quantitative loops, and the test gas inlet branch and the test gas outlet branch. The ten-way valve A has ten connection points, marked A1-A10 in clockwise direction. The gas inlet branch to be tested is connected to A10, and the gas outlet branch to be tested is connected to A5; a quantitative loop is connected between A1 and A4, and between A6 and A9 through pipelines respectively; a carrier gas inlet branch is connected to A2 and A8 respectively; A3 serves as the carrier gas outlet and is connected to the first detection branch, and A7 serves as another carrier gas outlet and is connected to the second detection branch.

4. The valve circuit system for analyzing trace or micro-impurities in a plurality of high-purity gases according to claim 3, characterized in that: The gas inlet branch to be tested includes an inlet pipe and a first pressure balancing valve. The inlet pipe is connected between A10 and the external gas source to be tested. The first pressure balancing valve is located on the inlet pipe. The outlet branch of the gas to be measured includes an outlet pipe and a second pressure balancing valve. The outlet pipe is connected between A5 and an external gas collection device to be measured, or between A5 and the atmosphere. The second pressure balancing valve is located on the outlet pipe.

5. The valve circuit system for analyzing trace or micro-impurities in a plurality of high-purity gases according to claim 1 or 2, characterized in that: The first detection branch includes a pre-separation unit, a pipeline with a first main separation column, a main separation unit and a pipeline with a second main separation column. The end of the pipeline with the second main separation column is connected to a pulse discharge helium ionization detector. The first main separation column and the second main separation column separate the gas passing through into multiple gas segments according to the components. The pre-separation unit is equipped with a ten-way valve B, a first pre-separation column and a second pre-separation column, a carrier gas inlet branch, an exhaust branch, and a carrier gas outlet connected to the pipeline equipped with the first main separation column. Depending on the main component of the gas to be tested, the gas to be tested is passed into the first pre-separation column or the second pre-separation column, and the first pre-separation column or the second pre-separation column separates the gas to be tested into multiple gas segments according to the components. Based on the required detection components of the gas to be tested, the gas segments containing the detection components in the multiple gas segments are transported to the carrier gas outlet of the pre-separation unit, and the remaining gas segments are transported to the exhaust branch. The main separation unit is equipped with a six-way valve a, a carrier gas outlet connected to the pipeline with the second main separation column, an exhaust branch, and a carrier gas inlet branch. The six-way valve a transports the components to be detected in the gas segment transported by the first main separation column to the carrier gas outlet of the main separation unit, and the remaining gas segments are transported to the exhaust branch. Among them, the first pre-separation column for analyzing impurities in high-purity hydrogen adopts a high specific surface area carbon molecular sieve column; the second pre-separation column, the first main separation column, and the second main separation column for analyzing high-purity oxygen, high-purity argon, and high-purity nitrogen all adopt 13X molecular sieve analysis columns; for analyzing impurities in high-purity helium, either the first pre-separation column or the second pre-separation column can be selected.

6. The valve circuit system for analyzing trace or micro-impurities in a plurality of high-purity gases according to claim 5, characterized in that: Ten-way valve B has ten connection points, marked B1-B10 in clockwise order. The carrier gas outlet of the detection gas inlet assembly is connected to B10, and the pipeline with the first main separation column is connected to B5. The first pre-separation column is connected between B1 and B6, and the second pre-separation column is connected between B4 and B9. The carrier gas inlet branch is connected to B2. B3 and B8 are directly connected by a pipeline. The exhaust branch is connected to B7. The six-way valve a is provided with 6 connection points, which are marked as a1-a6 in clockwise direction; the pipeline with the first main separation column is connected to a6, the exhaust branch is connected to a1, the pipeline with the second main separation column is connected to a5, a2 and a4 are directly connected by a pipeline, and the carrier gas inlet branch is connected to a3.

7. The valve circuit system for analyzing trace or micro-impurities in a plurality of high-purity gases according to claim 5, characterized in that: The second detection branch sequentially includes a pipeline provided with a third pre-separation column, a second separation unit, and a pipeline provided with a third main separation column. The end of the pipeline provided with the third main separation column is connected to a pulsed discharge helium ionization detector. The third pre-separation column and the third main separation column separate the passing gas into multiple gas segments according to the components. The second separation unit is provided with a six-way valve b, a carrier gas outlet connected to the pipeline provided with the third main separation column, an exhaust branch, and a carrier gas inlet branch. The six-way valve b transports the components to be detected in the gas segment transported by the first main separation column to the carrier gas outlet of the main separation unit, and transports the remaining gas segment to the exhaust branch. The third pre-separation column and the third main separation column adopt polymer porous microsphere analysis columns.

8. The valve circuit system for analyzing trace or micro-impurities in a plurality of high-purity gases according to claim 7, characterized in that: The six-way valve b is provided with 6 connection points, which are marked as b1-b6 in clockwise direction; the pipeline with the first main separation column is connected to b6, the exhaust branch is connected to b1, the pipeline with the second main separation column is connected to b5, b2 and b4 are directly connected by a pipeline, and the carrier gas inlet branch is connected to b3.

9. The valve circuit system for analyzing trace or micro-impurities in a plurality of high-purity gases according to claim 2, characterized in that: A carrier gas inlet branch is provided on the pulse discharge helium ionization detector for purging the air inside the pulse discharge helium ionization detector. The carrier gas inlet branch is also connected to the protective atmosphere component, and passes through the cavity including the six-way valve b, the ten-way valve A, the ten-way valve B, and the six-way valve a in sequence, and is connected to the outside world after a damping column is provided at the end.

10. The valve circuit system for analyzing trace or micro-amount impurities in a plurality of high-purity gases according to claim 1, characterized in that: A plurality of exhaust branches and carrier gas inlet branches are provided in the valve circuit system. The exhaust branch includes an exhaust pipe and a damping column provided on the exhaust pipe, and the end of the exhaust pipe is directly connected to the outside world; the carrier gas inlet branch includes a carrier gas pipe, a pressure controller and a purifier provided in the carrier gas pipe, and the head end of the carrier gas pipe is connected to the carrier gas source; A carrier gas inlet branch is provided in the six-way valve a, and a damping column is also provided on the carrier gas inlet branch of the six-way valve a for balancing the pressure.

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