A high-precision separation device and method for dissolved gas components in transformer oil

Abstract

A high-precision separation device and method for dissolved gas components in transformer oil, belonging to the technical field of transformer fault detection, relates to solving the problems of large error and low precision in existing detection technologies due to low content of dissolved gas components in transformer oil; the high-precision separation device for dissolved gas components in transformer oil adopts a central cutting analysis method to fully analyze the dissolved gas hydrogen, methane, carbon monoxide, carbon dioxide, ethylene, ethane, acetylene, propylene, propane and propyne components in transformer oil through the connection and switching between a first switching valve, a second switching valve, a third switching valve, a fourth switching valve and a first chromatographic column, a second chromatographic column, a third chromatographic column and a fourth chromatographic column, without interference peaks between the components, and a quantitative loop is set in the device for sampling, thereby realizing quantitative and accurate analysis, greatly reducing the sampling error, and the sensitivity can reach the μmol / mol level.

Description

Technical Field

[0001] The invention belongs to the technical field of transformer fault detection, and relates to a device and method for separating dissolved gas components in transformer oil with high precision. Background Art

[0002] Transformers are often filled with mineral insulating oil for insulation. It is a mixture of hydrocarbon molecules of different molecular weights, containing CH3-, CH2-, and CH- chemical groups bonded together by CC bonds. When an electrical or thermal fault occurs, some C-CH bonds and CH bonds break, accompanied by the generation of a small amount of active hydrogen atoms and unstable hydrocarbon free radicals such as CH3 * 、CH2 * , CH * , C * , and these hydrogen atoms or free radicals quickly recombine through complex chemical reactions to generate hydrogen and low molecular hydrocarbon gases, such as methane, ethane, ethylene, acetylene, propylene, propane, propyne, etc. These components include inorganic and organic components and the content is often at the μmol / mol level. Currently, thermal conductivity cell detectors, hydrogen flame ionization detectors combined with nickel catalytic converters are used to analyze their component content, and manual sampling has a large error.

[0003] At present, the laboratory detection of dissolved gas in oil mainly adopts gas chromatography, which uses carrier gas to transport gas samples into the chromatographic column for gas separation, and then uses thermal conductivity cell (TCD) or hydrogen flame ionization detector (FID) to detect the volume fraction of gas components. The advantages of this method are good selectivity and high separation performance, but there are still some shortcomings: 1) The oil sample is sent to the laboratory after being collected from the site. In this process, it not only takes time, but also the collection, transportation, and storage will cause changes in the concentration of dissolved gas in the oil; 2) When quantitatively analyzing the gas, the operation steps are cumbersome, not only there may be errors in the degassing link, but also the manual correction of the detection curve will cause errors. The results obtained by different staff using the same gas chromatograph sometimes differ by 10%. The cumbersome operation, inevitable errors and the inability to track the transformer operation status in real time have limited the gas chromatography technology to play a better early warning role in transformer fault detection.

[0004] Backflushing means that the heavy components that do not need to be analyzed and have a long elution time are not separated, but are directly blown out of the chromatographic column in the opposite direction by switching the gas path. Backflushing can improve the operating efficiency of the instrument, save separation time, protect the chromatographic column, extend the service life of the column, and reduce detector contamination. In addition to backflushing heavy components, backflushing is also often used to analyze impurities in electronic gases such as sulfur hexafluoride and octafluoropropane. The components to be analyzed generally elute earlier, and the bottom gas generally elutes later. Backflushing can directly avoid the interference of the bottom gas on the components to be analyzed.

[0005] Heart cutting refers to the process of transferring the effluent from one column to a second column with a different stationary phase at a specific moment or within a specific time period during the chromatographic operation. Heart cutting simply means cutting out the material that comes out after the main component for analysis. Its main function is to reduce the impact of high-content substances on low concentrations, improve detection efficiency, and optimize detection limits. Heart cutting is generally used in conjunction with two-dimensional chromatography (GC+GC): some components pre-separated from the first column enter the second column directly or by cutting for further separation, while other components in the sample are vented. For example, in the analysis of hydrogen and nitrogen impurities in oxygen, when the hydrogen component enters the second column from the pre-column, the oxygen is continuously vented to prevent it from entering the second column; when the nitrogen is about to leave the pre-column, the valve is changed to allow it to enter the second column for further separation, thereby achieving the heart cutting of nitrogen. Summary of the invention

[0006] The technical problem to be solved by the present invention is how to design a high-precision separation device for dissolved gas components in transformer oil to solve the problems of large error and low precision in existing detection technology due to low content of dissolved gas components in transformer oil.

[0007] The present invention solves the above technical problems through the following technical solutions:

[0008] A high-precision separation device for dissolved gas components in transformer oil, comprising: a first switching valve (1), a quantitative ring (2), a first chromatographic column (3), a second chromatographic column (4), a second switching valve (5), a third switching valve (6), a third chromatographic column (7), a fourth chromatographic column (8), a fourth switching valve (9), a first plane tee (10), a second plane tee (11), a third plane tee (12), a fourth plane tee (13), a fifth plane tee (14), a sixth plane tee (15), a seventh plane tee (16), a first needle valve (17), a second needle valve (18), and a third needle valve (19); the first switching valve (1) is a ten-way switching valve, the second switching valve (5) is a four-way switching valve, the third switching valve (6) is a ten-way switching valve, and the fourth switching valve (9) is a four-way switching valve;

[0009] Port 1 of the first switching valve (1) is connected to the sample inlet, port 10 of the first switching valve (1) is connected to the input port of the quantitative ring (2), the output port of the quantitative ring (2) is connected to port 3 of the first switching valve (1), port 2 of the first switching valve (1) is connected to the sample outlet, port 4 of the first switching valve (1) is connected to port 2 of the fourth plane three-way (13), and the output port of the quantitative ring (2) is connected to the output port of the first switching valve (1). # The interface is connected, the port 5 of the first switching valve (1) is connected to the output end of the first chromatographic column (3), the input end of the first chromatographic column (3) is connected to the port 9 of the first switching valve (1), and the port 7 of the first switching valve (1) is connected to the port 3 of the third plane tee (12). # The interface is connected between port 8 of the first switching valve (1) and port 2 of the first needle valve (17). # The interface is connected, the port 6 of the first switching valve (1) is connected to the input end of the second chromatographic column (4); the output end of the second chromatographic column (4) is connected to the port 2 of the second switching valve (5); the port 3 of the second switching valve (5) is connected to the port 1 of the third switching valve (6); the port 4 of the second switching valve (5) is connected to the port 3 of the fifth flat tee (14); # The interface is connected, the No. 5 port of the second switching valve (5) is connected to the No. 6 port of the second switching valve (5), and the No. 1 port of the second switching valve (5) is connected to the No. 3 port of the sixth plane tee (15). # Interface connection; port 2 of the third switching valve (6) is connected to the input end of the fourth chromatographic column (8), the output end of the fourth chromatographic column (8) is connected to port 5 of the third switching valve (6), and port 3 of the third switching valve (6) is connected to port 1 of the fourth planar tee (13). # The interface is connected between port 4 of the third switching valve (6) and port 2 of the second needle valve (18). # The interface is connected between the No. 6 port of the third switching valve (6) and the No. 2 port of the sixth flat tee (15). # The interface is connected, the port 7 of the third switching valve (6) is connected to the output end of the third chromatographic column (7), the input end of the third chromatographic column (7) is connected to the port 10 of the third switching valve (6), and the port 8 of the third switching valve (6) is connected to the port 2 of the third needle valve (19). # The interface is connected between the No. 9 port of the third switching valve (6) and the No. 2 port of the fifth flat tee (14). # Interface connection; port 1 of the fourth switching valve (9) is connected to the carrier gas port, and port 2 of the fourth switching valve (9) is connected to port 3 of the second plane tee (11). # The interface is connected between the No. 3 port of the fourth switching valve (9) and the No. 3 port of the first plane tee (10). # The interface is connected, the No. 4 port of the fourth switching valve (9) is connected to the exhaust port; the No. 1 port of the first plane tee (10) is connected to the exhaust port; # Interface with the seventh plane tee (16) 1 # Interface connection, first plane tee (10) 2# Interface with the first needle valve (17) 1 # Interface connection, second plane tee (11) 1 # Interface with the fifth plane tee (14) 1 # Interface connection, second plane tee (11) 2 # Interface with the third plane tee (12) 1 # Interface connection, third plane tee (12) 2 # Interface with the fourth plane tee (13) 3 # Interface connection, sixth plane tee (15) 1 # The interface is connected to the detection port, 2 of the seventh plane tee (16) # Interface with the second needle valve (18) 1 # Interface connection, seventh plane tee (16) 3 # Interface with the third needle valve (19) 1 # Interface connection.

[0010] The high-precision gas component separation device for dissolved gas in transformer oil of the present invention is connected and switched between a first switching valve (1), a second switching valve (5), a third switching valve (6), a fourth switching valve (9) and a first chromatographic column (3), a second chromatographic column (4), a third chromatographic column (7), and a fourth chromatographic column (8), and adopts a heart-cutting analysis method to fully analyze the hydrogen, methane, carbon monoxide, carbon dioxide, ethylene, ethane, acetylene, propylene, propane, and propyne components dissolved in the transformer oil, and there are no interference peaks between the components. The device is provided with a quantitative loop (2) for sampling, thereby achieving quantitative and accurate analysis, greatly reducing sampling errors, and achieving a sensitivity of up to μmol / mol level.

[0011] Furthermore, it also includes: a plasma detector, a carrier gas device and an exhaust gas recovery device, wherein the plasma detector is connected to the detection port; the carrier gas device is connected to port No. 1 of the fourth switching valve (9); and the exhaust gas recovery device is connected to port No. 4 of the fourth switching valve (9).

[0012] Furthermore, the first chromatographic column (3), the second chromatographic column (4), and the fourth chromatographic column (8) are all polymer chromatographic columns, and the third chromatographic column (7) is a molecular sieve chromatographic column.

[0013] A method applied to the high-precision transformer oil dissolved gas component separation device includes the following processes: S1, sampling process; S2, sample pre-separation process; S3, process of detecting hydrogen, methane and carbon monoxide combined peak; S4, process of detecting carbon dioxide, ethylene, ethane and acetylene combined peak; S5, process of detecting propylene, propane and propyne combined peak.

[0014] Furthermore, the sampling process described in step S1 is specifically as follows: the No. 1 port of the first switching valve (1) is connected to the No. 10 port, and the No. 2 port of the first switching valve (1) is connected to the No. 3 port. The sample enters from the inlet port, passes through the No. 1 port of the first switching valve (1), the No. 10 port of the first switching valve (1), the quantitative ring (2), the No. 3 port of the first switching valve (1), and finally flows from the No. 2 port of the first switching valve (1) to the outlet port. The quantitative ring (2) stores a certain amount of sample, thereby completing the sampling process.

[0015] Furthermore, the sample pre-separation process described in step S2 is specifically as follows: the carrier gas passes through port No. 4 of the first switching valve (1), port No. 3 of the first switching valve (1), the quantitative ring (2), port No. 10 of the first switching valve (1), and port No. 9 of the first switching valve (1) in sequence, carrying the sample stored in the quantitative ring (2) into the first chromatographic column (3); the sample is pre-separated in the first chromatographic column (3), and the pre-separated sample flows through port No. 5 of the first switching valve (1) and port No. 6 of the first switching valve (1) to the second chromatographic column (4) to be separated into three combined peaks, and the order in which the three combined peaks flow out of the second chromatographic column (4) is: hydrogen methane carbon monoxide combined peak, carbon dioxide ethylene ethane acetylene combined peak, and propylene propane propyne combined peak.

[0016] Furthermore, the process of detecting the combined peak of hydrogen, methane and carbon monoxide in step S3 is as follows: the combined peak of hydrogen, methane and carbon monoxide flows out from the second chromatographic column (4), passes through port No. 2 of the second switching valve (5), port No. 3 of the second switching valve (5), port No. 1 of the third switching valve (6), and port No. 10 of the third switching valve (6) in sequence to flow to the third chromatographic column (7), is separated again into hydrogen, methane and carbon monoxide in the third chromatographic column (7), and then flows through port No. 7 of the third switching valve (6) and port No. 6 of the third switching valve (6) to port No. 2 of the sixth flat tee (15). # Interface, sixth plane tee (15) 1 # The gas flows into the detection port to detect the content of hydrogen, methane and carbon monoxide.

[0017] Furthermore, the process of detecting the carbon dioxide, ethylene, ethane and acetylene combined peak described in step S4 is specifically as follows: after the detection of the hydrogen, methane and carbon monoxide combined peak is completed, the third switching valve (6) is switched, and the carrier gas carrying the carbon dioxide, ethylene, ethane and acetylene combined peak flows out from the second chromatographic column (4), passes through port No. 2 of the second switching valve (5), port No. 3 of the second switching valve (5), port No. 1 of the third switching valve (6), and port No. 2 of the third switching valve (6) to the fourth chromatographic column (8), and is separated into carbon dioxide, ethylene, ethane and acetylene again in the fourth chromatographic column (8), and then flows through port No. 5 of the third switching valve (6) and port No. 6 of the third switching valve (6) to port 2 of the sixth flat tee (15). #Interface, sixth plane tee (15) 1 # The gas flows into the detection port to detect the component contents of carbon dioxide, ethylene, ethane and acetylene.

[0018] Furthermore, the process of detecting the propylene, propane, and propyne combined peak in step S5 is as follows: after the detection of the carbon dioxide, ethylene, ethane, and acetylene combined peak is completed, the second switching valve (5) is switched, and the carrier gas carrying the propylene, propane, and propyne combined peak is separated into propylene, propane, and propyne in the second chromatographic column (4), and flows through the No. 2 port of the second switching valve (5) and the No. 1 port of the second switching valve (5) to the No. 3 port of the sixth plane tee (15). # Interface, sixth plane tee (15) 1 # The gas flows into the detection port to detect the component contents of propylene, propane and propyne.

[0019] The advantages of the present invention are:

[0020] The high-precision gas component separation device for dissolved gas in transformer oil of the present invention is connected and switched between a first switching valve (1), a second switching valve (5), a third switching valve (6), a fourth switching valve (9) and a first chromatographic column (3), a second chromatographic column (4), a third chromatographic column (7), and a fourth chromatographic column (8), and adopts a heart-cutting analysis method to fully analyze the hydrogen, methane, carbon monoxide, carbon dioxide, ethylene, ethane, acetylene, propylene, propane, and propyne components dissolved in the transformer oil, and there are no interference peaks between the components. The device is provided with a quantitative loop (2) for sampling, thereby achieving quantitative and accurate analysis, greatly reducing sampling errors, and achieving a sensitivity of up to μmol / mol level. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 2 is a schematic structural diagram of a device for separating dissolved gas components in transformer oil with high precision according to a first embodiment of the present invention;

[0022] Figure 2 It is a schematic diagram of the sampling state and analysis and detection of hydrogen, methane and carbon monoxide of the high-precision transformer oil dissolved gas component separation device in Example 1 of the present invention;

[0023] Figure 3 It is a schematic diagram of analyzing and detecting the states of ethylene, ethane and acetylene components of a high-precision gas component separation device in transformer oil according to a first embodiment of the present invention;

[0024] Figure 4 It is a schematic diagram of analyzing and detecting the component states of carbon dioxide, propylene, propane, and propyne by a high-precision gas component separation device in transformer oil according to a first embodiment of the present invention;

[0025] Figure 52 is a schematic diagram of carrier gas flow path analysis of a high-precision transformer oil dissolved gas component separation device according to a first embodiment of the present invention;

[0026] Figure 6 This is a working flow chart of a device for separating dissolved gas components in high-precision transformer oil according to Embodiment 1 of the present invention. DETAILED DESCRIPTION

[0027] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be clearly and completely described below in combination with the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0028] The technical solution of the present invention is further described below in conjunction with the accompanying drawings and specific embodiments:

[0029] Embodiment 1

[0030] 1. Structure of the device

[0031] like Figure 1 As shown, a high-precision gas component separation device in transformer oil comprises: a first switching valve (1), a quantitative ring (2), a first chromatographic column (3), a second chromatographic column (4), a second switching valve (5), a third switching valve (6), a third chromatographic column (7), a fourth chromatographic column (8), a fourth switching valve (9), a first plane tee (10), a second plane tee (11), a third plane tee (12), a fourth plane tee (13), a fifth plane tee (14), a sixth plane tee (15), a seventh plane tee (16), a first needle valve (17), a second needle valve (18), and a third needle valve (19); the first switching valve (1) is a ten-way switching valve, the second switching valve (5) is a four-way switching valve, the third switching valve (6) is a ten-way switching valve, and the fourth switching valve (9) is a four-way switching valve; the first chromatographic column (3), the second chromatographic column (4), and the fourth chromatographic column (8) are all polymer chromatographic columns, and the third chromatographic column (7) is a molecular sieve chromatographic column.

[0032] Port 1 of the first switching valve (1) is connected to the sample inlet, port 10 of the first switching valve (1) is connected to the input port of the quantitative ring (2), the output port of the quantitative ring (2) is connected to port 3 of the first switching valve (1), port 2 of the first switching valve (1) is connected to the sample outlet, port 4 of the first switching valve (1) is connected to port 2 of the fourth plane three-way (13), and the output port of the quantitative ring (2) is connected to the output port of the first switching valve (1). #The interface is connected, the port 5 of the first switching valve (1) is connected to the output end of the first chromatographic column (3), the input end of the first chromatographic column (3) is connected to the port 9 of the first switching valve (1), and the port 7 of the first switching valve (1) is connected to the port 3 of the third plane tee (12). # The interface is connected between port 8 of the first switching valve (1) and port 2 of the first needle valve (17). # The interface is connected, the port 6 of the first switching valve (1) is connected to the input end of the second chromatographic column (4); the output end of the second chromatographic column (4) is connected to the port 2 of the second switching valve (5); the port 3 of the second switching valve (5) is connected to the port 1 of the third switching valve (6); the port 4 of the second switching valve (5) is connected to the port 3 of the fifth flat tee (14); # The interface is connected, the No. 5 port of the second switching valve (5) is connected to the No. 6 port of the second switching valve (5), and the No. 1 port of the second switching valve (5) is connected to the No. 3 port of the sixth plane tee (15). # Interface connection; port 2 of the third switching valve (6) is connected to the input end of the fourth chromatographic column (8), the output end of the fourth chromatographic column (8) is connected to port 5 of the third switching valve (6), and port 3 of the third switching valve (6) is connected to port 1 of the fourth planar tee (13). # The interface is connected between port 4 of the third switching valve (6) and port 2 of the second needle valve (18). # The interface is connected between the No. 6 port of the third switching valve (6) and the No. 2 port of the sixth flat tee (15). # The interface is connected, the port 7 of the third switching valve (6) is connected to the output end of the third chromatographic column (7), the input end of the third chromatographic column (7) is connected to the port 10 of the third switching valve (6), and the port 8 of the third switching valve (6) is connected to the port 2 of the third needle valve (19). # The interface is connected between the No. 9 port of the third switching valve (6) and the No. 2 port of the fifth flat tee (14). # Interface connection; port 1 of the fourth switching valve (9) is connected to the carrier gas device, and port 2 of the fourth switching valve (9) is connected to port 3 of the second plane tee (11) # The interface is connected between the No. 3 port of the fourth switching valve (9) and the No. 3 port of the first plane tee (10). # The No. 4 port of the fourth switching valve (9) is connected to the exhaust gas recovery device; the No. 1 port of the first plane tee (10) is connected to the exhaust gas recovery device; # Interface with the seventh plane tee (16) 1 # Interface connection, first plane tee (10) 2 # Interface with the first needle valve (17) 1 # Interface connection, second plane tee (11) 1 # Interface with the fifth plane tee (14) 1 # Interface connection, second plane tee (11) 2 #Interface with the third plane tee (12) 1 # Interface connection, third plane tee (12) 2 # Interface with the fourth plane tee (13) 3 # Interface connection, sixth plane tee (15) 1 # The interface is connected to the detection port, the detection port is connected to the plasma detector, and the seventh plane tee (16) is 2 # Interface with the second needle valve (18) 1 # Interface connection, seventh plane tee (16) 3 # Interface with the third needle valve (19) 1 # Interface connection.

[0033] 2. Path of carrier gas flow

[0034] like Figure 5 As shown, before the sample enters the device, the entire device is filled with carrier gas. In this embodiment, nitrogen is selected as the carrier gas. The carrier gas has three functions: first, to protect the first chromatographic column (3), the second chromatographic column (4), the third chromatographic column (7), and the fourth chromatographic column (8); second, to carry out the components separated from the first chromatographic column (3), the second chromatographic column (4), the third chromatographic column (7), and the fourth chromatographic column (8); and third, after the detection is completed, to carry out the exhaust gas in the device and input it into the exhaust gas treatment device for treatment.

[0035] (1) The path of the first carrier gas flow is as follows:

[0036] Port 1 of the fourth switching valve (9) → Port 2 of the fourth switching valve (9) → Port 3 of the second flat tee (11) # Interface → Second flat tee (11) 2 # Interface → Third plane tee (12) 1 # Interface → Third plane tee (12) 3 # Interface → Port 7 of the first switching valve (1) → Port 6 of the first switching valve (1) → Second chromatographic column (4) → Port 2 of the second switching valve (5) → Port 3 of the second switching valve (5) → Port 1 of the third switching valve (6) → Port 10 of the third switching valve (6) → Third chromatographic column (7) → Port 7 of the third switching valve (6) → Port 6 of the third switching valve (6) → Port 2 of the sixth flat tee (15) # Interface → Sixth plane tee (15) 1 # Interface → plasma detector;

[0037] (2) The path of the second carrier gas flow is as follows:

[0038] Port 1 of the fourth switching valve (9) → Port 2 of the fourth switching valve (9) → Port 3 of the second flat tee (11) # Interface → Second flat tee (11) 2 # Interface → Third plane tee (12) 1 # Interface → Third plane tee (12) 2 # Interface → Fourth plane tee (13) 3 # Interface → 2 of the fourth plane tee (13) # Interface → Port 4 of the first switching valve (1) → Port 5 of the first switching valve (1) → First chromatographic column (3) → Port 9 of the first switching valve (1) → Port 8 of the first switching valve (1) → Port 2 of the first needle valve (17) # Interface → 1st needle valve (17) # Interface → 2 of the first flat tee (10) # Interface → First plane tee (10) 3 # Interface→Port No. 3 of the fourth switching valve (9)→Port No. 4 of the fourth switching valve (9)→Exhaust gas treatment device;

[0039] (3) The path of the third carrier gas flow is as follows:

[0040] Port 1 of the fourth switching valve (9) → Port 2 of the fourth switching valve (9) → Port 3 of the second flat tee (11) # Interface → 1 of the second plane tee (11) # Interface → Fifth plane tee (14) 1 # Interface → Fifth plane tee (14) 3 # Interface → Port 4 of the second switching valve (5) → Port 5 of the second switching valve (5) → Port 6 of the second switching valve (5) → Port 1 of the second switching valve (5) → Port 3 of the sixth flat tee (15) # Interface → Sixth plane tee (15) 1 # Interface → plasma detector;

[0041] (4) The path of the fourth carrier gas flow is as follows:

[0042] Port 1 of the fourth switching valve (9) → Port 2 of the fourth switching valve (9) → Port 3 of the second flat tee (11) # Interface → 1 of the second plane tee (11) # Interface → Fifth plane tee (14) 1 # Interface → Port 9 of the third switching valve (6) → Port 8 of the third switching valve (6) → Port 2 of the third needle valve (19) # Interface → 1 of the third needle valve (19) # Interface → 3 of the seventh plane tee (16) #Interface → Seventh plane tee (16) 1 # Interface → 1st flat tee (10) # Interface → First plane tee (10) 3 # Interface→Port No. 3 of the fourth switching valve (9)→Port No. 4 of the fourth switching valve (9)→Exhaust gas treatment device;

[0043] (5) The path of the fifth carrier gas flow is as follows:

[0044] Port 1 of the fourth switching valve (9) → Port 2 of the fourth switching valve (9) → Port 3 of the second flat tee (11) # Interface → Second flat tee (11) 2 # Interface → Third plane tee (12) 1 # Interface → Third plane tee (12) 2 # Interface → Fourth plane tee (13) 3 # Interface → 1 of the fourth plane tee (13) # Interface → Port 3 of the third switching valve (6) → Port 2 of the third switching valve (6) → Fourth chromatographic column (8) → Port 5 of the third switching valve (6) → Port 4 of the third switching valve (6) → Port 2 of the second needle valve (18) # Interface → 1 of the second needle valve (18) # Interface → Seventh plane tee (16) 2 # Interface → Seventh plane tee (16) 1 # Interface → 1st flat tee (10) # Interface → First plane tee (10) 3 # Interface→Port No. 3 of the fourth switching valve (9)→Port No. 4 of the fourth switching valve (9)→Exhaust gas treatment device.

[0045] 3. Workflow of the device

[0046] like Figure 6 As shown, the working process of the device includes the following processes:

[0047] 3.1 Sampling process

[0048] like Figure 1 As shown, the first switching valve (1) is switched, and the port No. 1 of the first switching valve (1) is connected to the port No. 10, and the port No. 2 of the first switching valve (1) is connected to the port No. 3. The sample enters from the inlet, passes through the port No. 1 of the first switching valve (1), the port No. 10 of the first switching valve (1), the quantitative ring (2), the port No. 3 of the first switching valve (1), and finally flows from the port No. 2 of the first switching valve (1) to the outlet. In this process, the quantitative ring (2) stores a certain amount of sample to complete the sampling.

[0049] 3.2 Sample pre-separation process

[0050] like Figure 2 The first switching valve (1) is switched as shown, and the second carrier gas passes through port No. 4 of the first switching valve (1), port No. 3 of the first switching valve (1), the quantitative ring (2), port No. 10 of the first switching valve (1), and port No. 9 of the first switching valve (1) in sequence, carrying the sample stored in the quantitative ring (2) into the first chromatographic column (3); the sample is pre-separated in the first chromatographic column (3), and the pre-separated sample flows through port No. 5 of the first switching valve (1) and port No. 6 of the first switching valve (1) to the second chromatographic column (4) to be separated into three combined peaks, and the order in which the three combined peaks flow out of the second chromatographic column (4) is: hydrogen, methane, carbon monoxide combined peak, carbon dioxide, ethylene, ethane, acetylene combined peak, and propylene, propane, and propyne combined peak.

[0051] A plasma detector is connected to the detection port of the device to detect the component contents of the three combined peaks. The processes are as follows:

[0052] 3.3. Process of detecting the combined peak of hydrogen, methane and carbon monoxide

[0053] like Figure 2 As shown, the combined peak of hydrogen, methane and carbon monoxide first flows out from the second chromatographic column (4), passes through port 2 of the second switching valve (5), port 3 of the second switching valve (5), port 1 of the third switching valve (6), and port 10 of the third switching valve (6) to the third chromatographic column (7), is separated into hydrogen, methane and carbon monoxide again in the third chromatographic column (7), and then flows through port 7 of the third switching valve (6) and port 6 of the third switching valve (6) to port 2 of the sixth flat tee (15). # Interface, sixth plane tee (15) 1 # The gas flows into the plasma detector to detect the content of hydrogen, methane and carbon monoxide.

[0054] 3.4. Process of detecting the combined peak of carbon dioxide, ethylene, ethane and acetylene

[0055] After the combined peak of hydrogen, methane and carbon monoxide is detected, Figure 3 The third switching valve (6) is switched as shown, and the first carrier gas carrying the combined peak of carbon dioxide, ethylene, ethane and acetylene flows out from the second chromatographic column (4), passes through port No. 2 of the second switching valve (5), port No. 3 of the second switching valve (5), port No. 1 of the third switching valve (6), and port No. 2 of the third switching valve (6) to flow to the fourth chromatographic column (8), and is separated again into carbon dioxide, ethylene, ethane and acetylene in the fourth chromatographic column (8), and then flows through port No. 5 of the third switching valve (6) and port No. 6 of the third switching valve (6) to port No. 2 of the sixth flat tee (15). # Interface, sixth plane tee (15) 1 #The gas flows into the plasma detector to detect the content of carbon dioxide, ethylene, ethane and acetylene.

[0056] 3.5. Detection process of propylene, propane and propyne combined peak

[0057] After the combined peak of carbon dioxide, ethylene, ethane and acetylene is detected, Figure 4 The second switching valve (5) is switched as shown, and the first carrier gas carrying the propylene, propane and propyne peak is separated into propylene, propane and propyne in the second chromatographic column (4), and flows through the No. 2 port of the second switching valve (5) and the No. 1 port of the second switching valve (5) to the No. 3 port of the sixth plane tee (15). # Interface, sixth plane tee (15) 1 # The gas flows into the plasma detector to detect the content of propylene, propane and propyne.

[0058] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit the same. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that the technical solutions described in the aforementioned embodiments may still be modified, or some of the technical features may be replaced by equivalents. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A high-precision separation device for dissolved gas components in transformer oil, characterized in that: include: a first switching valve (1), a quantitative ring (2), a first chromatographic column (3), a second chromatographic column (4), a second switching valve (5), a third switching valve (6), a third chromatographic column (7), a fourth chromatographic column (8), a fourth switching valve (9), a first plane tee (10), a second plane tee (11), a third plane tee (12), a fourth plane tee (13), a fifth plane tee (14), a sixth plane tee (15), a seventh plane tee (16), a first needle valve (17), a second needle valve (18) and a third needle valve (19); the first switching valve (1) is a ten-way switching valve, the second switching valve (5) is a four-way switching valve, the third switching valve (6) is a ten-way switching valve, and the fourth switching valve (9) is a four-way switching valve; Port 1 of the first switching valve (1) is connected to the sample inlet, port 10 of the first switching valve (1) is connected to the input port of the quantitative ring (2), the output port of the quantitative ring (2) is connected to port 3 of the first switching valve (1), port 2 of the first switching valve (1) is connected to the sample outlet, port 4 of the first switching valve (1) is connected to port 2 of the fourth plane three-way (13), and the output port of the quantitative ring (2) is connected to the output port of the first switching valve (1). # The interface is connected, the port 5 of the first switching valve (1) is connected to the output end of the first chromatographic column (3), the input end of the first chromatographic column (3) is connected to the port 9 of the first switching valve (1), and the port 7 of the first switching valve (1) is connected to the port 3 of the third plane tee (12). # The interface is connected between port 8 of the first switching valve (1) and port 2 of the first needle valve (17). # The interface is connected, the port 6 of the first switching valve (1) is connected to the input end of the second chromatographic column (4); the output end of the second chromatographic column (4) is connected to the port 2 of the second switching valve (5); the port 3 of the second switching valve (5) is connected to the port 1 of the third switching valve (6); the port 4 of the second switching valve (5) is connected to the port 3 of the fifth flat tee (14); # The interface is connected, the No. 5 port of the second switching valve (5) is connected to the No. 6 port of the second switching valve (5), and the No. 1 port of the second switching valve (5) is connected to the No. 3 port of the sixth plane tee (15). # Interface connection; port 2 of the third switching valve (6) is connected to the input end of the fourth chromatographic column (8), the output end of the fourth chromatographic column (8) is connected to port 5 of the third switching valve (6), and port 3 of the third switching valve (6) is connected to port 1 of the fourth planar tee (13). # The interface is connected between port 4 of the third switching valve (6) and port 2 of the second needle valve (18). # The interface is connected between port 6 of the third switching valve (6) and port 2 of the sixth flat tee (15). # The interface is connected, the port 7 of the third switching valve (6) is connected to the output end of the third chromatographic column (7), the input end of the third chromatographic column (7) is connected to the port 10 of the third switching valve (6), and the port 8 of the third switching valve (6) is connected to the port 2 of the third needle valve (19). # The interface is connected between the No. 9 port of the third switching valve (6) and the No. 2 port of the fifth flat tee (14). # Interface connection; port 1 of the fourth switching valve (9) is connected to the carrier gas port, and port 2 of the fourth switching valve (9) is connected to port 3 of the second plane tee (11). # The interface is connected between the No. 3 port of the fourth switching valve (9) and the No. 3 port of the first plane tee (10). # The interface is connected, the No. 4 port of the fourth switching valve (9) is connected to the exhaust port; the No. 1 port of the first plane tee (10) is connected to the exhaust port; # Interface with the seventh plane tee (16) 1 # Interface connection, first plane tee (10) 2 # Interface with the first needle valve (17) 1 # Interface connection, second plane tee (11) 1 # Interface with the fifth plane tee (14) 1 # Interface connection, second plane tee (11) 2 # Interface with the third plane tee (12) 1 # Interface connection, third plane tee (12) 2 # Interface with the fourth plane tee (13) 3 # Interface connection, sixth plane tee (15) 1 # The interface is connected to the detection port, 2 of the seventh plane tee (16) # Interface with the second needle valve (18) 1 # Interface connection, seventh plane tee (16) 3 # Interface with the third needle valve (19) 1 # Interface connection; The first chromatographic column (3), the second chromatographic column (4), and the fourth chromatographic column (8) are all polymer chromatographic columns, and the third chromatographic column (7) is a molecular sieve chromatographic column; The sample is pre-separated in the first chromatographic column (3). The pre-separated sample flows into the second chromatographic column (4) through the No. 5 port of the first switching valve (1) and the No. 6 port of the first switching valve (1) to be separated into three combined peaks. The order in which the three combined peaks flow out of the second chromatographic column (4) is: hydrogen, methane, and carbon monoxide combined peak, carbon dioxide, ethylene, ethane, and acetylene combined peak, and propylene, propane, and propyne combined peak. The hydrogen, methane, and carbon monoxide combined peak is further separated into hydrogen, methane, and carbon monoxide in the third chromatographic column (7). The carbon dioxide, ethylene, ethane, and acetylene combined peak is further separated into carbon dioxide, ethylene, ethane, and acetylene in the fourth chromatographic column (8). The propylene, propane, and propyne combined peak is separated into propylene, propane, and propyne in the second chromatographic column (4).

2. The high-precision gas component separation device in transformer oil according to claim 1, characterized in that: Also includes: A plasma detector, a gas carrier device and an exhaust gas recovery device, wherein the plasma detector is connected to the detection port; the gas carrier device is connected to port No. 1 of the fourth switching valve (9); and the exhaust gas recovery device is connected to port No. 4 of the fourth switching valve (9).

3. A method for separating dissolved gas components in high-precision transformer oil according to any one of claims 1 to 2, characterized in that: The method comprises the following processes: S1, sampling process; S2, sample pre-separation process; S3, process of detecting the combined peak of hydrogen, methane and carbon monoxide; S4, process of detecting the combined peak of carbon dioxide, ethylene, ethane and acetylene; S5, process of detecting the combined peak of propylene, propane and propyne.

4. The method according to claim 3, characterized in that The sampling process described in step S1 is specifically as follows: the No. 1 port of the first switching valve (1) is connected to the No. 10 port, and the No. 2 port of the first switching valve (1) is connected to the No. 3 port. The sample enters from the inlet port, passes through the No. 1 port of the first switching valve (1), the No. 10 port of the first switching valve (1), the quantitative ring (2), the No. 3 port of the first switching valve (1), and finally flows from the No. 2 port of the first switching valve (1) to the outlet port. The quantitative ring (2) stores a certain amount of sample, thereby completing the sampling process.

5. The method according to claim 4, characterized in that The sample pre-separation process described in step S2 is specifically as follows: the carrier gas passes through port No. 4 of the first switching valve (1), port No. 3 of the first switching valve (1), the quantitative loop (2), port No. 10 of the first switching valve (1), and port No. 9 of the first switching valve (1) in sequence, carrying the sample stored in the quantitative loop (2) into the first chromatographic column (3); the sample is pre-separated in the first chromatographic column (3), and the pre-separated sample flows through port No. 5 of the first switching valve (1) and port No. 6 of the first switching valve (1) to the second chromatographic column (4) to be separated into three combined peaks, and the order in which the three combined peaks flow out of the second chromatographic column (4) is: hydrogen methane carbon monoxide combined peak, carbon dioxide ethylene ethane acetylene combined peak, and propylene propane propyne combined peak.

6. The method according to claim 5, characterized in that The process of detecting the combined peak of hydrogen, methane and carbon monoxide in step S3 is as follows: the combined peak of hydrogen, methane and carbon monoxide flows out from the second chromatographic column (4), passes through port No. 2 of the second switching valve (5), port No. 3 of the second switching valve (5), port No. 1 of the third switching valve (6), and port No. 10 of the third switching valve (6) in sequence to flow to the third chromatographic column (7), is separated again into hydrogen, methane and carbon monoxide in the third chromatographic column (7), and then flows through port No. 7 of the third switching valve (6) and port No. 6 of the third switching valve (6) to port No. 2 of the sixth flat tee (15). # Interface, sixth plane tee (15) 1 # The gas flows into the detection port to detect the content of hydrogen, methane and carbon monoxide.

7. The method according to claim 6, characterized in that The process of detecting the carbon dioxide, ethylene, ethane and acetylene combined peak described in step S4 is specifically as follows: after the detection of the hydrogen, methane and carbon monoxide combined peak is completed, the third switching valve (6) is switched, and the carrier gas carrying the carbon dioxide, ethylene, ethane and acetylene combined peak flows out from the second chromatographic column (4), passes through port No. 2 of the second switching valve (5), port No. 3 of the second switching valve (5), port No. 1 of the third switching valve (6), and port No. 2 of the third switching valve (6) to the fourth chromatographic column (8), and is separated into carbon dioxide, ethylene, ethane and acetylene again in the fourth chromatographic column (8), and then flows through port No. 5 of the third switching valve (6) and port No. 6 of the third switching valve (6) to port No. 2 of the sixth flat tee (15). # Interface, sixth plane tee (15) 1 # The gas flows into the detection port to detect the component contents of carbon dioxide, ethylene, ethane and acetylene.

8. The method according to claim 7, characterized in that The process of detecting the propylene, propane, and propyne combined peak in step S5 is as follows: after the detection of the carbon dioxide, ethylene, ethane, and acetylene combined peak is completed, the second switching valve (5) is switched, and the carrier gas carrying the propylene, propane, and propyne combined peak is separated into propylene, propane, and propyne in the second chromatographic column (4), and flows through the No. 2 port of the second switching valve (5) and the No. 1 port of the second switching valve (5) to the No. 3 port of the sixth plane tee (15). # Interface, sixth plane tee (15) 1 # The gas flows into the detection port to detect the component contents of propylene, propane and propyne.

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