System and method for analyzing impurities in high-purity disilane

Abstract

The invention discloses an analysis system and an analysis method for impurities in high-purity disilane. The analysis system comprises a first ten-way valve, a first quantitative tube, a first chromatographic column, a first six-way valve, a second quantitative tube, a second chromatographic column, a second six-way valve, a first PDD detector, a third chromatographic column, a second twenty-way valve, a third quantitative tube, a fourth chromatographic column, a third six-way valve, a fifth chromatographic column and a second PDD detector. According to the analysis system and the analysis method for the impurities in the high-purity disilane, a five-valve five-column double-detector configuration mode is adopted, different impurities are distributed on different detectors, the working state of a multi-way valve is controlled, and the valve switching time is regulated and controlled, so that sample introduction of the same gas path and separation and analysis of multiple gas paths are realized, and the detection accuracy is improved. Therefore, analysis results of all impurities in the sample gas can be obtained in one analysis process, main components or silane impurities can be reversely blown out, interference of a main peak background is removed, and the efficiency and accuracy of the analysis process are improved.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of analytical testing technology, and particularly relates to a system and method for analyzing impurities in high-purity disilane. BACKGROUND

[0002] The impurities in high-purity disilane gas include the following categories: air impurities, such as oxygen, nitrogen, carbon monoxide, carbon dioxide, and hydrogen; organic impurities, such as methane, ethane, ethylene, acetylene, propane, butane, and other hydrocarbons; and other silicon impurities, such as silane and propylsilane. The current method for testing the purity of disilane is to use gas chromatography with a PDD (Pulsed Discharge Detector) detector for detection. This method separates the components at different levels through a chromatographic column, and then captures the ionized signal value for quantitative and qualitative analysis. However, the main problem with this method is that high-purity disilane gas includes multiple types of impurities, and the types of components to be analyzed are numerous and complex, resulting in a long time required for sample testing. In addition, the peak of the main component of disilane will affect the separation of silane and propylsilane, silicon compounds will affect the chromatographic column, and organic compounds with the same number of carbon molecules are difficult to separate.

[0003] The information disclosed in this Background section is only for the purpose of increasing the understanding of the background of the present application and should not be taken as admitting that this information forms prior art that is already known to those of ordinary skill in the art. SUMMARY

[0004] The present application aims to provide a system for analyzing impurities in high-purity disilane, which adopts a configuration mode of five valves, five columns, and double detectors, can distribute different impurities to different detectors, realizes simultaneous sampling, and simultaneously analyzes impurities, and can obtain the analysis results of all impurity components in one analysis process.

[0005] In order to achieve the above object, one specific embodiment of the present application provides a system for analyzing impurities in high-purity disilane, which comprises a first ten-way valve, a first constant-volume tube, a first chromatographic column, a first six-way valve, a second constant-volume tube, a second chromatographic column, a second six-way valve, a first PDD detector, a third chromatographic column, a second ten-way valve, a third constant-volume tube, a fourth chromatographic column, a third six-way valve, a fifth chromatographic column, and a second PDD detector. Sample gas of disilane is introduced from the first ten-way valve; the first constant-volume tube is in communication with the first ten-way valve at both ends and is used to store the sample gas; the first chromatographic column is in communication with the first ten-way valve at both ends and is used to pre-separate the sample gas; the first six-way valve is in communication with the first ten-way valve; the second constant-volume tube is in communication with the first six-way valve at both ends and is used to store the sample gas; one end of the second chromatographic column is in communication with the first ten-way valve and is used to separate hydrogen, oxygen, nitrogen, and carbon monoxide in the sample gas; the second six-way valve is in communication with the other end of the second chromatographic column; the first PDD detector is in communication with the second six-way valve and is used to detect the impurity content in the sample gas; the first carrier gas and the second carrier gas are introduced from the first ten-way valve to send the sample gas in the first constant-volume tube into the first chromatographic column and the second chromatographic column for separation; one end of the third chromatographic column is in communication with the first six-way valve, and the other end is in communication with the second six-way valve, and is used to separate propylsilane and butane in the sample gas; the third carrier gas is introduced from the second six-way valve to send the sample gas in the second constant-volume tube to the third chromatographic column for separation and to the first PDD detector for detection; the second ten-way valve is in communication with the first six-way valve; the third constant-volume tube is in communication with the second ten-way valve at both ends and is used to store the sample gas; the sample gas can be introduced from the first ten-way valve to sequentially fill the first constant-volume tube, the second constant-volume tube, and the third constant-volume tube through the first six-way valve and the second ten-way valve; the fourth chromatographic column is in communication with the second ten-way valve at both ends and is used to pre-separate the sample gas; the third six-way valve is in communication with the second ten-way valve; the fifth chromatographic column is in communication with the third six-way valve at both ends and is used to separate methane, carbon dioxide, ethane, ethylene, acetylene, and propane in the sample gas; the second PDD detector is in communication with the fifth chromatographic column and the third six-way valve; the fourth carrier gas is introduced from the second ten-way valve to send the sample gas in the third constant-volume tube into the fourth chromatographic column and the fifth chromatographic column for separation and into the second PDD detector for analysis; the fifth carrier gas is introduced from the third six-way valve to clean the gas path, and the sixth carrier gas is introduced from the second ten-way valve to blow the sample gas in the fifth chromatographic column into the second PDD detector for analysis.

[0006] In one or more embodiments of the present application, the first ten-way valve has A1 to A10 ports, the sample gas is introduced from the A8 port, the first carrier gas is introduced from the A10 port, and the second carrier gas is introduced from the A3 port; one end of the first constant-volume tube is in communication with the A9 port, and the other end is in communication with the A6 port; one end of the first chromatographic column is in communication with the A1 port, and the other end is in communication with the A5 port.

[0007] The first six-way valve has B1 to B10 ports, the B3 port is in communication with the A7 port, and the third carrier gas is introduced from the B1 port; one end of the second constant-volume tube is in communication with the B2 port, and the other end is in communication with the B5 port; the second six-way valve has C1 to C6 ports, and the C4 port is in communication with the C6 port.

[0008] One end of the second chromatographic column is in communication with the A2 port, and the other end is in communication with the C3 port; one end of the third chromatographic column is in communication with the B6 port, and the other end is in communication with the C1 port; the first PDD detector is in communication with the C2 port.

[0009] The second ten-way valve has D1 to D10 ports, the D8 port is in communication with the B4 port, and the fourth carrier gas is introduced from the D10 port; one end of the third constant-volume tube is in communication with the D9 port, and the other end is in communication with the D6 port; one end of the fourth chromatographic column is in communication with the D1 port, and the other end is in communication with the D5 port.

[0010] The third six-way valve has E1 to E6 ports, the E4 port is in communication with the D2 port, the E2 port is in communication with the E6 port, the fifth carrier gas is introduced from the E1 port, and the sixth carrier gas is introduced from the D3 port; one end of the fifth chromatographic column is in communication with the E5 port, and the other end is in communication with the E3 port; the second PDD detector is in communication with the other end of the fifth chromatographic column and the E3 port.

[0011] In one or more embodiments of the present application, the first ten-way valve has an OFF state and an ON state, in the OFF state, the A10 port is in communication with the A1 port, the A8 port is in communication with the A9 port, the A6 port is in communication with the A7 port, the A3 port is in communication with the A2 port, and the A5 port is in communication with the A4 port; in the ON state, the A9 port is in communication with the A10 port, the A8 port is in communication with the A7 port, the A6 port is in communication with the A5 port, the A2 port is in communication with the A1 port, and the A3 port is in communication with the A4 port.

[0012] The first six-way valve has an OFF state and an ON state, in the OFF state, the B3 port is in communication with the B2 port, the B5 port is in communication with the B4 port, and the B1 port is in communication with the B6 port; in the ON state, the B3 port is in communication with the B4 port, the B5 port is in communication with the B6 port, and the B1 port is in communication with the B2 port.

[0013] The second six-way valve has an OFF state and an ON state, in the OFF state, C3 port communicates with C2 port, C4 port communicates with C5 port; C1 port communicates with C6 port; in the ON state, C3 port communicates with C4 port, C6 port communicates with C5 port; C1 port communicates with C2 port.

[0014] The twentieth valve has an OFF state and an ON state, in the OFF state, D10 port communicates with D1 port, D8 port communicates with D9 port, D6 port communicates with D7 port, D3 port communicates with D2 port, D5 port communicates with D4 port; in the ON state, D9 port communicates with D10 port, D8 port communicates with D7 port, D6 port communicates with D5 port, D2 port communicates with D1 port, D3 port communicates with D4 port.

[0015] The third six-way valve has an OFF state and an ON state, in the OFF state, E3 port communicates with E2 port, E4 port communicates with E5 port; E1 port communicates with E6 port; in the ON state, E3 port communicates with E4 port, E6 port communicates with E5 port; E1 port communicates with E2 port.

[0016] In one or more embodiments of the present application, the first chromatographic column is a modified activated carbon pre-column filled with activated carbon particles, the particle size of the activated carbon is 60 to 80 mesh. The second chromatographic column is a 5A column filled with 5A molecular sieve, the pore size of the molecular sieve is 60-80 mesh. The third chromatographic column is a capillary column with an inner diameter of 0.53 to 0.55 mm, the capillary column is filled with methyl polysiloxane. The fourth chromatographic column is an R column filled with porous polymer monomers, the pore size of the porous polymer monomers is 60 to 80 mesh. The fifth chromatographic column is a Q column filled with high molecular porous microspheres, the pore size of the high molecular porous microspheres is 60-80 mesh.

[0017] Another specific embodiment of the present application provides a method for analyzing impurities in high-purity disilane using the above-mentioned analysis system, which comprises: S1: the first ten-way valve, the first six-way valve, the second six-way valve, the second ten-way valve and the third six-way valve are all in the OFF state, sample gas is introduced from the A8 port, and the first, second and third dosing tubes are sequentially filled; S2: the first ten-way valve, the first six-way valve, the second ten-way valve and the third six-way valve are simultaneously switched to the ON state, the second six-way valve remains in the OFF state, the sample gas in the first dosing tube is sequentially swept into the first and second chromatographic columns by the first carrier gas introduced from the A10 port for separation, and the hydrogen, oxygen, nitrogen and carbon monoxide in the sample gas are separated and sent into the first PDD detector for analysis to obtain the corresponding contents; the sample gas in the second dosing tube is swept into the third chromatographic column by the third carrier gas introduced from the B1 port for separation, and the propylsilane and butane in the sample gas are left in the third chromatographic column, and the remaining components are discharged from the C5 port; the sample gas in the third dosing tube is swept into the fourth chromatographic column by the fourth carrier gas introduced from the D10 port for separation, and the separated methane and carbon dioxide are sent into the second PDD detector, and the residual sample gas remains in the fourth chromatographic column; S3: the first ten-way valve, the third six-way valve and the first six-way valve are sequentially switched to the OFF state, the second ten-way valve remains in the ON state, and the residual sample gas in the fourth chromatographic column is swept into the fifth chromatographic column by the fourth carrier gas; S4: the second ten-way valve is switched to the OFF state at the same time as the second six-way valve is switched to the ON state, the propylsilane and butane in the third chromatographic column are sent into the first PDD detector by the third carrier gas from the B1 port for analysis to obtain the corresponding contents; the ethane, ethylene, acetylene and propane separated from the fifth chromatographic column are sent into the second PDD detector for analysis to obtain the corresponding contents.

[0018] In one or more embodiments of the present application, in steps S2 to S3, the first ten-way valve remains in the ON state for 1 to 2 minutes and is then switched to the OFF state; the third six-way valve remains in the ON state for 4 to 6 minutes and is then switched to the OFF state; the first six-way valve remains in the ON state for 4.05 to 6.05 minutes and is then switched to the OFF state, and the first six-way valve is switched to the OFF state after the third six-way valve is switched to the OFF state; and the second ten-way valve remains in the ON state for 12 to 14 minutes and is then switched to the OFF state.

[0019] In one or more embodiments of the present application, in step S3, after the first ten-way valve is switched to the OFF state, the first carrier gas sequentially passes through the A10 port and the A1 port to discharge the residual silicon impurities in the first chromatographic column from the A5 port and the A4 port.

[0020] In one or more embodiments of the present invention, in step S4, after the second ten-way valve is switched to the OFF state, the fourth carrier gas sequentially passes through port D10 and port D1 to discharge the residual silane in the fourth chromatographic column from port D5 and port D4.

[0021] In one or more embodiments of the present invention, S1 specifically refers to: the first ten-way valve, the first six-way valve, the second six-way valve, the second ten-way valve, and the third six-way valve are all in the OFF state, and the sample gas is introduced from the A8 port and passes sequentially through the A9 port, the first metering tube, the A6 port, the A7 port, the B3 port, the B2 port, the second metering tube, the B5 port, the B4 port, the D8 port, the D9 port, and the third metering tube, filling the first metering tube, the second metering tube, and the third metering tube.

[0022] In one or more embodiments of the present invention, S2 specifically involves: simultaneously switching the first ten-way valve, the first six-way valve, the second ten-way valve, and the third six-way valve to the ON state, while the second six-way valve remains in the OFF state. The first carrier gas is introduced through port A10 and sequentially passes through port A9, the first quantitative tube, port A6, and port A5 to purge the sample gas in the first quantitative tube into the first chromatographic column for pre-separation. The sample gas pre-separated by the first chromatographic column is purged into the second chromatographic column through ports A1 and A2 for separation. Hydrogen, oxygen, nitrogen, and carbon monoxide are separated in the second chromatographic column and sequentially sent to the first PDD detector through ports C3 and C2 for analysis to obtain the content of hydrogen, oxygen, nitrogen, and carbon monoxide. The third carrier gas enters through port B1, purges the sample gas from the second quantitative tube through port B2, and then purges the sample gas into the third chromatographic column through ports B5 and B6, leaving propane and butane in the third chromatographic column. The remaining components are discharged through ports C1, C6, C4, and C5. The fourth carrier gas enters through port D10, purges the sample gas from the third quantitative tube through port D9, and then sends the sample gas into the fourth chromatographic column for separation through ports D6 and D5. The fourth chromatographic column separates the sample gas, and the separated methane and carbon dioxide are then sent to the second PDD detector for analysis through ports D1, D2, E4, and E3. The remaining sample gas remains in the fourth chromatographic column.

[0023] In one or more embodiments of the present invention, S3 specifically involves: the first ten-way valve, the third six-way valve, and the first six-way valve being switched to the OFF state in sequence, the second ten-way valve remaining in the ON state, and the residual sample gas in the fourth chromatographic column being sent to the fifth chromatographic column for separation by the fourth carrier gas through the D1 port, D2 port, E4 port, and E5 port in sequence.

[0024] In one or more embodiments of the present invention, S4 specifically involves: simultaneously switching the second ten-way valve to the OFF state and the second six-way valve to the ON state; the third carrier gas sequentially passes through ports B1 and B6 to send the propane and butane in the third chromatographic column to the first PDD detector for analysis via ports C1 and C2 to obtain the corresponding content; the sixth carrier gas sequentially passes through ports D3, D2, E4, and E6 to send the ethane, ethylene, acetylene, and propane separated from the fifth chromatographic column to the second PDD detector for analysis to obtain the corresponding content.

[0025] In one or more embodiments of the present invention, the first carrier gas, the second carrier gas, the third carrier gas, the fourth carrier gas, the fifth carrier gas, and the sixth carrier gas are helium gases with a purity of 6N or higher, and are continuously supplied to the first ten-way valve, the first six-way valve, the second ten-way valve, and the third six-way valve from the same gas source through different gas paths.

[0026] Compared with existing technologies, the analytical system and method for analyzing impurities in high-purity silane of the present invention adopts a five-valve, five-column, dual-detector configuration, distributing different impurities to different detectors. By controlling the working state of the multi-way valve and adjusting the valve switching time, the same gas path can be used for sample injection, while multiple gas paths can be separated and analyzed. Thus, the analytical results of all impurities in the sample gas can be obtained in one analysis process, and the main component or silane impurities can be backflushed to remove the interference of the main peak background. This avoids interference from the main component or impurities, improving the efficiency and accuracy of the analytical process. Attached Figure Description

[0027] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0028] Figure 1 This is a first schematic diagram of an analysis system for impurities in high-purity silane according to an embodiment of the present invention;

[0029] Figure 2 This is a second schematic diagram of an analysis system for impurities in high-purity silane according to an embodiment of the present invention;

[0030] Figure 3 This is a third schematic diagram of an analysis system for impurities in high-purity silane according to an embodiment of the present invention;

[0031] Figure 4 This is a fourth schematic diagram of an analysis system for impurities in high-purity silane according to an embodiment of the present invention.

[0032] Explanation of key figure labels:

[0033] 1-First 10-port valve, 2-First 6-port valve, 3-Second 6-port valve, 4-Second 10-port valve, 5-Third 6-port valve, 6-First quantitative tube, 7-First chromatographic column, 8-Second quantitative tube, 9-Second chromatographic column, 10-First PDD detector, 11-Third chromatographic column, 12-Third quantitative tube, 13-Fourth chromatographic column, 14-Fifth chromatographic column, 15-Second PDD detector. Detailed Implementation

[0034] To enable those skilled in the art to better understand the technical solutions in this disclosure, the technical solutions in the embodiments of this disclosure will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this disclosure, and not all embodiments. Based on the embodiments in this disclosure, all other embodiments obtained by those skilled in the art without creative effort should fall within the scope of protection of this disclosure.

[0035] like Figure 1As shown, an embodiment of the present invention discloses an analytical system for impurities in high-purity silane, comprising a first ten-way valve 1, a first metering tube 6, a first chromatographic column 7, a first six-way valve 2, a second metering tube 8, a second chromatographic column 9, a second six-way valve 3, a first PDD detector 10, a third chromatographic column 11, a second ten-way valve 4, a third metering tube 12, a fourth chromatographic column 13, a third six-way valve 5, a fifth chromatographic column 14, and a second PDD detector 15. The silane sample gas is introduced through the first ten-way valve 1, and can then be introduced from the first ten-way valve 1 into other multi-way valves, metering tubes, and chromatographic columns. The first metering tube 6 is connected to the first ten-way valve 1 at both ends and is used to store the sample gas. The first chromatographic column 7 is connected to the first ten-way valve 1 at both ends and is used for pre-separation of the sample gas. The first six-way valve 2 is connected to the first ten-way valve 1. The second metering tube 8 is connected to the first six-way valve 2 at both ends and is used to store the sample gas. One end of the second chromatographic column 9 is connected to the first ten-way valve 1 and is used to separate hydrogen, oxygen, nitrogen, and carbon monoxide from the sample gas. The second six-way valve 3 is connected to the other end of the second chromatographic column 9. The first PDD detector 10 is connected to the second six-way valve 3 to detect the impurity content in the sample gas. The first carrier gas and the second carrier gas are introduced through the first ten-way valve 1 to send the sample gas in the first metering tube 6 to the first chromatographic column 7 and the second chromatographic column 9 for separation. One end of the third chromatographic column 11 is connected to the first six-way valve 2, and the other end is connected to the second six-way valve 3, for separating propane and butane in the sample gas. The third carrier gas is introduced through the second six-way valve 2 to transport the sample gas in the second metering tube 6 to the third chromatographic column 11 for separation and to the first PDD detector 10 for detection. The second ten-way valve 4 is connected to the first six-way valve 2. Both ends of the third metering tube 12 are connected to the second ten-way valve 4 for storing the sample gas. The sample gas can be introduced from the first ten-way valve 1 and sequentially filled through the first six-way valve 2 and the second ten-way valve 4 to fill the first metering tube 6, the second metering tube 8, and the third metering tube 12. Both ends of the fourth chromatographic column 13 are connected to the second ten-way valve 4 for pre-separation of the sample gas. The third six-way valve 5 is connected to the twenty-way valve 4. The fifth column 14 is connected to both ends of the third six-way valve 5, used to separate methane, carbon dioxide, ethane, ethylene, acetylene, and propane from the sample gas. The second PDD detector 15 is connected to the fifth column 14 and the third six-way valve 5. The fourth carrier gas is introduced through the twenty-way valve 4 to send the sample gas from the third metering tube 12 into the fourth column 13 and the fifth column 14 for separation and then into the second PDD detector 15 for analysis; the fifth carrier gas is introduced through the third six-way valve 5 into the purge gas path, and the sixth carrier gas is introduced through the twenty-way valve 4 to purge the sample gas from the fifth column 14 into the second PDD detector 15 for analysis.

[0036] In the above embodiments, the analysis system for impurities in high-purity silane adopts a configuration mode of five valves, five columns, and dual detectors, which can distribute different impurities to different detectors for simultaneous injection and analysis of impurities. The analysis results of all impurity components can be obtained in one analysis process.

[0037] Specifically, the first ten-way valve 1 has ports A1 to A10. Sample gas is introduced through port A8, the first carrier gas is introduced through port A10, and the second carrier gas is introduced through port A3. One end of the first metering tube 6 is connected to port A9, and the other end is connected to port A6; one end of the first chromatographic column 7 is connected to port A1, and the other end is connected to port A5.

[0038] The first six-way valve 2 has ports B1 to B10, port B3 is connected to port A7, and the third carrier gas is introduced through port B1. One end of the second metering tube 8 is connected to port B2, and the other end is connected to port B5; the second six-way valve 3 has ports C1 to C6, and ports C4 and C6 are connected through an external pipeline.

[0039] One end of the second chromatographic column 9 is connected to port A2, and the other end is connected to port C3. One end of the third chromatographic column 11 is connected to port B6, and the other end is connected to port C1. The first PDD detector 10 is connected to port C2.

[0040] The twentieth valve 4 has ports D1 to D10, port D8 is connected to port B4, and the fourth carrier gas is introduced through port D10. One end of the third metering tube 12 is connected to port D9, and the other end is connected to port D6. One end of the fourth chromatographic column 13 is connected to port D1, and the other end is connected to port D5.

[0041] The third six-way valve 5 has ports E1 to E6. Port E4 is connected to port D2, and ports E2 and E6 are connected via external piping. The fifth carrier gas is introduced through port E1, and the sixth carrier gas is introduced through port D3. One end of the fifth chromatographic column 14 is connected to port E5, and the other end is connected to port E3. The second PDD detector 15 is connected to the other end of the fifth chromatographic column 14 and port E3.

[0042] Furthermore, the tenth-way valve 1 has an OFF state and an ON state. In the OFF state, port A10 is connected to port A1, port A8 is connected to port A9, port A6 is connected to port A7, port A3 is connected to port A2, and port A5 is connected to port A4. In the ON state, port A9 is connected to port A10, port A8 is connected to port A7, port A6 is connected to port A5, port A2 is connected to port A1, and port A3 is connected to port A4.

[0043] The first six-way valve 2 has an OFF state and an ON state. In the OFF state, port B3 is connected to port B2, port B5 is connected to port B4, and port B1 is connected to port B6. In the ON state, port B3 is connected to port B4, port B5 is connected to port B6, and port B1 is connected to port B2.

[0044] The second six-way valve 3 has an OFF state and an ON state. In the OFF state, port C3 is connected to port C2, port C4 is connected to port C5, and port C1 is connected to port C6. In the ON state, port C3 is connected to port C4, port C6 is connected to port C5, and port C1 is connected to port C2.

[0045] The 20th port valve 4 has an OFF state and an ON state. In the OFF state, port D10 is connected to port D1, port D8 is connected to port D9, port D6 is connected to port D7, port D3 is connected to port D2, and port D5 is connected to port D4. In the ON state, port D9 is connected to port D10, port D8 is connected to port D7, port D6 is connected to port D5, port D2 is connected to port D1, and port D3 is connected to port D4.

[0046] The third six-way valve 5 has an OFF state and an ON state. In the OFF state, the E3 port is connected to the E2 port, the E4 port is connected to the E5 port, and the E1 port is connected to the E6 port. In the ON state, the E3 port is connected to the E4 port, the E6 port is connected to the E5 port, and the E1 port is connected to the E2 port.

[0047] By configuring the pipelines of the five multi-port valves and switching the operating state of each multi-port valve, the sample gas can be separated in multiple chromatographic columns and then delivered to the corresponding PDD detector for detection through carrier gas at different gas paths. At the same time, by adjusting the operating state of the multi-port valves, the separated components that do not need to be detected can be discharged from the multi-port valves in a timely manner, thereby reducing the impact on the analytical results.

[0048] In one embodiment, the first chromatographic column 7 is a modified activated carbon pre-column packed with activated carbon particles, used for pre-separation of the sample gas to ensure more thorough separation in subsequent separations. Preferably, the first chromatographic column 7 is made of stainless steel, with an inner diameter of 1 / 8 inch and a length of 1.5 m. The activated carbon particle size is 60 to 80 mesh.

[0049] The second chromatographic column 9 is a 5A column packed with 5A molecular sieves, used to separate hydrogen, oxygen, nitrogen, and carbon monoxide from the sample gas, especially to separate the sample gas pre-separated by the first chromatographic column 7. Preferably, the second chromatographic column 9 is made of stainless steel, with an inner diameter of 1 / 8 inch and a length of 1.5 m. The molecular sieve has a pore size of 60-80 mesh.

[0050] The third chromatographic column 11 is a capillary column with an inner diameter of 0.53 to 0.55 mm, used to separate propane and butane in the sample gas. Preferably, the third chromatographic column 11 is an SE-30 capillary column with a length of 120 m. The capillary column is packed with methyl polysiloxane.

[0051] The fourth chromatographic column 13 is an R-column packed with porous polymer monomers for pre-separation of the sample gas. Preferably, the fourth chromatographic column 13 is made of stainless steel, with an inner diameter of 1 / 16 inch and a length of 4 m. The porous polymer monomers have a pore size of 60 to 80 mesh, and the porous polymer monomers can be one or more of diethylphenylene and alkenylpyrrole.

[0052] The fifth chromatographic column 14 is a Q-column packed with porous polymer microspheres, used to separate methane, carbon dioxide, ethane, ethylene, acetylene, and propane from the sample gas. Preferably, the fifth chromatographic column 14 is made of stainless steel, with an inner diameter of 1 / 16 inch and a length of 4 m. The porous polymer microspheres have a pore size of 60-80 mesh. The porous polymer microspheres can be divinylbenzene-ethylvinylbenzene copolymer.

[0053] In one embodiment, the first quantitative tube has a capacity of 1 ml; the second quantitative tube 8 has a capacity of 0.1 ml; and the third quantitative tube 12 has a capacity of 0.5 ml.

[0054] In summary, this high-purity silane impurity analysis system employs a five-valve, five-column, dual-detector configuration. The multi-port valves and five columns allow different impurities to be distributed to different detectors, enabling simultaneous sample gas injection and impurity analysis, presenting all analytical results at once. By configuring the piping of the five multi-port valves and switching their operating states, the sample gas can be separated within multiple columns and then delivered to the corresponding PDD detectors via carrier gases at different gas paths. Furthermore, by adjusting the operating states of the multi-port valves, backflushing of the main component or silane impurities can be achieved to avoid interference, while also allowing for the venting of the main peak and selection of the desired gas path.

[0055] Another embodiment of the present invention provides a method for analyzing impurities in high-purity silane using the analytical system described in any of the above embodiments, comprising steps S1-S4.

[0056] Step S1: The first ten-way valve 1, the first six-way valve 2, the second six-way valve 3, the second ten-way valve 4, and the third six-way valve 5 are all in the OFF state. The sample gas is introduced from the A8 port and fills the first quantitative tube 6, the second quantitative tube 8, and the third quantitative tube 12 in sequence.

[0057] Specifically, such as Figure 1As shown, in step S1, the first ten-way valve 1, the first six-way valve 2, the second six-way valve 3, the second ten-way valve 4, and the third six-way valve 5 are all in the OFF state. The sample gas enters from port A8 and passes sequentially through port A9, the first quantitative tube 6, port A6, port A7, port B3, port B2, the second quantitative tube 8, port B5, port B4, port D8, port D9, and the third quantitative tube 12, filling the first quantitative tube 6, the second quantitative tube 8, and the third quantitative tube 12. Excess sample gas is discharged from ports D6 and D7.

[0058] With the above-mentioned gas path setup, sample gas can fill three quantitative tubes through a single gas path, thus saving sample gas filling time.

[0059] In addition, in step S1, the first to sixth carrier gases are continuously supplied. At this time, the first carrier gas is purged to the first chromatographic column 7 through the A10 and A1 ports of the first ten-way valve 1 and then discharged through the A5 and A4 ports.

[0060] The second carrier gas is purged to the second chromatographic column 9 through the A3 and A2 ports of the first ten-way valve 1, and then through the C3 and C2 ports of the second six-way valve 3 before being purged to the first PDD detector 10.

[0061] The third carrier gas is purged through the B1 and B6 ports of the first six-way valve 2 to the third chromatographic column 11, and then sequentially passes through the C1, C6, C4, and C5 ports of the second six-way valve 3 before being discharged.

[0062] The fourth carrier gas is purged through the D10 and D1 ports of the 20th valve 4 to the fourth chromatographic column 13, and then discharged through the D5 and D4 ports.

[0063] The sixth carrier gas passes sequentially through the D3 port, D2 port of the 20th port valve 4, the E4 port, and the E5 port of the third flow valve before being purged to the fifth chromatographic column 14, and then to the second PDD detector 15.

[0064] The fifth carrier gas is purged sequentially through the E1 port, E6 port, E2 port and E3 port of the third six-way valve 5 to the second PDD detector 15.

[0065] With this configuration, each carrier gas can blow out air and other impurities from the corresponding gas path into the analysis system, avoiding interference with the analysis process. At the same time, continuous purging ensures that the gas pressure inside the analysis system is greater than that outside, preventing air and other impurities from re-entering.

[0066] In addition, the first, second, third, fourth, fifth, and sixth carrier gases are helium gases with a purity of 6N or higher, and are continuously supplied from the same gas source to the first ten-way valve 1, the first six-way valve 2, the second ten-way valve 4, and the third six-way valve 5 through different gas paths. This can avoid the influence of differences in purity between carrier gases or differences between different gas paths on the analysis results.

[0067] Step S2: The first ten-way valve 1, the first six-way valve 2, the second ten-way valve 4, and the third six-way valve 5 are simultaneously switched to the ON state, while the second six-way valve 3 remains in the OFF state. The sample gas in the first quantitative tube 6 is purged sequentially into the first chromatographic column 7 and the second chromatographic column 9 by the first carrier gas introduced through port A10. Hydrogen, oxygen, nitrogen, and carbon monoxide in the sample gas are separated and sent to the first PDD detector 10 for analysis to obtain their corresponding concentrations. The sample gas in the second quantitative tube 8 is purged into the third chromatographic column 11 by the third carrier gas introduced through port B1. Propylene silane and butane in the sample gas remain in the third chromatographic column 11, while the remaining components are discharged through port C5. The sample gas in the third quantitative tube 12 is purged into the fourth chromatographic column 13 by the fourth carrier gas introduced through port D10. The separated methane and carbon dioxide are sent to the second PDD detector 15 for analysis, while the remaining sample gas remains in the fourth chromatographic column 13.

[0068] Specifically, such as Figure 2 As shown, in step S2, the first ten-way valve 1, the first six-way valve 2, the second ten-way valve 4, and the third six-way valve 5 are simultaneously switched to the ON state, while the second six-way valve 3 remains in the OFF state. The first carrier gas enters through port A10 and sequentially passes through port A9, the first quantitative tube 6, port A6, and port A5, purging the sample gas in the first quantitative tube 6 into the first chromatographic column 7 for pre-separation. The sample gas pre-separated by the first chromatographic column 7 is then purged into the second chromatographic column 9 through ports A1 and A2 for further separation. Hydrogen, oxygen, nitrogen, and carbon monoxide in the sample gas are separated in the second chromatographic column 9 and sequentially sent to the first PDD detector 10 through ports C3 and C2 for analysis to obtain the content of hydrogen, oxygen, nitrogen, and carbon monoxide.

[0069] The first chromatographic column 7 pre-separates the sample gas, allowing it to be separated more thoroughly in the second chromatographic column 9, so that hydrogen, oxygen, nitrogen, and carbon monoxide can sequentially enter the first PDD detector 10.

[0070] The third carrier gas enters through port B1, purges the sample gas from the second quantitative tube 8 through port B2, and then purges the sample gas into the third chromatographic column 11 through ports B5 and B6. The third chromatographic column 11 separates the sample gas, leaving propane and butane in the sample gas for subsequent analysis. Other components, such as impurity silane and the main component ethyl silane, are discharged through ports C1, C6, C4, and C5 to avoid interfering with subsequent analytical steps and results.

[0071] The fourth carrier gas is introduced through port D10, purging the sample gas in the third quantitative tube 12 through port D9, and then sending the sample gas into the fourth chromatographic column 13 for separation through ports D6 and D5. The methane and carbon dioxide separated by the fourth chromatographic column 13 are then sent into the second PDD detector 15 through ports D1, D2, E4, and E3, while the residual sample gas remains in the fourth chromatographic column 13.

[0072] At this time, the fifth carrier gas sequentially passes through port D1, port D2, port D6, port D5 and the fifth chromatographic column 14 to purge to the second PDD detector 15. Thus, the gas in the gas path always flows to the second PDD detector 15. Therefore, although the second PDD detector 15 is connected to both the fifth chromatographic column 14 and the third six-way valve 5, the separated methane and carbon dioxide will not flow to the fifth chromatographic column 14 at the connection point of the three due to the action of the fifth carrier gas, but will only flow to the second PDD detector 15.

[0073] In this step, hydrogen, oxygen, nitrogen, and carbon monoxide are analyzed in the first PDD detector 10, while methane and carbon dioxide are analyzed in the second PDD detector 15. The remaining components remain in their respective columns awaiting further analysis. Excess components are removed from the analytical system to avoid affecting the analytical results.

[0074] Step S3: The first ten-way valve 1, the third six-way valve 5 and the first six-way valve 2 are switched to the OFF state in sequence, the second ten-way valve 4 is kept in the ON state, and the residual sample gas in the fourth chromatographic column 13 is purged into the fifth chromatographic column 14 by the fourth carrier gas for separation.

[0075] Specifically, such as Figure 3As shown, in step S3, the first ten-way valve 1, the third six-way valve 5, and the first six-way valve 2 are sequentially switched to the OFF state, while the second ten-way valve 4 remains in the ON state. The residual sample gas in the fourth column 13 is sequentially fed into the fifth column 14 by the fourth carrier gas through ports D1, D2, E4, and E5 for separation. After the first ten-way valve 1 is switched to the OFF state, the first carrier gas sequentially passes through ports A10 and A1, discharging residual silicon impurities in the first column 7 through ports A5 and A4, preventing contamination in the second column 9 during subsequent steps.

[0076] In steps S2 to S3, the first ten-way valve 1 remains ON for 1 to 2 minutes before switching to OFF. The third six-way valve 5 remains ON for 4 to 6 minutes before switching to OFF. The first six-way valve 2 remains ON for 4.05 to 6.05 minutes before switching to OFF, and switches to OFF only after the third six-way valve 5 switches to OFF. The second ten-way valve 4 remains ON for 12 to 14 minutes before switching to OFF. By controlling the valve switching times described above, the switching between sample injection, separation, and analysis states can be achieved, thus enabling the analysis of multiple components using a single analytical system.

[0077] Step S4: Simultaneously, the 20th-port valve 4 is switched to the OFF state, and the 26th-port valve 3 is switched to the ON state. Propylsilane and butane in the third column 11 are sent to the first PDD detector 10 through port B1 by the third carrier gas for analysis, yielding the corresponding concentrations. The sixth carrier gas is introduced through port D3, and ethane, ethylene, acetylene, and propane separated from the fifth column 14 are sent to the second PDD detector 15 for analysis, yielding the corresponding concentrations.

[0078] Specifically, such as Figure 4 As shown, in step S4, while the 20th-port valve 4 is switched to the OFF state, the 26th-port valve 3 is switched to the ON state. The third carrier gas sequentially passes through ports B1 and B6 to send the propane and butane in the third chromatographic column 11 to the first PDD detector 10 for analysis via ports C1 and C2, obtaining the corresponding contents. The sixth carrier gas passes through port D3 to send the ethane, ethylene, acetylene, and propane separated from the fifth chromatographic column 14 to the second PDD detector 15 for analysis, obtaining the corresponding contents. Simultaneously, in step S4, after the 20th-port valve 4 is switched to the OFF state, the fourth carrier gas sequentially passes through ports D10 and D1 to discharge the residual propane in the fourth chromatographic column 13 via ports D5 and D4, preventing it from entering the first PDD detector and causing contamination. After all analyses are completed, the 26th-port valve 3 is switched to the OFF state, and the remaining multi-port valves are also in the OFF state.

[0079] Through steps S1 to S4 above, all impurities in the silane sample gas have been analyzed and corresponding chromatograms have been obtained. The content of each component can be calculated by comparing these chromatograms with those of the standard gas. The standard gas is a gas with helium as the background gas and containing 2 ppm of various impurity components. If it is necessary to measure other hydrocarbons or chlorosilanes, the standard gas composition can be increased accordingly.

[0080] The component content in the sample gas is calculated according to the following formula (1):

[0081] Φ i =( A i / A s )* Φ s ——(1)

[0082] In the formula:

[0083] Φ i The concentration of component i in the sample gas is expressed in ppm.

[0084] Φ s The concentration of component i in the standard gas is expressed in ppm.

[0085] A i denoted as peak area (pA.s) in the spectrum corresponding to component i in the sample gas.

[0086] A s The peak area (pA.s) in the spectrum corresponding to component i in the standard gas.

[0087] The arithmetic mean of two parallel measurements of the sample is taken as the final analytical result, and the relative deviation between the two measurements is no greater than ±10%.

[0088] In summary, the analytical method for impurities in high-purity silane of the present invention utilizes the five-valve, five-column, dual-detector configuration of the above-mentioned analytical system to distribute different impurities to different detectors. By controlling the working state of the multi-way valve and adjusting the valve switching time, it achieves sample injection through the same gas path, separation and analysis of multiple gas paths. Thus, the analytical results of all impurities in the sample gas can be obtained in a single analysis process, and the main component or silane impurities can be backflushed to remove interference from the main peak background. This avoids interference from the main component or impurities, improving the efficiency and accuracy of the analytical process.

[0089] It will be apparent to those skilled in the art that this disclosure is not limited to the details of the exemplary embodiments described above, and that this disclosure can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of this disclosure is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within this disclosure. No reference numerals in the claims should be construed as limiting the scope of the claims.

[0090] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. An analytical system for impurities in high-purity silane, characterized in that, include: The sample gas of silane is introduced through the tenth valve; The first quantitative tube is connected at both ends to the first ten-way valve and is used to store the sample gas; The first chromatographic column, with both ends connected to the first ten-way valve, is used for pre-separation of the sample gas; The first six-way valve is connected to the first ten-way valve; The second quantitative tube is connected at both ends to the first six-way valve and is used to store the sample gas; The second chromatographic column is connected at one end to the first ten-way valve and is used to separate hydrogen, oxygen, nitrogen and carbon monoxide in the sample gas. The second six-way valve is connected to the other end of the second chromatographic column; The first PDD detector is connected to the second six-way valve and is used to detect the impurity content in the sample gas; the first carrier gas and the second carrier gas are introduced from the first ten-way valve to send the sample gas in the first quantitative tube into the first chromatographic column and the second chromatographic column for separation. The third chromatographic column is connected at one end to the first six-way valve and at the other end to the second six-way valve, and is used to separate propane and butane in the sample gas; the third carrier gas is introduced from the second six-way valve to transport the sample gas in the second quantitative tube to the third chromatographic column for separation and to the first PDD detector for detection. The twentieth valve is connected to the first six-way valve; The third metering tube is connected to the second ten-way valve at both ends and is used to store the sample gas; the sample gas can be introduced from the first ten-way valve and sequentially pass through the first six-way valve and the second ten-way valve to fill the first metering tube, the second metering tube and the third metering tube. The fourth chromatographic column is connected to the second ten-way valve at both ends, and the fourth chromatographic column is used for pre-separation of the sample gas; The third six-way valve is connected to the second ten-way valve; The fifth chromatographic column, connected at both ends to the third six-way valve, is used to separate methane, carbon dioxide, ethane, ethylene, acetylene, and propane from the sample gas; and The second PDD detector is connected to the fifth chromatographic column and the third six-way valve. The fourth carrier gas is introduced from the second ten-way valve to send the sample gas in the third quantitative tube into the fourth and fifth chromatographic columns for separation and then into the second PDD detector for analysis. The fifth carrier gas is introduced from the third six-way valve into the purge gas path, and the sixth carrier gas is introduced from the second ten-way valve to blow the sample gas in the fifth chromatographic column into the second PDD detector for analysis.

2. The analytical system for impurities in high-purity silane according to claim 1, characterized in that, The first ten-way valve has ports A1 to A10. The sample gas is introduced through port A8, the first carrier gas is introduced through port A10, and the second carrier gas is introduced through port A3. One end of the first quantitative tube is connected to port A9, and the other end is connected to port A6. One end of the first chromatographic column is connected to port A1, and the other end is connected to port A5. The first six-way valve has ports B1 to B10, port B3 is connected to port A7, and the third carrier gas is introduced through port B1; one end of the second metering tube is connected to port B2, and the other end is connected to port B5; the second six-way valve has ports C1 to C6, and port C4 is connected to port C6. One end of the second chromatographic column is connected to port A2, and the other end is connected to port C3; one end of the third chromatographic column is connected to port B6, and the other end is connected to port C1; the first PDD detector is connected to port C2. The second ten-way valve has ports D1 to D10, port D8 is connected to port B4, and the fourth carrier gas is introduced through port D10; one end of the third metering tube is connected to port D9, and the other end is connected to port D6; one end of the fourth chromatographic column is connected to port D1, and the other end is connected to port D5. The third six-way valve has ports E1 to E6, port E4 is connected to port D2, port E2 is connected to port E6, the fifth carrier gas is introduced through port E1, and the sixth carrier gas is introduced through port D3; one end of the fifth chromatographic column is connected to port E5, and the other end is connected to port E3; the second PDD detector is connected to the other end of the fifth chromatographic column and port E3.

3. The analytical system for impurities in high-purity silane according to claim 2, characterized in that, The first ten-way valve has an OFF state and an ON state. In the OFF state, port A10 is connected to port A1, port A8 is connected to port A9, port A6 is connected to port A7, port A3 is connected to port A2, and port A5 is connected to port A4. In the ON state, port A9 is connected to port A10, port A8 is connected to port A7, port A6 is connected to port A5, port A2 is connected to port A1, and port A3 is connected to port A4. The first six-way valve has an OFF state and an ON state. In the OFF state, port B3 is connected to port B2, port B5 is connected to port B4, and port B1 is connected to port B6. In the ON state, port B3 is connected to port B4, port B5 is connected to port B6, and port B1 is connected to port B2. The second six-way valve has an OFF state and an ON state. In the OFF state, port C3 is connected to port C2, port C4 is connected to port C5, and port C1 is connected to port C6. In the ON state, port C3 is connected to port C4, port C6 is connected to port C5, and port C1 is connected to port C2. The 20th port valve has an OFF state and an ON state. In the OFF state, port D10 is connected to port D1, port D8 is connected to port D9, port D6 is connected to port D7, port D3 is connected to port D2, and port D5 is connected to port D4. In the ON state, port D9 is connected to port D10, port D8 is connected to port D7, port D6 is connected to port D5, port D2 is connected to port D1, and port D3 is connected to port D4. The third six-way valve has an OFF state and an ON state. In the OFF state, the E3 port is connected to the E2 port, the E4 port is connected to the E5 port, and the E1 port is connected to the E6 port. In the ON state, the E3 port is connected to the E4 port, the E6 port is connected to the E5 port, and the E1 port is connected to the E2 port.

4. The analytical system for impurities in high-purity silane according to claim 1, characterized in that, The first chromatographic column is a modified activated carbon pre-column filled with activated carbon particles, wherein the particle size of the activated carbon is 60 to 80 mesh. The second chromatographic column is a 5A column filled with 5A molecular sieves, the pore size of which is 60-80 mesh. The third chromatographic column is a capillary column with an inner diameter of 0.53 to 0.55 mm, and the capillary column is filled with methyl polysiloxane. The fourth chromatographic column is an R column packed with porous polymer monomers, the pore size of which is 60 to 80 mesh; and The fifth chromatographic column is a Q column filled with porous polymer microspheres, the porous polymer microspheres having a pore size of 60-80 mesh.

5. A method for analyzing impurities in high-purity silane using the analytical system of claim 4, characterized in that, include: S1: The first ten-way valve, the first six-way valve, the second six-way valve, the second ten-way valve, and the third six-way valve are all in the OFF state. The sample gas is introduced from the A8 port and fills the first quantitative tube, the second quantitative tube, and the third quantitative tube in sequence. S2: The first ten-way valve, the first six-way valve, the second ten-way valve, and the third six-way valve are simultaneously switched to the ON state, while the second six-way valve remains in the OFF state. The sample gas in the first quantitative tube is purged into the first chromatographic column and the second chromatographic column by the first carrier gas introduced through port A10. The hydrogen, oxygen, nitrogen, and carbon monoxide in the sample gas are separated and sent to the first PDD detector for analysis to obtain the corresponding content. The sample gas in the second quantitative tube is purged into the third chromatographic column by the third carrier gas introduced through port B1. The propane and butane in the sample gas are retained in the third chromatographic column, while the remaining components are discharged from port C5. The sample gas in the third quantitative tube is purged into the fourth chromatographic column by the fourth carrier gas introduced through port D10. The separated methane and carbon dioxide are sent to the second PDD detector, while the remaining sample gas remains in the fourth chromatographic column. S3: The first ten-way valve, the third six-way valve and the first six-way valve are switched to the OFF state in sequence, while the second ten-way valve remains in the ON state. The residual sample gas in the fourth chromatographic column is purged into the fifth chromatographic column by the fourth carrier gas for separation. S4: When the second ten-way valve is switched to the OFF state, the second six-way valve is switched to the ON state. The propane and butane in the third chromatographic column are sent to the first PDD detector for analysis by the third carrier gas through port B1 to obtain the corresponding content. The sixth carrier gas is introduced through port D3 to send the ethane, ethylene, acetylene and propane separated from the fifth chromatographic column to the second PDD detector for analysis to obtain the corresponding content.

6. The method for analyzing impurities in high-purity silane according to claim 5, characterized in that, In steps S2 to S3, the first ten-way valve remains in the ON state for 1 to 2 minutes and then switches to the OFF state. The third six-way valve remains in the ON state for 4 to 6 minutes before switching to the OFF state. The first six-way valve remains in the ON state for 4.05 to 6.05 minutes before switching to the OFF state, and the first six-way valve switches to the OFF state after the third six-way valve switches to the OFF state; The second ten-way valve remains in the ON position for 12 to 14 minutes before switching to the OFF position.

7. The method for analyzing impurities in high-purity silane according to claim 5, characterized in that, In step S3, after the first ten-way valve is switched to the OFF state, the first carrier gas sequentially passes through port A10 and port A1, and discharges the residual silicon impurities in the first chromatographic column through ports A5 and A4.

8. The method for analyzing impurities in high-purity silane according to claim 5, characterized in that, In step S4, after the second ten-way valve is switched to the OFF state, the fourth carrier gas sequentially passes through port D10 and port D1 to discharge the residual silane in the fourth chromatographic column through ports D5 and D4.

9. The method for analyzing impurities in high-purity silane according to claim 5, characterized in that, S1 specifically refers to the following: the first ten-way valve, the first six-way valve, the second six-way valve, the second ten-way valve, and the third six-way valve are all in the OFF state; the sample gas is introduced from port A8 and passes sequentially through port A9, the first metering tube, port A6, port A7, port B3, port B2, the second metering tube, port B5, port B4, port D8, port D9, and the third metering tube, filling the first metering tube, the second metering tube, and the third metering tube; and / or; S2 specifically involves: simultaneously switching the first ten-way valve, the first six-way valve, the second ten-way valve, and the third six-way valve to the ON state, while keeping the second six-way valve in the OFF state. The first carrier gas enters through port A10 and sequentially passes through port A9, the first quantitative tube, port A6, and port A5 to purge the sample gas in the first quantitative tube into the first chromatographic column for pre-separation. The sample gas pre-separated by the first chromatographic column is then purged into the second chromatographic column through ports A1 and A2 for further separation. Hydrogen, oxygen, nitrogen, and carbon monoxide are separated in the second chromatographic column and sequentially sent to the first PDD detector through ports C3 and C2 for analysis to obtain the content of hydrogen, oxygen, nitrogen, and carbon monoxide. The third carrier gas enters through port B1. A fourth carrier gas is introduced through port D10, purging the sample gas from the second quantitative tube through port D9, and then sending the sample gas into the third chromatographic column through ports D6 and D5 for separation. The fourth chromatographic column separates the sample gas, and the separated methane and carbon dioxide are then sent to the second PDD detector for analysis through ports D1, D2, E4, and E3. The remaining sample gas remains in the fourth chromatographic column; and / or; S3 specifically refers to: the first ten-way valve, the third six-way valve, and the first six-way valve being switched to the OFF state in sequence, the second ten-way valve being kept in the ON state, and the residual sample gas in the fourth chromatographic column being sent to the fifth chromatographic column for separation by the fourth carrier gas through the D1 port, D2 port, E4 port, and E5 port in sequence; and / or; S4 specifically involves: simultaneously switching the second ten-way valve to the OFF state and the second six-way valve to the ON state; the third carrier gas sequentially passes through ports B1 and B6 to send the propane and butane in the third chromatographic column to the first PDD detector for analysis via ports C1 and C2 to obtain the corresponding content; the sixth carrier gas sequentially passes through ports D3, D2, E4, and E6 to send the ethane, ethylene, acetylene, and propane separated from the fifth chromatographic column to the second PDD detector for analysis to obtain the corresponding content.

10. The method for analyzing impurities in high-purity silane according to claim 5, characterized in that, The first carrier gas, the second carrier gas, the third carrier gas, the fourth carrier gas, the fifth carrier gas, and the sixth carrier gas are helium gases with a purity of 6N or higher, and are continuously supplied to the first ten-way valve, the first six-way valve, the second ten-way valve, and the third six-way valve from the same gas source through different gas paths.

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