Analysis system for hydrocarbon components in ultrapure ammonia

Abstract

An analysis system for hydrocarbon components in ultrapure ammonia. The analysis system comprises: a sample storage tank (1), an electronic refrigeration and concentration apparatus (7), a carrier gas apparatus (10) and a detection apparatus, wherein the electronic refrigeration and concentration apparatus (7) is connected to the sample storage tank (1), and the electronic refrigeration and concentration apparatus (7) is also connected to both the carrier gas apparatus (10) and the detection apparatus; and the detection apparatus comprises a chromatographic column (12) and a hydrogen flame ionization detector (13). The electronic refrigeration and concentration apparatus (7) refrigerates and concentrates samples, and on this basis, hydrocarbon components in ultrapure ammonia can be detected by means of the chromatographic column (12) and / or the hydrogen flame ionization detector (13), without the need for using a pulse discharge helium ionization detector, thereby reducing the costs of detecting hydrocarbon components in ultrapure ammonia.

Description

A system for analyzing hydrocarbon components in ultra-pure ammonia

[0001] This application claims priority to the Chinese patent application filed with the China Patent Office on October 12, 2023, with application number 202311323506.1 and invention name “A System for Analyzing Hydrocarbon Components in Ultra-Pure Ammonia”, the entire contents of which are incorporated by reference into this application. Technical Field

[0002] The present invention relates to the technical field of component detection, and in particular to a hydrocarbon component analysis system in ultrapure ammonia. Background Art

[0003] GB / T 14601-2009, "Ammonia Gases for the Electronics Industry," requires that electronic-grade NH3 products have a purity of ≥99.9995% by volume and a hydrocarbon (C1-C3) content of less than 1 μmol / mol. Optoelectronic-grade NH3 products have a purity of ≥99.99994% by volume and a hydrocarbon (C1-C3) content of less than 0.05 μmol / mol. Detecting hydrocarbon content during the use of gases used in the electronics industry is crucial. Currently, the detection of hydrocarbons in ultrapure ammonia is typically performed using a pulsed discharge helium ionization detector, which is expensive.

[0004] Summary of the Invention

[0005] The object of the present invention is to provide a system for analyzing hydrocarbon components in ultrapure ammonia gas, so as to reduce the cost of detecting hydrocarbon components in ultrapure ammonia gas.

[0006] To achieve the above object, the present invention provides the following solutions:

[0007] The present invention provides a system for analyzing hydrocarbon components in ultrapure ammonia, the analysis system comprising: a sample storage tank, an electronic refrigeration and concentration device, a carrier gas device, and a detection device;

[0008] The electronic refrigeration and concentration device is connected to the sample storage tank, and the electronic refrigeration and concentration device is also connected to the carrier gas device and the detection device respectively;

[0009] The electronic refrigeration and concentration device is used to refrigerate and concentrate the sample to be tested taken out from the sample storage tank;

[0010] The gas carrier device is used to load the sample to be tested after refrigeration and concentration in the electronic refrigeration and concentration device into the detection device;

[0011] The detection device is used to detect hydrocarbon components in the sample to be tested after refrigeration concentration;

[0012] The detection device comprises a chromatographic column and a hydrogen flame ionization detector.

[0013] Optionally, the analysis system further comprises: an automatic switching six-way valve;

[0014] The electronic refrigeration and concentration device and the sample storage tank, the electronic refrigeration and concentration device and the carrier gas device, and the electronic refrigeration and concentration device and the detection device are all connected through the automatic switching six-way valve, specifically:

[0015] The sample storage tank is connected to the first port of the automatic switching six-way valve;

[0016] The electronic refrigeration concentrating device is connected to the sixth port and the third port of the automatic switching six-way valve respectively;

[0017] The gas carrier device is connected to the fifth port of the automatic switching six-way valve;

[0018] The detection device is connected to the fourth port of the automatic switching six-way valve;

[0019] During the sample sampling process, the automatic switching six-way valve is in a first state, wherein the first port and the sixth port of the automatic switching six-way valve are connected, the second port and the third port are connected, and the fourth port and the fifth port are connected;

[0020] During the analysis and detection process, the automatic switching six-way valve is in the second state, which is a state in which the first port and the second port of the automatic switching six-way valve are connected, the third port and the fourth port are connected, and the fifth port and the sixth port are connected.

[0021] Optionally, the analysis system further comprises: a sample recovery device;

[0022] The sample recovery device is connected to the second port of the automatic switching six-way valve.

[0023] Optionally, the analysis system further comprises: a first three-way selection valve, a second three-way selection valve and a third three-way selection valve;

[0024] The sample storage tank and the sample recovery device are connected to the automatic switching six-way valve through the first three-way selection valve, the second three-way selection valve and the third three-way selection valve, specifically:

[0025] The a port, b port and c port of the first three-way selector valve are connected to the a port of the third three-way selector valve, the sample storage tank and the carrier gas device respectively;

[0026] The b port and the c port of the third three-way selector valve are connected to the first port of the automatic switching six-way valve and the b port of the second three-way selector valve respectively;

[0027] The a port and the c port of the second three-way selection valve are connected to the sample recovery device and the second port of the automatic switching six-way valve respectively.

[0028] Optionally, the analysis system further comprises: a planar tee;

[0029] The carrier gas device is connected to the automatic switching six-way valve through the planar three-way connection, specifically:

[0030] The three interfaces of the planar tee are respectively connected to the carrier gas device, the C interface of the first three-way selection valve and the fifth port of the automatic switching six-way valve.

[0031] Optionally, a first pressure reducing valve is provided at the outlet of the sample storage tank.

[0032] Optionally, a second pressure reducing valve is provided at the outlet of the gas carrier device.

[0033] According to the specific embodiments provided by the present invention, the present invention discloses the following technical effects:

[0034] An embodiment of the present invention provides an analysis system for hydrocarbon components in ultrapure ammonia, the analysis system comprising: a sample storage tank, an electronic refrigeration and concentration device, a carrier gas device, and a detection device; the electronic refrigeration and concentration device is connected to the sample storage tank, and the electronic refrigeration and concentration device is also connected to the carrier gas device and the detection device, respectively; the electronic refrigeration and concentration device is used to refrigerate and concentrate a sample to be tested removed from the sample storage tank; the carrier gas device is used to load the sample to be tested, which has been refrigerated and concentrated in the electronic refrigeration and concentration device, into the detection device; the detection device is used to detect hydrocarbon components in the sample to be tested, which has been refrigerated and concentrated; the detection device comprises a chromatographic column and a hydrogen flame ionization detector. In an embodiment of the present invention, an electronic refrigeration and concentration device is provided to refrigerate and concentrate the sample, and on this basis, hydrocarbon components in ultrapure ammonia can be detected using a chromatographic column and / or a hydrogen flame ionization detector, without the need for a pulsed discharge helium ionization detector, thereby reducing the cost of detecting hydrocarbon components in ultrapure ammonia.

[0035] Figures in the specification

[0036] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0037] FIG1 is a schematic diagram of a system for analyzing hydrocarbon components in ultrapure ammonia during a sample sampling process according to an embodiment of the present invention;

[0038] FIG2 is a schematic diagram of the status of a system for analyzing hydrocarbon components in ultrapure ammonia during the analysis and detection process provided by an embodiment of the present invention.

[0039] Explanation of the accompanying symbols: 1. Sample storage tank; 2. First pressure reducing valve; 3. First three-way selection valve; 4. Second three-way selection valve; 5. Third three-way selection valve; 6. Sample recovery device; 7. Electronic refrigeration and concentration device; 8. Second pressure reducing valve; 9. Flat three-way valve; 10. Carrier gas device; 11. Automatic switching six-way valve; 12. Chromatographic column; 13. Hydrogen flame ionization detector. DETAILED DESCRIPTION

[0040] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only 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 making creative efforts are within the scope of protection of the present invention.

[0041] The object of the present invention is to provide a system for analyzing hydrocarbon components in ultrapure ammonia gas, so as to reduce the cost of detecting hydrocarbon components in ultrapure ammonia gas.

[0042] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0043] An embodiment of the present invention provides a system for analyzing hydrocarbon components in ultrapure ammonia. As shown in Figures 1 and 2, the analysis system includes: a sample storage tank 1, an electronic refrigeration and concentration device 7, a carrier gas device 10, and a detection device; the electronic refrigeration and concentration device 7 is connected to the sample storage tank 1, and the electronic refrigeration and concentration device 7 is also connected to the carrier gas device 10 and the detection device respectively; the electronic refrigeration and concentration device 7 is used to refrigerate and concentrate the sample to be tested taken out of the sample storage tank 1; the carrier gas device 10 is used to load the sample to be tested after refrigeration and concentration in the electronic refrigeration and concentration device 7 into the detection device; the detection device is used to detect hydrocarbon components in the sample to be tested after refrigeration and concentration; in this embodiment of the present invention, the detection device includes a chromatographic column 12 and a hydrogen flame ionization detector 13.

[0044] The chromatographic column 12 in the embodiment of the present invention is filled with porapak QS chromatographic support or other equivalent chromatographic supports.

[0045] The analysis system further includes: an automatic switching six-way valve 11; the electronic refrigeration and concentration device 7 and the sample storage tank 1, the electronic refrigeration and concentration device 7 and the carrier gas device 10, and the electronic refrigeration and concentration device 7 and the detection device are all connected through the automatic switching six-way valve 11, specifically: the sample storage tank 1 is connected to the first port of the automatic switching six-way valve 11; the electronic refrigeration and concentration device 7 is respectively connected to the sixth port and the third port of the automatic switching six-way valve 11; the carrier gas device 10 is connected to the fifth port of the automatic switching six-way valve 11 The detection device is connected to the fourth port of the automatic switching six-way valve 11; during the sample sampling process, the automatic switching six-way valve 11 is in a first state, wherein the first state is a state in which the first port of the automatic switching six-way valve 11 is connected to the sixth port, the second port is connected to the third port, and the fourth port is connected to the fifth port; during the analysis and detection process, the automatic switching six-way valve 11 is in a second state, wherein the second state is a state in which the first port of the automatic switching six-way valve 11 is connected to the second port, the third port is connected to the fourth port, and the fifth port is connected to the sixth port. The first port, the second port, the third port, the fourth port, the fifth port, and the sixth port in the embodiment of the present invention correspond to port ①, port ②, port ③, port ④, port ⑤, and port ⑥ in FIG. 1 , respectively.

[0046] Exemplarily, as a preferred embodiment, the analysis system further includes: a sample recovery device 6; the sample recovery device 6 is connected to the second port of the automatic switching six-way valve 11. The analysis system further includes: a first three-way selection valve 3, a second three-way selection valve 4, and a third three-way selection valve 5; the sample storage tank 1 and the sample recovery device 6 are connected to the automatic switching six-way valve 11 through the first three-way selection valve 3, the second three-way selection valve 4, and the third three-way selection valve 5, specifically: the a port, b port, and c port of the first three-way selection valve 3 are connected to the a port of the third three-way selection valve 5, the sample storage tank 1, and the carrier gas device 10, respectively; the b port and c port of the third three-way selection valve 5 are connected to the first port of the automatic switching six-way valve 11 and the b port of the second three-way selection valve 4, respectively; the a port and c port of the second three-way selection valve 4 are connected to the sample recovery device 6 and the second port of the automatic switching six-way valve 11, respectively. The first three-way selector valve 3, the second three-way selector valve 4 and the third three-way selector valve 5 in the embodiment of the present invention all include an a port, a b port and a c port, wherein an a port is a common end and there are two directions of gas flow: one is that the a port is connected to the b port, and the other is that the a port is connected to the c port.

[0047] The analysis system also includes a planar tee 9; the gas carrier device 10 is connected to the automatic switching six-way valve 11 via the planar tee 9. Specifically, the three ports of the planar tee 9 are respectively connected to the gas carrier device 10, the C port of the first three-way selector valve 3, and the fifth port of the automatic switching six-way valve 11. The outlet of the sample storage tank 1 is provided with a first pressure reducing valve 2. The outlet of the gas carrier device 10 is provided with a second pressure reducing valve 8.

[0048] Based on the above structure, the working principle of the hydrocarbon component analysis system in ultra-pure ammonia according to the embodiment of the present invention is as follows:

[0049] The sample does not pass through the electronic refrigeration device process: after the sample flows out of the sample storage tank 1, it is reduced in pressure through the first pressure reducing valve 2, and then flows to the first three-way selection valve 3 (at this time, the a interface is connected to the b interface) → the third three-way selection valve 5 (at this time, the a interface is connected to the c interface) → the second three-way selection valve 4 (at this time, the a interface is connected to the b interface) → the sample recovery device 6.

[0050] The carrier gas does not pass through the electronic refrigeration device process: after the carrier gas flows out of the carrier gas device 10, it is reduced in pressure through the second pressure reducing valve 8, flows to the flat tee 9, and flows from one interface of the flat tee 9 to the first three-way selection valve 3 (at this time, the a interface is connected to the c interface) → the third three-way selection valve 5 (at this time, the a interface is connected to the c interface) → the second three-way selection valve 4 (at this time, the a interface is connected to the b interface) → the sample recovery device 6.

[0051] Pipeline purging process: After the carrier gas flows out from the carrier gas device 10, it is reduced in pressure through the second pressure reducing valve 8 and flows to the flat tee 9. From one interface of the flat tee 9, it flows to the first three-way selection valve 3 (at this time, a and c are connected) → the third three-way selection valve 5 (at this time, a and b are connected) → the automatic switching port ① and port ⑥ of the six-way valve 11, the electronic refrigeration concentration device 7, the automatic switching port ③ and port ② of the six-way valve 11 → the second three-way selection valve 4 (at this time, the a interface is connected to the c interface) → the sample recovery device 6.

[0052] Sample sampling process: During this process, the six-way valve 11 is automatically switched to the first state, as shown in Figure 1. After the sample flows out of the sample storage tank 1, it is reduced in pressure through the first pressure reducing valve 2 and flows to the first three-way selection valve 3 (at this time a and b are connected) → the third three-way selection valve 5 (at this time a and b are connected) → automatically switching the six-way valve 11's ports 1, 6, electronic refrigeration concentration device 7, port 3, and port 2 → the second three-way selection valve 4 (at this time a and c are connected) → the sample recovery device 6.

[0053] Analysis and detection process: During this process, the automatic switching six-way valve 11 is in the second state, as shown in Figure 2. After the carrier gas flows out from the carrier gas device 10, it is reduced in pressure through the second pressure reducing valve 8 and flows to the flat tee 9. From the other interface of the flat tee 9, it flows out to the No. 5 and No. 6 ports of the automatic switching six-way valve 11. The sample carrying the electronic refrigeration and concentration device 7 enters the chromatographic column 12 through the No. 3 and No. 4 ports of the automatic switching six-way valve 11, and is separated into methane, acetylene, ethylene, ethane, propylene, and propane by the chromatographic column 12, and is detected by the hydrogen flame ionization detector 13.

[0054] According to the specific embodiments provided by the present invention, the present invention discloses the following technical effects:

[0055] The present invention automatically switches the six-way valve 11 for sample injection, cooperates with an electronic refrigeration and concentration device, and detects the hydrocarbon (C1-C3) content through hydrogen flame ionization, thereby reducing the hydrocarbon detection cost.

[0056] The various embodiments in this specification are described in a progressive manner, and each embodiment focuses on the differences from other embodiments. The same and similar parts between the various embodiments can be referenced to each other. Specific examples are used herein to illustrate the principles and implementation methods of the present invention. The description of the above embodiments is only used to help understand the method of the present invention and its core idea; at the same time, for those of ordinary skill in the art, according to the ideas of the present invention, there will be changes in the specific implementation methods and scope of application. In summary, the contents of this specification should not be understood as limiting the present invention.

Claims

1. A system for analyzing hydrocarbon components in ultrapure ammonia, characterized in that: The analysis system comprises: a sample storage tank, an electronic refrigeration concentration device, a gas carrier device and a detection device; The electronic refrigeration and concentration device is connected to the sample storage tank, and the electronic refrigeration and concentration device is also connected to the gas carrier device and the detection device respectively; The electronic refrigeration and concentration device is used to refrigerate and concentrate the sample to be tested taken out from the sample storage tank; The gas carrier device is used to load the sample to be tested after refrigeration and concentration in the electronic refrigeration and concentration device into the detection device; The detection device is used to detect hydrocarbon components in the sample to be tested after refrigeration and concentration; The detection device comprises a chromatographic column and a hydrogen flame ionization detector.

2. The hydrocarbon component analysis system in ultrapure ammonia according to claim 1, characterized in that: The analysis system further comprises: an automatically switching six-way valve; The electronic refrigeration and concentration device and the sample storage tank, the electronic refrigeration and concentration device and the carrier gas device, and the electronic refrigeration and concentration device and the detection device are all connected through the automatic switching six-way valve, specifically: The sample storage tank is connected to the first port of the automatic switching six-way valve; The electronic refrigeration concentrating device is respectively connected to the sixth port and the third port of the automatic switching six-way valve; The gas carrier device is connected to the fifth port of the automatic switching six-way valve; The detection device is connected to the fourth port of the automatic switching six-way valve; During the sample sampling process, the automatic switching six-way valve is in a first state, wherein the first port of the automatic switching six-way valve is connected to the sixth port, the second port is connected to the third port, and the fourth port is connected to the fifth port; During the analysis and detection process, the automatic switching six-way valve is in the second state, where the first port of the automatic switching six-way valve is connected to the second port, the third port is connected to the fourth port, and the fifth port is connected to the sixth port.

3. The hydrocarbon component analysis system in ultrapure ammonia according to claim 2, characterized in that: The analysis system further comprises: a sample recovery device; The sample recovery device is connected to the second port of the automatic switching six-way valve.

4. The hydrocarbon component analysis system in ultrapure ammonia according to claim 3 is characterized in that: The analysis system further comprises: a first three-way selection valve, a second three-way selection valve and a third three-way selection valve; The sample storage tank and the sample recovery device are connected to the automatic switching six-way valve through the first three-way selection valve, the second three-way selection valve and the third three-way selection valve, specifically: The a interface, b interface and c interface of the first three-way selection valve are respectively connected to the a interface of the third three-way selection valve, the sample storage tank and the carrier gas device; The b interface and the c interface of the third three-way selection valve are respectively connected to the first port of the automatic switching six-way valve and the b interface of the second three-way selection valve; The a interface and the c interface of the second three-way selection valve are connected to the sample recovery device and the second port of the automatic switching six-way valve respectively.

5. The hydrocarbon component analysis system in ultrapure ammonia according to claim 4, characterized in that: The analysis system further comprises: a planar tee; The gas carrier device is connected to the automatic switching six-way valve through the planar three-way valve, specifically: The three interfaces of the planar tee are respectively connected to the carrier gas device, the c interface of the first three-way selection valve and the fifth port of the automatic switching six-way valve.

6. The hydrocarbon component analysis system in ultrapure ammonia according to claim 5, characterized in that: The outlet of the sample storage tank is provided with a first pressure reducing valve.

7. The hydrocarbon component analysis system in ultrapure ammonia according to claim 5, characterized in that: The outlet of the gas carrier device is provided with a second pressure reducing valve.

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