CN115236244A - Gas chromatography detection system and method for analyzing impurities in molybdenum hexafluoride product - Google Patents
Gas chromatography detection system and method for analyzing impurities in molybdenum hexafluoride product Download PDFInfo
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- CN115236244A CN115236244A CN202211066983.XA CN202211066983A CN115236244A CN 115236244 A CN115236244 A CN 115236244A CN 202211066983 A CN202211066983 A CN 202211066983A CN 115236244 A CN115236244 A CN 115236244A
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- 238000001514 detection method Methods 0.000 title claims abstract description 40
- WSWMGHRLUYADNA-UHFFFAOYSA-N 7-nitro-1,2,3,4-tetrahydroquinoline Chemical compound C1CCNC2=CC([N+](=O)[O-])=CC=C21 WSWMGHRLUYADNA-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 239000012535 impurity Substances 0.000 title claims abstract description 26
- 238000004817 gas chromatography Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims description 12
- 239000012159 carrier gas Substances 0.000 claims abstract description 92
- 239000007789 gas Substances 0.000 claims abstract description 62
- 238000002347 injection Methods 0.000 claims abstract description 5
- 239000007924 injection Substances 0.000 claims abstract description 5
- 239000001307 helium Substances 0.000 claims description 19
- 229910052734 helium Inorganic materials 0.000 claims description 19
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 19
- 238000000926 separation method Methods 0.000 claims description 17
- 238000004458 analytical method Methods 0.000 claims description 10
- 230000008878 coupling Effects 0.000 claims description 8
- 238000010168 coupling process Methods 0.000 claims description 8
- 238000005859 coupling reaction Methods 0.000 claims description 8
- 239000002808 molecular sieve Substances 0.000 claims description 6
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 6
- 238000004587 chromatography analysis Methods 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000010926 purge Methods 0.000 claims 1
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000011010 flushing procedure Methods 0.000 abstract description 2
- 238000013022 venting Methods 0.000 description 4
- 239000000945 filler Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000011002 quantification Methods 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical group [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005372 isotope separation Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910001512 metal fluoride Inorganic materials 0.000 description 1
- 229910021344 molybdenum silicide Inorganic materials 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a gas chromatography detection system and a gas chromatography detection method for analyzing impurities in a molybdenum hexafluoride product, wherein the gas chromatography detection system comprises a first carrier gas branch, a second carrier gas branch, a third carrier gas branch and a fourth carrier gas branch, a first chromatographic column, a second chromatographic column, a third chromatographic column, a fourth chromatographic column, a first switching valve, a second switching valve and a third switching valve, the second chromatographic column is arranged between the first switching valve and the third switching valve, and the fourth chromatographic column is arranged between the second switching valve and the third switching valve. According to the invention, the sample injection of the first quantitative ring and the second quantitative ring is completed at one time through the pipeline between the first switching valve and the second switching valve, then the sample gas is sequentially detected, the two detections are not interfered with each other, the accuracy of the detection result is improved, and after the sample injection and the detection are finished, the carrier gas is respectively used for back flushing, so that the corrosion of molybdenum hexafluoride to the pipeline and equipment is reduced.
Description
Technical Field
The invention belongs to the technical field of chemical product analysis devices, and particularly relates to a gas chromatography detection system and a gas chromatography detection method for analyzing impurities in a molybdenum hexafluoride product.
Background
The fluorine and the fluoride generally refer to all fluorine-containing elements and derivatives thereof, and are widely applied to various industries, and molybdenum hexafluoride is mainly applied to the isotope separation of molybdenum as a metal fluoride, can be used for vapor deposition of molybdenum silicide or molybdenum in the micro-electricity industry to manufacture interconnecting wires with low resistance and high melting point, and has wide application and requirements.
Commercially produced molybdenum hexafluoride often contains impurities including H 2 、N 2 、O 2 、CO、CO 2 And CF 4 And the like, the existence of the impurities seriously influences the use performance of the molybdenum hexafluoride product, so that the analysis and research on the components and the content of the impurities are indispensable, the purity of the molybdenum hexafluoride product is judged according to the detection result, or the molybdenum hexafluoride product is subjected to deep purification to meet the use requirement, but at present, few methods are used for analyzing the impurities. Therefore, the simple, accurate, fast and reliable analysis method has important significance for production control and product quality control.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a gas chromatography detection system method for analyzing impurities in a molybdenum hexafluoride product, which is used for detecting whether the impurity content of the molybdenum hexafluoride product reaches a practical standard, and provides a reliable detection method for detecting the molybdenum hexafluoride product.
In order to solve the technical problems, the invention adopts the technical scheme that: a gas chromatography detection system for analyzing impurities in a molybdenum hexafluoride product is characterized by comprising a carrier gas first branch, a carrier gas second branch, a carrier gas third branch and a carrier gas fourth branch, a first chromatographic column, a second chromatographic column, a third chromatographic column and a fourth chromatographic column, a first switching valve, a second switching valve and a third switching valve;
and two ends of the second chromatographic column are respectively connected with the first switching valve and the third switching valve, and two ends of the fourth chromatographic column are respectively connected with the second switching valve and the third switching valve.
The carrier gas first branch is connected with an interface (4) of the first switching valve, the carrier gas second branch is connected with an interface (7) of the first switching valve, the sample inlet is connected with an interface (1) of the first switching valve, an interface (3) and an interface (R) of the first switching valve are connected through a first quantitative ring, an interface (2) of the first switching valve is connected with the second switching valve, an interface (6) of the first switching valve is connected with the third switching valve through a pipeline, and the pipeline is provided with the second chromatographic column.
No. 5 interface and No. 9 interface of first switching valve pass through the tube coupling, are provided with on this pipeline first chromatographic column, no. 8 interface connection of first switching valve has first blowdown needle valve.
The third carrier gas branch is connected with an interface (4) of the second switching valve, the fourth carrier gas branch is connected with an interface (7) of the second switching valve, the sample outlet is connected with an interface (2) of the second switching valve, interfaces (3) and (r) of the second switching valve are connected through a pipeline, a second quantitative ring is arranged on the pipeline, an interface (1) of the second switching valve is connected with the first switching valve, an interface (6) of the second switching valve is connected with the third switching valve through a pipeline, and the pipeline is provided with the fourth chromatographic column.
No. 5 interface and No. 9 interface of second diverter valve pass through the tube coupling, are provided with on this pipeline third chromatography post, no. 8 interface connection of second diverter valve has the second needle valve of emptying.
Interface (1) of third diverter valve with first diverter valve passes through the tube coupling, is provided with on this pipeline the second chromatographic column, interface (5) of third diverter valve with the second diverter valve passes through the tube coupling, is provided with on this pipeline the fourth chromatographic column, interface (4) of third diverter valve has the third needle valve that empties, interface (2) of third diverter valve has the fourth needle valve that empties, interface (2) and interface (3) of third diverter valve connect, interface (6) of third diverter valve connect the helium ionization detector.
The first chromatographic column is a carbon molecular sieve chromatographic column, the second chromatographic column is a 5A molecular sieve chromatographic column, and the third chromatographic column and the fourth chromatographic column are Hayesep Q chromatographic columns.
A method for analyzing impurities in a molybdenum hexafluoride product is characterized in that sample gas is injected once, and the sample gas is subjected to H pre-separation in a first chromatographic column 2 、O 2 、Ar、N 2 And a CO component, H 2 、O 2 、Ar、N 2 And the CO component enters a second chromatographic column for re-separation and then enters a helium ionization detector for detection; pre-separating H from sample gas in third chromatographic column 2 、O 2 、Ar、N 2 And a CO component, H 2 、O 2 、Ar、N 2 And the CO component enters a fourth chromatographic column and is discharged, and the component CF separated after the third chromatographic column 4 、CO 2 、N 2 O and SF 6 And (4) separating again in a fourth chromatographic column, and then detecting in a helium ionization detector.
The method comprises the following specific steps:
s1, sample gas to be detected sequentially passes through interface (1), interface (R) and a first quantitative ring of a first switching valve from a sample inlet, after the first quantitative ring is filled with the sample gas to be detected, the sample gas to be detected enters interface (1), interface (R) and a second quantitative ring of a second switching valve through interface (3) and interface (2) of the first switching valve, and after the second quantitative ring is filled with the sample gas to be detected, the sample gas to be detected enters a sample outlet along interface (3) and interface (2) of the second switching valve;
s2, after the sample introduction is finished, opening a first switching valve, opening a carrier gas first branch, and opening the carrier gas first branchThe carrier gas in the channel flows to interface (3) through interface (4) of the first switching valve, the sample gas carrying a certain quantity flows to interface (9) through interface (R) to enter the first chromatographic column for pre-separation, and H which flows out first 2 、O 2 、Ar、N 2 And after CO flows out along the interface No. 5, closing the first switching valve, opening a carrier gas second branch, and carrying the carrier gas H by the carrier gas second branch 2 、O 2 、Ar、N 2 And CO enters the second chromatographic column from the interface No. 6 and enters H of the second chromatographic column 2 、O 2 、Ar、N 2 And the CO is separated again through the second chromatographic column, flows to the interface (6) through the interface (1) of the third switching valve and enters a helium ionization detector for detection, the carrier gas of the first branch of the carrier gas flows to the interface (5) through the interface (4) of the first switching valve in sequence and enters the first chromatographic column, then flows to the interface (8) through the interface (9) and enters a first venting needle valve, and the sample gas in the first chromatographic column is purged and vented;
s3, opening the second switching valve, allowing the carrier gas in the third branch of the carrier gas to flow to the interface (3) through the interface (4) of the second switching valve, allowing the carrier gas carrying a certain amount of sample gas to flow to the interface (9) through the interface (4) of the second switching valve, allowing the carrier gas to enter a third chromatographic column for pre-separation, and allowing the H gas flowing out first to flow out 2 、O 2 、Ar、N 2 And after CO flows out along the interface No. 5, the CO enters a fourth chromatographic column along the interface No. 6, and H 2 、O 2 、Ar、N 2 After CO flows out of the fourth chromatographic column, the CO flows to a No. 4 interface along a No. 5 interface of the third switching valve, and enters a fourth emptying needle valve from the No. 4 interface of the third switching valve for emptying;
s4, CF separated after third chromatographic column 4 、CO 2 、N 2 O and SF 6 Flowing to interface (6) along interface (5) of the second switching valve, closing the second switching valve, opening the third switching valve, opening the fourth branch of carrier gas, flowing the carrier gas of the fourth branch of carrier gas to interface (6) through interface (7) of the second switching valve, and carrying CF 4 、CO 2 、N 2 O and SF 6 And the separated gas flows to the interface (6) through the interface (5) of the third switching valve and enters the helium ionization detector for detection.
Preferably, the first and second dosing rings have a volume of 0.1-1ml, more preferably 0.55ml.
Compared with the prior art, the invention has the following advantages:
the invention provides a gas chromatography detection system and a gas chromatography detection method, which can detect impurity components and content of a molybdenum hexafluoride product, judge the purity of the molybdenum hexafluoride according to a detection result and facilitate deep purification of the molybdenum hexafluoride product. According to the invention, the sample injection of the first quantitative ring and the second quantitative ring is completed at one time through the pipeline between the first switching valve and the second switching valve, then the sample gas is sequentially detected, the two detections are not interfered with each other, the accuracy of the detection result is improved, and after the sample injection and the detection are finished, the carrier gas is respectively used for back flushing, so that the corrosion of molybdenum hexafluoride to the pipeline and equipment is reduced.
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Drawings
Fig. 1 is a schematic diagram of the gas circuit flow of the present invention.
Description of the reference numerals:
1-a first branch of carrier gas; 2-sample inlet; 3-a first quantification ring;
4-a first chromatographic column; 5-a second branch of carrier gas; 6-a first venting needle valve;
7-a second chromatographic column; 8-a helium ionization detector; 9 — second quantification loop;
10-a sample outlet; 11-third branch of carrier gas; 12-a third chromatographic column;
13-carrier gas fourth branch; 14-second vent needle valve; 15-a fourth chromatography column;
16-a third vent needle valve; 17-a fourth vent needle valve; 18 — a first switching valve;
19-second switching valve; 20-third switching valve.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, embodiments accompanying figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms than those specifically described herein, and it will be apparent to those skilled in the art that many more modifications are possible without departing from the spirit and scope of the invention.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only and do not represent the only embodiments.
As shown in fig. 1, the present invention provides a gas chromatography detection system for analyzing impurities in a molybdenum hexafluoride product, including a carrier gas first branch 1, a carrier gas second branch 5, a carrier gas third branch 11, and a carrier gas fourth branch 13, a first chromatographic column 4, a second chromatographic column 7, a third chromatographic column 12, and a fourth chromatographic column 15, and a first switching valve 18, a second switching valve 19, and a third switching valve 20;
the first switching valve 18 and the third switching valve 20 are connected to both ends of the second column 7, respectively, and the second switching valve 19 and the third switching valve 20 are connected to both ends of the fourth column 15, respectively.
The carrier gas first branch 1 is connected with an interface (4) of the first switching valve 18, the carrier gas second branch 5 is connected with an interface (7) of the first switching valve 18, the sample inlet 2 is connected with an interface (1) of the first switching valve 18, interfaces (3) and (3) of the first switching valve 18 are connected through a first quantitative ring 3, an interface (2) of the first switching valve 18 is connected with the second switching valve 19, an interface (6) of the first switching valve 18 is connected with the third switching valve 20 through a pipeline, and the second chromatographic column 7 is arranged on the pipeline.
The interface (5) and the interface (9) of the first switching valve 18 are connected through a pipeline, the first chromatographic column 4 is arranged on the pipeline, and the interface (8) of the first switching valve 18 is connected with a first emptying needle valve 6.
The carrier gas third branch 11 is connected to the interface (4) of the second switching valve 19, the carrier gas fourth branch 13 is connected to the interface (7) of the second switching valve 19, the sample outlet 10 is connected to the interface (2) of the second switching valve 19, the interfaces (3) and (r) of the second switching valve 19 are connected through a pipeline, the pipeline is provided with a second quantitative ring 9, the interface (1) of the second switching valve 19 is connected to the first switching valve 18, the interface (6) of the second switching valve 19 is connected to the third switching valve 20 through a pipeline, and the pipeline is provided with the fourth chromatographic column 15.
No. 5 interface and No. 9 interface of second diverter valve 19 pass through the tube coupling, are provided with on this pipeline third chromatography post 12, no. 8 interface connection of second diverter valve 19 has second needle valve 14 that empties.
The interface (1) of the third switching valve 20 is connected with the first switching valve 18 through a pipeline, the second chromatographic column 7 is arranged on the pipeline, the interface (5) of the third switching valve 20 is connected with the second switching valve 19 through a pipeline, the fourth chromatographic column 15 is arranged on the pipeline, the interface (4) of the third switching valve 20 is connected with a third emptying needle valve 16, the interface (2) of the third switching valve 20 is connected with a fourth emptying needle valve 17, the interface (2) and the interface (3) of the third switching valve 20 are connected, and the interface (6) of the third switching valve 20 is connected with the helium ionization detector 8.
The first chromatographic column 4 is a carbon molecular sieve chromatographic column, the column length × the inner diameter =0.6m × 0.32m, and the filler particle size is 60 to 80 meshes, the second chromatographic column 7 is a 5A molecular sieve chromatographic column, the column length × the inner diameter =2m × 0.32m, and the filler particle size is 60 to 80 meshes, the third chromatographic column 12 and the fourth chromatographic column 15 are Hayesep Q chromatographic columns, the column length × the inner diameter =2m × 0.32m, and the filler particle size is 60 to 80 meshes.
Method for analyzing impurities in molybdenum hexafluoride productIt is characterized in that sample gas is injected once, and the sample gas is pre-separated from H in a first chromatographic column 4 2 、O 2 、Ar、N 2 And a CO component, H 2 、O 2 、Ar、N 2 And the CO component enters a second chromatographic column 7 for separation again and then enters a helium ionization detector 8 for detection; pre-separating H from the sample gas in the third chromatographic column 12 2 、O 2 、Ar、N 2 And a CO component, H 2 、O 2 、Ar、N 2 And the CO component enters a fourth chromatographic column 15 and is discharged, and the component CF separated after the third chromatographic column 12 4 、CO 2 、N 2 O and SF 6 Enters a fourth chromatographic column 15 for separation again and then enters a helium ionization detector 8 for detection.
The method comprises the following specific steps:
s1, sample gas to be detected sequentially passes through a port (1) of a first switching valve 18, a port (R) and a first quantitative ring 3 from a sample inlet 2, after the sample gas to be detected is filled in the first quantitative ring 3, the sample gas to be detected enters a port (1) of a second switching valve 19, a port (R) and a second quantitative ring 9 from the port (3) and the port (2) of the first switching valve 18, and after the sample gas to be detected is filled in the second quantitative ring 9, the sample gas to be detected enters a sample outlet 10 along the port (3) and the port (2) of the second switching valve 19;
s2, after sample introduction is finished, opening a first switching valve 18, opening a carrier gas first branch 1, enabling carrier gas of the carrier gas first branch 1 to flow to a port (3) through a port (4) of the first switching valve 18, enabling the carrier gas carrying a certain amount of sample gas to flow to a port (9) through a port (4) of the first switching valve 18 to enter a first chromatographic column 4 for pre-separation, and enabling the sample gas flowing out firstly to flow to a port (9) through a port (C) of the first chromatographic column to enter a second chromatographic column 4 for pre-separation, wherein the sample gas flows out firstly 2 、O 2 、Ar、N 2 And CO flows out along the interface No. 5, the first switching valve 18 is closed, the carrier gas second branch 5 is opened, and the carrier gas carrying belt H of the carrier gas second branch 5 2 、O 2 、Ar、N 2 And H of CO entering the second chromatographic column 7 from the interface No. 6 and entering the second chromatographic column 7 2 、O 2 、Ar、N 2 And CO is separated again through the second chromatographic column 7, flows to the interface (6) through the interface (1) of the third switching valve 20 and enters the helium ionization detector 8 for detection, and the carrier gas of the first carrier gas branch 1 sequentially flows through the interface (4) of the first switching valve 18The sample gas flows to the interface (5) and enters the first chromatographic column 4, then flows to the interface (8) from the interface (9) and enters the first emptying needle valve 6, and the sample gas in the first chromatographic column 4 is purged and emptied;
s3, then opening second switching valve 19, the carrier gas of carrier gas third branch 11 flows to interface (3) through interface (4) of second switching valve 19, the carrier gas carrying a certain quantity of sample gas flows to interface (9) through interface (r) into third chromatographic column 12 for pre-separation, and H flowing out first 2 、O 2 、Ar、N 2 And CO flows out along the interface No. 5, enters a fourth chromatographic column 15 along the interface No. 6 2 、O 2 、Ar、N 2 After CO flows out of the fourth chromatographic column 15, the CO flows to a connector (4) along a connector (5) of the third switching valve 20, and enters the fourth emptying needle valve 16 from the connector (4) of the third switching valve 20 for emptying;
s4, CF separated after the third chromatographic column 12 4 、CO 2 、N 2 O and SF 6 Flowing to interface (6) along interface (5) of second switching valve 19, closing second switching valve 19, opening third switching valve 20, opening carrier gas fourth branch 13, flowing carrier gas of carrier gas fourth branch 13 to interface (6) through interface (7) of second switching valve 19, and carrying CF 4 、CO 2 、N 2 O and SF 6 And the separated gas enters the fourth chromatographic column 15 for separation again, and flows to the interface (6) through the interface (5) of the third switching valve 20 to enter the helium ionization detector 8 for detection.
In this embodiment, the volume of the first dosing ring 3 and the second dosing ring 9 is preferably 0.25ml.
When the device is used, sample gas to be detected sequentially passes through the interface (1), the interface (R) and the first quantitative ring (3) of the first switching valve (18) from the sample inlet (2), and after the first quantitative ring (3) is filled with the sample gas to be detected, the sample gas to be detected enters the interface (1), the interface (R) and the second quantitative ring (9) of the second switching valve (19) through the interface (3) and the interface (2) of the first switching valve (18), and after the second quantitative ring (9) is filled with the sample gas to be detected, the sample gas to be detected enters the sample outlet (10) along the interface (3) and the interface (2) of the second switching valve (19).
After the sample introduction is finished, the first switching valve 18 is opened, and the carrier is openedThe carrier gas of the first carrier gas branch 1 flows to the interface (3) through the interface (4) of the first switching valve 18, the carrier gas carrying a certain amount of sample gas flows to the interface (9) through the interface (4) of the third switching valve 18 to enter the first chromatographic column 4 for pre-separation, and H which flows out firstly flows out 2 、O 2 、Ar、N 2 And after CO flows out along the interface No. 5, the first switching valve 18 is closed, the carrier gas second branch 5 is opened, and the carrier gas carrier tape H of the carrier gas second branch 5 2 、O 2 、Ar、N 2 And H of CO entering the second chromatographic column 7 from the interface No. 6 and entering the second chromatographic column 7 2 、O 2 、Ar、N 2 And CO is separated again through the second chromatographic column 7, flows to the interface (6) through the interface (1) of the third switching valve 20 and enters the helium ionization detector 8 for detection, the carrier gas of the first carrier gas branch 1 sequentially flows to the interface (5) through the interface (4) of the first switching valve 18 and enters the first chromatographic column 4, then flows to the interface (8) through the interface (9) and enters the first venting needle valve 6, and the sample gas in the first chromatographic column 4 is purged and vented.
Then second switching valve 19 is opened, the carrier gas in carrier gas third branch 11 flows into interface (3) through interface (4) of second switching valve 19, the sample gas carrying a certain quantity flows into interface (9) through interface (4) of second switching valve 19 and enters third chromatographic column 12 to make pre-separation, and the H gas flowing out first flows out 2 、O 2 、Ar、N 2 And CO flows out along the interface No. 5, enters a fourth chromatographic column 15 along the interface No. 6 2 、O 2 、Ar、N 2 And CO flows out of the fourth chromatographic column 15 and then flows to a connector (4) along a connector (5) of the third switching valve 20, and enters the fourth vent needle valve 16 from the connector (4) of the third switching valve 20 for venting.
CF separated after the third chromatographic column 12 4 、CO 2 、N 2 O and SF 6 The carrier gas flows to the interface (6) along the interface (5) of the second switching valve 19, the second switching valve 19 is closed, the third switching valve 20 is opened, the carrier gas fourth branch 13 is opened, the carrier gas of the carrier gas fourth branch 13 flows to the interface (6) through the interface (7) of the second switching valve 19, and then the CF is carried 4 、CO 2 、N 2 O and SF 6 Enters a fourth chromatographic column 15 for re-separation, and the separated gas passes through a third switching valve 2Interface (5) of 0 flows to interface (6) to be detected by helium ionization detector 8.
The molybdenum hexafluoride sample is detected, and the following results are obtained:
| impurities | H 2 | O 2 +Ar | N 2 | CO | CF 4 | CO 2 | N 2 O | SF 6 |
| Content/10 -6 | 0.02 | 0.05 | 0.03 | 0.05 | 1.8 | 0.07 | 0.05 | 0.12 |
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modifications, alterations and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (10)
1. A gas chromatography detection system for analyzing impurities in a molybdenum hexafluoride product is characterized by comprising a carrier gas first branch (1), a carrier gas second branch (5), a carrier gas third branch (11) and a carrier gas fourth branch (13), a first chromatographic column (4), a second chromatographic column (7), a third chromatographic column (12) and a fourth chromatographic column (15), a first switching valve (18), a second switching valve (19) and a third switching valve (20);
the two ends of the second chromatographic column (7) are respectively connected with the first switching valve (18) and the third switching valve (20), and the two ends of the fourth chromatographic column (15) are respectively connected with the second switching valve (19) and the third switching valve (20).
2. A gas chromatography detection system for the analysis of impurities in molybdenum hexafluoride products, according to claim 1, characterized in that the first branch (1) of the carrier gas is connected to the interface No. 4 of the first switching valve (18), the second branch (5) of the carrier gas is connected to the interface No. 7 of the first switching valve (18), the sample inlet (2) is connected to the interface No. 1 of the first switching valve (18), the interfaces No. 3 and No. r of the first switching valve (18) are connected by a first dosing ring (3), the interface No. 2 of the first switching valve (18) is connected to the second switching valve (19), the interface No. 6 of the first switching valve (18) is connected to the third switching valve (20) by a pipeline, on which the second chromatography column (7) is arranged;
no. 5 interface and No. 9 interface of first switching valve (18) pass through the tube coupling, are provided with on this pipeline first chromatographic column (4), no. 8 interface connection of first switching valve (18) has first blowdown needle valve (6).
3. The gas chromatography detection system for the analysis of impurities in a molybdenum hexafluoride product according to claim 1, wherein the carrier gas third branch (11) is connected to interface No. (4) of the second switching valve (19), the carrier gas fourth branch (13) is connected to interface No. (7) of the second switching valve (19), the sample outlet (10) is connected to interface No. (2) of the second switching valve (19), and interfaces No. (3) and No. (r) of the second switching valve (19) are connected through a pipeline, on which a second quantitative ring (9) is disposed;
the interface (1) of the second switching valve (19) is connected with the first switching valve (18), the interface (6) of the second switching valve (19) is connected with the third switching valve (20) through a pipeline, and the fourth chromatographic column (15) is arranged on the pipeline;
no. 5 interface and No. 9 interface of second diverter valve (19) pass through the tube coupling, are provided with on this pipeline third chromatographic column (12), no. 8 interface connection of second diverter valve (19) has second blow-off needle valve (14).
4. A gas chromatography detection system for the analysis of impurities in molybdenum hexafluoride products, according to claim 1, wherein the number (1) interface of the third switching valve (20) is connected to the first switching valve (18) by a line on which the second chromatography column (7) is arranged;
no. 5 interface of third diverter valve (20) with second diverter valve (19) pass through the tube coupling, are provided with on this pipeline fourth chromatographic column (15), no. 4 interface connection of third diverter valve (20) has third evacuation needle valve (16), no. 2 interface connection of third diverter valve (20) has fourth evacuation needle valve (17), no. 2 interface and No. 3 interface connection of third diverter valve (20), no. 6 interface connection helium ionization detector (8) of third diverter valve (20).
5. A gas chromatography detection system for the analysis of impurities in molybdenum hexafluoride products, according to claim 1, characterised in that the first chromatographic column (4) is a carbon molecular sieve chromatographic column, the second chromatographic column (7) is a 5A molecular sieve chromatographic column, and the third (12) and fourth (15) chromatographic columns are Hayesep Q chromatographic columns.
6. A gas chromatography detection system for the analysis of impurities in molybdenum hexafluoride products, according to claim 1, wherein the first and second switching valves (18, 19) are ten-way valves and the third switching valve (20) is a six-way valve.
7. A method for analyzing impurities in a molybdenum hexafluoride product, comprising the steps of using the gas chromatography detection system of any one of claims 1-6, including:
s1, sample gas to be detected sequentially passes through a port (1) of a first switching valve (18), a port (R) and a first quantitative ring (3) from a sample inlet (2), after the first quantitative ring (3) is filled with the sample gas to be detected, the sample gas to be detected enters the port (1) of a second switching valve (19), a port (R) of the second switching valve (19) through the port (3) and the port (2) and the second quantitative ring (9), and after the second quantitative ring (9) is filled with the sample gas to be detected, the sample gas to be detected enters a sample outlet (10) along the port (3) and the port (2) of the second switching valve (19);
s2, after sample injection is finished, a first switching valve (18) is opened, a carrier gas first branch (1) is opened, carrier gas of the carrier gas first branch (1) flows to a port (3) through a port (4) of the first switching valve (18), a certain amount of sample gas flows to a port (9) through a port at the position of the No. 5 to enter a first chromatographic column (4) for pre-separation, the first mixed gas which flows out firstly flows out along the port (5), the first switching valve (18) is closed, a carrier gas second branch (5) is opened, carrier gas of the carrier gas second branch (5) carries the first mixed gas to enter a second chromatographic column (7) from the port (6), the first mixed gas which enters the second chromatographic column (7) is separated again through the second chromatographic column (7), the carrier gas flows to the port (6) through the port (1) of a third switching valve (20) to enter a helium ionization detector (8) for detection, the carrier gas of the first branch (1) sequentially flows into the port (6) of the first chromatographic column (4) through the port (4) of the first switching valve (18), and then flows into a helium ionization detector (8) for detection, and the carrier gas of the sample purging;
s3, then opening a second switching valve (19), enabling carrier gas of a carrier gas third branch (11) to flow to a port (3) through a port (4) of the second switching valve (19), enabling a certain amount of sample gas to flow to a port (9) through a port (4) of the second switching valve (19) to enter a third chromatographic column (12) for pre-separation, enabling first mixed gas flowing out firstly to flow out along the port (5) and then enter a fourth chromatographic column (15) along the port (6), enabling the first mixed gas to flow to the port (4) along the port (5) of a third switching valve (20) after flowing out from the fourth chromatographic column (15), and enabling the first mixed gas to flow to the port (4) through the port (4) of the third switching valve (20) to enter a fourth emptying needle valve (16) for emptying;
s4, the second mixed gas separated after the third chromatographic column (12) flows to the interface (6) along the interface (5) of the second switching valve (19), the second switching valve (19) is closed, the third switching valve (20) is opened, the carrier gas fourth branch (13) is opened, the carrier gas of the carrier gas fourth branch (13) flows to the interface (6) through the interface (7) of the second switching valve (19), then the second mixed gas is carried to enter the fourth chromatographic column (15) for re-separation, and the separated gas flows to the interface (6) through the interface (5) of the third switching valve (20) and enters the helium ionization detector (8) for detection.
8. A method for the analysis of impurities in molybdenum hexafluoride products according to claim 7, characterized in that the first dosing ring (3) and the second dosing ring (9) have a volume of 0.1-1ml.
9. The method for analyzing the impurities in the molybdenum hexafluoride product according to claim 7, wherein the sample gas is fed once, the sample gas is pre-separated into the first mixed gas in the first chromatographic column (4), and the first mixed gas is re-separated in the second chromatographic column (7) and then is detected in the helium ionization detector (8).
10. A method for the analysis of impurities in molybdenum hexafluoride products according to claim 7, characterized in that the sample gas is pre-separated from H in a third chromatographic column (12) 2 、O 2 、Ar、N 2 And a CO component, H 2 、O 2 、Ar、N 2 And CO component enters a fourth chromatographic column (15) and then is dischargedFraction CF separated after empty, third column (12) 4 、CO 2 、N 2 O and SF 6 Enters a fourth chromatographic column (15) for re-separation and then enters a helium ionization detector (8) for detection.
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