CN111024801A - Sample injection system and method for analyzing content of rare gas in collected gas by drainage method - Google Patents
Sample injection system and method for analyzing content of rare gas in collected gas by drainage method Download PDFInfo
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- CN111024801A CN111024801A CN201911327156.XA CN201911327156A CN111024801A CN 111024801 A CN111024801 A CN 111024801A CN 201911327156 A CN201911327156 A CN 201911327156A CN 111024801 A CN111024801 A CN 111024801A
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- 238000000034 method Methods 0.000 title claims abstract description 46
- 238000002347 injection Methods 0.000 title claims description 76
- 239000007924 injection Substances 0.000 title claims description 76
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000000741 silica gel Substances 0.000 claims abstract description 41
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 41
- 238000010790 dilution Methods 0.000 claims abstract description 32
- 239000012895 dilution Substances 0.000 claims abstract description 32
- 238000000746 purification Methods 0.000 claims abstract description 27
- 238000005070 sampling Methods 0.000 claims abstract description 13
- 239000007789 gas Substances 0.000 claims description 191
- 239000002184 metal Substances 0.000 claims description 135
- 229910052751 metal Inorganic materials 0.000 claims description 135
- 229910001220 stainless steel Inorganic materials 0.000 claims description 49
- 239000010935 stainless steel Substances 0.000 claims description 49
- 238000007789 sealing Methods 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000012544 monitoring process Methods 0.000 claims description 8
- 238000004949 mass spectrometry Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000003507 refrigerant Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 3
- 229910052710 silicon Inorganic materials 0.000 abstract 3
- 239000010703 silicon Substances 0.000 abstract 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 239000011521 glass Substances 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 238000003466 welding Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 150000003839 salts Chemical class 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
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2226—Sampling from a closed space, e.g. food package, head space
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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Abstract
The invention belongs to the field of determination of the content of rare gas dissolved in water, and particularly relates to a sample introduction system and a sample introduction method for analyzing the content of the rare gas in gas collected by adopting a drainage method, wherein the sample introduction system comprises a sample introduction needle, a gas collection bottle, a spiral cold trap, a gas dilution tank, a capacitance gauge and a molecular pump set, and the mouth of the gas collection bottle is sealed by a silica gel plug; in the sample introduction method, after the gas collection bottle is erected, the sample introduction needle is inserted into the silicon plug but does not penetrate through the silicon plug, the molecular pump set pumps away air in the sample introduction system, a molecular pump valve is closed, the spiral cold trap is sleeved with alcohol-dry ice, the sample introduction needle penetrates through the silicon plug, the gas is dried and diffused to the dilution tank through the cold trap, the capacitance gauge reads the gas pressure, and then the gas is intercepted and enters the purification system to remove active gas. The invention effectively avoids the problem of pollution of air inside the needle head to the sample gas in the process of sampling by using the injector, and simultaneously, can effectively remove water and dry the gas rich in water vapor before entering the purification system.
Description
Technical Field
The invention belongs to the field of determination of content of rare gas dissolved in water, and particularly relates to a sample injection system and method for analyzing content of rare gas in collected gas by a drainage method.
Background
As a traditional gas collection method, the drainage method has the advantages of simplicity in operation, high sampling efficiency and the like. The gas is collected in the glass bottle, and after the collection is accomplished, the glass bottle adopts the plug to seal the inversion, and the gas is sealed in the glass bottle bottom by the dual effect of saturated salt solution and plug.
The traditional sample injection analysis method for collecting rare gases in gases by a drainage method is to erect a glass bottle, drive the gases to the bottle mouth of the glass bottle, penetrate a rubber plug by adopting a syringe needle, transfer the gases into the syringe, pull out the syringe, transfer sample gases into a purification system for gas purification, adsorb active gases except the rare gases, and analyze the rare gases. This approach suffers from two major problems: 1) before the syringe needle is inserted into the bottle body, the air in the needle can pollute the sample gas, and even a small amount of air can cause remarkable influence on the content analysis of rare gases, particularly argon, in the sample gas because the content of argon in the air is high (about 9320 ppm); 2) because the gas adopts saturated salt solution to seal, consequently there is a large amount of vapor in the gas, and vapor can seriously influence the vacuum degree of purification system, and then causes the influence to the purification of gas, and uses the syringe directly to pour into purification system and is difficult to effectively get rid of vapor.
Disclosure of Invention
The invention aims to provide a sample introduction system and a sample introduction method for analyzing the content of rare gas in collected gas by a drainage method, which can effectively avoid the pollution of air to sample gas, and can effectively dry gas to be detected with high humidity so as to accurately determine the content of the rare gas in the gas.
The technical scheme for realizing the purpose of the invention is as follows: a kind of sample introduction system of rare gas content analysis in the drainage method collection gas, this system includes the silica gel stopper, gas collection bottle, sample introduction needle, first metal valve, spiral cold trap, second metal valve, quick seal joint, third metal valve, capacitance gauge, stainless steel dilution tank, fourth metal valve, molecular pump group, fifth metal valve, small volume container, sixth metal valve and gas purification system, one end of the sample introduction needle inserts in the silica gel stopper, the silica gel stopper is in the bottleneck of the gas collection bottle, another end of the sample introduction needle connects with air inlet of the first metal valve; the air inlet of the spiral cold trap is connected with the air outlet of the first metal valve, the air outlet of the spiral cold trap is connected with the air inlet of the second metal valve, and the air outlet of the second metal valve is connected with the air inlet of the third metal valve through the quick sealing joint; the gas inlet of the stainless steel dilution tank is connected with the gas outlet of the third metal valve, the gas outlet of the stainless steel dilution tank is respectively connected with the gas inlet of the fourth metal valve and the gas inlet of the fifth metal valve, and a capacitance gauge is arranged at a monitoring port at the top of the stainless steel dilution tank; the air inlet of the fourth metal valve is communicated with the air inlet of the molecular pump group; the gas inlet of the small-volume container is connected with the gas outlet of the fifth metal valve, the gas outlet of the small-volume container is connected with the gas inlet of the sixth metal valve, and the gas outlet of the sixth metal valve is connected with the gas inlet of the gas purification system.
The sampling needle comprises a stainless steel flange and a sampling needle, one end of the sampling needle is positioned in the center of the stainless steel flange, and the other end of the sampling needle is inserted into the silica gel plug.
And the stainless steel flange of the sample injection needle is connected with the air inlet of the first metal valve.
The end part of the sample injection needle inserted into the silica gel plug is beveled by 30 degrees along the end surface by a stainless steel tube to form a sharp shape.
The sample injection needle is connected with the gas inlet of the first metal valve, the gas inlet of the spiral cold trap is connected with the gas outlet of the first metal valve, the gas outlet of the spiral cold trap is connected with the gas inlet of the second metal valve, the gas inlet of the stainless steel dilution tank is connected with the gas outlet of the third metal valve, the gas outlet of the stainless steel dilution tank is connected with the gas inlet of the fourth metal valve, the gas outlet of the stainless steel dilution tank is connected with the gas inlet of the fifth metal valve, and the stainless steel dilution tank is connected with the capacitance gauge through metal clamping sleeves.
And the gas inlet of the fourth metal valve is connected with the gas inlet of the molecular pump group, and the gas outlet of the sixth metal valve is connected with the gas inlet of the gas purification system through stainless steel flanges.
And the air inlet of the small-volume container is welded with the air outlet of the fifth metal valve, and the air outlet of the small-volume container is welded with the air inlet of the sixth metal valve.
The molecular pump group is an oil-free vacuum pump.
A sample injection method for analyzing the content of rare gas in collected gas by a drainage method comprises the following specific steps:
step 1, erecting a gas collection bottle filled with saturated salt water and a silica gel plug plugged at the bottle mouth, driving the collected gas to the bottle mouth of the gas collection bottle, and inserting a sample injection needle into the silica gel plug;
step 4, keeping for a period of time, and fully balancing the collected gas in the gas collection bottle and the gas in the sample introduction system;
step 6, opening a sixth metal valve, and introducing the intercepted gas into a gas purification system for purification and mass spectrometry;
and 8, connecting the spiral cold trap to an air inlet of a high-pressure nitrogen bottle through a quick sealing joint, blowing out condensed moisture in the spiral cold trap by the high-pressure nitrogen bottle, placing the spiral cold trap in an oven for drying, and connecting the spiral cold trap to a sample introduction system through the quick sealing joint again for sample introduction of a next gas sample.
And (3) inserting a sample injection needle head of the sample injection needle in the step (1) into the silica gel plug, wherein the sample injection needle head does not penetrate through the silica gel plug.
And in the step 2, until the pressure reading of the capacitance gauge at the monitoring port of the stainless steel dilution tank is less than 1 Pa.
The period of time in the step 3 is 5 min; and a sample injection needle head of the sample injection needle penetrates through the silica gel plug to enter the gas collection bottle.
The period of time in the step 4 is 1 min.
And intercepting gas with the volume of 0.1cc in the step 5.
The drying temperature of the oven in the step 8 is 80 ℃.
The invention has the beneficial technical effects that: the invention effectively avoids the problem of pollution of air inside the needle head to the sample gas in the process of sampling by using the injector, and simultaneously can effectively remove water and dry the gas rich in water vapor before entering the purification system.
The sample introduction system comprises a flange for welding a sample introduction needle, a spiral cold trap, a gas dilution tank, a capacitance gauge and a molecular pump set, wherein the bottle mouth of a gas collection bottle is sealed by a silica gel plug with a certain thickness. After the gas collection bottle is erected, the sample injection needle is inserted into the gas collection bottle without penetrating through the silica gel plug, the molecular pump set pumps away air in the sample injection needle and other parts in the sample injection system, a molecular pump valve is closed, the spiral cold trap is sleeved with alcohol-dry ice, the sample injection needle penetrates through the silica gel plug, after the gas is dried and diffused to the dilution tank through the cold trap, the capacitance gauge reads the gas pressure, and then 0.1cc of gas is intercepted and enters the purification system to remove active gas.
The gas collection bottle is sealed by the silica gel plug with a certain thickness, and the silica gel plug not only can be used as a sealing plug for initial vacuum preparation of a sample injection system such as a needle head, but also can prevent the needle head from being blocked by scrap colloidal particles; a stainless steel tube made of 316L material and with the outer diameter of 1.6mm is adopted, the stainless steel tube is obliquely cut by 30 degrees along the end face to be made into a needle shape, and then the other end face of the stainless steel tube is internally welded to a CF16 flange and is in sealing connection with a spiral cold trap, so that the reliable sealing performance of the needle and the system can be ensured; a copper tube with the outer diameter of 6.35mm is adopted to be made into a spiral cold trap to adsorb water vapor, so that the gas can be dried more thoroughly; the spiral cold trap and the gas dilution tank are sealed by adopting a quick sealing joint, so that the cold trap is convenient to disassemble and dry to remove moisture after each sample is dried; the high-precision capacitance gauge designed on the gas dilution tank can accurately measure the gas pressure, and can realize the measurement of the gas sample introduction amount by matching with a gas separator with the calibrated volume of 0.1cc, thereby realizing the measurement of the content of the rare gas.
Drawings
FIG. 1 is a schematic diagram of a sample injection system for analyzing the content of rare gases in collected gases by a drainage method according to the present invention;
FIG. 2 is a schematic structural diagram of a sample injection needle according to the present invention;
FIG. 3 is a schematic structural diagram of a spiral cold trap provided in the present invention;
in fig. 1: 1 is saturated saline solution, 2 is collected gas, 3 is a silica gel plug, 4 is a gas collection bottle, 5 is a sample injection needle, 6 is a first metal valve, 7 is a spiral cold trap, 8 is a second metal valve, 9 is a quick sealing joint, 10 is a third metal valve, 11 is a capacitance gauge, 12 is a stainless steel gas dilution tank, 13 is a fourth metal valve, 14 is a molecular pump group, 15 is a fifth metal valve, 16 is a small-volume container, 17 is a fifth metal valve, and 18 is a gas purification system;
in fig. 2: 19 is a sample injection needle, and 20 is a stainless steel flange.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
As shown in fig. 1, 2 and 3, the sample injection system for analyzing the content of rare gas in collected gas by using a drainage method provided by the invention comprises a silica gel plug 3, a gas collection bottle 4, a sample injection needle 5, a first metal valve 6, a spiral cold trap 7, a second metal valve 8, a quick seal joint 9, a third metal valve 10, a capacitance gauge 11, a stainless steel dilution tank 12, a fourth metal valve 13, a molecular pump group 14, a fifth metal valve 15, a small-volume container 16, a sixth metal valve 17 and a gas purification system 18. The sample injection needle 5 is formed by welding a CF16 stainless steel flange 20 and a sample injection needle 19, one end of the sample injection needle 19 is positioned at the center of the CF16 stainless steel flange 20, the other end of the sample injection needle 19 is inserted into a silica gel plug 3, the silica gel plug 3 is plugged in the bottle mouth of the gas collection bottle 4, and the CF16 stainless steel flange 20 of the sample injection needle 5 is hermetically connected with the gas inlet of the first metal valve 6 through a metal ferrule; the air inlet of the spiral cold trap 7 is hermetically connected with the air outlet of the first metal valve 6 through a metal sleeve, the air outlet of the spiral cold trap 7 is hermetically connected with the air inlet of the second metal valve 8 through a metal sleeve, and the air outlet of the second metal valve 8 is hermetically connected with the air inlet of the third metal valve 10 through a quick seal joint 9; an air inlet of the stainless steel dilution tank 12 is hermetically connected with an air outlet of the third metal valve 10 through a metal ferrule, an air outlet of the stainless steel dilution tank 12 is hermetically connected with an air inlet of the fourth metal valve 13 and an air inlet of the fifth metal valve 15 through a three-way metal ferrule, a capacitance gauge 11 is arranged at a monitoring port at the top of the stainless steel dilution tank 12, and the two are hermetically connected through a metal ferrule; the gas inlet of the fourth metal valve 13 is hermetically connected with the gas inlet of the molecular pump group 14 through a CF63 stainless steel flange; the air inlet of the small-volume container 16 is welded with the air outlet of the fifth metal valve 15 through argon arc welding, the air outlet of the small-volume container 16 is welded with the air inlet of the sixth metal valve 17 through argon arc welding, and the air outlet of the sixth metal valve 17 is connected with the air inlet of the purification system 18 through a CF16 stainless steel flange in a sealing mode.
The metal cutting ferrule and the valve of the whole set of system are all made of 316L stainless steel, the inner walls of the pipeline and the metal cutting ferrule are all subjected to polishing treatment, the outer diameter of the metal cutting ferrule is 6.35mm, and the inner diameter of the metal cutting ferrule is 4.20 mm.
The thickness of the silica gel plug 3 of the gas collection bottle is 15 mm.
The material of the sample injection needle 19 is 316L stainless steel, the end part of the sample injection needle 19 inserted into the silica gel plug 3 is a stainless steel tube with the outer diameter of 1.6mm and the inner diameter of 0.8mm, the end part is obliquely cut by 30 degrees along one end face to form a tip shape, and the other end face is internally welded in the center of a CF16 stainless steel flange 20.
The spiral cold trap 7 is made of a copper tube, the outer diameter of the copper tube is 6.35mm, and the inner diameter of the copper tube is 4.6 mm.
The measuring range of the capacitance gauge 11 is 1-20000 Pa, and the measuring precision is 0.25% of the reading.
The molecular pump group 14 is an oil-free vacuum pump with the pumping speed of 70L/s and the ultimate vacuum of 10-8Pa。
The small volume container 16 has a nominal volume of 0.1 cc.
As shown in figures 1, 2 and 3, the invention provides a sample injection method for analyzing the content of rare gases in collected gases by a drainage method, which comprises the following specific steps:
step 1, erecting a gas collection bottle 4 containing saturated saline solution 1 and a silica gel plug 3 plugged at the bottle mouth, driving collected gas 2 to the bottle mouth of the gas collection bottle 4, inserting a sample injection needle 19 of a sample injection needle 5 into the silica gel plug 3 for 7mm, and ensuring that the sample injection needle 19 does not penetrate through the silica gel plug 3;
step 4, keeping for 1min to ensure that the collected gas 2 in the gas collection bottle 4 is fully balanced with the gas in the sample introduction system;
step 6, opening a sixth metal valve 17, introducing 0.1cc of gas into a gas purification system 18 for purification, and performing mass spectrometry by adopting a mass spectrometer; step 7, closing the third metal valve 10 after the purification and mass spectrometry, pulling out the sample injection needle 19 of the sample injection needle 5 from the silica gel plug 3, and removing the vacuum cup with the alcohol-dry ice mixed refrigerant outside the spiral cold trap 7; then the spiral cold trap 7 is removed from the sampling system by removing the quick sealing joint 9 from the third metal valve 10;
and 8, connecting the spiral cold trap 7 to an air inlet of a high-pressure nitrogen bottle through a quick sealing joint 9, blowing out condensed moisture in the spiral cold trap 7 by using the high-pressure nitrogen bottle, placing the spiral cold trap 7 in an oven for drying at 80 ℃, and connecting the spiral cold trap 7 to a sample introduction system through the quick sealing joint 9 again for preparing the next gas sample for sample introduction.
The present invention has been described in detail with reference to the drawings and examples, but the present invention is not limited to the examples, and various changes can be made within the knowledge of those skilled in the art without departing from the spirit of the present invention. The prior art can be adopted in the content which is not described in detail in the invention.
Claims (15)
1. A kind of drainage method collects the sample injection system of rare gas content analysis in the gas, its characterized in that: the system comprises a silica gel plug (3), a gas collection bottle (4), a sampling needle (5), a first metal valve (6), a spiral cold trap (7), a second metal valve (8), a quick sealing joint (9), a third metal valve (10), a capacitance gauge (11), a stainless steel dilution tank (12), a fourth metal valve (13), a molecular pump set (14), a fifth metal valve (15), a small-volume container (16), a sixth metal valve (17) and a gas purification system (18), wherein one end of the sampling needle (5) is inserted into the silica gel plug (3), the silica gel plug (3) is plugged into the bottle mouth of the gas collection bottle (4), and the other end of the sampling needle (5) is connected with a gas inlet of the first metal valve (6); the air inlet of the spiral cold trap (7) is connected with the air outlet of the first metal valve (6), the air outlet of the spiral cold trap (7) is connected with the air inlet of the second metal valve (8), and the air outlet of the second metal valve (8) is connected with the air inlet of the third metal valve (10) through the quick sealing joint (9); an air inlet of the stainless steel dilution tank (12) is connected with an air outlet of the third metal valve (10), an air outlet of the stainless steel dilution tank (12) is respectively connected with an air inlet of the fourth metal valve (13) and an air inlet of the fifth metal valve (15), and a capacitance gauge (11) is arranged at a monitoring port at the top of the stainless steel dilution tank (12); the air inlet of the fourth metal valve (13) is communicated with the air inlet of the molecular pump group (14); the gas inlet of the small-volume container (16) is connected with the gas outlet of the fifth metal valve (15), the gas outlet of the small-volume container (16) is connected with the gas inlet of the sixth metal valve (17), and the gas outlet of the sixth metal valve (17) is connected with the gas inlet of the gas purification system (18).
2. The sample injection system for analyzing the rare gas content in the collected gas by the drainage method according to claim 1, characterized in that: the sample injection needle (5) consists of a stainless steel flange (20) and a sample injection needle head (19), one end of the sample injection needle head (19) is positioned at the center of the stainless steel flange (20), and the other end of the sample injection needle head (19) is inserted into the silica gel plug (3).
3. The sample injection system for analyzing the rare gas content in the collected gas by the drainage method according to claim 2, characterized in that: and a stainless steel flange (20) of the sample injection needle (5) is connected with an air inlet of the first metal valve (6).
4. The sample injection system for analyzing the rare gas content in the collected gas by the drainage method according to claim 1, 2 or 3, wherein: the end part of the sample injection needle (19) inserted into the silica gel plug (3) is beveled by a stainless steel pipe for 30 degrees along the end surface to form a sharp shape.
5. The sample injection system for analyzing the rare gas content in the collected gas by the drainage method according to claim 4, wherein the sample injection system comprises: the gas inlet of appearance needle (5) and first metal valve (6) between, between the gas inlet of heliciform cold trap (7) and the gas outlet of first metal valve (6), between the gas outlet of heliciform cold trap (7) and the gas inlet of second metal valve (8), between the gas inlet of stainless steel dilution tank (12) and the gas outlet of third metal valve (10), between the gas outlet of stainless steel dilution tank (12) and the gas inlet of fourth metal valve (13), between the gas outlet of stainless steel dilution tank (12) and the gas inlet of fifth metal valve (15), all be connected through the metal cutting ferrule respectively between stainless steel dilution tank (12) and electric capacity rule (11).
6. The sample injection system for analyzing the rare gas content in the collected gas by the drainage method according to claim 5, wherein the sample injection system comprises: the gas inlet of the fourth metal valve (13) is connected with the gas inlet of the molecular pump group (14), and the gas outlet of the sixth metal valve (17) is connected with the gas inlet of the gas purification system (18) through stainless steel flanges.
7. The sample injection system for analyzing the rare gas content in the collected gas by the drainage method according to claim 6, wherein: the air inlet of the small-volume container (16) is welded with the air outlet of the fifth metal valve (15), and the air outlet of the small-volume container (16) is welded with the air inlet of the sixth metal valve (17).
8. The sample injection system for analyzing the rare gas content in the collected gas by the drainage method according to claim 7, characterized in that: the molecular pump set (14) is an oil-free vacuum pump.
9. A sample injection method for analyzing the rare gas content in the collected gas by drainage method by using the sample injection system according to any one of claims 1 to 8, which is characterized in that: the method comprises the following specific steps:
step 1, erecting a gas collection bottle (4) containing saturated saline solution (1) and a silica gel plug (3) plugged at the bottle mouth, driving the collected gas (2) to the bottle mouth of the gas collection bottle (4), and inserting a sample injection needle (5) into the silica gel plug (3);
step 2, opening a first metal valve (6), a second metal valve (8), a third metal valve (10), a fourth metal valve (13) and a fifth metal valve (15), closing a sixth metal valve (17), and vacuumizing the system by adopting a molecular pump set (14) until the pressure reading of a capacitance gauge (11) at a monitoring port of a stainless steel dilution tank (12) is less than a certain value;
step 3, sleeving a thermos cup with an alcohol-dry ice refrigerant outside the spiral cold trap (7), closing a fourth metal valve (13) and a fifth metal valve (15) after a period of time, and enabling the sample injection needle (5) to penetrate through the silica gel plug (3) to enter the gas collection bottle (4);
step 4, keeping for a period of time, and fully balancing the collected gas (2) in the gas collection bottle (4) and the gas in the sample introduction system;
step 5, closing the third metal valve (10), opening the fifth metal valve (15), keeping for a period of time, recording the pressure reading of the capacitance gauge (11), closing the fifth metal valve (15), and intercepting gas with a certain volume;
step 6, opening a sixth metal valve (17), and introducing the intercepted gas into a gas purification system (18) for purification and mass spectrometry;
step 7, after the purification and mass spectrometry are finished, closing the third metal valve (10), pulling out a sample injection needle head (19) of the sample injection needle (5) from the silica gel plug (3), and removing the vacuum cup with the alcohol-dry ice refrigerant outside the spiral cold trap (7); then the spiral cold trap (7) is removed from the sampling system through the quick sealing joint (9) and the third metal valve (10);
and 8, connecting the spiral cold trap (7) to an air inlet of a high-pressure nitrogen bottle through a quick sealing joint (9), blowing out condensed moisture in the spiral cold trap (7) by the high-pressure nitrogen bottle, placing the spiral cold trap (7) in an oven for drying, and connecting the spiral cold trap (7) to a sample introduction system through the quick sealing joint (9) again for preparing the next gas sample for sample introduction.
10. The sample injection method for analyzing the rare gas content in the collected gas by the drainage method according to claim 9, characterized in that: and (2) inserting a sample injection needle head (19) of the sample injection needle (5) into the silica gel plug (3) in the step (1), wherein the sample injection needle head (19) does not penetrate through the silica gel plug (3).
11. The sample injection method for analyzing the rare gas content in the collected gas by the drainage method according to claim 10, characterized in that: and in the step 2, until the pressure reading of a capacitance gauge (11) at the monitoring port of the stainless steel dilution tank (12) is less than 1 Pa.
12. The sample injection method for analyzing the rare gas content in the collected gas by the drainage method according to claim 11, characterized in that: the period of time in the step 3 is 5 min; and a sample injection needle head (19) of the sample injection needle (5) penetrates through the silica gel plug (3) to enter the gas collection bottle (4).
13. The sample injection method for analyzing the rare gas content in the collected gas by the drainage method according to claim 12, characterized in that: the period of time in the step 4 is 1 min.
14. The sample injection method for analyzing the rare gas content in the collected gas by the drainage method according to claim 13, characterized in that: and intercepting gas with the volume of 0.1cc in the step 5.
15. The sample injection method for analyzing the rare gas content in the collected gas by the drainage method according to claim 14, characterized in that: the drying temperature of the oven in the step 8 is 80 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911327156.XA CN111024801A (en) | 2019-12-20 | 2019-12-20 | Sample injection system and method for analyzing content of rare gas in collected gas by drainage method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911327156.XA CN111024801A (en) | 2019-12-20 | 2019-12-20 | Sample injection system and method for analyzing content of rare gas in collected gas by drainage method |
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| CN109813794A (en) * | 2018-12-25 | 2019-05-28 | 核工业北京地质研究院 | A kind of drainage collects the sampling system and sample injection method of gas |
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| JP2002062285A (en) * | 2000-08-17 | 2002-02-28 | Air Water Inc | Head space sampler for analyzing volatile organic compound in-site |
| CN102042920A (en) * | 2009-10-23 | 2011-05-04 | 中国石油化工股份有限公司 | Trace hydrogen fractionation-free quantitative enrichment system and enrichment method |
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Application publication date: 20200417 |