CN110609077B - Natural gas neon isotope composition measuring device and method - Google Patents
Natural gas neon isotope composition measuring device and method Download PDFInfo
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- CN110609077B CN110609077B CN201810615650.5A CN201810615650A CN110609077B CN 110609077 B CN110609077 B CN 110609077B CN 201810615650 A CN201810615650 A CN 201810615650A CN 110609077 B CN110609077 B CN 110609077B
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- 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
Abstract
The invention relates to a natural gas neon isotope composition measuring device which comprises a rare gas mass spectrometer, active carbon cold traps I and II and a natural gas steel cylinder. The natural gas steel cylinder is connected with a high vacuum system through a high vacuum pipeline by an active carbon cold trap I; the high vacuum pipeline is connected with an ultrahigh vacuum pipeline through a pipeline, and the ultrahigh vacuum pipeline is connected with an activated carbon cold trap II, a rare gas mass spectrometer and an ultrahigh vacuum system; a pressure reducing valve, high vacuum valves I, II and a film vacuum gauge are arranged between the natural gas steel cylinder and the active carbon cold trap I; the active carbon cold trap I is connected with a high vacuum pipeline through a high vacuum valve III; a high vacuum valve IV is arranged between the high vacuum system and the pipeline; the pipeline is provided with an ultrahigh vacuum valve I; an ultrahigh vacuum valve II is arranged between the ultrahigh vacuum system and the pipeline; the active carbon cold trap II is connected with an ultrahigh vacuum pipeline through an ultrahigh vacuum valve III; an ultra-high vacuum valve IV is arranged between the rare gas mass spectrometer and the activated carbon cold trap II. The invention also discloses a using method of the device. The invention has accurate measurement result and no interference.
Description
Technical Field
The invention relates to an analysis method of neon content and neon isotope composition of natural gas, in particular to a measurement device and method of neon isotope composition of natural gas.
Background
Noble gases include helium, neon, argon, krypton, xenon and radon, wherein stable isotope compositions of helium, neon, argon, krypton and xenon are commonly analyzed by a rare gas mass spectrometer, and in order to obtain accurate data, helium, neon, argon, krypton and xenon are generally prepared from gas samples and separated by components, and then the isotope compositions of the components are analyzed by the rare gas mass spectrometer. The process of preparing a gas sample to contain only rare gases is called purging.
The rare gas neon isotope composition of the atmosphere, crust and mantle has different values, so that information such as the source of the rare gas neon isotope can be obtained. The content of neon in natural gas is very low, much lower than the content of helium or argon in natural gas, typically 1/1000 of the helium content or less than 1/100 of the argon content. When detecting the rare gas isotope composition in natural gas, each laboratory usually carries out one-time sample injection, firstly purifies the natural gas into pure rare gas, then separates each component, carries out isotope composition mass spectrometry detection, and chemical reagents required for purification usually comprise titanium sponge, zirconium aluminum getter, active carbon and the like, and uses an electric furnace. In order to meet the requirements of neon isotope composition mass spectrometry detection, a large amount of natural gas needs to be purified, and only a small part of purified gas is used for helium or argon isotope composition detection. The process of purifying all rare gases by one sample injection requires a large amount of chemical reagents and time, and the method of using a small part of purified gases for helium or argon isotope composition detection is unfavorable for analysis of helium and argon contents and is easy to generate isotope split.
Disclosure of Invention
The invention aims to solve the technical problem of providing a natural gas neon isotope composition measuring device with more accurate measurement results and no interference.
The invention aims to provide a method for using a natural gas neon isotope composition measuring device.
In order to solve the problems, the device for measuring the composition of the natural gas neon isotope is characterized in that: the device comprises a rare gas mass spectrometer, an activated carbon cold trap I, an activated carbon cold trap II and a natural gas steel cylinder; the natural gas steel cylinder is connected with a high vacuum system through a high vacuum pipeline by the active carbon cold trap I; the high vacuum pipeline is connected with an ultrahigh vacuum pipeline through a pipeline, one end of the ultrahigh vacuum pipeline is sequentially connected with the activated carbon cold trap II and the rare gas mass spectrometer, and the other end of the ultrahigh vacuum pipeline is connected with an ultrahigh vacuum system; a pressure reducing valve, a high vacuum valve I, a high vacuum valve II and a film vacuum gauge are sequentially arranged on the high vacuum pipeline between the natural gas steel cylinder and the active carbon cold trap I; the activated carbon cold trap I is connected with the high vacuum pipeline through a high vacuum valve III; a high vacuum valve IV is arranged on the high vacuum pipe between the high vacuum system and the pipeline; the pipeline is provided with an ultrahigh vacuum valve I; an ultrahigh vacuum valve II is arranged on the ultrahigh vacuum pipe between the ultrahigh vacuum system and the pipeline; the active carbon cold trap II is connected with the ultrahigh vacuum pipeline through an ultrahigh vacuum valve III; and an ultrahigh vacuum valve IV is arranged on the ultrahigh vacuum tube between the rare gas mass spectrometer and the activated carbon cold trap II.
The natural gas steel cylinder is provided with a valve.
The control temperature of the activated carbon cold trap II is 30K-300K.
The application method of the natural gas neon isotope composition measuring device comprises the following steps:
the method comprises the steps of closing an ultrahigh vacuum valve I and an ultrahigh vacuum valve IV, opening the high vacuum valve I, the high vacuum valve II, the high vacuum valve III and the high vacuum valve IV, opening the ultrahigh vacuum valve II and the ultrahigh vacuum valve III, and vacuumizing; simultaneously, the active carbon cold trap I and the active carbon cold trap II are respectively warmed to room temperature;
closing the ultrahigh vacuum valve III; setting 30K for the activated carbon cold trap II, and starting to cool;
setting the pressure at the outlet of the pressure reducing valve to be 0.1MPa, closing the high vacuum valve I, opening a valve of a natural gas steel cylinder, waiting 10 seconds, and closing the valve; closing the high vacuum valve II, opening the high vacuum valve I, waiting for 10 seconds, and closing the high vacuum valve I; closing the high vacuum valve III and the high vacuum valve IV, opening the high vacuum valve II, waiting for 10 seconds, and closing the high vacuum valve II; recording the pressure of gas, opening the high vacuum valve III, and freezing the activated carbon cold trap I by using liquid nitrogen for 3min;
fourthly, closing the ultrahigh vacuum valve II, closing the high vacuum valve III, opening the ultrahigh vacuum valve I, waiting for 10 seconds, closing the ultrahigh vacuum valve I, and introducing gas into a sample ultrahigh vacuum area;
opening the ultrahigh vacuum valve III, and waiting for 10min after the activated carbon cold trap II reaches 30K; opening the ultrahigh vacuum valve II, waiting for 1min, and closing the ultrahigh vacuum valve II;
setting 70K for the active carbon cold trap II, and waiting for 10min after 70K is reached;
and closing the ultra-high vacuum valve III, opening the ultra-high vacuum valve IV for 10 seconds, closing the ultra-high vacuum valve IV, and measuring 20 Ne mass spectrum peak height and neon isotope composition, and calculating the content of neon in natural gas.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, aiming at the characteristic that the neon content in natural gas is far lower than the helium or argon content, the sample for mass spectrum detection of the neon isotope composition of natural gas is prepared independently, and the sample quantity is more suitable for the requirement of neon isotope composition detection, so that the measurement result is more accurate.
2. According to the invention, the active carbon cold trap I frozen by liquid nitrogen removes argon, krypton, xenon and active gases in natural gas, the active carbon can be regenerated after being used, chemical reagents except liquid nitrogen are not required to be consumed, and a sample entering a mass spectrometer meets the detection requirement of neon isotope composition as much as possible, and whether helium and argon meet the detection requirement or not is not required to be considered, so that the quantitative determination is more accurate.
3. The invention separates argon, helium and neon by using the active carbon cold trap II, separates argon by using the active carbon cold traps (I and II) twice, separates helium by using the active carbon cold trap (II) once, and makes neon enter mass spectrum separately for analysis, and does not interfere with other rare gas measurement, in particular eliminates 40 Secondary ion pair of Ar 20 Interference of Ne mass spectrum peaks.
Drawings
The following describes the embodiments of the present invention in further detail with reference to the drawings.
Fig. 1 is a schematic structural view of the present invention.
In the figure: 1-a rare gas mass spectrometer; 2-an active carbon cold trap I; 3-an active carbon cold trap II; 4-a natural gas steel cylinder; 40-valve; 5-high vacuum line; 51-high vacuum valve I; 52-a high vacuum valve II; 53-high vacuum valve iii; 54-a high vacuum valve IV; 6-a high vacuum system; 7-an ultra-high vacuum pipeline; 71-an ultrahigh vacuum valve I; 72-an ultrahigh vacuum valve II; 73-an ultra-high vacuum valve III; 74-an ultrahigh vacuum valve IV; 8-an ultra-high vacuum system; 9-a pressure reducing valve; 10-film vacuum gauge.
Detailed Description
As shown in fig. 1, the natural gas neon isotope composition measuring device comprises a rare gas mass spectrometer 1, an activated carbon cold trap I2, an activated carbon cold trap II 3 and a natural gas steel cylinder 4.
The natural gas steel cylinder 4 is connected with a high vacuum system 6 through a high vacuum pipeline 5 and an active carbon cold trap I2; the high vacuum pipeline 5 is connected with an ultrahigh vacuum pipeline 7 through a pipeline, one end of the ultrahigh vacuum pipeline 7 is sequentially connected with an activated carbon cold trap II 3 and a rare gas mass spectrometer 1, and the other end of the ultrahigh vacuum pipeline 7 is connected with an ultrahigh vacuum system 8; a pressure reducing valve 9, a high vacuum valve I51, a high vacuum valve II 52 and a film vacuum gauge 10 are sequentially arranged on a high vacuum pipeline 5 between the natural gas steel cylinder 4 and the active carbon cold trap I2; the activated carbon cold trap I2 is connected with a high vacuum pipeline 5 through a high vacuum valve III 53; a high vacuum valve IV 54 is arranged on the high vacuum pipeline 5 between the high vacuum system 6 and the pipeline; the pipeline is provided with an ultrahigh vacuum valve I71; an ultrahigh vacuum valve II 72 is arranged on the ultrahigh vacuum pipeline 7 between the ultrahigh vacuum system 8 and the pipeline; the activated carbon cold trap II 3 is connected with an ultrahigh vacuum pipeline 7 through an ultrahigh vacuum valve III 73; an ultra-high vacuum valve IV 74 is arranged on the ultra-high vacuum pipeline 7 between the rare gas mass spectrometer 1 and the activated carbon cold trap II 3.
The natural gas cylinder 4 is provided with a valve 40.
The control temperature of the activated carbon cold trap II 3 is 30K-300K.
The application method of the natural gas neon isotope composition measuring device comprises the following steps:
the method comprises the steps of closing an ultra-high vacuum valve I71 and an ultra-high vacuum valve IV 74, opening a high vacuum valve I51, a high vacuum valve II 52, a high vacuum valve III 53 and a high vacuum valve IV 54, opening an ultra-high vacuum valve II 72 and an ultra-high vacuum valve III 73, and vacuumizing; simultaneously, the active carbon cold trap I2 and the active carbon cold trap II 3 are respectively warmed to room temperature;
closing the ultrahigh vacuum valve III 73; setting the activated carbon cold trap II 3 at 30K, and starting to cool;
setting the outlet pressure of the pressure reducing valve 9 to be 0.1MPa, closing the high vacuum valve I51, opening the valve 40 of the natural gas steel cylinder 4 for 10 seconds, and closing the valve 40; closing the high vacuum valve II 52, opening the high vacuum valve I51, waiting 10 seconds, and closing the high vacuum valve I51; closing the high vacuum valve III 53 and the high vacuum valve IV 54, opening the high vacuum valve II 52, waiting 10 seconds, and closing the high vacuum valve II 52; recording the pressure of the gas, opening a high vacuum valve III 53, freezing an active carbon cold trap I2 by liquid nitrogen, and waiting for 3min; this step removes argon, krypton, xenon and reactive gases from the natural gas, leaving only helium and neon;
fourth, a Guan Chaogao vacuum valve II 72 is opened, a high vacuum valve III 53 is closed, an ultra-high vacuum valve I71 is opened, 10s is equal, and Guan Chaogao vacuum valve I71 is equal, and gas is introduced into a sample ultra-high vacuum area;
opening an ultrahigh vacuum valve III 73, waiting for 10min after the activated carbon cold trap II 3 reaches 30K; opening an ultrahigh vacuum valve II 72, waiting for 1min, and opening a Guan Chaogao vacuum valve II 72; this step separates helium and neon and removes the helium;
setting 70K in a cold trap II 3 of active carbon, and waiting for 10min after 70K is reached;
vacuum valve III 73 of Ru Guan Chaogao, open ultra high vacuum valve IV 74, wait 10s, vacuum valve IV 74 of Guan Chaogao, measure 20 Ne mass spectrum peak height and neon isotope composition, and calculating the content of neon in natural gas.
The natural gas cylinder 4 and the pressure reducing valve 9 were removed, a reference gas (air) was introduced from the high vacuum valve I51, and the pressure of the reference gas was measured in the same manner, 20 Ne mass spectrum peak height and neon isotope composition, and the content of neon in natural gas and the isotope composition thereof are calculated by a comparison method.
When the invention is used for separately carrying out the analysis of natural gas helium and argon isotopes, only a small amount of sample is needed, the invention does not need to be carried out simultaneously with the neon isotope composition, and the detection of each sample is improved.
Example 1 taking a neon isotope composition measurement of a natural gas sample in a tarius basin as an example, a method for using a natural gas neon isotope composition measurement apparatus includes the following steps:
the method comprises the steps of closing an ultra-high vacuum valve I71 and an ultra-high vacuum valve IV 74, opening a high vacuum valve I51, a high vacuum valve II 52, a high vacuum valve III 53 and a high vacuum valve IV 54, opening an ultra-high vacuum valve II 72 and an ultra-high vacuum valve III 73, and vacuumizing; simultaneously, the active carbon cold trap I2 and the active carbon cold trap II 3 are respectively warmed to room temperature;
closing the ultrahigh vacuum valve III 73; setting the activated carbon cold trap II 3 at 30K, and starting to cool;
setting the outlet pressure of the pressure reducing valve 9 to be 0.1MPa, closing the high vacuum valve I51, opening the valve 40 of the natural gas steel cylinder 4 for 10 seconds, and closing the valve 40; closing the high vacuum valve II 52, opening the high vacuum valve I51, waiting 10 seconds, and closing the high vacuum valve I51; closing the high vacuum valve III 53 and the high vacuum valve IV 54, opening the high vacuum valve II 52, waiting 10 seconds, and closing the high vacuum valve II 52; recording the pressure P of the gas s Opening a high vacuum valve III 53, freezing an activated carbon cold trap I2 by liquid nitrogen, and waiting for 3min; this step removes argon, krypton, xenon and reactive gases from the natural gas, leaving only helium and neon;
fourth, a Guan Chaogao vacuum valve II 72 is opened, a high vacuum valve III 53 is closed, an ultra-high vacuum valve I71 is opened, 10s is equal, and Guan Chaogao vacuum valve I71 is equal, and gas is introduced into a sample ultra-high vacuum area;
opening an ultrahigh vacuum valve III 73, and waiting for 10min after the activated carbon cold trap II 3 reaches 30K; opening an ultrahigh vacuum valve II 72, waiting for 1min, and opening a Guan Chaogao vacuum valve II 72; this step separates helium and neon and removes the helium;
setting 70K in a cold trap II 3 of active carbon, and waiting for 10min after 70K is reached;
vacuum valve III 73 of Ru Guan Chaogao, open ultra high vacuum valve IV 74, wait 10s, vacuum valve IV 74 of Guan Chaogao, measure 20 Ne mass spectrum peak height 20 I s And neon isotope composition (R) 20/22 ) s 、(R 21/22 ) s 。
The natural gas cylinder 4 and the pressure reducing valve 9 are removed, a reference gas (air) is introduced from the high vacuum valve I51, and the pressure P of the reference gas is measured by the same procedure 0 、 20 Ne mass spectrum peak height 20 I 0 And neon isotope composition (R) 20/22 ) 0 、(R 21/22 ) 0 。
Calculating parameters:
P 0 = 183Pa，P s = 76800Pa，I 0 = 22.5V，I s = 2.1V
(R 20/22 ) s = 7.8，(R 21/22 ) s = 0.056，(R 20/22 ) 0 = 9.9，(R 21/22 ) 0 =0.029；
calculation results:
natural gas neon content = ( 20 I s /P s )/( 20 I 0 /P 0 ) × 1.8 × 10 -5 = 4 × 10 -9
Natural gas 20 Ne/ 22 Ne = (R 20/22 ) s /(R 20/22 ) 0 × 9.8 = 7.7
Natural gas 21 Ne/ 22 Ne = (R 21/22 ) s /(R 21/22 ) 0 × 0.029 = 0.056。
Claims (1)
1. The application method of the natural gas neon isotope composition measuring device is characterized by comprising the following steps of: the measuring device comprises a rare gas mass spectrometer (1), an active carbon cold trap I (2), an active carbon cold trap II (3) and a natural gas steel bottle (4); the natural gas steel cylinder (4) is connected with a high vacuum system (6) through a high vacuum pipeline (5) and the active carbon cold trap I (2); the high vacuum pipeline (5) is connected with an ultrahigh vacuum pipeline (7) through a pipeline, one end of the ultrahigh vacuum pipeline (7) is sequentially connected with the activated carbon cold trap II (3) and the rare gas mass spectrometer (1), and the other end of the ultrahigh vacuum pipeline is connected with an ultrahigh vacuum system (8); a pressure reducing valve (9), a high vacuum valve I (51), a high vacuum valve II (52) and a film vacuum gauge (10) are sequentially arranged on the high vacuum pipeline (5) between the natural gas steel cylinder (4) and the active carbon cold trap I (2); the active carbon cold trap I (2) is connected with the high vacuum pipeline (5) through a high vacuum valve III (53); a high vacuum valve IV (54) is arranged on the high vacuum pipeline (5) between the high vacuum system (6) and the pipeline; the pipeline is provided with an ultrahigh vacuum valve I (71); an ultrahigh vacuum valve II (72) is arranged on the ultrahigh vacuum pipeline (7) between the ultrahigh vacuum system (8) and the pipeline; the active carbon cold trap II (3) is connected with the ultrahigh vacuum pipeline (7) through an ultrahigh vacuum valve III (73); an ultrahigh vacuum valve IV (74) is arranged on the ultrahigh vacuum pipeline (7) between the rare gas mass spectrometer (1) and the activated carbon cold trap II (3); the using method of the measuring device comprises the following steps:
the method comprises the steps of closing an ultrahigh vacuum valve I (71) and an ultrahigh vacuum valve IV (74), opening the high vacuum valve I (51), a high vacuum valve II (52), a high vacuum valve III (53) and a high vacuum valve IV (54), opening the ultrahigh vacuum valve II (72) and the ultrahigh vacuum valve III (73), and vacuumizing; simultaneously, the active carbon cold trap I (2) and the active carbon cold trap II (3) are respectively heated to room temperature;
closing the ultrahigh vacuum valve III (73); the activated carbon cold trap II (3) is set to be 30K, and cooling is started;
setting the outlet pressure of the pressure reducing valve (9) to be 0.1MPa, closing the high vacuum valve I (51), opening the valve (40) of the natural gas steel cylinder (4), and closing the valve (40) for 10 seconds; closing the high vacuum valve II (52), opening the high vacuum valve I (51), and closing the high vacuum valve I (51) 10 seconds; closing the high vacuum valve III (53), the high vacuum valve IV (54), opening the high vacuum valve II (52), and the like for 10 seconds, and closing the high vacuum valve II (52); recording the pressure of the gas, opening the high vacuum valve III (53), and freezing the activated carbon cold trap I (2) by using liquid nitrogen for 3min;
fourth, closing the ultra-high vacuum valve II (72), closing the high vacuum valve III (53), opening the ultra-high vacuum valve I (71), waiting 10 seconds, closing the ultra-high vacuum valve I (71), and introducing gas into a sample ultra-high vacuum area;
opening the ultrahigh vacuum valve III (73), and waiting for 10min after the activated carbon cold trap II (3) reaches 30K; opening the ultrahigh vacuum valve II (72), waiting for 1min, and closing the ultrahigh vacuum valve II (72);
setting 70K for the active carbon cold trap II (3), and waiting for 10min after 70K is reached;
and (3) closing the ultra-high vacuum valve III (73), opening the ultra-high vacuum valve IV (74), and measuring after 10 seconds, closing the ultra-high vacuum valve IV (74) 20 Ne mass spectrum peak height and neon isotope composition, and calculating the content of neon in natural gas.
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| CN113908591B (en) * | 2020-07-07 | 2023-03-17 | 中国科学院西北生态环境资源研究院 | Device and method for extracting dissolved gas in water sample of high-vacuum double-valve glass bottle |
| CN114813450A (en) * | 2022-05-06 | 2022-07-29 | 中国科学院西北生态环境资源研究院 | Method for measuring freezing pressure of helium content in natural gas |
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