CN207439998U - A kind of high argon isotope ratio measuring device of natural gas - Google Patents
A kind of high argon isotope ratio measuring device of natural gas Download PDFInfo
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- CN207439998U CN207439998U CN201721601676.1U CN201721601676U CN207439998U CN 207439998 U CN207439998 U CN 207439998U CN 201721601676 U CN201721601676 U CN 201721601676U CN 207439998 U CN207439998 U CN 207439998U
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Abstract
The utility model is related to a kind of high argon isotope ratio measuring device of natural gas, which includes rare gas mass spectrograph, activated carbon cold-trap, titanium sponge stove, quadrupole mass spectrometer, U-shaped cold-trap and natural gas steel cylinder.Natural gas steel cylinder is connected with high vacuum system by high vacuum pipeline through U-shaped cold-trap, quadrupole mass spectrometer；High vacuum pipeline is connected with ultrahigh vacuum pipeline by pipeline, which is connected with titanium sponge stove, activated carbon cold-trap, rare gas mass spectrograph, ultra-high vacuum system；Pressure reducing valve, high vacuum valve I, II, diagram vacuum gauge are equipped between natural gas steel cylinder and U-shaped cold-trap；High vacuum valve III is equipped between U-shaped cold-trap and pipeline；High vacuum valve IV is equipped between high vacuum system and pipeline；Ultrahigh vacuum valve IV is equipped between ultra-high vacuum system and pipeline；Ultrahigh vacuum valve V is equipped between activated carbon cold-trap and titanium sponge stove；Ultrahigh vacuum valve VI is equipped between rare gas mass spectrograph and activated carbon cold-trap.The utility model has the characteristics that high certainty of measurement.
Description
Technical field
The utility model is related to natural gas argon isotope ratio (40Ar/36Ar analysis method more particularly to one kind) is natural
The high argon isotope ratio measuring device of gas.
Background technology
Rare gas He-Ar isotope composition has different numerical value in earth layers, it is possible thereby to obtain rare gas
The information such as source and Formed age.In structurally stable region, the natural gas adsorption age is older, and storage time is longer in geologic body,
Its argon isotope ratio (40Ar/36Ar it is) higher, thus by argon isotope ratio (40Ar/36Ar) can obtain natural gas formation and
Age information is stored, is of great significance for natural gas exploration and exploitation.It is limited by factors such as instrument and experimental techniques, with
Toward measure natural gas argon isotope ratio (40Ar/36Ar) it is less than 10000.
In natural gas sampling, transport, storage and analytic process, it is easy to micro-air is mixed into, this micro-air
Be mixed into affect argon isotope ratio (40Ar/36Ar detection data) can use the ratio between argon content and oxygen content to correct this mistake
Difference.But when argon isotope ratio (40Ar/36Ar when) very high, the air of trace, which is mixed into, can also generate larger error, and at this time
The content of oxygen can not have been measured with previous detection method.20Ne is typically derived from air, so measurement20The content of Ne is similary
Can estimate air be mixed into argon isotope ratio (40Ar/36Ar influence).
Utility model content
The technical problem to be solved by the utility model is to provide a kind of high argon isotopes of the natural gas of high certainty of measurement
Compare measuring device.
To solve the above problems, a kind of high argon isotope ratio measuring device of natural gas described in the utility model, special
Sign is：The device include rare gas mass spectrograph, activated carbon cold-trap, titanium sponge stove, quadrupole mass spectrometer, liquid nitrogen frozen it is U-shaped
Cold-trap and natural gas steel cylinder；The natural gas steel cylinder is connected with by high vacuum pipeline through the U-shaped cold-trap, the quadrupole mass spectrometer
High vacuum system；The high vacuum pipeline is connected with ultrahigh vacuum pipeline by pipeline, and one end of the ultrahigh vacuum pipeline connects successively
There are the titanium sponge stove, the activated carbon cold-trap, the rare gas mass spectrograph, the other end is connected with ultra-high vacuum system；Institute
It states and is equipped with pressure reducing valve, high vacuum valve I, Gao Zhen on the high vacuum pipeline between natural gas steel cylinder and the U-shaped cold-trap successively
Empty valve II, diagram vacuum gauge；The high vacuum pipeline between the U-shaped cold-trap and the pipeline is equipped with high vacuum valve III；
The high vacuum pipeline between the high vacuum system and the pipeline is equipped with high vacuum valve IV；The ultra-high vacuum system
The ultrahigh vacuum pipeline between the pipeline is equipped with ultrahigh vacuum valve IV；The activated carbon cold-trap and the titanium sponge
The ultrahigh vacuum pipeline between stove is equipped with ultrahigh vacuum valve V；The rare gas mass spectrograph and the activated carbon cold-trap
Between the ultrahigh vacuum pipeline be equipped with ultrahigh vacuum valve VI.
The natural gas steel cylinder is equipped with valve.
The quadrupole mass spectrometer is connected through high vacuum valve V with the high vacuum pipeline.
On the pipeline between the high vacuum pipeline and the ultrahigh vacuum pipeline successively be equipped with ultrahigh vacuum valve I,
Ultrahigh vacuum valve II, ultrahigh vacuum valve III.
The activated carbon cold-trap is connected through ultrahigh vacuum valve VII with the ultrahigh vacuum pipeline.
The titanium sponge stove is connected through ultrahigh vacuum valve VIII with the ultrahigh vacuum pipeline.
The utility model has the following advantages compared with prior art：
1st, natural gas is quickly introduced ultrahigh vacuum area by the utility model, during avoiding sampling analysis to the utmost
Air pollution.
2nd, the utility model natural gas is being not take up Sample introduction ultrahigh vacuum area by the U-shaped cold-trap of liquid nitrogen frozen
In the case of time, sulfur-containing compound, carbon dioxide and high-carbon hydrocarbon have been rapidly removed, sample is made to obtain preliminary purification, has kept super
High vacuum region it is pure.
3rd, the utility model titanium sponge stove is in ultrahigh vacuum region, and can be extracted into ultrahigh vacuum, makes Sample Purification on Single mistake
Journey Air Contamination can be neglected.
4th, the utility model40The mass spectra peak of Ar is up to more than 10V, when natural gas argon isotope ratio (40Ar/36Ar it is) higher
When, it improves36The signal-to-noise ratio of Ar, so that argon isotope ratio (40Ar/36Ar) measurement keeps preferable precision.
5th, the utility model can be detected in sample20The content of Ne, for estimating that trace air is mixed into argon isotope ratio
(40Ar/36Ar influence).
Description of the drawings
Specific embodiment of the present utility model is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 is the structure diagram of the utility model.
In figure：1-rare gas mass spectrograph；2-activated carbon cold-trap；3-titanium sponge stove；4-diagram vacuum gauge；5-four
Pole mass spectrograph；6-U-shaped cold-trap；7-natural gas steel cylinder；70-valve；8-high vacuum pipeline；81-high vacuum valve I；82-high
Vacuum valve II；83-high vacuum valve III；84-high vacuum valve IV；85-high vacuum valve V；9-high vacuum system；10-superelevation
Vacuum pipeline；101-ultrahigh vacuum valve I；102-ultrahigh vacuum valve II；103-ultrahigh vacuum valve III；104-ultrahigh vacuum valve
Ⅳ；105-ultrahigh vacuum valve V；106-ultrahigh vacuum valve VI；107-ultrahigh vacuum valve VII；108-ultrahigh vacuum valve VIII；
11-ultra-high vacuum system；12-pressure reducing valve.
Specific embodiment
As shown in Figure 1, a kind of high argon isotope ratio measuring device of natural gas, the device include rare gas mass spectrograph 1,
Activated carbon cold-trap 2, titanium sponge stove 3, quadrupole mass spectrometer 5, the U-shaped cold-trap 6 of liquid nitrogen frozen and natural gas steel cylinder 7.
Natural gas steel cylinder 7 is connected with high vacuum system 9 by high vacuum pipeline 8 through U-shaped cold-trap 6, quadrupole mass spectrometer 5；Gao Zhen
Blank pipe line 8 is connected with ultrahigh vacuum pipeline 10 by pipeline, and one end of the ultrahigh vacuum pipeline 10 is sequentially connected with titanium sponge stove 3, lives
Property charcoal cold-trap 2, rare gas mass spectrograph 1, the other end are connected with ultra-high vacuum system 11；Natural gas steel cylinder 7 and U-shaped cold-trap 6 it
Between high vacuum pipeline 8 on successively be equipped with pressure reducing valve 12, high vacuum valve I 81, high vacuum valve II 82, diagram vacuum gauge 4；It is U-shaped cold
High vacuum pipeline 8 between trap 6 and pipeline is equipped with high vacuum valve III 83；High-vacuum tube between high vacuum system 9 and pipeline
Line 8 is equipped with high vacuum valve IV 84；Ultrahigh vacuum pipeline 10 between ultra-high vacuum system 11 and pipeline is equipped with ultrahigh vacuum
Valve IV 104；Ultrahigh vacuum pipeline 10 between activated carbon cold-trap 2 and titanium sponge stove 3 is equipped with ultrahigh vacuum valve V 105；It is rare
Ultrahigh vacuum pipeline 10 between mass spectrometer 1 and activated carbon cold-trap 2 is equipped with ultrahigh vacuum valve VI 106.
Wherein：Natural gas steel cylinder 7 is equipped with valve 70.
Quadrupole mass spectrometer 5 is connected through high vacuum valve V 85 with high vacuum pipeline 8.
Ultrahigh vacuum valve I 101 is equipped on the pipeline between high vacuum pipeline 8 and ultrahigh vacuum pipeline 10 successively, is surpassed
High vacuum valve II 102, ultrahigh vacuum valve III 103.
Activated carbon cold-trap 2 is connected through ultrahigh vacuum valve VII 107 with ultrahigh vacuum pipeline 10.
Titanium sponge stove 3 is connected through ultrahigh vacuum valve VIII 108 with ultrahigh vacuum pipeline 10.
The measuring method of the high argon isotope ratio measuring device of the natural gas, comprises the following steps：
(1) high vacuum valve V 85 is closed, closes ultrahigh vacuum valve I 101 and ultrahigh vacuum valve VI 106, opens high vacuum valve I
81st, high vacuum valve II 82, high vacuum valve III 83, high vacuum valve IV 84 open ultrahigh vacuum valve II 102, ultrahigh vacuum valve III
103rd, ultrahigh vacuum valve IV 104, ultrahigh vacuum valve VIII 108, ultrahigh vacuum valve V 105, ultrahigh vacuum valve VII 107, vacuumize.Together
When U-shaped cold-trap 6 be warming up to room temperature, titanium sponge stove 3 is warming up to 700 DEG C, and activated carbon cold-trap 2 is warming up to 300K.
(2) ultrahigh vacuum valve VII 107 is closed, and activated carbon cold-trap 2 sets 70K, starts to cool down.
(3) 12 back pressure of pressure reducing valve is set to 0, with the U-shaped cold-trap 6 of liquid nitrogen frozen, closes high vacuum valve I 81, open natural gas steel
Valve 70 on bottle 7, waits 10s, closing valve 70；High vacuum valve II 82 is closed, opens high vacuum valve I 81, waits 10s, closes high vacuum valve I
81；High vacuum valve IV 84 is closed, opens high vacuum valve II 82, waits 10s, closes high vacuum valve II 82；Ultrahigh vacuum valve II 102 is closed, is opened super
High vacuum valve I 101 waits 10s, closes ultrahigh vacuum valve I 101；High vacuum valve V 85 is opened, quadrupole mass spectrometer 5 quickly measures argon gas
Content.
Natural gas is quickly introduced into ultrahigh vacuum area, avoids the air pollution during sampling analysis to the utmost.
By natural gas by the U-shaped cold-trap 6 of liquid nitrogen frozen, in the case where being not take up the time in Sample introduction ultrahigh vacuum area, quickly
Sulfur-containing compound, carbon dioxide and high-carbon hydrocarbon are eliminated, sample is made to obtain preliminary purification, keeps the pure of ultrahigh vacuum region.
(4) ultrahigh vacuum valve III 103, ultrahigh vacuum valve IV 104, ultrahigh vacuum valve VIII 108 are closed；According to the content of argon gas, lead to
Cross it is one or many open ultrahigh vacuum valve II 102, wait 5s, close ultrahigh vacuum valve II 102；Ultrahigh vacuum valve III 103 is opened, waits 5s,
The method for closing ultrahigh vacuum valve III 103 introduces gas into Sample Purification on Single area.
(5) ultrahigh vacuum valve VIII 108 is opened, and titanium sponge stove 3 is warming up to 800 DEG C, waits 10min, is opened simultaneously in waiting process
High vacuum valve IV 84.
Titanium sponge stove 3 can be extracted into ultrahigh vacuum in ultrahigh vacuum region, make sample purification process Air Contamination
It is negligible.
(6) ultrahigh vacuum valve VIII 108 is closed, opens ultrahigh vacuum valve VII 107, activated carbon cold-trap 2 waits again after reaching 70K
10min。
(7) ultrahigh vacuum valve VII 107 is closed, opens ultrahigh vacuum valve VI 106, waits 10s, closes ultrahigh vacuum valve VI 106, measurement20Ne
Content；Open simultaneously ultrahigh vacuum valve IV 104.
It detects in sample20The content of Ne, for estimate trace air be mixed into argon isotope ratio (40Ar/36Ar influence).
⑻20Ne measurements finish, and close ultrahigh vacuum valve IV 104, open ultrahigh vacuum valve VII 107；Activated carbon cold-trap 2 heats up, and reaches
10min is waited again after to 250K.
(9) ultrahigh vacuum valve VII 107 is closed, according to the content of step (3) argon gas, ultrahigh vacuum valve V 105 is closed if necessary, opens super
High vacuum valve VI 106 waits 10s, closes ultrahigh vacuum valve VI 106；Measure argon isotope ratio40Ar/36Ar.
The combination of step (3), (4) and (9), makes40The mass spectra peak of Ar is up to more than 10V, improves height40Ar/36Ar natural gases
's36The signal-to-noise ratio of Ar.
Embodiment illustrates by taking the argon isotope ratio test of Sichuan Basin Weiyuan gas field natural gas sample as an example.
The measuring method of the high argon isotope ratio measuring device of natural gas, comprises the following steps：
(1) high vacuum valve V 85 is closed, closes ultrahigh vacuum valve I 101 and ultrahigh vacuum valve VI 106, opens high vacuum valve I
81st, high vacuum valve II 82, high vacuum valve III 83, high vacuum valve IV 84 open ultrahigh vacuum valve II 102, ultrahigh vacuum valve III
103rd, ultrahigh vacuum valve IV 104, ultrahigh vacuum valve VIII 108, ultrahigh vacuum valve V 105, ultrahigh vacuum valve VII 107, vacuumize.Together
When U-shaped cold-trap 6 be warming up to room temperature, titanium sponge stove 3 is warming up to 700 DEG C, and activated carbon cold-trap 2 is warming up to 300K.Diagram vacuum gauge 4
Pressure is shown as 2 Pa, and the pressure of ultra-high vacuum system 11 is shown as 8 × 10-6Pa。
(2) ultrahigh vacuum valve VII 107 is closed, and activated carbon cold-trap 2 sets 70K, starts to cool down.
(3) 12 back pressure of pressure reducing valve is set to 0, with the U-shaped cold-trap 6 of liquid nitrogen frozen, closes high vacuum valve I 81, open natural gas steel
Valve 70 on bottle 7, waits 10s, closing valve 70；High vacuum valve II 82 is closed, opens high vacuum valve I 81, waits 10s, closes high vacuum valve I
81；High vacuum valve IV 84 is closed, opens high vacuum valve II 82, waits 10s, closes high vacuum valve II 82；Ultrahigh vacuum valve II 102 is closed, is opened super
High vacuum valve I 101 waits 10s, closes ultrahigh vacuum valve I 101；High vacuum valve V 85 is opened, quadrupole mass spectrometer 5 quickly measures argon gas
Volumn concentration is 0.06%.
(4) ultrahigh vacuum valve III 103, ultrahigh vacuum valve IV 104, ultrahigh vacuum valve VIII 108 are closed.According to the content of argon gas, open
Ultrahigh vacuum valve II 102 waits 5s, closes ultrahigh vacuum valve II 102；Ultrahigh vacuum valve III 103 is opened, waits 5s, closes ultrahigh vacuum valve III
103, circulation primary introduces gas into Sample Purification on Single area.
(5) ultrahigh vacuum valve VIII 108 is opened, and titanium sponge stove 3 is warming up to 800 DEG C, waits 10min, is opened simultaneously in waiting process
High vacuum valve IV 84.
(6) ultrahigh vacuum valve VIII 108 is closed, opens ultrahigh vacuum valve VII 107, activated carbon cold-trap 2 waits again after reaching 70K
10min。
(7) ultrahigh vacuum valve VII 107 is closed, opens ultrahigh vacuum valve VI 106, waits 10s, closes ultrahigh vacuum valve VI 106.Measurement20Ne
Content, do not detect20Ne.Open simultaneously ultrahigh vacuum valve IV 104.
⑻20Ne measurements finish, and close ultrahigh vacuum valve IV 104, open ultrahigh vacuum valve VII 107；Activated carbon cold-trap 2 heats up, and reaches
10min is waited again after to 250K.
(9) ultrahigh vacuum valve VII 107 is closed, ultrahigh vacuum valve V 105 is closed, opens ultrahigh vacuum valve VI 106, waits 10s, closes superelevation
Vacuum valve VI 106.Measurement40Ar mass spectrum peak heights show value is 41.0109V,36Ar mass spectrum peak heights show value is 2.51667mV,
After standard specimen corrects, the argon isotope ratio of the natural gas (40Ar/36Ar it is) 16052.
Explanation：According to step (3) argon gas content judge, (4) (9) circulation primary, step should close ultrahigh vacuum valve VII to step
107 and ultrahigh vacuum valve V 105, it could keep40Ar mass spectrums peak height is in rare gas mass spectrometric range (mass spectrum peak height<50V)
Within.
Data show this area's natural gas in the whole country argon isotope ratio (40Ar/36Ar) highest, the data of announcement
Peak be 9255.This example measurement argon isotope ratio (40Ar/36Ar it is) 16052, the appearance of new data will be helpful to section
Scholar improves and is based on40Ar/36The natural gas of Ar estimates formula into hydrocarbon Oil-gas pool forming age.
(7) step does not detect20Ne illustrates, from sampling in analysis whole process, do not have trace air in natural gas
It is mixed into, argon isotope ratio (40Ar/36Ar) it is not affected.
Claims (6)
1. a kind of high argon isotope ratio measuring device of natural gas, it is characterised in that：The device includes rare gas mass spectrograph
（1）, activated carbon cold-trap（2）, titanium sponge stove（3）, quadrupole mass spectrometer（5）, liquid nitrogen frozen U-shaped cold-trap（6）And natural gas steel cylinder
（7）；The natural gas steel cylinder（7）Pass through high vacuum pipeline（8）Through the U-shaped cold-trap（6）, the quadrupole mass spectrometer（5）It is connected with
High vacuum system（9）；The high vacuum pipeline（8）Ultrahigh vacuum pipeline is connected with by pipeline（10）, the ultrahigh vacuum pipeline
（10）One end be sequentially connected with the titanium sponge stove（3）, the activated carbon cold-trap（2）, the rare gas mass spectrograph（1）,
The other end is connected with ultra-high vacuum system（11）；The natural gas steel cylinder（7）With the U-shaped cold-trap（6）Between the high vacuum
Pipeline（8）On successively be equipped with pressure reducing valve（12）, high vacuum valve I（81）, high vacuum valve II（82）, diagram vacuum gauge（4）；The U
Type cold-trap（6）The high vacuum pipeline between the pipeline（8）It is equipped with high vacuum valve III（83）；The high vacuum system
（9）The high vacuum pipeline between the pipeline（8）It is equipped with high vacuum valve IV（84）；The ultra-high vacuum system（11）
The ultrahigh vacuum pipeline between the pipeline（10）It is equipped with ultrahigh vacuum valve IV（104）；The activated carbon cold-trap（2）
With the titanium sponge stove（3）Between the ultrahigh vacuum pipeline（10）It is equipped with ultrahigh vacuum valve V（105）；The rare gas
Constitution spectrometer（1）With the activated carbon cold-trap（2）Between the ultrahigh vacuum pipeline（10）It is equipped with ultrahigh vacuum valve VI
（106）.
2. a kind of high argon isotope ratio measuring device of natural gas as described in claim 1, it is characterised in that：The natural gas
Steel cylinder（7）It is equipped with valve（70）.
3. a kind of high argon isotope ratio measuring device of natural gas as described in claim 1, it is characterised in that：The quadrupole matter
Spectrometer（5）Through high vacuum valve V（85）With the high vacuum pipeline（8）It is connected.
4. a kind of high argon isotope ratio measuring device of natural gas as described in claim 1, it is characterised in that：The high vacuum
Pipeline（8）With the ultrahigh vacuum pipeline（10）Between the pipeline on successively be equipped with ultrahigh vacuum valve I（101）, superelevation it is true
Empty valve II（102）, ultrahigh vacuum valve III（103）.
5. a kind of high argon isotope ratio measuring device of natural gas as described in claim 1, it is characterised in that：The activated carbon
Cold-trap（2）Through ultrahigh vacuum valve VII（107）With the ultrahigh vacuum pipeline（10）It is connected.
6. a kind of high argon isotope ratio measuring device of natural gas as described in claim 1, it is characterised in that：The titanium sponge
Stove（3）Through ultrahigh vacuum valve VIII（108）With the ultrahigh vacuum pipeline（10）It is connected.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201721601676.1U CN207439998U (en) | 2017-11-27 | 2017-11-27 | A kind of high argon isotope ratio measuring device of natural gas |
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| CN201721601676.1U CN207439998U (en) | 2017-11-27 | 2017-11-27 | A kind of high argon isotope ratio measuring device of natural gas |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110609077A (en) * | 2018-06-14 | 2019-12-24 | 中国科学院地质与地球物理研究所兰州油气资源研究中心 | Natural gas neon isotope composition measuring device and method |
| CN114397354A (en) * | 2021-12-31 | 2022-04-26 | 四川红华实业有限公司 | Device and method for separating standard substance of gas uranium isotope abundance |
-
2017
- 2017-11-27 CN CN201721601676.1U patent/CN207439998U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110609077A (en) * | 2018-06-14 | 2019-12-24 | 中国科学院地质与地球物理研究所兰州油气资源研究中心 | Natural gas neon isotope composition measuring device and method |
| CN110609077B (en) * | 2018-06-14 | 2023-08-08 | 中国科学院西北生态环境资源研究院 | Natural gas neon isotope composition measuring device and method |
| CN114397354A (en) * | 2021-12-31 | 2022-04-26 | 四川红华实业有限公司 | Device and method for separating standard substance of gas uranium isotope abundance |
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Effective date of registration: 20200825 Address after: 730000 No.318, Donggang West Road, Chengguan District, Lanzhou City, Gansu Province Patentee after: NORTHWEST INSTITUTE OF ECO-ENVIRONMENT AND RESOURCES, CAS Address before: Chengguan District of Gansu city of Lanzhou province Donggang West Road 730000 No. 382 Patentee before: Lanzhou Center for Oil and Gas Resources, Institute of Geology and Geophysics, CAS |