CN205538816U - Aerochemistry and noble gas isotopic content while measuring device - Google Patents

Aerochemistry and noble gas isotopic content while measuring device Download PDF

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Publication number
CN205538816U
CN205538816U CN201620352296.8U CN201620352296U CN205538816U CN 205538816 U CN205538816 U CN 205538816U CN 201620352296 U CN201620352296 U CN 201620352296U CN 205538816 U CN205538816 U CN 205538816U
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vacuum pipeline
vacuum valve
rare
aerochemistry
ultrahigh vacuum
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CN201620352296.8U
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李立武
曹春辉
贺坚
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Northwest Institute of Eco Environment and Resources of CAS
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Lanzhou Center for Oil and Gas Resources of Institute of Geology and Geophysics of CAS
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Abstract

The utility model relates to an aerochemistry and noble gas isotopic content while measuring device, the device include noble gas mass spectrograph system, quadrupole mass spectrometer, are equipped with high vacuum system, cold -trap and the titanium sponge stove of being responsible for the line. Be responsible for the line link respectively has vacuum pipeline I, vacuum pipeline II, vacuum pipeline III, vacuum pipeline I terminal with noble gas mass spectrograph system links to each other, the end of vacuum pipeline II links respectively has vacuum pipeline IV, vacuum pipeline V, vacuum pipeline IV terminal with quadrupole mass spectrometer links to each other, vacuum pipeline V terminal with the titanium sponge stove links to each other, III warps of vacuum pipeline the cold -trap even has the introduction port. The utility model discloses an inferiorly advance appearance, measuring result is comprehensive, has not only rectified the air of sneaking into in gas sampling and the transportation and has disturbed, has rectified the interference that instrument analysis in -process entrained air was transferred to to the sample moreover.

Description

Aerochemistry forms simultaneous measuring apparatus with rare and refractory metals
Technical field
This utility model relates to gas geochemistry technical field, particularly relates to aerochemistry and forms simultaneous measuring apparatus with rare and refractory metals.
Background technology
Gas geochemistry research relates to numerous field of earth sciences: the effect of gas in gas transmission in the material circulation of the whole world, volcanic earthquake activity, oil-gas resource, earth interior gas and the interaction of rock, mantle degassing, the geological reservoir of gas, etc..Main research: gaseous sample (such as air, natural gas etc.), the gas dissolved in fluid sample (such as subsoil water, thermal water, sea water etc.), the gas deposited of composing in solid sample (such as shale, natural gas hydrocarbons source rock or reservoir, minerogenic rock etc.), these gas (H2、N2、O2、CO、CO2、H2S、CH4、C2H2n+2, He, Ne, Ar, Kr and Xe etc.) chemical composition and stable isotopic composition of authigenic, to inquire into the origin cause of formation of these gases, source, Geochemical Characteristics, coupling coexistence mechanism, and the Geodynamic setting that reflected and evolution.
Wherein the measurement of aerochemistry composition and rare gas (He, Ne, Ar, Kr and Xe) stable isotope composition is the important means of gas geochemistry research.In conventional research work, the measurement of aerochemistry composition and rare gas stable isotope composition is carried out separately, i.e. need two samples, the chemical composition of a sample is measured with gas chromatograph or gas component mass spectrograph, the stable isotope composition of the rare gas of another sample is measured with rare gas mass spectrograph, sample size requires more, the measurement cycle is longer, the situation causing air pollution during sample introduction is inconsistent, and the measurement result of aerochemistry composition cannot be used for He-Ar isotope air interference correction during measuring.
Some unit quadrupole mass spectrometer and rare gas mass spectrograph measuring samples simultaneously, but its quadrupole mass spectrometer only measures the chemical composition of rare gas after purification, measurement result is not comprehensive, can not carry out He-Ar isotope air interference correction during measuring.
Utility model content
Technical problem to be solved in the utility model is to provide a kind of single injected sampling, the comprehensive aerochemistry of measurement result forms simultaneous measuring apparatus with rare and refractory metals.
For solving the problems referred to above, aerochemistry described in the utility model forms simultaneous measuring apparatus with rare and refractory metals, it is characterised in that: this device includes rare gas spectrometer system, quadrupole mass spectrometer, is provided with the high vacuum system of Trunk Line, cold-trap and titanium sponge stove;Described Trunk Line is connected with vacuum pipeline I, vacuum pipeline II, vacuum pipeline III respectively;The end of described vacuum pipeline I is connected with described rare gas spectrometer system;The end of described vacuum pipeline II is connected with vacuum pipeline IV, vacuum pipeline V respectively;The end of described vacuum pipeline IV is connected with described quadrupole mass spectrometer;The end of described vacuum pipeline V is connected with described titanium sponge stove;Described vacuum pipeline III is connected with injection port through described cold-trap.
Described rare gas spectrometer system purification separation device in rare gas.
Described quadrupole mass spectrometer uses the work of micropore input mode.
Described Trunk Line is provided with ultrahigh vacuum valve IV.
Ultrahigh vacuum valve VI, ultrahigh vacuum valve VII it is sequentially provided with on described vacuum pipeline I.
Described vacuum pipeline II is provided with ultrahigh vacuum valve V.
Described vacuum pipeline IV is provided with ultrahigh vacuum valve Ⅸ.
Diagram vacuum gauge, ultrahigh vacuum valve VIII it is respectively equipped with on described vacuum pipeline V.
Ultrahigh vacuum valve III, ultrahigh vacuum valve II, ultrahigh vacuum valve I it is sequentially provided with on described vacuum pipeline III.
This utility model compared with prior art has the advantage that
1, this utility model forms measurement result according to rare_gas chemistry to be measured, suitable gas flow segmentation is introduced rare gas spectrometer system, it is purified, divides the analysis of variance, to avoid gas flow not enough or too much, in the range of making rare gas mass spectrograph be operated in optimum linear.
2, this utility model single injected sampling, measure aerochemistry composition simultaneously and rare and refractory metals forms, the test result of aerochemistry composition is measured for follow-up rare gas and is provided the reference of content, and the air interference correction for follow-up rare gas measurement result provides foundation.
3, this utility model corrects the air interference of rare gas measurement result according to the chemical composition of gaseous sample, not only corrects the air interference being mixed in gas sampling and transportation, and corrects the interference being mixed into air during Instrumental Analysis transferred to by sample.
Accompanying drawing explanation
Below in conjunction with the accompanying drawings detailed description of the invention of the present utility model is described in further detail.
Fig. 1 is structural representation of the present utility model.
In figure: 1 rare gas spectrometer system;2 quadrupole mass spectrometer;3 high vacuum systems;31 ultrahigh vacuum valves I;32 ultrahigh vacuum valves II;33 ultrahigh vacuum valves III;34 ultrahigh vacuum valves IV;35 ultrahigh vacuum valves V;36 ultrahigh vacuum valves VI;37 ultrahigh vacuum valves VII;38 ultrahigh vacuum valves VIII;39 ultrahigh vacuum valves Ⅸ;4 cold-traps;5 titanium sponge stoves;6 injection ports;7 diagram vacuum gauges.
Detailed description of the invention
As it is shown in figure 1, aerochemistry forms simultaneous measuring apparatus with rare and refractory metals, this device includes rare gas spectrometer system 1, quadrupole mass spectrometer 2, is provided with the high vacuum system 3 of Trunk Line, cold-trap 4 and titanium sponge stove 5.
Trunk Line is connected with vacuum pipeline I, vacuum pipeline II, vacuum pipeline III respectively;The end of vacuum pipeline I is connected with rare gas spectrometer system 1;The end of vacuum pipeline II is connected with vacuum pipeline IV, vacuum pipeline V respectively;The end of vacuum pipeline IV is connected with quadrupole mass spectrometer 2;The end of vacuum pipeline V is connected with titanium sponge stove 5;Vacuum pipeline III is connected with injection port 6 through cold-trap 4.
Wherein:
Rare gas spectrometer system 1 purification separation device in rare gas.
Quadrupole mass spectrometer 2 uses micropore input mode to work.
Trunk Line is provided with ultrahigh vacuum valve IV 34.
Ultrahigh vacuum valve VI 36, ultrahigh vacuum valve VII 37 it is sequentially provided with on vacuum pipeline I.
Vacuum pipeline II is provided with ultrahigh vacuum valve V 35.
Vacuum pipeline IV is provided with ultrahigh vacuum valve Ⅸ 39.
Diagram vacuum gauge 7, ultrahigh vacuum valve VIII 38 it is respectively equipped with on vacuum pipeline V.
Ultrahigh vacuum valve III 33, ultrahigh vacuum valve II 32, ultrahigh vacuum valve I 31 it is sequentially provided with on vacuum pipeline III.
This aerochemistry forms, with rare and refractory metals, the method simultaneously measured, and comprises the following steps:
(1) close ultrahigh vacuum valve I 31, ultrahigh vacuum valve VII 37, ultrahigh vacuum valve Ⅸ 39, open ultrahigh vacuum valve II 32, ultrahigh vacuum valve III 33, ultrahigh vacuum valve IV 34, ultrahigh vacuum valve V 35, ultrahigh vacuum valve VI 36, ultrahigh vacuum valve VIII 38, to vacuum pipeline evacuation, the background pressure of recording sheet vacuometer 7;
(2) connecting gaseous sample container to be measured at injection port 6, gaseous sample the most to be measured does not connects with injection port 6, opens ultrahigh vacuum valve I 31, evacuation;
(3) closing ultrahigh vacuum valve II 32, gaseous sample to be measured connects with injection port 6, is introduced by gaseous sample to be measured, closes ultrahigh vacuum valve I 31;
(4) close ultrahigh vacuum valve IV 34, ultrahigh vacuum valve VI 36, ultrahigh vacuum valve VIII 38, open ultrahigh vacuum valve II 32, record the pressure of now diagram vacuum gauge 7;
(5) open ultrahigh vacuum valve Ⅸ 39, quadrupole mass spectrometer 2 measure the chemical composition of gaseous sample to be measured;
(6) measure complete, cold-trap 4 is adjusted to-196 DEG C, then measured the chemical composition of gaseous sample to be measured by quadrupole mass spectrometer 2, then, close ultrahigh vacuum valve Ⅸ 39;
If measure is Xe isotopics, then this step changes into: close ultrahigh vacuum valve Ⅸ 39;
(7) close ultrahigh vacuum valve III 33, open ultrahigh vacuum valve VIII 38, titanium sponge stove 5 temperature is risen to 800 DEG C, keep 10min;
(8) according to the chemical composition of rare gas to be measured, calculate the gas flow needing to enter rare gas spectrometer system 1, by being repeatedly opened ultrahigh vacuum valve VI 36, close ultrahigh vacuum valve VI 36, open ultrahigh vacuum valve VII 37, close ultrahigh vacuum valve VII 37;Or close ultrahigh vacuum valve V 35, open ultrahigh vacuum valve VI 36 and ultrahigh vacuum valve VII 37 simultaneously;Or closing ultrahigh vacuum valve VIII 38, open ultrahigh vacuum valve VI 36 and ultrahigh vacuum valve VII 37, desired gas amount is introduced rare gas spectrometer system 1 by segmentation, carries out rare and refractory metals composition analysis simultaneously;
(9) the air interference of rare gas measurement result is corrected according to the chemical composition of gaseous sample.
Embodiment 1 Illustrate as a example by the Ar isotopics of steel cylinder natural gas are tested,OnePlant aerochemistry and rare and refractory metals composition measuring method simultaneously, comprise the following steps
(1) close ultrahigh vacuum valve I 31, ultrahigh vacuum valve VII 37, ultrahigh vacuum valve Ⅸ 39, open ultrahigh vacuum valve II 32, ultrahigh vacuum valve III 33, ultrahigh vacuum valve IV 34, ultrahigh vacuum valve V 35, ultrahigh vacuum valve VI 36, ultrahigh vacuum valve VIII 38, to vacuum pipeline evacuation, the background pressure P of recording sheet vacuometer 70
(2) at injection port 6, connect testing sample, as natural gas steel cylinder connects the extraordinary air relief valve of band air-tightness, fine vacuum connects air relief valve outlet and injection port 6, now natural gas steel cylinder valve closing, air relief valve back pressure is adjusted to less than 1atm, this pressure is the pressure that ultrahigh vacuum valve can bear, and opens ultrahigh vacuum valve I 31, evacuation.
(3) after vacuum reaches fine vacuum, close ultrahigh vacuum valve II 32, open natural gas steel cylinder valve, natural gas sample to be measured is introduced, close ultrahigh vacuum valve I 31.
(4) close ultrahigh vacuum valve IV 34, ultrahigh vacuum valve VI 36, ultrahigh vacuum valve VIII 38, open ultrahigh vacuum valve II 32, record the pressure P of now diagram vacuum gauge 71
(5) open ultrahigh vacuum valve Ⅸ 39, quadrupole mass spectrometer 2 measure the chemical composition of natural gas sample to be measured.
(6) measure complete, cold-trap 4 is adjusted to-196 DEG C, to remove CO2And C3H8Above higher carbon number hydrocarbon class, then the chemical composition of testing sample is measured by quadrupole mass spectrometer 2, then, close ultrahigh vacuum valve Ⅸ 39.
Bound gas pressure data (P1-P0), calculate H2、He、CH4、N2、C2H6、O2, Ar and CO2Volumn concentration Deng composition.
Illustrate: when again measuring by quadrupole mass spectrometer 2, O2Do not affected by higher molecular weight gas with the mass spectrum of Ar.
(7) close ultrahigh vacuum valve III 33, open ultrahigh vacuum valve VIII 38, titanium sponge stove 5 temperature is risen to 800 DEG C, keep 10min, tentatively remove H2、CH4、N2And O2Isoreactivity composition.
(8) according to the volumn concentration of the surveyed Ar of step, calculate the gas flow needing to enter rare gas spectrometer system 1, the generally content of Ar is higher, by opening ultrahigh vacuum valve VI 36, close ultrahigh vacuum valve VI 36, open ultrahigh vacuum valve VII 37, close ultrahigh vacuum valve VII 37, the gas of a small amount of volume is introduced rare gas spectrometer system 1, carries out rare gas Ar isotopics and analyze.
(9) with the surveyed O of step2With the air interference that the volumn concentration of Ar corrects Ar isotope measure result.

Claims (9)

1. aerochemistry forms simultaneous measuring apparatus with rare and refractory metals, it is characterised in that: this device includes rare gas spectrometer system (1), quadrupole mass spectrometer (2), is provided with the high vacuum system (3) of Trunk Line, cold-trap (4) and titanium sponge stove (5);Described Trunk Line is connected with vacuum pipeline I, vacuum pipeline II, vacuum pipeline III respectively;The end of described vacuum pipeline I is connected with described rare gas spectrometer system (1);The end of described vacuum pipeline II is connected with vacuum pipeline IV, vacuum pipeline V respectively;The end of described vacuum pipeline IV is connected with described quadrupole mass spectrometer (2);The end of described vacuum pipeline V is connected with described titanium sponge stove (5);Described vacuum pipeline III is connected with injection port (6) through described cold-trap (4).
2. aerochemistry as claimed in claim 1 forms simultaneous measuring apparatus with rare and refractory metals, it is characterised in that: described rare gas spectrometer system (1) purification separation device in rare gas.
3. aerochemistry as claimed in claim 1 forms simultaneous measuring apparatus with rare and refractory metals, it is characterised in that: described quadrupole mass spectrometer (2) uses the work of micropore input mode.
4. aerochemistry as claimed in claim 1 forms simultaneous measuring apparatus with rare and refractory metals, it is characterised in that: described Trunk Line is provided with ultrahigh vacuum valve IV (34).
5. aerochemistry as claimed in claim 1 forms simultaneous measuring apparatus with rare and refractory metals, it is characterised in that: it is sequentially provided with ultrahigh vacuum valve VI (36), ultrahigh vacuum valve VII (37) on described vacuum pipeline I.
6. aerochemistry as claimed in claim 1 forms simultaneous measuring apparatus with rare and refractory metals, it is characterised in that: described vacuum pipeline II is provided with ultrahigh vacuum valve V (35).
7. aerochemistry as claimed in claim 1 forms simultaneous measuring apparatus with rare and refractory metals, it is characterised in that: described vacuum pipeline IV is provided with ultrahigh vacuum valve Ⅸ (39).
8. aerochemistry as claimed in claim 1 forms simultaneous measuring apparatus with rare and refractory metals, it is characterised in that: it is respectively equipped with diagram vacuum gauge (7), ultrahigh vacuum valve VIII (38) on described vacuum pipeline V.
9. aerochemistry as claimed in claim 1 forms simultaneous measuring apparatus with rare and refractory metals, it is characterised in that: it is sequentially provided with ultrahigh vacuum valve III (33), ultrahigh vacuum valve II (32), ultrahigh vacuum valve I (31) on described vacuum pipeline III.
CN201620352296.8U 2016-04-25 2016-04-25 Aerochemistry and noble gas isotopic content while measuring device Active CN205538816U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106680359A (en) * 2017-01-16 2017-05-17 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 Online analysis method and system of components of shale residual gas and rare gas
CN107045016A (en) * 2017-02-05 2017-08-15 中国科学院地质与地球物理研究所 A kind of objects outside Earth Atmospheric components and radioisotope gauge and measuring method

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106680359A (en) * 2017-01-16 2017-05-17 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 Online analysis method and system of components of shale residual gas and rare gas
CN107045016A (en) * 2017-02-05 2017-08-15 中国科学院地质与地球物理研究所 A kind of objects outside Earth Atmospheric components and radioisotope gauge and measuring method
CN107045016B (en) * 2017-02-05 2018-09-14 中国科学院地质与地球物理研究所 A kind of objects outside Earth Atmospheric components and radioisotope gauge and measurement method

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C14 Grant of patent or utility model
GR01 Patent grant
TR01 Transfer of patent right

Effective date of registration: 20200821

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

TR01 Transfer of patent right