CN103048412A - Online analysis pretreatment device for trace hydrogen isotopes in natural gas - Google Patents
Online analysis pretreatment device for trace hydrogen isotopes in natural gas Download PDFInfo
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- CN103048412A CN103048412A CN2011103150844A CN201110315084A CN103048412A CN 103048412 A CN103048412 A CN 103048412A CN 2011103150844 A CN2011103150844 A CN 2011103150844A CN 201110315084 A CN201110315084 A CN 201110315084A CN 103048412 A CN103048412 A CN 103048412A
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Abstract
The invention discloses an online analysis pretreatment device for trace hydrogen isotopes in natural gas. The device comprises a sample chamber, a six-way valve, an absorption cold trap, a preenrichment cold trap and an enrichment cold trap, wherein the sample chamber is connected with the absorption cold trap, the absorption cold trap is connected with the six-way valve, two ends of the preenrichment cold trap are respectively connected with the six-way valve, one end of the enrichment cold trap is connected with the six-way valve, and the other end of the enrichment cold trap is connected with a chromatographic column, and the six-way valve is respectively connected with a helium pressure regulating valve B and a gas circuit release valve D; an inlet and an outlet of the sample chamber are respectively provided with a gas circuit release valve; and a gas circuit release valve is arranged between the absorption cold trap and the six-way valve. The device disclosed by the invention can be used for realizing the online enrichment of a trace hydrogen component in a natural gas sample, separating the trace hydrogen component from other gas components so as to detect the hydrogen isotopes.
Description
Technical field
The present invention relates to the analytical chemistry field, say further, relate to the pretreating device of microscratch amount hydrogen isotope on-line analysis in a kind of rock gas.
Background technology
Rock gas isotope analysis technical elements, domestic and international many advanced laboratory technique strength concentrate on the test of hydrocarbon gas isotope, are used for the rock gas tracer study.Mainly be by high-temp combustion interface or Pintsch process interface that isotope mass spectrometer and chromatograph is online, analyze CH in the rock gas
4Deng the hydrocarbon isotopics of hydrocarbon gas.And to the non-hydrocarbon gas H of microscratch amount in the gas reservoir
2Relate to less, and microscratch amount gas composition H in the gas reservoir
2As the important component part of gas reservoir, must record geological information relevant in the process of natural gas pool formation.But it is subjected to the restriction of microscratch amount gas composition isotope analysis technical bottleneck, and the research work in this field almost is in blank both at home and abroad at present.
Document " on-line analysis of Irish touchstone pyrolysis hydrogen isotope " (author: " test of rock ore deposit " 4 phases of 25 volumes in 2006 such as Wang Guang, Li Liwu: the 311-314 page or leaf) disclose: utilize the degassed free carbon of rock fever/hydrogen isotopic composition analytical equipment, by the method for high temperature pyrolysis, step heating, pyrolysis H in the alkaline basalt total rock fluid components
2Hydrogen isotope has carried out mass spectrometric analysis for isotope.Said apparatus comprises solid particles of rock sample heating tank, and six-way valve, injection annulus (the inner activated charcoal of filling), absorption tube, surge flask (external vacuum pump), stop valve that NaOH is housed form with relevant pipeline.Principle of work: pyrolysis produces a large amount of CO in the alkaline basalt total rock fluid components
2, H
2, CH
4Deng gas composition, CO
2Absorbed by alkali, after the relative enrichment of other components, be adsorbed in the injection annulus.Then heat injection annulus, H
2, CH
4Discharge Deng component, bring chromatogram into by carrier gas He, each component is carried out chromatographic resolution, isotope mass spectrometer is analyzed its isotopics.
(author: Shangguan's will hat, Huo Weiguo " Science Bulletin " 15 phases of 46 volumes calendar year 2001: the 314-318 page or leaf) disclose: analytic target is that geothermal spring discharges gas, H to document " δ D value and the origin cause of formation thereof of Tengchong Rehai geothermal area effusion H2 "
2Component has high level, and directly by syringe sampling, after the chromatographic resolution, isotope mass spectrometer records its H
2Isotopics.
Chinese patent (application number: 200710138976 denominations of invention: a kind of hydrogen, the method that hydrogen deuteride and deuterium hydrogen isotope quantitatively detect) disclose: this invention relates to a kind of hydrogen, the method that hydrogen deuteride and deuterium hydrogen isotope quantitatively detect, the method is as carrier gas with neon, gas chromatograph has adopted the two warm systems of twin columns, by syringe or gas sampling valve injection, the gas of sample gas after gas chromatographic column separates produces electric signal by detecting device, after prime amplifier amplifies signal, by chromatographic work station record chromatographic peak hydrogen, hydrogen deuteride, the peak area of deuterium gas adopts volume correction factor normalization method or external standard method hydrogen, hydrogen deuteride and deuterium gas content.
Chinese patent (application number: 200510027030 denominations of invention: the analytical equipment of a kind of O2 of containing, N2 and H2 mixed gas) disclose: a kind of analytical equipment that mixes gas that contains.Mainly solve in the past H
2, O
2, N
2Need at least two chromatograms to analyze in the analytical approach, and complicated operation, data are processed loaded down with trivial details, the technical matterss such as error is larger, the present invention is by adopting a gas transfer valve to realize that different carrier gas switch, so that do carrier gas with nitrogen or argon gas when measuring hydrogen, does carrier gas with hydrogen or helium when measuring remaining gas, and the detection of all components is all carried out at single thermal conductivity detector (TCD), thereby realizing that the separate unit analytical equipment is finished contains H
2, O
2, N
2The analysis of mixed gas.
The prior art Main Problems is: (1) existing H
2The enriching apparatus off-line carries out pre-treatment to testing sample, and the operation of its processing procedure takes a lot of work, time-consuming; Two processes of pretreatment process and isotope analysis disconnect mutually simultaneously, bring inconvenience to test job.(2) traditional chromatogram split sampling pattern can cause the isotope fractionation of H2, can't satisfy the analysis of low hydrogen concentration natural gas sample simultaneously.Key issue is how to make up a cover without the split sampling device at present, and this device can be realized the enrichment of microscratch amount hydrogen simultaneously, and separates with other gas composition.
Summary of the invention
For solving problems of the prior art, the invention provides the pretreating device of microscratch amount hydrogen isotope on-line analysis in a kind of rock gas.Can realize microscratch amount hydrogen component on-line preconcentration in the rock gas sample, and separate with other gas compositions, detect its isotope.
The pretreating device that the purpose of this invention is to provide microscratch amount hydrogen isotope on-line analysis in a kind of rock gas.
Described device comprises sample chamber 103, six-way valve 109, absorption cold-trap 105, preenrichment cold-trap 107 and enrichment cold-trap 111,
Described sample chamber 103 connects absorption cold-trap 105, and absorption cold-trap 105 connects six-way valve 109, and preenrichment cold-trap 107 two ends connect respectively six-way valve 109, and enrichment cold-trap 111 1 ends connect six-way valve 109, and the other end connects chromatographic column,
Described six-way valve 109 connects respectively helium pressure variable valve B108 and gas circuit atmospheric valve D110;
When six-way valve 109 places the sampling state, absorption cold- trap 105 and 107 series connection of preenrichment cold-trap, preenrichment cold-trap 107 and enrichment cold-trap 111 disconnect;
Put 109 in sampling during state when six-way valve, absorption cold-trap 105 and preenrichment cold-trap 107 disconnect, preenrichment cold- trap 107 and 111 series connection of enrichment cold-trap;
103 imports of described sample chamber and outlet are provided with the gas circuit atmospheric valve;
Be provided with gas circuit atmospheric valve C106 between described absorption cold-trap 105 and the six-way valve 109.
Described absorption cold-trap 105 adopts the stainless steel pipeline to fill 40～60 order 5A molecular sieve and 100～120 order divinyl benzene polymers molecular sieve, and the content of wherein said 5A molecular sieve is 20%～80wt%;
Described preenrichment cold-trap 107 adopts the stainless steel pipeline to fill 40～100 order 5A molecular sieve;
Described enrichment cold-trap 111 adopts the stainless steel pipeline to fill 80～100 order 5A molecular sieve.
The temperature of described absorption cold-trap 105 is 159 ± 15K; The stainless steel pipeline
The temperature of described preenrichment cold-trap 107 is 77 ± 10K; The stainless steel pipeline
The temperature of described enrichment cold-trap 111 is 77 ± 10K, the stainless steel pipeline
In the practical operation,
A sample thief gas is in the sample chamber, and the access continuous-flow system, opens valve 102,104,106 usefulness He gas are taken the pipeline Air out of;
B places the sampling state with six-way valve 109, and shut-off valve 102,104,106 is opened the sample chamber valve simultaneously.Carrier gas He brings sample gas into absorption cold-trap 105 (liquid nitrogen+alcohol 159K), and hydro carbons and part inorganic gas are adsorbed, and H
2Pass through smoothly, and in preenrichment cold-trap 107 (liquid nitrogen 77K) enrichment, carrier gas He discharges through drain 110;
C is converted to the sample presentation state with six-way valve 109, to adsorb cold-trap 105 this moment and from (liquid nitrogen+alcohol) cryostat, mention hydro carbons and the part inorganic gas that the heating chamber removal of putting into 150 ℃ is adsorbed, and preenrichment cold-trap 107 is mentioned from the liquid nitrogen cryostat, at room temperature discharges H
2, and brought into enrichment cold-trap 111 (liquid nitrogen 77K) by carrier gas, enriching and purifying is 2 minutes again
D six-way valve 109 returns to the sampling state, and enrichment cold-trap 111 placed under the room temperature discharges H
2, and brought into GC-IRMS system measurement H by carrier gas
2Isotopic ratio.
Above process is set according to time series successively by the mass spectrum workstation, and fully automatically control, and be complementary with the Spectrometry process, thus the consistance of assurance analytic process.
Device of the present invention be a kind of for the on-line analysis of rock gas microscratch amount H2 isotope without the split sampling device, be to use for reference the pneumatic valve sampling technique and adsorbent of molecular sieve is finished the performance design of each gas composition selective adsorption under condition of different temperatures.Described device is used for the sample introduction of chromatogram-gas isotope mass spectrograph analytic system.Under continuous flow mode, utilize molecular sieve in the absorption property difference of different temperature points, the H2 of microscratch amount in the rock gas sample is separated with hydro carbons and other gas compositions, H2 is enriched in the 5A molecular sieve liquid nitrogen cold trap simultaneously, cold-trap placed H2 discharges under the room temperature, brought into chromatogram-isotope mass spectrometer analytic system by carrier gas He, measure its isotope.
The content that innovation of the present invention is to take into full account H2 in the rock gas sample is low, and its isotope test is subject to the characteristics of isotope fractionation impact and the needs of continuous stream on-line analysis, utilize the difference of hydrogen and other gas composition physicochemical property, development and design for the pretreating device of microscratch amount H2 isotope on-line analysis in the rock gas.
The invention effect:
1 utilize this device can realize the rock gas sample without split sampling; And the H2 component of microscratch amount wherein carried out enrichment, separate with other gas composition in the sample.
2 devices can be online for the on-line analysis of hydrogen isotope with gas chromatography mass spectrometric analysis for isotope system, and can automatically control.Can satisfy density of hydrogen is 5 * 10
-6(V/V) analysis of rock gas sample has higher analysis precision and accuracy.
3 utilize said apparatus to measure the H2 isotope, and analytical cycle is 20 minutes, and realizes the automatic control of sample analysis flow process, has avoided numerous and diverse pretreatment process, has greatly improved analysis efficiency.
Description of drawings
Fig. 1 pretreating device sampling of the present invention view
Fig. 2 pretreating device sample presentation of the present invention view
The analysis of spectra of Fig. 3 embodiment
Description of drawings:
101-helium pressure variable valve A 102-gas circuit atmospheric valve A 103-sample chamber
104-gas circuit atmospheric valve B 105-absorption cold-trap 106-gas circuit atmospheric valve C
107-preenrichment cold-trap 108-helium pressure variable valve B 109-six-way valve
110-gas circuit atmospheric valve D 111-enrichment cold-trap
Embodiment
Below in conjunction with embodiment, further specify the present invention.
Embodiment:
As depicted in figs. 1 and 2, the pretreating device of microscratch amount hydrogen isotope on-line analysis in a kind of rock gas comprises:
Described sample chamber 103 connects absorption cold-trap 105, and absorption cold-trap 105 connects six-way valve 109, and preenrichment cold-trap 107 two ends connect respectively six-way valve 109, and enrichment cold-trap 111 1 ends connect six-way valve 109, and the other end connects chromatographic column,
Described six-way valve 109 connects respectively helium pressure variable valve B108 and gas circuit atmospheric valve D110;
103 imports of described sample chamber and outlet are provided with gas circuit atmospheric valve A101 and gas circuit atmospheric valve B102;
Be provided with gas circuit atmospheric valve C106 between described absorption cold-trap 105 and the six-way valve 109;
When six-way valve 109 places the sampling state, absorption cold- trap 105 and 107 series connection of preenrichment cold-trap, preenrichment cold-trap 107 and enrichment cold-trap 111 disconnect;
Put 109 in sampling during state when six-way valve, absorption cold-trap 105 and preenrichment cold-trap 107 disconnect, preenrichment cold- trap 107 and 111 series connection of enrichment cold-trap.
Described absorption cold-trap 105 (temperature is 159K) adopts
The stainless steel pipeline fill 40～60 order 5A molecular sieve and 100～120 order divinyl benzene polymers molecular sieve (HAYESEP-D), two kinds of molecular sieve mixed by weight 1: 1; Preenrichment cold-trap 107 (temperature is 77K) adopts
The stainless steel pipeline fill 40～100 order 5A molecular sieve; Enrichment cold-trap 111 (temperature is 77K) adopts
The stainless steel pipeline fill 80～100 order 5A molecular sieve.
When testing:
A sample thief gas is in the sample chamber, and the access continuous-flow system, opens valve 102,104,106 usefulness He gas are taken the pipeline Air out of;
B places six-way valve under the sampling state, and shut-off valve 102,104,106 is opened the sample chamber valve simultaneously.Carrier gas He brings sample gas into absorption cold-trap 105 (liquid nitrogen+alcohol 159K), and hydro carbons and part inorganic gas are adsorbed, and H
2Pass through smoothly, and in preenrichment cold-trap 107 (liquid nitrogen 77K) enrichment, carrier gas He discharges through drain 110;
C is converted to the sample presentation state with six-way valve 109, to adsorb cold-trap 105 this moment and from (liquid nitrogen+alcohol) cryostat, mention hydro carbons and the part inorganic gas that the heating chamber removal of putting into 150 ℃ is adsorbed, and preenrichment cold-trap 107 is mentioned from the liquid nitrogen cryostat, at room temperature discharges H
2, and brought into enrichment cold-trap 111 (liquid nitrogen 77K) by carrier gas, enriching and purifying is 2 minutes again;
D six-way valve 109 returns to the sampling state, and enrichment cold-trap 111 is mentioned from the liquid nitrogen cryostat, places under the room temperature to discharge H
2, and brought into chromatogram-isotope mass spectrometer system measurement H by carrier gas
2Isotopic ratio.
Claims (6)
1. the pretreating device of microscratch amount hydrogen isotope on-line analysis in the rock gas is characterized in that:
Described device comprises sample chamber (103), six-way valve (109), absorption cold-trap (105), preenrichment cold-trap (107) and enrichment cold-trap (111),
The import of described sample chamber connects helium pressure variable valve A (101), sample chamber (103) outlet connects absorption cold-trap (105), absorption cold-trap (105) connects six-way valve (109), preenrichment cold-trap (107) two ends connect respectively six-way valve (109), enrichment cold-trap (111) one ends connect six-way valve (109), the other end connects chromatographic column
Described six-way valve (109) connects respectively helium pressure variable valve B (108) and gas circuit atmospheric valve D (110);
When six-way valve (109) places the sampling state, absorption cold-trap (105) and preenrichment cold-trap (107) series connection, preenrichment cold-trap (107) and enrichment cold-trap (111) disconnect;
When six-way valve was put (109) in the sampling state, absorption cold-trap (105) and preenrichment cold-trap (107) disconnected, preenrichment cold-trap (107) and enrichment cold-trap (111) series connection.
2. the pretreating device of microscratch amount hydrogen isotope on-line analysis in the rock gas as claimed in claim 1 is characterized in that:
(103) import of described sample chamber and outlet are provided with the gas circuit atmospheric valve.
3. the pretreating device of microscratch amount hydrogen isotope on-line analysis in the rock gas as claimed in claim 2 is characterized in that:
Be provided with gas circuit atmospheric valve C (106) between described absorption cold-trap (105) and the six-way valve (109).
4. such as the pretreating device of microscratch amount hydrogen isotope on-line analysis in the described rock gas of one of claim 1～3, it is characterized in that:
Described absorption cold-trap (105) adopts the stainless steel pipeline to fill 40～60 order 5A molecular sieve and 100～120 order divinyl benzene polymers molecular sieve, and the content of wherein said 5A molecular sieve is 20%～80wt%;
Described preenrichment cold-trap (107) adopts the stainless steel pipeline to fill 40～100 order 5A molecular sieve;
Described enrichment cold-trap (111) adopts the stainless steel pipeline to fill 80～100 order 5A molecular sieve.
5. the pretreating device of microscratch amount hydrogen isotope on-line analysis in the rock gas as claimed in claim 4 is characterized in that:
The temperature of described absorption cold-trap (105) is 159 ± 15K;
The temperature of described preenrichment cold-trap (107) is 77 ± 10K;
The temperature of described enrichment cold-trap (111) is 77 ± 10K.
6. the pretreating device of microscratch amount hydrogen isotope on-line analysis in the rock gas as claimed in claim 4 is characterized in that:
The stainless steel pipeline of described absorption cold-trap (105)
The stainless steel pipeline of described preenrichment cold-trap (107)
The stainless steel pipeline of described enrichment cold-trap (111)
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| CN103472157A (en) * | 2013-09-29 | 2013-12-25 | 中国寰球工程公司 | Heat exchanger liquefied natural gas sampling and proximate analyzing system |
| CN105403613A (en) * | 2015-10-23 | 2016-03-16 | 中国科学技术大学 | Vacuum step heating and element-isotope enrichment analysis apparatus |
| CN107209154A (en) * | 2015-02-06 | 2017-09-26 | 沙特基础工业全球技术有限公司 | Online gas chromatography system and its purposes for analysis of catalysed reactions |
| CN108414633A (en) * | 2018-02-12 | 2018-08-17 | 中国科学院地质与地球物理研究所 | A kind of determining instrument of micro nitrogen isotope and its application |
| CN109603413A (en) * | 2018-12-14 | 2019-04-12 | 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 | Hydrogen and methane and the device and method for measuring hydrogen isotope in a kind of separable mixed gas |
| CN109946407A (en) * | 2017-12-20 | 2019-06-28 | 核工业北京地质研究院 | A kind of mineral inclusion water sample extraction element for H isotope analysis |
| CN110095575A (en) * | 2019-05-08 | 2019-08-06 | 中国科学技术大学 | The enriching and purifying equipment of pure gas in mixed gas |
| CN111474284A (en) * | 2020-04-09 | 2020-07-31 | 中国工程物理研究院材料研究所 | Feed gas pretreatment and automatic sample introduction system for gas chromatography |
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| CN103472157A (en) * | 2013-09-29 | 2013-12-25 | 中国寰球工程公司 | Heat exchanger liquefied natural gas sampling and proximate analyzing system |
| CN107209154A (en) * | 2015-02-06 | 2017-09-26 | 沙特基础工业全球技术有限公司 | Online gas chromatography system and its purposes for analysis of catalysed reactions |
| CN105403613A (en) * | 2015-10-23 | 2016-03-16 | 中国科学技术大学 | Vacuum step heating and element-isotope enrichment analysis apparatus |
| CN105403613B (en) * | 2015-10-23 | 2018-12-14 | 中国科学技术大学 | Vacuum step heating-element-isotope enrichment analytical equipment |
| CN109946407A (en) * | 2017-12-20 | 2019-06-28 | 核工业北京地质研究院 | A kind of mineral inclusion water sample extraction element for H isotope analysis |
| CN108414633A (en) * | 2018-02-12 | 2018-08-17 | 中国科学院地质与地球物理研究所 | A kind of determining instrument of micro nitrogen isotope and its application |
| CN108414633B (en) * | 2018-02-12 | 2019-06-14 | 中国科学院地质与地球物理研究所 | A kind of determining instrument of micro nitrogen isotope and its application |
| CN109603413A (en) * | 2018-12-14 | 2019-04-12 | 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 | Hydrogen and methane and the device and method for measuring hydrogen isotope in a kind of separable mixed gas |
| CN110095575A (en) * | 2019-05-08 | 2019-08-06 | 中国科学技术大学 | The enriching and purifying equipment of pure gas in mixed gas |
| WO2020224304A1 (en) * | 2019-05-08 | 2020-11-12 | 中国科学技术大学 | Enrichment and purification device for single gas in mixed gas |
| CN111474284A (en) * | 2020-04-09 | 2020-07-31 | 中国工程物理研究院材料研究所 | Feed gas pretreatment and automatic sample introduction system for gas chromatography |
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