CN112345667A - Gaseous hydrocarbon preparation and online carbon isotope analysis device and method - Google Patents
Gaseous hydrocarbon preparation and online carbon isotope analysis device and method Download PDFInfo
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- CN112345667A CN112345667A CN202011226558.3A CN202011226558A CN112345667A CN 112345667 A CN112345667 A CN 112345667A CN 202011226558 A CN202011226558 A CN 202011226558A CN 112345667 A CN112345667 A CN 112345667A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Abstract
The invention relates to a method for preparing and analyzing a carbon isotope sample, in particular to a device and a method for preparing gaseous hydrocarbon and analyzing a carbon isotope online. The device comprises a sample reaction device, a hydrocarbon gas enrichment and separation device, a combustion device and an isotope mass spectrometer. The gaseous hydrocarbon preparation and on-line carbon isotope analysis device of the invention adds a liquid nitrogen cold trap in front of a gas chromatographic column to effectively extract hydrocarbon compounds in a sample, the invention adopts the first time that a quartz sample tube is added into a vaporization chamber, the sample can be heated by setting the temperature of a sample inlet cylinder, and the same sample can be continuously measured for C generated at different temperature points1‑C5The carbon isotope ratio of the hydrocarbon is simple and quick, the analysis time is shortened, and the labor cost is reduced; the determination of carbon isotopes from hydrocarbon generation to monomer hydrocarbon is completely and continuously carried out on line without any intermediate transfer link, overcomes the defects of the existing analysis method, and is the direct connection of natural gas and gas source rocksThe comparison provides more accurate isotope data.
Description
Technical Field
The invention relates to a method for preparing and analyzing a carbon isotope sample, in particular to a device and a method for preparing gaseous hydrocarbon and analyzing a carbon isotope online.
Background
Compared with petroleum, the natural gas has more complex cause, runs through the whole evolution process of organic matters, is relatively easy to move, and is easy to dissipate after being gathered into a reservoir. Direct comparison of natural gas with source rock has long been one of the problems that laboratory workers have attempted to solve, and analysis of gaseous hydrocarbons in source rock has typically been performed by means of hydrocarbon source rock thermal simulation experimental techniques. The hydrocarbon source rock hydrocarbon generation thermal simulation experiment basically adopts an autoclave closed system thermal simulation method, however, deep analysis finds that the traditional thermal simulation device is a completely closed system, organic matter thermal evolution products are continuously accumulated along with the increase of simulation temperature and time, and can not move to the space outside the source rock, the method can only measure the accumulated biomass amount of each simulation temperature point, and the gaseous products collected at different temperature points are the mixture of the source rock kerogen primary degradation gas and the liquid hydrocarbon secondary cracking gas, on the other hand, the experiment method needs large sample amount, long flow path and high cost. Therefore, it is difficult to obtain accurate geochemical information, and the cause and the mechanism of transport, aggregation and accumulation of natural gas cannot be accurately grasped.
On the other hand, in the conventional sample analysis process, gaseous hydrocarbons (C) in the source rock are generated due to volatilization and the like1-C5Hydrocarbon) component is quickly lost, and C1-C5The carbon isotope analysis of hydrocarbon comprises the steps of firstly removing adsorbed gas in source rock by a heating degasser or carrying out hydrocarbon generation thermal simulation on the source rock by a hydrocarbon generation thermal simulation device (high-pressure kettle), then transferring a product into a sample bottle, and preparing each single component into pure CO by a natural gas carbon isotope preparation system2And finally, measuring the carbon isotope ratio on an isotope mass spectrometer. The experimental process is complex in flow, long in time consumption, multiple in sample transfer links, and the components to be measured are easy to lose due to leakage or be polluted due to air entering, so that the analysis is time-consuming and labor-consuming, and the accuracy of data is influenced.
Chinese patent application CN109387577A is an analysis device for analyzing gaseous hydrocarbon isotopes in fluid inclusions, comprising: the system comprises a laser micro-sampling system, a sample purification and enrichment system and a sample separation system, wherein the laser micro-sampling system comprises a laser and a sample chamber, the laser excites a fluid inclusion in the sample chamber to extract gaseous hydrocarbons, the gaseous hydrocarbons are purified by the sample purification and enrichment system, and the purified gaseous hydrocarbons detect gaseous hydrocarbon carbon hydrogen isotopes by the sample separation system; the sample purification and enrichment system comprises a plurality of cold traps, cold trap tanks and a heating furnace which are communicated, wherein the cold traps are communicated with the sample chamber through pipelines; the sample separation system comprises in sequence: a gas chromatographic column, an oxidation furnace and/or a pyrolysis furnace and an isotope mass spectrometer which are communicated. The device is still relatively complex.
Disclosure of Invention
The invention mainly aims to provide a device and a method for preparing gaseous hydrocarbon and analyzing carbon isotopes on line.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a gaseous hydrocarbon preparation and on-line carbon isotope analysis device, which comprises a sample reaction device, a hydrocarbon gas enrichment and separation device, a combustion device and an isotope mass spectrometer, wherein the sample reaction device is connected with the combustion device; the sample reaction device comprises a quartz sample tube, a vaporizing chamber and a sample feeding cylinder, wherein the vaporizing chamber is arranged in the sample feeding cylinder, the quartz sample tube is arranged in the vaporizing chamber, and one end of the sample feeding cylinder is connected with a three-way valve.
The hydrocarbon gas enrichment and separation device comprises a U-shaped enrichment pipe, a liquid nitrogen cold trap and a gas chromatograph, wherein the U-shaped enrichment pipe is arranged in the liquid nitrogen cold trap and is connected with the sample injection cylinder through a six-way valve; the gas chromatograph is connected with the gas-carrying chromatographic pipeline through a six-way valve.
The combustion device comprises a combustion furnace and a water removal device;
the combustion furnace is respectively connected with the gas chromatograph and the water removal device, and the water removal device is connected with the isotope mass spectrometer.
Further, the quartz sample tube was 2cm long and 3mm in inner diameter, and both ends were plugged with quartz wool.
Further, the U-shaped enrichment pipe is made of stainless steel.
The invention also provides a method for preparing gaseous hydrocarbon in source rock and carrying out online carbon isotope analysis by using the device, which comprises the following steps:
step 1, grinding a rock sample into particles of 20-60 meshes;
step 2, putting the sample obtained in the step 1 into a quartz sample tube, and placing the quartz sample tube into a vaporizing chamber;
step 3, adding liquid nitrogen into the liquid nitrogen cold trap, opening a three-way valve, introducing high-purity carrier gas, setting the temperature of a vaporization chamber, heating the quartz sample tube to a preset temperature, keeping the temperature for 15-20min, and enriching hydrocarbon compounds in the sample in the liquid nitrogen cold trap;
step 4, after the enrichment is finished, rotating the six-way valve, removing the liquid nitrogen cold trap, starting the gas chromatograph and the isotope mass spectrometer, and allowing the gaseous hydrocarbon in the source rock to enter the chromatographic column for separation along with the carrier gas through the six-way valve;
step 5, opening a combustion furnace to combust the separated monomolecular hydrocarbon components into CO2Purifying by a water removal device, removing impurity gas generated at the same time, and finally obtaining pure CO2A gas;
step 6, determining CO by using an isotope mass spectrometer2Carbon isotope ratio of (a);
and 7, changing the preset temperature, and repeating the steps 3-6.
Further, in step 1, liquid nitrogen was continuously introduced during the grinding of the sample.
Further, in step 4, the gas chromatography conditions were:
the chromatographic column is as follows: CP-PoraPLOT Q-HT quartz capillary column, 27.5m × 0.32mm × 10 μm;
carrier gas: helium with purity of 99.999% and carrier gas flow rate of 1 ml/min;
and (3) sample introduction mode: a split mode with a split ratio of 5: 1;
temperature rising procedure: the initial temperature is 40 ℃, the temperature is kept for 1min, the temperature is increased to 180 ℃ at the speed of 5 ℃/min, and the temperature is kept for 20 min.
Further, the temperature of the interface of the chromatograph and the combustion furnace is 200 ℃, and the temperature of the combustion furnace is 910 ℃.
Further, in step 7, the preset temperature is increased from 50 ℃ to 350 ℃, and the circulation is stopped when the temperature interval of each circulation is 50 ℃ or 100 ℃ to 350 ℃.
The gaseous hydrocarbon preparation and online carbon isotope analysis device is not limited to the preparation of the gaseous hydrocarbon in the source rock sample and the online carbon isotope analysis, and is also suitable for other samples containing the gaseous hydrocarbon.
Compared with the prior art, the invention has the following advantages:
the gaseous hydrocarbon preparation and on-line carbon isotope analysis device of the invention adds a liquid nitrogen cold trap in front of a gas chromatographic column to effectively extract hydrocarbon compounds in a sample, the invention adopts the first time that a quartz sample tube is added into a vaporization chamber, the sample can be heated by setting the temperature of a sample inlet cylinder, and the same sample can be continuously measured for C generated at different temperature points1-C5The carbon isotope ratio of the hydrocarbon is simple and quick, the analysis time is shortened, and the labor cost is reduced; the isotope determination from hydrocarbon generation to monomer hydrocarbon carbon is carried out on line completely and continuously without any intermediate transfer link, thereby overcoming the defects of the existing analysis method and providing more accurate isotope data for the direct comparison of natural gas and gas source rock.
The method of the invention enables the sample to be in a low temperature environment through liquid nitrogen as much as possible in the processes of sample storage, crushing, weighing and analysis processing so as to obtain relatively complete components in the sample, thereby overcoming the problem of hydrocarbon gas loss in the sample and enabling the detection result to be more accurate.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
Fig. 1 is a schematic structural diagram of a device for preparing gaseous hydrocarbons and analyzing carbon isotopes online in source rocks according to an embodiment of the present invention;
FIG. 2 is a flow chart illustrating an embodiment of a method for gaseous hydrocarbon production and online carbon isotope analysis in a source rock according to an embodiment of the present invention;
fig. 3 is a graph illustrating the results of carbon isotope analysis of gaseous hydrocarbons in a source rock sample according to an embodiment of the present invention.
Wherein, 1, three-way valve; 2. a quartz sample tube; 3. a vaporization chamber; 4. a sample feeding cylinder; 5. a six-way valve; 6. a U-shaped enrichment pipe; 7. liquid nitrogen cold trap; 8. a gas chromatograph; 9. a combustion furnace; 10. a water removal device; 11. an isotope mass spectrometer; a. a reaction device; b. a hydrocarbon gas enrichment and separation device; c. a combustion apparatus.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the stated features, steps, operations, and/or combinations thereof, unless the context clearly indicates otherwise.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
Example 1
As shown in fig. 1, the apparatus for preparing gaseous hydrocarbons and analyzing carbon isotopes on line in source rocks comprises a sample reaction device a, a hydrocarbon gas enrichment and separation device b, a combustion device c and an isotope mass spectrometer 11.
The sample reaction device a comprises a quartz sample tube 2, a vaporizing chamber 3 and a sample inlet 4. The sample after freezing grinding is put into a quartz sample tube 2, the length of the quartz sample tube is 2cm, the inner diameter of the quartz sample tube is 3mm, two ends of the quartz sample tube are plugged by quartz wool and are arranged in a vaporization chamber 3, the vaporization chamber 3 is arranged in a sample feeding cylinder, and hydrocarbon gas in source rock can be effectively released by setting the temperature of the sample feeding cylinder 4.
The hydrocarbon gas enrichment and separation device b is connected with the sample reaction device a through a six-way valve 5, and the hydrocarbon gas generated by desorption and hydrocarbon generation in the sample is enriched in a U-shaped enrichment pipe 6 immersed in a liquid nitrogen cold trap 7 under the carrying of enrichment carrier gas.
The complete separation of each monomolecular component in the gaseous hydrocarbon compound is realized by the chromatograph 8, if the chromatograph 8 is not used, the isotope numerical values of methane, ethane, propane, butane and pentane cannot be respectively obtained, and only the isotope numerical value of the mixed hydrocarbon gas can be obtained, but the mixed hydrocarbon gas has small significance for exploration and research.
The combustion device c comprises a combustion furnace 9 and a water removal device 10, the temperature of the interface between the chromatograph 8 and the combustion furnace 9 is 200 ℃, and the temperature of the combustion furnace is 910 ℃. The single molecular components in the gaseous hydrocarbon compound separated by the chromatograph 8 enter the combustion furnace 9 under the drive of the carrier gas, and are sequentially reacted with O in the combustion furnace 92Reaction to CO2(ii) a CO produced2The gas is purified by cooling by means of a water removal device 10, removing H formed at the same time2O and other impurity gases to finally obtain pure CO2A gas.
Determination of pure CO from oxidation of individual monomolecular components of gaseous hydrocarbon compounds by means of an isotope mass spectrometer 112Carbon isotope ratio of (a).
Example 2
As shown in fig. 2, the method for preparing gaseous hydrocarbons and performing online carbon isotope analysis in source rock by using the device described in example 1 comprises the following steps:
(1) performing liquid nitrogen freezing treatment on tools such as a hammer, a pair of tweezers and the like, pouring liquid nitrogen into a mortar, taking a proper amount of sample, putting the sample into the mortar which is cooled, adding the liquid nitrogen, rapidly grinding the sample, continuously adding the proper amount of liquid nitrogen in the grinding process, and repeating for many times until the rock sample is ground into particles of 20-60 meshes;
(2) quickly taking a certain amount of sample, putting the sample into a quartz sample tube 2 which is cooled in advance, filling two ends of the sample tube with quartz wool, and placing the sample tube into a vaporizing chamber 3;
(3) introducing liquid nitrogen into the liquid nitrogen cold trap 7, opening the three-way valve 1, introducing high-purity carrier gas, setting the temperature of the sample inlet cylinder 4 at 50 ℃, keeping the temperature for 20min, and enriching hydrocarbon gas generated by desorption and hydrocarbon generation in the sample in the U-shaped enrichment tube 6 under the carrying of the carrier gas;
(4) setting working parameters of a gas chromatograph 8: the chromatographic column is a CP-PoraPLOT Q-HT quartz capillary column, and is 27.5m multiplied by 0.32mm multiplied by 10 mu m; carrier gas: helium with purity of 99.999% and carrier gas flow rate of 1 ml/min; and (3) sample introduction mode: a split mode with a split ratio of 5: 1; temperature rising procedure: the initial temperature is 40 ℃, the temperature is kept for 1min, the temperature is increased to 180 ℃ at the speed of 5 ℃/min, and the temperature is kept for 20 min. And (3) rotating the six-way valve 5, removing the liquid nitrogen cold trap 7, starting the gas chromatograph 8 and the isotope mass spectrometer 11, and completely separating each monomolecular component in the gaseous hydrocarbon compound in the sample by the chromatographic column.
(5) The separated gaseous hydrocarbon monomolecular hydrocarbon component enters the combustion furnace 9 under the drive of the carrier gas and is sequentially reacted with O in the combustion furnace 92Reaction to CO2CO formed2The gas is purified by cooling by means of a water removal device 10, removing H formed at the same time2O and other impurity gases to finally obtain pure CO2A gas.
(6) CO after water removal2The gas is introduced into the isotope mass spectrometer 11 with the carrier gas, the carbon isotope ratio is measured, and a spectrum is generated as shown in fig. 3.
(7) And (4) setting the temperature of the injection port to 100 ℃, 200 ℃, 300 ℃ and 350 ℃, and repeating the steps (3) to (6) respectively until the carbon isotope ratio and the spectrogram of the gaseous hydrocarbon in the source rock at all preset temperatures are obtained.
In conclusion, the invention makes the sample in the low-temperature environment through liquid nitrogen as much as possible in the processes of sample storage, crushing, weighing and analysis processing so as to obtain relatively complete components in the sample, and overcomes the problem of hydrocarbon gas loss in the sample. By adding a liquid nitrogen cold trap in front of the gas chromatographic column, hydrocarbon compounds in the source rock are effectively extracted. The method has the advantages that the quartz sample tube is added into the vaporizing chamber of the sample feeding cylinder for the first time, the sample can be heated by setting the temperature of the sample feeding cylinder, the method is simple and rapid, and the gaseous hydrocarbon (C) generated at different temperature points can be simply, rapidly and continuously measured for the same source rock sample1-C5) The carbon isotope ratio of the hydrocarbon shortens the analysis time and reduces the labor cost.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (8)
1. A gaseous hydrocarbon preparation and on-line carbon isotope analysis device is characterized by comprising a sample reaction device, a hydrocarbon gas enrichment and separation device, a combustion device and an isotope mass spectrometer; the sample reaction device comprises a quartz sample tube, a vaporization chamber and a sample feeding cylinder, wherein the vaporization chamber is arranged in the sample feeding cylinder, the quartz sample tube is arranged in the vaporization chamber, and one end of the sample feeding cylinder is connected with a three-way valve;
the hydrocarbon gas enrichment and separation device comprises a U-shaped enrichment pipe, a liquid nitrogen cold trap and a gas chromatograph, wherein the U-shaped enrichment pipe is arranged in the liquid nitrogen cold trap and is connected with the sample injection cylinder through a six-way valve; the gas chromatograph is connected with the gas-carrying chromatographic pipeline through a six-way valve;
the combustion device comprises a combustion furnace and a water removal device;
the combustion furnace is respectively connected with the gas chromatograph and the water removal device, and the water removal device is connected with the isotope mass spectrometer.
2. The apparatus of claim 1, wherein the quartz sample tube has a length of 2cm and an inner diameter of 3mm, and is plugged at both ends with quartz wool.
3. The apparatus of claim 1, wherein the U-shaped enrichment tube is made of stainless steel.
4. A method for gaseous hydrocarbon production and online carbon isotope analysis in source rock using the apparatus of any one of claims 1-3, comprising the steps of:
step 1, grinding a rock sample into particles of 20-60 meshes;
step 2, putting the sample obtained in the step 1 into a quartz sample tube, and placing the quartz sample tube into a vaporizing chamber;
step 3, adding liquid nitrogen into the liquid nitrogen cold trap, opening a three-way valve, introducing high-purity carrier gas, setting the temperature of a sample injection cylinder, heating the quartz sample tube to a preset temperature, keeping the temperature for 15-20min, and enriching hydrocarbon compounds in the sample in the liquid nitrogen cold trap;
step 4, after the enrichment is finished, rotating the six-way valve, removing the liquid nitrogen cold trap, starting the gas chromatograph and the isotope mass spectrometer, and allowing the gaseous hydrocarbon in the source rock to enter the chromatographic column for separation along with the carrier gas through the six-way valve;
step 5, opening a combustion furnace to combust the separated monomolecular hydrocarbon components into CO2Purifying by a water removal device, removing impurity gas generated at the same time, and finally obtaining pure CO2A gas;
step 6, determining CO by using an isotope mass spectrometer2Carbon isotope ratio of (a);
and 7, changing the preset temperature, and repeating the steps 3-6.
5. The method of claim 4, wherein the liquid nitrogen is continuously introduced during the grinding of the sample in step 1.
6. The method of claim 4, wherein in step 4, the gas chromatography conditions are:
the chromatographic column is as follows: CP-PoraPLOT Q-HT quartz capillary column, 27.5m × 0.32mm × 10 μm;
carrier gas: helium with purity of 99.999% and carrier gas flow rate of 1 ml/min;
and (3) sample introduction mode: a split mode with a split ratio of 5: 1;
temperature rising procedure: the initial temperature is 40 ℃, the temperature is kept for 1min, the temperature is increased to 180 ℃ at the speed of 5 ℃/min, and the temperature is kept for 20 min.
7. The method of claim 4, wherein the chromatograph and furnace interface temperature is 200 ℃ and the furnace temperature is 910 ℃.
8. The method of claim 4, wherein the predetermined temperature is increased from 50 ℃ to 350 ℃, and the cycling is stopped at a temperature interval of 50 ℃ or 100 ℃ for each cycle to 350 ℃.
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Cited By (3)
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| CN107219245A (en) * | 2017-05-26 | 2017-09-29 | 国家地质实验测试中心 | A kind of hydrocarbon source rock organic carbon pyrolysis analysis apparatus and method |
| CN113252421A (en) * | 2021-06-17 | 2021-08-13 | 西南石油大学 | Device and method for measuring trace carbon isotopes and heavy components in natural gas |
| CN114062550A (en) * | 2021-11-16 | 2022-02-18 | 西南石油大学 | Natural gas all-component analysis device and method |
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| CN107831250A (en) * | 2017-05-27 | 2018-03-23 | 中国石油化工股份有限公司 | Hydrocarbon compound carbon isotope analysis chromatography separating method in natural gas |
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| CN103245735A (en) * | 2013-03-29 | 2013-08-14 | 中国石油天然气股份有限公司 | Online analysis method for hydrocarbon carbon isotope of light dydrocarbon monomer of source rock pyrolysis product |
| CN107831250A (en) * | 2017-05-27 | 2018-03-23 | 中国石油化工股份有限公司 | Hydrocarbon compound carbon isotope analysis chromatography separating method in natural gas |
| CN109387577A (en) * | 2017-08-10 | 2019-02-26 | 中国石油化工股份有限公司 | For analyzing the analytical equipment of gaseous hydrocarbon carbon-hydrogen isotopes in fluid inclusion |
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| CN107219245A (en) * | 2017-05-26 | 2017-09-29 | 国家地质实验测试中心 | A kind of hydrocarbon source rock organic carbon pyrolysis analysis apparatus and method |
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| CN113252421A (en) * | 2021-06-17 | 2021-08-13 | 西南石油大学 | Device and method for measuring trace carbon isotopes and heavy components in natural gas |
| CN113252421B (en) * | 2021-06-17 | 2021-09-21 | 西南石油大学 | Device and method for measuring trace carbon isotopes and heavy components in natural gas |
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| CN114062550B (en) * | 2021-11-16 | 2024-02-02 | 西南石油大学 | Natural gas full-component analysis device and method |
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