CN113804807A - Carbon isotope separation and enrichment device for hydrocarbon gas components in natural gas and sample preparation method - Google Patents

Carbon isotope separation and enrichment device for hydrocarbon gas components in natural gas and sample preparation method Download PDF

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CN113804807A
CN113804807A CN202010539902.8A CN202010539902A CN113804807A CN 113804807 A CN113804807 A CN 113804807A CN 202010539902 A CN202010539902 A CN 202010539902A CN 113804807 A CN113804807 A CN 113804807A
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gas
sample
temperature
vacuum
valve
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翟正
王学军
李祥臣
綦艳丽
刘庆
鲍燕
林晶
韩冬梅
王�忠
张蕾
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China Petroleum and Chemical Corp
Exploration and Development Research Institute of Sinopec Shengli Oilfield Co
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China Petroleum and Chemical Corp
Exploration and Development Research Institute of Sinopec Shengli Oilfield Co
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • G01N30/08Preparation using an enricher
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • G01N2030/067Preparation by reaction, e.g. derivatising the sample

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Abstract

The invention aims to provide a device for quickly separating and enriching carbon isotopes of hydrocarbon components in natural gas and a sample preparation method. The device is provided with a plurality of sample reactors and sample collecting pipes, so that the reaction, transfer and purification time of hydrocarbon components in natural gas is prolonged, and the accuracy of the test process is ensured; based on the device, the chromatographic separation conditions of the natural gas hydrocarbon components are optimized, the retention time intervals of different components are shortened, and the sample separation and preparation efficiency is improved; the method selects oxygen as reaction carrier gas, thereby ensuring that the sample can react completely at high temperature, ensuring the accuracy of sample preparation and reducing sample preparation steps.

Description

Carbon isotope separation and enrichment device for hydrocarbon gas components in natural gas and sample preparation method
Technical Field
The invention belongs to the technical field of natural gas analysis methods, and relates to a separation and enrichment device for carbon isotopes of hydrocarbon gas components in natural gas and a sample preparation method.
Background
Natural gas can be detected as either trace gas in deposits or gas accumulated in reservoirs. Over a long period of time, hydrocarbon gases are produced from organic matter through bacterial action and conversion by heat generation. The natural gas isotope can accurately judge the cause type of the natural gas, evaluate the maturity of the natural gas, and realize the prediction of the oil-gas relationship and the CO in the natural gas2And (4) risk evaluation, identification of the fingerprint characteristics of the natural gas in the gas reservoir and prediction of the change trend of the oil and gas field. Therefore, the method has important theoretical and practical significance for accurately measuring the carbon isotope characteristics of the hydrocarbon components in the natural gas.
At present, people adopt an on-line analysis technology of carbon isotopes, however, in actual analysis, the amount of samples entering a detector is small, data fluctuation is often generated, and for substances with low content, the content is lower than a detection line, so that the detection cannot be performed. At present, a separation technology of hydrocarbon gas components is also developed, a chromatographic method is used for detecting the content of different components in natural gas, although different components can be separated, a capillary column is generally adopted in the process of testing and separating, the sample injection amount is often less than 10 mu L, different components can only be effectively separated, and subsequent further operation is inconvenient. In order to meet the requirements of analysis and test, the sample introduction amount of a sample is usually required to be more than 3mL, chromatographic analysis conditions are obviously different based on the increase of the sample introduction amount, and the chromatographic analysis conditions of natural gas hydrocarbon components based on the preparation chromatogram are required to be established; the patent "method for chromatographic separation of carbon isotopes of hydrocarbon compounds in natural gas (2017103883344)" was previously reported, which proposed chromatographic separation conditions for carbon isotopes of hydrocarbon compounds in natural gas, but the chromatographic preparation method established in the patent was based on a single set of reaction and collection device, and as the mixing of gas components is ensured in the preparation of different components, the reaction and collection of hydrocarbon components are required to be completed within a chromatographic retention time interval, and thus the chromatographic retention time of components in natural gas must be ensured to reach a certain time interval (at least more than 3 min), so that the chromatographic conditions are harsh and the chromatographic reaction time is long. Therefore, it is needed to develop a new automatic separation and preparation device for chromatography and a dual-path analysis system combined with a carbon isotope mass spectrometer.
Disclosure of Invention
The invention aims to provide a device for quickly separating and enriching carbon isotopes of hydrocarbon components in natural gas and a sample preparation method, which optimize a chromatographic separation method of the hydrocarbon components in the natural gas, establish a quick enrichment method aiming at low-content hydrocarbon components in the natural gas, and adopt oxygen as reaction gas and carrier gas, thereby ensuring that a sample completely reacts at high temperature and simplifying operation steps. The method ensures the accuracy of preparing the hydrocarbon component sample in the natural gas, not only can form a set of simple and easy standardized operation flow, but also can coordinate a plurality of operation stations, thereby realizing the standardization and automation of the operation.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a hydrocarbon gas component carbon isotope separation and enrichment device, which comprises a hydrocarbon gas separation device, a gas transmission device, two gas flowmeters, a plurality of sample reactors, a plurality of valves, a plurality of sample collection and vacuum degree control devices, which are sequentially connected together;
the hydrocarbon gas separation device comprises a sample inlet, a chromatograph and a program switching valve which are connected in sequence;
the sample reactor is connected with a gas flowmeter through a valve; the two gas flow meters are respectively connected with the gas transmission device through valves;
the sample collection and vacuum degree control device comprises a bubble meter, eight vacuum valves, an alcohol cold trap, two liquid nitrogen cold traps, a collection pipe, an auxiliary gas device and a vacuum pump; the sample reactor is respectively connected with a first vacuum valve and a second vacuum valve; the bubble meter is connected with the second vacuum valve; the alcohol cold trap is respectively connected with the first vacuum valve and the third vacuum valve; the first liquid nitrogen cold trap is respectively connected with a third vacuum valve and a fourth vacuum valve, the fifth vacuum valve is respectively connected with a fourth vacuum valve, a sixth vacuum valve, a seventh vacuum valve and a second liquid nitrogen cold trap, and the eighth vacuum valve is respectively connected with the second liquid nitrogen cold trap and a vacuum pump; the sixth vacuum valve is connected with the sample collecting pipe, and the seventh vacuum valve is connected with the auxiliary gas device.
Preferably, the program switching valve can be one of a two-way valve, a three-way valve and a four-way valve.
Preferably, the number of the sample reactors, the number of the sample collecting devices and the number of the vacuum degree control devices correspond to the number of the program switching valves in communication respectively. Preferably, the sample reactor is a quartz reaction tube.
Preferably, a vacuum gauge is arranged in the vacuum pump; preferably, a graduated U-shaped tube is placed in the liquid nitrogen trap, the amount of which is observed when the collected gas solidifies to a solid state.
In a second aspect of the present invention, there is provided a method for preparing a sample by separating and enriching carbon isotopes in hydrocarbon gas components by using the above-mentioned apparatus, comprising the following steps:
opening a valve between a gas transmission device and a sample reactor, inputting oxygen into the device, raising the temperature of the sample reactor when continuous bubbles are generated in a bubble meter, pushing a sample into a chromatograph when the temperature of the sample reactor reaches 900 ℃, separating hydrocarbon gas, and sequentially introducing the separated gas into the corresponding sample reactors through a program switching valve;
turning on the vacuum pump, controlling the vacuum degree of the device, and controlling the opening or closing state of each vacuum valve to generate gas H2O and CO2Sequentially passing through alcohol cold hydrazine and liquid nitrogen cold hydrazine, and making CO be in the presence of different temperatures of alcohol cold hydrazine and liquid nitrogen cold hydrazine2Gas is stored in liquid nitrogen cold hydrazine, H2Storing O in alcohol cold hydrazine; cooling CO in hydrazine with liquid nitrogen2The temperature is raised to normal temperature, and a required sample is collected;
by opening and closing the vacuum valve, H in the system is pumped away2O and residual gases.
According to the third aspect of the invention, the carbon isotope separation and enrichment sample preparation method for the hydrocarbon gas components in the natural gas is provided, and the sample preparation of the hydrocarbon gas components in the natural gas by utilizing the device and setting the chromatographic separation parameters by controlling the sample injection amount or the sample injection times.
Preferably, the full component chromatographic separation parameters in natural gas are:
a chromatographic column: a Propack Q packed column;
carrier gas: oxygen gas;
flow rate of carrier gas: 16 mL/min;
temperature: the initial temperature is 40 ℃, and the temperature is raised to 165 ℃ at 3 ℃/min;
sample introduction volume: 5 mL.
Preferably, the chromatographic separation parameters for ethane in natural gas are:
a chromatographic column: a Propack Q packed column;
carrier gas: oxygen gas;
flow rate of carrier gas: 16 mL/min;
temperature: the initial temperature is 40 ℃, the temperature is increased to 70 ℃ at the speed of 6 ℃/min, and then the temperature is increased to 120 ℃ at the speed of 3 ℃/min;
sample introduction volume: 9 mL.
Preferably, the chromatographic separation parameters for propane in natural gas are:
a chromatographic column: a Propack Q packed column;
carrier gas: oxygen gas;
flow rate of carrier gas: 18 mL/min;
temperature: the initial temperature is 40 ℃, the temperature is increased to 80 ℃ at 6 ℃/min, and then the temperature is increased to 150 ℃ at 5 ℃/min;
preferably, the chromatographic separation parameters for butane in natural gas are:
a chromatographic column: a Propack Q packed column;
carrier gas: oxygen gas;
flow rate of carrier gas: 20 mL/min;
temperature: the initial temperature is 40 ℃, the temperature is raised to 100 ℃ at 8 ℃/min, and then the temperature is raised to 165 ℃ at 7 ℃/min.
Compared with the prior art, the invention has the following beneficial effects:
the device is provided with a plurality of sample reactors and sample collecting pipes, so that the reaction, transfer and purification time of hydrocarbon components in natural gas is prolonged, and the accuracy of the test process is ensured; the device provided by the invention is provided with the U-shaped pipe with the scale marks in the liquid nitrogen cold trap, so that the relative contents of different components in the natural gas can be estimated.
Based on the device, the chromatographic separation conditions of the natural gas hydrocarbon components are optimized, the retention time intervals of different components are shortened, and the sample separation and preparation efficiency is improved; the invention also optimizes the chromatographic enrichment condition of low-content hydrocarbon components in the natural gas, ensures the quick and effective enrichment of each component and effectively shortens the enrichment time of low-content samples.
The method selects oxygen as reaction carrier gas, thereby ensuring that the sample can react completely at high temperature, ensuring the accuracy of sample preparation and reducing sample preparation steps.
Drawings
The accompanying drawings, which form a part hereof, are included to provide a further explanation 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 view of a device for rapidly separating and enriching carbon isotopes in hydrocarbon components according to example 1 of the present invention;
FIG. 2 is a sample collection and vacuum control apparatus;
FIG. 3 ethane separation enrichment chromatogram;
FIG. 4 a propane separation enrichment chromatogram;
FIG. 5 butane separation enrichment chromatogram.
1. Sample inlet, 2, chromatograph, 3, switching valve, 4, valve, 5, sample reactor, 6, valve, 7, sample reactor, 8, valve, 9, sample reactor, 10, valve, 11, sample reactor, 12, valve, 13, first flowmeter, 14, valve, 15, second flowmeter, 16, sample collection and vacuum degree control device, 17, sample collection and vacuum degree control device, 18, sample collection and vacuum degree control device, 19, sample collection and vacuum degree control device, 20, first vacuum valve, 21, second vacuum valve, 22, bubble gauge, 23, alcohol cold trap, 24, third vacuum valve, 25, first liquid nitrogen cold trap, 26, fourth vacuum valve, 27, sixth vacuum valve, 28, sample collection pipe, 29, seventh vacuum valve, 30, auxiliary gas device, 31, fifth vacuum valve, 32, second liquid nitrogen cold trap, 33. an eighth vacuum valve, 34, a vacuum pump, 35, a first gas transmission device, 36 and a second gas transmission device.
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 device for separating and enriching carbon isotopes in hydrocarbon gas components in natural gas
As shown in figure 1, the device comprises a hydrocarbon gas separation device, a gas transmission device (35, 36), two gas flow meters (13, 15), four sample reactors (5, 7, 9, 11), valves (4, 6, 8, 10, 12, 14), four sample collection and vacuum degree control devices (16, 17, 18, 19) which are connected together in sequence,
the hydrocarbon gas separation device comprises a sample inlet 1, a chromatograph 2 and a program switching valve 3 which are connected in sequence; the program switching valve is a four-way valve (a, b, c, d);
the sample reactors 5, 7, 9, 11 are connected with a gas flow meter through valves 4, 6, 8, 10, 12 or 14 respectively; the first gas transmission device 35 and the second gas transmission device 36 are respectively connected with the gas flow meters 13 and 15; the sample reactor 5 is respectively connected with the end a of the program switching valve and the sample collection and vacuum degree control device 16; the sample reactor 7 is respectively connected with the end b of the program switching valve and a sample collection and vacuum degree control device 17; the sample reactor 9 is respectively connected with the end c of the program switching valve and a sample collection and vacuum degree control device 18; the sample reactor 11 is connected with a program switching valve d end and a sample collecting and vacuum degree control device 19 respectively.
The sample collection and vacuum degree control device comprises a bubble meter 22, eight vacuum valves (20, 21, 24, 26, 27, 29, 31, 33), an alcohol cold trap 23, two liquid nitrogen cold traps (25, 33), a collecting pipe 28, an auxiliary gas device 30 and a vacuum pump 34; the sample reactor is respectively connected with a first vacuum valve 20 and a second vacuum valve 21; the bubble meter 22 is connected with the second vacuum valve 21; the alcohol cold trap 23 is respectively connected with the first vacuum valve 20 and the third vacuum valve 24; the first liquid nitrogen cold trap 25 is respectively connected with a third vacuum valve 24 and a fourth vacuum valve 26, the fifth vacuum valve 31 is respectively connected with the fourth vacuum valve 26, a sixth vacuum valve 27, a seventh vacuum valve 29 and a second liquid nitrogen cold trap 32, and the eighth vacuum valve 33 is respectively connected with the second liquid nitrogen cold trap 32 and a vacuum pump 34; the sixth vacuum valve 27 is connected to the sample collection tube 28, and the seventh vacuum valve 29 is connected to the auxiliary gas device 30.
The sample reactor is a quartz reaction tube, and a vacuum gauge is arranged in a vacuum pump.
Example 2 method for separating and enriching carbon isotopes in hydrocarbon gas components in natural gas
Sample preparation was carried out using the apparatus described in example 1, the method comprising the steps of:
(1) closing the reaction tube, and vacuumizing the system by controlling the switch of the touch button vacuum valve;
(2) closing the valve 27, the fifth vacuum valve 31 and the eighth vacuum valve 33, disconnecting the rest vacuum valves and valves, and vacuumizing the sample collection pipe at the sampling port;
(3) closing valves 27, 31 and 33, closing valves 4 and 12, closing valves 20, 24 and 26, introducing oxygen and adjusting the flow of oxygen, when successive bubbles are generated in bubble gauge 22, indicating that the reaction apparatus is filled with oxygen.
(4) And (3) heating the quartz tube reaction tube, and injecting a 3mL natural gas sample into a chromatograph when the temperature of the quartz tube reaction tube reaches 900 ℃.
(5) According to the optimized chromatographic conditions, as shown in table 1 below, the separation of methane, ethane, propane, butane and pentane components can be achieved, and methane is introduced into the quartz reaction tube 5 by switching the four-way valve by a program.
(6) CO of methane in a reactor2CO formed2Flowing along the pipeline, storing the impurities in the alcohol cold hydrazine 23, and introducing CO2The gas is stored in a first liquid nitrogen cooled hydrazine 25.
(7) Disconnecting the first vacuum valve 20, the fifth vacuum valve 31 and the eighth vacuum valve 33, and pumping out the gas in the pipeline;
(8) when the vacuum degree reaches 10-2When the gas is in use, the fifth vacuum valve 31 and the eighth vacuum valve 33 are disconnected, and CO in the liquid nitrogen cold hydrazine is cooled2The temperature is raised to normal temperature, and the sample collecting pipe obtains the required sample, namely the preparation of the reaction gas of the methane gas in the natural gas is completed.
(9) According to the chromatographic conditions, when C appears in the chromatogram2And when the peak occurs, the four-way valve is switched by the program to be automatically connected to the b contact, and the operation is repeated. By analogy in sequence, do notCollecting the hydrocarbon gas reactant with the same carbon number.
TABLE 1 Natural gas full-component separation chromatography test conditions
Figure BDA0002536957810000061
Example 3 method for preparing sample by separating and enriching ethane carbon isotope in natural gas
The hydrocarbon composition in the selected natural gas was about 95% methane, about 2.6% ethane, about 1.3% propane, about 0.7% butane, and about 0.4% remaining heavy hydrocarbon components.
The difference from example 2 is that the sample amount is enlarged, 9mL of natural gas is injected into the chromatograph, the chromatographic separation conditions are shown in table 2 below, and the ethane separation enrichment chromatogram is shown in fig. 3. The other steps are similar to example 2.
TABLE 2 chromatographic analysis conditions for separation and enrichment of ethane in natural gas
Figure BDA0002536957810000062
Example 4 method for separating and enriching propane carbon isotope in natural gas
The hydrocarbon composition in the selected natural gas was about 95% methane, about 2.6% ethane, about 1.3% propane, about 0.7% butane, and about 0.4% remaining heavy hydrocarbon components.
The difference from example 2 is that the sample amount is enlarged, 15mL of natural gas is injected into the chromatograph, the chromatographic separation conditions are shown in the following Table 3, and the propane separation enrichment chromatogram is shown in FIG. 4. The other steps are similar to example 2.
TABLE 3 chromatographic analysis conditions for separation and enrichment of propane in natural gas
Figure BDA0002536957810000063
Example 5 method for preparing sample by isotopic separation and enrichment of butane carbon in natural gas
The hydrocarbon composition in the selected natural gas was about 95% methane, about 2.6% ethane, about 1.3% propane, about 0.7% butane, and about 0.4% remaining heavy hydrocarbon components.
The difference from example 2 is that the sample amount is enlarged, 20mL of natural gas is injected into the chromatograph, the chromatographic separation conditions are shown in the following Table 4, and the butane separation enrichment chromatogram is shown in FIG. 5. The other steps are similar to example 2.
TABLE 4 chromatographic analysis conditions for separation and enrichment of butane in natural gas
Figure BDA0002536957810000071
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 (10)

1. The separation and enrichment device for the carbon isotopes of hydrocarbon gas components is characterized by comprising a hydrocarbon gas separation device, a gas transmission device, two gas flowmeters, a plurality of sample reactors, a plurality of valves, a plurality of sample collection and vacuum degree control devices which are sequentially connected together;
the hydrocarbon gas separation device comprises a sample inlet, a chromatograph and a program switching valve which are connected in sequence;
the sample reactor is connected with a gas flowmeter through a valve; the two gas flow meters are respectively connected with the gas transmission device through valves;
the sample collection and vacuum degree control device comprises a bubble meter, eight vacuum valves, an alcohol cold trap, two liquid nitrogen cold traps, a collection pipe, an auxiliary gas device and a vacuum pump; the sample reactor is respectively connected with a first vacuum valve and a second vacuum valve; the bubble meter is connected with the second vacuum valve; the alcohol cold trap is respectively connected with the first vacuum valve and the third vacuum valve; the first liquid nitrogen cold trap is respectively connected with a third vacuum valve and a fourth vacuum valve, the fifth vacuum valve is respectively connected with a fourth vacuum valve, a sixth vacuum valve, a seventh vacuum valve and a second liquid nitrogen cold trap, and the eighth vacuum valve is respectively connected with the second liquid nitrogen cold trap and a vacuum pump; the sixth vacuum valve is connected with the sample collecting pipe, and the seventh vacuum valve is connected with the auxiliary gas device.
2. The hydrocarbon gas component carbon isotope separation and enrichment facility as claimed in claim 1, wherein the program switching valve is one of a two-way valve, a three-way valve, and a four-way valve.
3. The hydrocarbon gas component carbon isotope separation and enrichment device of claim 1 or 2, wherein the number of the sample reactors, the number of the sample collection and vacuum degree control devices respectively correspond to the number of the program switching valves.
4. The hydrocarbon gas component carbon isotope separation and enrichment facility as claimed in claim 1, wherein the sample reactor is a quartz reaction tube.
5. The hydrocarbon gas component carbon isotope separation and enrichment facility as claimed in claim 1, wherein a vacuum gauge is provided in the vacuum pump; preferably, a U-shaped pipe with scale marks is arranged in the liquid nitrogen cold trap.
6. The method for preparing the sample by separating and enriching the carbon isotopes in the hydrocarbon gas components by using the device of claims 1-5 is characterized by comprising the following steps:
opening a valve between a gas transmission device and a sample reactor, inputting oxygen into the device, raising the temperature of the sample reactor when continuous bubbles are generated in a bubble meter, pushing a sample into a chromatograph when the temperature of the sample reactor reaches 900 ℃, separating hydrocarbon gas, and sequentially introducing the separated gas into the corresponding sample reactors through a program switching valve;
the vacuum pump is turned on to control the vacuum degree of the device, and then the opening or closing state of each vacuum valve is controlled to generateGas H of2O and CO2Sequentially passing through alcohol cold hydrazine and liquid nitrogen cold hydrazine, and making CO be in the presence of different temperatures of alcohol cold hydrazine and liquid nitrogen cold hydrazine2Gas is stored in liquid nitrogen cold hydrazine, H2Storing O in alcohol cold hydrazine; cooling CO in hydrazine with liquid nitrogen2The temperature is raised to normal temperature, and a required sample is collected;
the H2O and residual gas in the system are pumped away by opening and closing the vacuum valve.
7. A method for preparing a sample by separating and enriching carbon isotopes of hydrocarbon gas components in natural gas is characterized in that the device of any one of claims 1 to 5 is used for realizing the separation and enrichment of the carbon isotopes of the hydrocarbon gas components in the natural gas by controlling the sample injection amount or the sample injection times and setting chromatographic separation parameters.
8. The method of claim 7, wherein the parameters for full component chromatography in natural gas are:
a chromatographic column: a Propack Q packed column;
carrier gas: oxygen gas;
flow rate of carrier gas: 16 mL/min;
temperature: the initial temperature is 40 ℃, and the temperature is raised to 165 ℃ at 3 ℃/min;
sample introduction volume: 5 mL.
9. The method of claim 7, wherein the chromatographic separation parameters for ethane in natural gas are:
a chromatographic column: a Propack Q packed column;
carrier gas: oxygen gas;
flow rate of carrier gas: 16 mL/min;
temperature: the initial temperature is 40 ℃, the temperature is increased to 70 ℃ at the speed of 6 ℃/min, and then the temperature is increased to 120 ℃ at the speed of 3 ℃/min;
sample introduction volume: 9 mL.
10. The method of claim 7, wherein the chromatographic separation parameters for propane in natural gas are:
a chromatographic column: a Propack Q packed column;
carrier gas: oxygen gas;
flow rate of carrier gas: 18 mL/min;
temperature: the initial temperature is 40 ℃, the temperature is increased to 80 ℃ at 6 ℃/min, and then the temperature is increased to 150 ℃ at 5 ℃/min;
preferably, the chromatographic separation parameters for butane in natural gas are:
a chromatographic column: a Propack Q packed column;
carrier gas: oxygen gas;
flow rate of carrier gas: 20 mL/min;
temperature: the initial temperature is 40 ℃, the temperature is raised to 100 ℃ at 8 ℃/min, and then the temperature is raised to 165 ℃ at 7 ℃/min.
CN202010539902.8A 2020-06-12 2020-06-12 Carbon isotope separation and enrichment device for hydrocarbon gas components in natural gas and sample preparation method Pending CN113804807A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113804769A (en) * 2020-06-15 2021-12-17 中国石油化工股份有限公司 Light hydrocarbon carbon isotope enrichment analytical equipment in natural gas

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Publication number Priority date Publication date Assignee Title
CN107478473A (en) * 2016-06-07 2017-12-15 中国石油化工股份有限公司 Trace methane Gas carbon isotopes sample-preparing system and its method for making sample
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
CN212586315U (en) * 2020-06-12 2021-02-23 中国石油化工股份有限公司 Carbon isotope separation and enrichment device for hydrocarbon gas components in natural gas

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107478473A (en) * 2016-06-07 2017-12-15 中国石油化工股份有限公司 Trace methane Gas carbon isotopes sample-preparing system and its method for making sample
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
CN212586315U (en) * 2020-06-12 2021-02-23 中国石油化工股份有限公司 Carbon isotope separation and enrichment device for hydrocarbon gas components in natural gas

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113804769A (en) * 2020-06-15 2021-12-17 中国石油化工股份有限公司 Light hydrocarbon carbon isotope enrichment analytical equipment in natural gas

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