CN107300498B - Device for measuring carbon stable isotope ratio in carbon dioxide - Google Patents

Device for measuring carbon stable isotope ratio in carbon dioxide Download PDF

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Publication number
CN107300498B
CN107300498B CN201710610001.1A CN201710610001A CN107300498B CN 107300498 B CN107300498 B CN 107300498B CN 201710610001 A CN201710610001 A CN 201710610001A CN 107300498 B CN107300498 B CN 107300498B
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sample bottle
sample
sealing gasket
carbon dioxide
carbon
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CN107300498A (en
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张少庆
张新艳
娄博坤
吴东辉
于洪文
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Northeast Institute of Geography and Agroecology of CAS
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Northeast Institute of Geography and Agroecology of CAS
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode

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  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Engineering & Computer Science (AREA)
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  • Molecular Biology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Investigating Or Analysing Biological Materials (AREA)

Abstract

A device for measuring the ratio of carbon stable isotopes in carbon dioxide relates to a device for measuring the ratio of carbon stable isotopes in carbon dioxide. The invention aims to solve the technical problems that the removal of impurity gas is time-consuming, high in cost and poor in effect when the ratio of carbon stable isotope in carbon dioxide is measured at present. The device for measuring the carbon stable isotope ratio in the carbon dioxide consists of a positioning frame, a sample bottle, an air bag, a sealing gasket and a sample bottle cap; the air bag is sleeved on the sealing gasket, the air bag extends into the sample bottle, the sealing gasket is clamped on the inner wall of the upper end of the sample bottle, the sample bottle cap is fixed with the upper end of the sample bottle through threads, and the positioning frame is sleeved on the outer wall of the sample bottle cap. The device of the invention is used for replacing the existing sample bottle, the test cost can be saved by 50 percent, and the time for exhausting the impurity gas and injecting the gas sample into the sample bottle can be saved by 50 percent; the device has the advantages of ingenious design, reasonable structure, easy disassembly and assembly, convenient transportation and convenient use.

Description

Device for measuring carbon stable isotope ratio in carbon dioxide
Technical Field
The invention relates to a device for measuring a carbon stable isotope ratio in carbon dioxide.
Background
Carbon dioxide carbon stable isotope has very important significance for the research of climate change, ecosystem function and the like. Laboratories typically employ a multi-purpose sample preparation device in conjunction with a stable isotope mass spectrometer to determine the carbon stable isotope ratio in carbon dioxide gas. Impurity gas which interferes with sample measurement in a sample bottle is removed before the sample bottle is filled with a sample, and two methods for removing the impurity gas exist at present, wherein one method is that high-purity helium gas is introduced for about ten minutes by using an insertion instrument with a double-hole needle, and a larger helium gas flow rate is needed for removing the impurity gas, so that the method is time-consuming and high in test cost; in the other method, the vacuum pump is used for vacuumizing the sample bottle, and the method is time-consuming and labor-consuming and has poor effect.
Disclosure of Invention
The invention provides a device for measuring the ratio of carbon stable isotopes in carbon dioxide, aiming at solving the technical problems that the removal of impurity gases in the prior art is time-consuming, high in cost and poor in effect when the ratio of the carbon stable isotopes in the carbon dioxide is measured.
The device for measuring the carbon stable isotope ratio in carbon dioxide consists of a positioning frame 1, a sample bottle 2, an air bag 3, a sealing gasket 4 and a sample bottle cap 5;
the positioning frame 1 consists of a positioning rod 1-1 and a clamping head 1-2; the positioning rod 1-1 is a cylinder, and a through hole 1-1-1 is formed in the positioning rod 1-1 along the axis direction; the clamping head 1-2 is a cylinder with a bottom on the end surface, and the circle center on the outer wall of the end surface with the bottom is fixed with one end of the positioning rod 1-1;
the sample bottle 2 consists of an upper end threaded port 2-3 and a lower end bottle body 2-2, the upper end threaded port 2-3 is fixed on the upper end face of the lower end bottle body 2-2, and the top of the side wall of the bottle body 2-2 is provided with a vent hole 2-1;
the sealing gasket 4 is a T-shaped rubber gasket and consists of a thin end 4-3 and a thick end 4-2, the thin end 4-3 and the thick end 4-2 are both cylinders and are coaxially fixed, a hollow cone 4-1 is arranged at the center of the end face of the thin end 4-3 of the sealing gasket 4, and the bottom surface of the hollow cone 4-1 is arranged on the end face of the thin end 4-3 of the sealing gasket 4;
the sample bottle cap 5 is a plastic cap with a hole 5-1 in the middle of the bottom surface, and threads are arranged inside the side wall of the sample bottle cap 5;
the air bag 3 is sleeved on the thin end 4-3 of the sealing gasket 4, the air bag 3 extends into the sample bottle 2, the thin end 4-3 of the sealing gasket 4 is clamped on the inner wall of the upper end threaded port 2-3 of the sample bottle 2, the sample bottle cap 5 is fixed with the upper end threaded port 2-3 of the sample bottle 2 through threads, and the clamping head 1-2 of the positioning frame 1 is sleeved on the outer wall of the sample bottle cap 5.
The use method of the device for determining the carbon stable isotope ratio in the carbon dioxide comprises the following steps:
firstly, removing impurity gas: inserting the needle head of the airtight needle into the through hole 1-1-1 in the positioning rod 1-1, penetrating the sealing gasket 4, pulling the piston of the airtight needle, pumping the gas in the air bag 3, introducing the external air from the vent hole 2-1, keeping the pressure balance inside and outside the sample bottle 2, and pulling out the airtight needle;
secondly, sample adding: inserting an airtight needle head into a sample air bag to extract sample gas, then inserting the airtight needle head into a through hole 1-1-1 in a positioning rod 1-1 to penetrate through a sealing gasket 4, wherein the needle point of the airtight needle head is just positioned in a hollow cone 4-1 on the sealing gasket 4 at the moment, preventing the needle point from puncturing an air bag 3, pushing a piston of the airtight needle, injecting the sample gas into the air bag 3, discharging air in a sample tube 2 from an air vent 2-1, keeping the pressure balance inside and outside the sample bottle 2, pulling out the airtight needle, and pulling out a positioning frame 1;
thirdly, sample determination: the sample bottle 2 added with the sample gas is placed on an automatic sample feeding rack, and the ratio of the carbon stable isotope in the carbon dioxide gas is measured by the combined use of the multipurpose sample preparation device and the stable isotope mass spectrometer.
The invention has the beneficial effects that:
the device of the invention is used for replacing the existing sample bottle, the test cost can be saved by 50 percent, and the time for exhausting the impurity gas and injecting the gas sample into the sample bottle can be saved by 50 percent;
the device has the advantages of ingenious design, reasonable structure, easy disassembly and assembly, convenient transportation and convenient use.
Drawings
FIG. 1 is a schematic view of an apparatus for determining a carbon stable isotope ratio in carbon dioxide according to a first embodiment in a natural state of an air bag;
FIG. 2 is a schematic diagram of an apparatus for determining the ratio of carbon stable isotopes in carbon dioxide according to a first embodiment when the gas bag is purged of miscellaneous gases;
FIG. 3 is a schematic diagram of the apparatus for determining the carbon stable isotope ratio in carbon dioxide according to the first embodiment when the gas bag is filled with the sample gas;
FIG. 4 is a schematic view of a gasket 4 according to a first embodiment;
FIG. 5 is a schematic view of a positioning frame 1 according to a first embodiment;
FIG. 6 is a schematic view of a sample vial 2 according to a first embodiment;
fig. 7 is a schematic front view of a sample bottle cap 5 according to a first embodiment;
fig. 8 is a schematic top view of a sample bottle cap 5 according to a first embodiment.
Detailed Description
The first embodiment is as follows: the embodiment is a device for measuring the ratio of carbon stable isotopes in carbon dioxide, and specifically comprises a positioning frame 1, a sample bottle 2, an air bag 3, a sealing gasket 4 and a sample bottle cap 5, as shown in fig. 1-8;
the positioning frame 1 consists of a positioning rod 1-1 and a clamping head 1-2; the positioning rod 1-1 is a cylinder, and a through hole 1-1-1 is formed in the positioning rod 1-1 along the axis direction; the clamping head 1-2 is a cylinder with a bottom on the end surface, and the circle center on the outer wall of the end surface with the bottom is fixed with one end of the positioning rod 1-1;
the sample bottle 2 consists of an upper end threaded port 2-3 and a lower end bottle body 2-2, the upper end threaded port 2-3 is fixed on the upper end face of the lower end bottle body 2-2, and the top of the side wall of the bottle body 2-2 is provided with a vent hole 2-1;
the sealing gasket 4 is a T-shaped rubber gasket and consists of a thin end 4-3 and a thick end 4-2, the thin end 4-3 and the thick end 4-2 are both cylinders and are coaxially fixed, a hollow cone 4-1 is arranged at the center of the end face of the thin end 4-3 of the sealing gasket 4, and the bottom surface of the hollow cone 4-1 is arranged on the end face of the thin end 4-3 of the sealing gasket 4;
the sample bottle cap 5 is a plastic cap with a hole 5-1 in the middle of the bottom surface, and threads are arranged inside the side wall of the sample bottle cap 5;
the air bag 3 is sleeved on the thin end 4-3 of the sealing gasket 4, the air bag 3 extends into the sample bottle 2, the thin end 4-3 of the sealing gasket 4 is clamped on the inner wall of the upper end threaded port 2-3 of the sample bottle 2, the sample bottle cap 5 is fixed with the upper end threaded port 2-3 of the sample bottle 2 through threads, and the clamping head 1-2 of the positioning frame 1 is sleeved on the outer wall of the sample bottle cap 5.
The method for using the device for measuring the carbon stable isotope ratio in carbon dioxide of the embodiment is as follows:
firstly, removing impurity gas: inserting the needle head of the airtight needle into the through hole 1-1-1 in the positioning rod 1-1, penetrating the sealing gasket 4, pulling the piston of the airtight needle, pumping the gas in the air bag 3, introducing the external air from the vent hole 2-1, keeping the pressure balance inside and outside the sample bottle 2, and pulling out the airtight needle;
secondly, sample adding: inserting an airtight needle head into a sample air bag to extract sample gas, then inserting the airtight needle head into a through hole 1-1-1 in a positioning rod 1-1 to penetrate through a sealing gasket 4, wherein the needle point of the airtight needle head is just positioned in a hollow cone 4-1 on the sealing gasket 4 at the moment, preventing the needle point from puncturing an air bag 3, pushing a piston of the airtight needle, injecting the sample gas into the air bag 3, discharging air in a sample tube 2 from an air vent 2-1, keeping the pressure balance inside and outside the sample bottle 2, pulling out the airtight needle, and pulling out a positioning frame 1;
thirdly, sample determination: the sample bottle 2 added with the sample gas is placed on an automatic sample feeding rack, and the ratio of the carbon stable isotope in the carbon dioxide gas is measured by the combined use of the multipurpose sample preparation device and the stable isotope mass spectrometer.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the air bag 3 is a latex balloon. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the sample bottle 2 is made of stainless steel. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the sample bottle 2 is made of high-silicon boron acid and alkali resistant glass. The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the sample bottle 2 is made of high-elasticity rubber. The rest is the same as one of the first to fourth embodiments.
The invention was verified with the following tests:
test one: the test is a device for measuring the ratio of carbon stable isotopes in carbon dioxide, and specifically comprises a positioning frame 1, a sample bottle 2, an air bag 3, a sealing gasket 4 and a sample bottle cap 5, as shown in figures 1-8;
the positioning frame 1 consists of a positioning rod 1-1 and a clamping head 1-2; the positioning rod 1-1 is a cylinder, and a through hole 1-1-1 is formed in the positioning rod 1-1 along the axis direction; the clamping head 1-2 is a cylinder with a bottom on the end surface, and the circle center on the outer wall of the end surface with the bottom is fixed with one end of the positioning rod 1-1;
the sample bottle 2 consists of an upper end threaded port 2-3 and a lower end bottle body 2-2, the upper end threaded port 2-3 is fixed on the upper end face of the lower end bottle body 2-2, and the top of the side wall of the bottle body 2-2 is provided with a vent hole 2-1;
the sealing gasket 4 is a T-shaped rubber gasket and consists of a thin end 4-3 and a thick end 4-2, the thin end 4-3 and the thick end 4-2 are both cylinders and are coaxially fixed, a hollow cone 4-1 is arranged at the center of the end face of the thin end 4-3 of the sealing gasket 4, and the bottom surface of the hollow cone 4-1 is arranged on the end face of the thin end 4-3 of the sealing gasket 4;
the sample bottle cap 5 is a plastic cap with a hole 5-1 in the middle of the bottom surface, and threads are arranged inside the side wall of the sample bottle cap 5;
the air bag 3 is sleeved on the thin end 4-3 of the sealing gasket 4, the air bag 3 extends into the sample bottle 2, the thin end 4-3 of the sealing gasket 4 is clamped on the inner wall of the upper end threaded port 2-3 of the sample bottle 2, the sample bottle cap 5 is fixed with the upper end threaded port 2-3 of the sample bottle 2 through threads, and the clamping head 1-2 of the positioning frame 1 is sleeved on the outer wall of the sample bottle cap 5.
The method of use of the apparatus for determining the carbon stable isotope ratio in carbon dioxide of this experiment was as follows:
firstly, removing impurity gas: inserting the needle head of the airtight needle into the through hole 1-1-1 in the positioning rod 1-1, penetrating the sealing gasket 4, pulling the piston of the airtight needle, pumping the gas in the air bag 3, introducing the external air from the vent hole 2-1, keeping the pressure balance inside and outside the sample bottle 2, and pulling out the airtight needle;
secondly, sample adding: inserting an airtight needle head into a sample air bag to extract sample gas, then inserting the airtight needle head into a through hole 1-1-1 in a positioning rod 1-1 to penetrate through a sealing gasket 4, wherein the needle point of the airtight needle head is just positioned in a hollow cone 4-1 on the sealing gasket 4 at the moment, preventing the needle point from puncturing an air bag 3, pushing a piston of the airtight needle, injecting the sample gas into the air bag 3, discharging air in a sample tube 2 from an air vent 2-1, keeping the pressure balance inside and outside the sample bottle 2, pulling out the airtight needle, and pulling out a positioning frame 1;
thirdly, sample determination: the sample bottle 2 added with the sample gas is placed on an automatic sample feeding rack, and the ratio of the carbon stable isotope in the carbon dioxide gas is measured by the combined use of the multipurpose sample preparation device and the stable isotope mass spectrometer.

Claims (5)

1. A device for measuring the ratio of carbon stable isotopes in carbon dioxide is characterized in that the device for measuring the ratio of the carbon stable isotopes in the carbon dioxide comprises a positioning frame (1), a sample bottle (2), an air bag (3), a sealing gasket (4) and a sample bottle cap (5); the positioning frame (1) consists of a positioning rod (1-1) and a clamping head (1-2); the positioning rod (1-1) is a cylinder, and a through hole (1-1-1) is formed in the positioning rod (1-1) along the axis direction; the clamping head (1-2) is a cylinder with an end surface with a bottom, and the circle center on the outer wall of the end surface with the bottom is fixed with one end of the positioning rod (1-1); the sample bottle (2) consists of an upper end threaded port (2-3) and a lower end bottle body (2-2), the upper end threaded port (2-3) is fixed on the upper end face of the lower end bottle body (2-2), and a vent hole (2-1) is formed in the top of the side wall of the bottle body (2-2); the sealing gasket (4) is a T-shaped rubber gasket and consists of a thin end (4-3) and a thick end (4-2), the thin end (4-3) and the thick end (4-2) are both cylinders and are coaxially fixed, a hollow cone (4-1) is arranged at the center of the end face of the thin end (4-3) of the sealing gasket (4), and the bottom face of the hollow cone (4-1) is arranged on the end face of the thin end (4-3) of the sealing gasket (4); the sample bottle cap (5) is a plastic cap with a hole (5-1) in the middle of the bottom surface, and threads are arranged inside the side wall of the sample bottle cap (5); the air bag (3) is sleeved on the thin end (4-3) of the sealing gasket (4), the air bag (3) extends into the sample bottle (2), the thin end (4-3) of the sealing gasket (4) is clamped on the inner wall of the upper threaded port (2-3) of the sample bottle (2), the sample bottle cap (5) is fixed with the upper threaded port (2-3) of the sample bottle (2) through threads, and the clamping head (1-2) of the positioning frame (1) is sleeved on the outer wall of the sample bottle cap (5);
the device for determining the carbon stable isotope ratio in carbon dioxide is used as follows:
removing miscellaneous gas: inserting a needle head of the airtight needle into a through hole (1-1-1) in a positioning rod (1-1), penetrating a sealing gasket (4), pulling a piston of the airtight needle, pumping the air in an air bag (3), introducing external air from a vent hole (2-1), keeping the pressure balance inside and outside a sample bottle (2), and pulling out the airtight needle;
sample adding: the airtight needle head is inserted into the sample air bag to extract sample air, then the airtight needle head is inserted into a through hole (1-1-1) in a positioning rod (1-1) to penetrate through a sealing gasket (4), the needle point of the airtight needle head is just positioned in a hollow cone (4-1) on the sealing gasket (4) at the moment, the air bag (3) is prevented from being punctured by the needle point, a piston of the airtight needle is pushed, the sample air is injected into the air bag (3), the air in the sample bottle (2) is discharged from a vent hole (2-1), the balance of the internal and external pressures of the sample bottle (2) is kept, and the airtight needle is pulled out;
and (3) sample determination: and (3) placing the sample bottle (2) added with the sample gas on an automatic sample feeding rack, and measuring the carbon stable isotope ratio in the carbon dioxide gas by using the multi-purpose sample preparation device and a stable isotope mass spectrometer.
2. An apparatus for determining the carbon stable isotope ratio in carbon dioxide as claimed in claim 1, characterized in that said balloon (3) is a latex balloon.
3. The apparatus for determining the carbon dioxide carbon stable isotope ratio according to claim 1, characterized in that the sample bottle (2) is made of stainless steel.
4. The device for determining the carbon stable isotope ratio in carbon dioxide according to claim 1, wherein the material of the sample bottle (2) is high silicon boron acid and alkali resistant glass.
5. The device for measuring the carbon dioxide stable isotope ratio according to claim 1, characterized in that the sample bottle (2) is made of elastomer.
CN201710610001.1A 2017-07-24 2017-07-24 Device for measuring carbon stable isotope ratio in carbon dioxide Expired - Fee Related CN107300498B (en)

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CN112305058A (en) * 2020-10-30 2021-02-02 上海化工研究院有限公司 Method for determining deuterium isotope abundance in water sample

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JP3464827B2 (en) * 1994-07-04 2003-11-10 株式会社鳥羽合成樹脂製作所 Sample vial
GB9623544D0 (en) * 1996-11-12 1997-01-08 Micromass Ltd Sample vial and vial closure device for use in gas analysis and method of using the same
CN101089619A (en) * 2006-06-14 2007-12-19 中国科学院大连化学物理研究所 Device for investigating low pressure easy explosion gas
CN201330012Y (en) * 2008-12-14 2009-10-21 史海刚 Pressure bottle
CN104634901B (en) * 2013-11-12 2017-11-21 中国石油化工股份有限公司 A kind of gas sample injection device and its application
CN203705228U (en) * 2014-03-07 2014-07-09 国家电网公司 Sulfur hexafluoride gas collecting device

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