CN112986447A - Gas chromatography device - Google Patents
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- CN112986447A CN112986447A CN202110439548.6A CN202110439548A CN112986447A CN 112986447 A CN112986447 A CN 112986447A CN 202110439548 A CN202110439548 A CN 202110439548A CN 112986447 A CN112986447 A CN 112986447A
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Abstract
The embodiment of the invention discloses a gas chromatography device, which comprises: a sample introduction part configured to: receiving a quantity of a sample gas carried by a first carrier gas, the sample gas comprising a hydrogen isotope component and an impurity component; the first chromatographic column is communicated with the sample injection part and is used for separating a hydrogen isotope component from an impurity component in the sample gas; a second chromatographic column for receiving the separated hydrogen isotope component and separating hydrogen isotopes in the hydrogen isotope component; a separation line for receiving the separated impurity components; a second carrier gas inlet line for providing a second carrier gas; a first switching section configured to introduce a second carrier gas into the hydrogen isotope component after the separated hydrogen isotope component flows out of the first chromatographic column to be carried into the second chromatographic column by the second carrier gas while introducing the separated impurity component into the separation line; and a gas analysis section for detecting and analyzing the gas component. The technical scheme of the invention can simplify the gas circuit.
Description
Technical Field
The invention relates to the technical field of radioactive gas detection, in particular to a gas chromatography analysis device.
Background
Tritium is a radioactive isotope of hydrogen, is an important strategic energy substance, and has important significance in other fields such as industry, national defense and scientific research. Since tritium has strong adsorption and memory effects, the hydrogen isotope content is generally analyzed by a gas chromatography method. In order to meet the detection requirements on hydrogen isotopes and impurities in tritium-containing gas, a gas chromatography system in the prior art has more gas circuits and more complex control.
Disclosure of Invention
The present invention provides a gas chromatography apparatus comprising:
a sample introduction part configured to: receiving a quantity of a sample gas carried by a first carrier gas, the sample gas comprising a hydrogen isotope component and an impurity component;
a first chromatographic column, which is communicated with the sample injection part and is used for separating the hydrogen isotope component from the impurity component in the sample gas, so that the separated hydrogen isotope component flows out of the first chromatographic column before the impurity component;
a second chromatographic column for receiving the separated hydrogen isotope component and separating hydrogen isotopes in the hydrogen isotope component;
a separation line for receiving the separated impurity components;
a second carrier gas inlet line for providing a second carrier gas;
a first switching section configured to introduce the second carrier gas into the hydrogen isotope component after the separated hydrogen isotope component flows out of the first chromatography column to carry the hydrogen isotope component with the second carrier gas into the second chromatography column while introducing the separated impurity component into the separation line; and
and the gas analysis part is used for detecting and analyzing the gas components flowing into the gas analysis part.
Drawings
Other objects and advantages of the present invention will become apparent from the following description of the invention which refers to the accompanying drawings, and may assist in a comprehensive understanding of the invention.
FIG. 1 is a schematic gas circuit diagram of a gas chromatography apparatus according to an embodiment of the invention;
FIG. 2 is a schematic diagram of a gas path for separating hydrogen isotopes and impurity components from a sample gas using the gas chromatography apparatus shown in FIG. 1;
fig. 3 is a schematic gas path diagram for detecting hydrogen isotopes after the separated hydrogen isotopes and impurity components are cut by the gas chromatography apparatus shown in fig. 1;
fig. 4 is a schematic gas path diagram for detecting impurities after the separated hydrogen isotopes and impurity components are cut by the gas chromatography apparatus shown in fig. 1;
FIG. 5 is an enlarged view of a portion of the seal box of FIG. 1;
FIG. 6 is a block diagram showing the structure of a gas chromatography apparatus according to an embodiment of the present invention;
fig. 7 is a chromatogram of a hydrogen isotope component and an impurity component obtained by the gas chromatography analysis apparatus of the embodiment of the invention; and
fig. 8 is a chromatogram of another set of hydrogen isotope components and impurity components obtained by the gas chromatography analysis apparatus according to the embodiment of the invention.
It is noted that the drawings are not necessarily to scale and are merely illustrative in nature and not intended to obscure the reader.
Description of reference numerals:
11. a first chromatographic column; 12. a second chromatography column; 121. a liquid nitrogen tank; 21. a first carrier gas inlet line; 20. a joint; 201. an electronic flow controller; 202. a damping pipeline; 22. a second carrier gas inlet line; 221. a damping pipeline; 23. separating the pipeline; 231. a damping pipeline; 24. a recovery pipeline; 31. a first switching section; 32. a second switching unit; 33. a sample injection valve; 40. a gas analysis section; 41. a plasma emission detector; 42. a thermal conductivity detector; 51. a sample inlet line; 511. a valve; 52. a quantitative section; 53. an air extraction pipeline; 531. a valve; 54. a vacuum pumping device; 55. a pressure sensor; 60. a sealing box; 61. a temperature sensor; 70. a control device; 80. and a gas carrying tank.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention. It should be apparent that the described embodiment is one embodiment of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention without any inventive step, are within the scope of protection of the invention.
It is to be noted that technical terms or scientific terms used herein should have the ordinary meaning as understood by those having ordinary skill in the art to which the present invention belongs, unless otherwise defined. If the description "first", "second", etc. is referred to throughout, the description of "first", "second", etc. is used only for distinguishing similar objects, and is not to be construed as indicating or implying a relative importance, order or number of technical features indicated, it being understood that the data described in "first", "second", etc. may be interchanged where appropriate.
Fig. 1 is a schematic gas circuit diagram of a gas chromatography apparatus according to an embodiment of the present invention. Referring to fig. 1, the gas chromatography apparatus includes: the sample injection section, the first chromatography column 11, the second chromatography column 12, the separation line 23, the second carrier gas inlet line 22, the first switching section 31, and the gas analysis section 40.
The gas analyzing section 40 is used for detecting and analyzing the gas components flowing therein.
The sample introduction part may be configured to: a quantity of a sample gas carried by a first carrier gas is received, the sample gas including a hydrogen isotope component and an impurity component. As will be readily understood by those skilled in the art, the hydrogen isotope component of the sample gas will typically comprise H2、D2、T2HD, HT, DT; the impurity component typically comprises N2、CH4CO, etc.
The first chromatographic column 11 is communicated with the sample injection part, and is used for separating the hydrogen isotope component from the impurity component in the sample gas, so that the separated hydrogen isotope component flows out of the first chromatographic column 11 before the impurity component. In other words, the first column 11 allows the hydrogen isotope component mixed in the sample gas to flow out of the first column 11 simultaneously with the impurity component, that is, allows the hydrogen isotope component to flow out of the first column 11 first and then allows the impurity component to flow out of the first column 11. The time for the impurity components and isotope components to flow out of the first chromatography column 11 can be adjusted by controlling the flow rate of the first carrier gas and the temperature of the first chromatography column 11.
It is easily understood by those skilled in the art that the first chromatographic column 11 can separate the hydrogen isotope component from the impurity component and the N in the impurity component2、CH4CO and the like are separated from each other; but the various hydrogen isotopes in the hydrogen isotope component cannot be separated from each other. It is easily understood that since the impurity components can be separated by the first chromatographic column 11, the impurity components flowing out of the first chromatographic column 11 can be directly introduced into the gas analyzing section 40 for analysis.
The separation line 23 is used to receive the separated impurity components. A secondary carrier gas inlet line 22 is used to provide a secondary carrier gas.
The first switching section 31 is configured to introduce the second carrier gas into the hydrogen isotope component after the separated hydrogen isotope component (i.e., the hydrogen isotope component flowing out of the first chromatographic column 11) flows out of the first chromatographic column 11 to carry the hydrogen isotope component into the second chromatographic column 12 with the second carrier gas, while introducing the separated impurity component (i.e., the impurity component flowing out of the first chromatographic column 11) into the separation line 23.
Those skilled in the art will readily appreciate that the secondary carrier gas inlet line 22 will provide secondary carrier gas continuously after the gas chromatography apparatus is powered on. Before the first switching part 31 introduces the second carrier gas into the hydrogen isotope component (i.e. before the second carrier gas is introduced into the gas path in which the separated hydrogen isotope component is located), the second carrier gas flows through other gas paths and enters the recovery system of the gas chromatography apparatus.
The second chromatographic column 12 is adapted to receive the separated hydrogen isotope fraction and to convert the hydrogenHydrogen isotopes in the isotope components are separated. In other words, the second column 12 allows different hydrogen isotopes to flow out of the second column 12 in a time-division manner. I.e. hydrogen isotopes (including H) from the second column 122、D2、T2At least two of HD, HT, and DT) are discharged from the second chromatographic column 12 in time divisions, and the hydrogen isotopes discharged in time divisions may be introduced into the gas analysis section 40 for detection and analysis.
Since the hydrogen isotope component flows out of the first chromatographic column 11 first and the impurity component flows out of the first chromatographic column 11 later, in the embodiment of the present application, after the hydrogen isotope component is separated from the first chromatographic column 11, the impurity component coming out of the first chromatographic column 11 is introduced into the separation pipeline 23 by using the first switching portion 31, so that the isotope component and the impurity component in the sample gas are respectively introduced into different gas paths. That is, in the embodiment of the present application, the first switching portion 31 is used to perform gas path cutting on the separated hydrogen isotope component and the impurity component, so that the separated hydrogen isotope component flows into the second chromatographic column 12, and the separated impurity component flows into the separation line 23. Thereby, the impurity components can be prevented from entering the second chromatography column 12, reducing the separation ability of the second chromatography column 12.
In some embodiments, the first switching part 31 may also be configured to introduce the second carrier gas into the second chromatography column 12 after the separated hydrogen isotope component flows into the second chromatography column 12, while introducing the separated impurity component (i.e., the impurity component flowing out of the first chromatography column 11) into the separation line 23. The time point at which the first switching portion 31 performs the air path cutting may be determined experimentally. For example, the gas analysis unit 40 may test the peak appearance time of the last hydrogen isotope exiting from the first column 11 and the peak appearance time of the impurity element exiting from the first column 11 in advance, and select a time point between the peak appearance times to perform gas path cutting.
Because first switching portion 31 introduces the impurity component that first carrier gas carried into separation pipeline 23 when accomplishing the gas circuit cutting to still introduce the second carrier gas in the isotope component, thereby make this application embodiment accessible once advance the appearance and can realize measuring respectively impurity component and isotope component, also make gas chromatography analytical equipment's gas circuit set up less simultaneously, control is simple.
In some embodiments, the first switching portion 31 may be configured to have a first operating state and a second operating state. When the first switching portion 31 is in the first operating state, the second chromatography column 12 communicates with the first chromatography column 11, and the second carrier gas inlet line 22 communicates with the separation line 23. In this operating state, the gas flowing out of the first column 11 can flow directly to the second column 12; the second carrier gas then flows into the separation line 23.
When the first switching portion 31 is in the second operating state, the second chromatography column 12 is communicated with the second carrier gas inlet line 22; and the first chromatographic column 11 is communicated with the separation line 23. In this operating state, the second carrier gas flows to the second chromatography column 12; the gas flowing out of the first column 11 flows into the separation line 23. Thus, the first switching unit 31 has the two operating states, and thus the air passage is divided.
In some embodiments, the first switching part 31 is set to the first operating state before the sample gas enters the first chromatographic column 11, so that the separated hydrogen isotope component can flow into the second chromatographic column 12 after the sample gas enters the first chromatographic column 11; after the isotopic element component flows out of the first chromatographic column 11 and before the impurity component flows out, the first switching portion 31 is switched to the second operating state, so that the impurity component flowing out of the first chromatographic column 11 enters the separation line 23 to divide the hydrogen isotopic element component and the impurity component into two gas paths.
Referring to fig. 1, the first switching part 31 includes a first port, a second port, a third port, and a fourth port. The first port of the first switching portion 31 communicates with the second column 12; the second port of the first switching portion 31 communicates with the second carrier gas intake conduit 22; the third port of the first switching portion 31 communicates with the separation line 23; the fourth port of the first switching portion 31 communicates with the first column 11. When the first switching portion 31 is in the first working state (see fig. 2), the first port is conducted with the fourth port, and the second port is conducted with the third port; when the first switching unit 31 is in the second operating state (see fig. 1, 3, and 4), the first port is in communication with the second port, and the third port is in communication with the fourth port.
In some embodiments, the first switching portion 31 is a four-way valve. In other embodiments, the first switching unit 31 may have more than five ports, four ports are used as the first port, the second port, the third port and the fourth port, and the rest of the ports may be left unused or have other purposes.
A damper line 221 may be provided on the secondary carrier gas inlet line 22 for adjusting the flow rate of the secondary carrier gas.
In some embodiments, the first chromatography column 11 may be a molecular sieve column.
In some embodiments, the second chromatography column 12 may be a modified alumina column.
In some embodiments, the modified alumina column can be made in the following manner. Mixing alumina powder and manganese chloride column powder according to a mass ratio of 19:100 to prepare a suspension, coating and modifying the suspension, and screening Al with the particle size of 90-110 meshes2O3/MnCl2Modifying powder, loading into a stainless steel column, aging the obtained packed column, and placing in a liquid nitrogen temperature-controlled environment; the preparation method of the liquid nitrogen temperature-controlled alumina-manganese chloride coating modified capillary column comprises the steps of preparing manganese chloride powder and distilled water into a solution according to a ratio of 19:100, then coating and modifying an alumina capillary column by using the solution, aging the obtained capillary column, and placing the aged capillary column in a liquid nitrogen temperature-controlled environment. Those skilled in the art will readily understand that the method for fabricating the modified alumina column is not limited in the embodiments of the present application, that is, any modified alumina column capable of separating hydrogen isotopes in the prior art can be used as the second chromatographic column 12 in the embodiments of the present application.
Those skilled in the art will readily understand that it is difficult for the second chromatography column 12 to separate hydrogen isotopes at normal temperatures, and therefore, in the present embodiment, the second chromatography column 12 is in a liquid nitrogen environment. Referring to FIG. 1, the second chromatography column 12 is in a liquid nitrogen tank 121.
In some embodiments of the present application, the gas analysis section 40 may include a Plasma Emission Detector (PED) 41. In other embodiments, the gas analysis section 40 may include a Thermal Conductivity Detector (TCD) 42.
In a preferred embodiment of the present application, the gas analysis section 40 may include PED41 and TCD42 in series.
PED has the characteristic of small dead volume, can test ppm-level gas, and has the detection range of 10-9-100%. The detection principle of PED is that light with different wavelengths is emitted in the plasma environment according to different components, and the interference of other components is avoided to the greatest extent by utilizing the selective optical filter in combination with the gas path design of the embodiment of the application.
TCD can test for percent gas. The detection principle is based on the fact that different gas components and carrier gases have different heat conductivities, when the composition and concentration of a thermal conductivity cell body change, the temperature on a thermosensitive element changes, resistance value changes caused by the temperature change can be measured through a Wheatstone bridge, and the content of each component can be measured according to the size of an obtained signal. TCD was detected in the range of 1000ppm to 100% content. During TCD detection, high-purity light gas is selected as carrier gas (in the embodiment of the application, the carrier gas can be high-purity neon), and the lower temperature of the cell body is selected, so that the analysis sensitivity can be improved.
According to the embodiment of the application, the measuring range of the detection gas is expanded by arranging the PED41 and the TCD42 which are connected in series, so that the detection of the tritium-containing gas with percentage content in the tritium extraction process and the trace H in the tritium-containing gas with high concentration in the tritium storage process can be realized2Detection of HT and impurity components.
In some embodiments, the gas chromatography apparatus may have two gas analysis portions 40 respectively communicating with the second chromatography column 12 and the separation line 23 to respectively measure the contents of the hydrogen isotope and the impurity.
In other embodiments, the gas chromatography apparatus is provided with only one gas analysis portion 40, and in such embodiments, the gas chromatography apparatus may further include: a second switching section 32 configured to: introducing the separated hydrogen isotopes (i.e., the hydrogen isotopes from the second chromatographic column 12 or the hydrogen isotopes flowing out of the second chromatographic column 12) into the gas analysis section 40; or the separated impurity components (i.e., the impurity components from the separation line 23 or the impurity components flowing out from the separation line 23) are introduced into the gas analysis section 40.
Those skilled in the art will readily understand that in such embodiments, the timing of the hydrogen isotopes and impurities entering the gas analysis portion 40 may be adjusted by setting the path lengths or gas flow rates of the hydrogen isotope gas path and the impurity gas path. The hydrogen isotope may be introduced into the gas analysis unit 40 first, or the impurity may be introduced into the gas analysis unit 40 first. In one embodiment of the present application, the impurities may be introduced into the gas analysis portion 40 first, and then the hydrogen isotopes may be introduced into the gas analysis portion 40.
In some embodiments, the separation line 23 is provided with a damping line 231, which can be used to reduce the flow rate of the gas in the gas path. The appropriate gas flow rate may be determined by selecting the amount and length of damping from damping line 231.
In some embodiments, the gas chromatography apparatus further comprises: a recovery line 24 in communication with the recovery system.
The second switching portion 32 is configured to have a first operating state and a second operating state. When the second switching portion 32 is in the first operating state, the separation line 23 communicates with the recovery line 24, and the second column 12 communicates with the gas analyzing portion 40. In this operating state, the gas flowing out of the second column 12 can directly flow into the gas analyzing section 40; the first carrier gas in the separation line 23 flows into the recovery line 24. It is easily understood by those skilled in the art that the impurity components cannot flow into the recovery line 24 because of the need to perform a detection analysis on the impurity components. When the second switching portion 32 is in the first operation state, the impurity components have either not flowed out of the first column 11 or flowed into the gas analyzing portion 40 to be analyzed.
When the second switching portion 32 is in the second operation state, the second column 12 is communicated with the recovery line 24; and the separation line 23 communicates with the gas analysis portion 40. In this operating state, the gas flowing out of the separation line 23 can directly flow into the gas analysis portion 40. The second carrier gas from the second chromatography column 12 flows into the recovery line 24. It is easily understood by those skilled in the art that the hydrogen isotope cannot flow into the recovery line 24 because of the need to perform detection analysis on the hydrogen isotope. When the second switching portion 32 is in the second operating state, the hydrogen isotopes either have not flowed out of the second chromatographic column 12 or have flowed into the gas analyzing portion 40 to complete the analysis.
In some embodiments, the time when the impurity component and the hydrogen isotope component reach the gas analysis portion 40 can be adjusted by adjusting the length of the gas path and the flow rate of the carrier gas, then the second switching portion 32 is first set to an operating state that enables the gas path where the gas component that reaches the gas analysis portion 40 first is in communication with the gas analysis portion 40, and after the detection and analysis of the gas component are completed, the operating state of the second switching portion 32 is switched to perform the detection and analysis of another gas component.
Referring to fig. 1, the second switching part 32 includes a first port, a second port, a third port, and a fourth port. The first port of the second switching portion 32 and the recovery line 24; the second port of the second switching portion 32 communicates with the second column 12; the third port of the second switching unit 32 communicates with the gas analyzing unit 40; the fourth port of the second switching portion 32 communicates with the separation line 23; when the second switching part 32 is in the first operating state (see fig. 1, 2 and 3), the first port is conducted with the fourth port, and the second port is conducted with the third port; when the second switching part 32 is in the second operating state (see fig. 4), the first port is conducted with the second port, and the third port is conducted with the fourth port.
In some embodiments, the second switching portion 32 is a four-way valve. In other embodiments, the second switch 32 may have more than five ports, four of the ports are the first port, the second port, the third port and the fourth port, and the rest of the ports may be idle or have other purposes.
In some embodiments, the sample introduction portion may comprise: a sample inlet line 51, a first carrier gas inlet line 21, a quantifying section 52, and an injection valve 33.
The sample gas inlet line 51 is used for introducing sample gas.
The primary carrier gas inlet line 21 is for supplying a primary carrier gas. The first carrier gas inlet line 21 is provided with a flow rate adjusting member for adjusting the flow rate of the first carrier gas. The flow regulating element may include a damper line 202 and/or an electronic flow controller 201. For example, when the gas path of the first carrier gas needs to flow through the first separation column 11 and the second separation column 12 in sequence (i.e., when the first switching portion 31 is in the first operating state), the flow rate of the first carrier gas is increased by the electronic flow controller 201; when the gas path of the first carrier gas only needs to flow through the first separation column 11 (i.e., when the first switching portion 31 is in the second operating state), the flow rate of the first carrier gas is adjusted to be small by the electronic flow controller 201.
The quantitative section 52 quantifies the sample gas.
Specifically, when the quantifying portion 52 communicates with the sample intake pipe 51, the sample gas enters the quantifying portion 52. When the quantitative section 52 is filled with the sample gas (for example, the sample injection time or the pressure indication of the pressure sensor 55 mentioned later), the injection valve 33 is switched to communicate the quantitative section 52 with the first carrier gas inlet line 21 and the first column 11, and the first carrier gas carries the sample gas in the quantitative section 52 into the first column 11.
When the sample injection valve 33 is in the second working state, two ends of the quantitative part 52 are respectively communicated with the first carrier gas inlet pipeline 21 and the first chromatographic column 11, and the sample inlet pipeline 51 is closed. In this operating state, the sample gas in the quantitative section 52 is carried by the first carrier gas into the first chromatographic column 11, that is, the sample gas carried by the first carrier gas in a fixed amount into the first chromatographic column 11 is realized.
In some embodiments, before sampling, the sampling valve 33 is set to the first working state, so that the sample gas enters the quantitative part 52; when the sample gas in the quantitative section 52 is full, the injection valve 33 is switched to the second operating state, so that the first carrier gas carries the quantitative sample gas into the first chromatographic column 11.
Referring to fig. 1, the sample valve 33 includes a first port, a second port, a third port, a fourth port, a fifth port, and a sixth port. The first port communicates with the first chromatographic column 11; the second port and the fifth port are respectively communicated with both ends of the quantitative section 52; the third port is a closed end; the fourth port communicates with the sample inlet line 51; the sixth port communicates with the first carrier gas inlet line 21.
When the sample injection valve 33 is in the first working state (see fig. 1), the first port is communicated with the sixth port, the second port is communicated with the third port, and the fourth port is communicated with the fifth port;
when the sample valve 33 is in the second working state (see fig. 2 to 4), the first port is conducted with the second port, the third port is conducted with the fourth port, and the fifth port is conducted with the sixth port.
In some embodiments, sample injection valve 33 is a six-way valve. In other embodiments, the sample valve 33 may also have more than seven ports, wherein six ports are used as the first port, the second port, the third port, the fourth port, the fifth port and the sixth port, and the rest of the ports may be left unused or have other uses.
The gas chromatography apparatus further comprises: and the air suction pipeline 53 and the sample air inlet pipeline 51 are jointly communicated with the fourth port of the sample injection valve 33. Referring to fig. 1, the air suction line 53 and the sample inlet line 51 may communicate with the fourth port of the injection valve 33 through a common line. A valve 531 may be provided on the suction line 53 and a valve 511 may be provided on the sample inlet line 51.
When the sample injection valve 33 is in the first working state, the valve 511 of the sample inlet pipeline 51 is closed, and the valve 531 of the air suction pipeline 53 is opened, the air suction pipeline 53 and the air path of the quantitative portion 52 may be firstly vacuumized by the vacuum pumping device 54, so that the air path of the quantitative portion 52 is in a vacuum state, then the valve 531 of the air suction pipeline 53 is closed, and the valve 511 of the sample inlet pipeline 51 is opened, so that the sample gas can enter the quantitative portion 52.
The gas chromatography apparatus further comprises: a vacuum-pumping device 54, in communication with the suction line 53, configured to: when the sample injection valve 33 is in the first working state, the valve 511 of the sample inlet pipeline 51 is closed, and the valve 531 of the air suction pipeline 53 is opened (i.e. before the sample inlet pipeline 51 injects the sample into the quantitative part 52), the air channels of the air suction pipeline 53 and the quantitative part 52 are controlled to be evacuated. Therefore, when the vacuum pumping is finished, the sample inlet pipeline 51 is communicated with the quantitative part 52, sample introduction of sample gas under negative pressure can be realized, further loss and leakage of high-dose gas are reduced, and personnel can be prevented from being exposed to overdose due to small gas sample introduction amount. Before the sample is introduced into the quantitative section 52 again, the quantitative section 52 may be cleaned by evacuating the quantitative section 52 by the evacuation device 54, that is, the sample gas remaining in the quantitative section 52 may be removed.
The gas chromatography apparatus further comprises: and the pressure sensor 55 is used for detecting the air pressure of the air paths of the sample air inlet pipeline 51 and the quantitative part 52 when the sample air inlet pipeline 51 is communicated with the quantitative part 52, so that the content of each component in the sample gas is determined according to the air pressure of the sample gas and the air pressure of the standard gas.
Referring to fig. 1 to 5, the gas chromatography apparatus further includes: a sealing box 60 filled with a shielding gas; the quantitative section 52, the injection valve 33, the first switching section 31, and the second switching section 32 may be disposed in the seal box 60. Through setting up seal box 60, can prevent that the air from getting into sample valve 33, first switching portion 31, inside second switching portion 32, preventing that it from causing the pollution to the gas that awaits measuring, influencing the accuracy that detects.
Both the valve 531 of the suction line 53 and the valve 511 of the sample intake line 51 may be provided in the hermetic container 60, thereby preventing air from entering the valve 531 and the valve 511.
The first carrier gas, the second carrier gas, and the shielding gas may be the same gas, and may be, for example, high purity neon. The primary carrier gas, secondary carrier gas, and shielding gas may be from the same carrier gas tank 80, connected by the connection 20. A two-stage purifier can be arranged between the carrier gas tank 80 and the joint 20 to purify high-purity Ne (5N) into ultra-pure Ne (7N-8N), and then the ultra-pure Ne can enter the first carrier gas inlet pipeline 21, so that the base line of PED41 is stable and the noise value is low. Those skilled in the art will readily appreciate that for a gas chromatography apparatus, carrier gas tank 80 will continue to supply primary and secondary carrier gases to primary and secondary carrier gas inlet lines 21, 22 from its start-up.
The gas chromatography apparatus further comprises: and a temperature sensor 61 for detecting the temperature inside the hermetic container 60. Temperature sensor 61 is used for making the temperature in seal box 60 stable (T), and rethread pressure sensor 55 makes the invariable (P) of pressure of the gas circuit that ration portion 52 belongs to, because the quantitative volume of ration portion 52 is invariable (V), can know according to krebs's equation n ═ PV/RT, and the quantitative gaseous material's of ration portion 52 quantity is invariable, so set up and can improve the accuracy that gas chromatography analytical equipment measured for the data of different periods of testing have comparability.
Referring to fig. 6, the gas chromatography apparatus further includes: a control device 70 configured to: according to the received command, the switching of the sample injection valve 33, the first switching part 31 and the second switching part 32 is controlled, and the on-off of the vacuum pumping device 54 is controlled.
In some embodiments, the control device 70 may also control the valve 531 of the suction line 53 and the valve 511 of the sample inlet line 51.
In some embodiments, the control device 70 is further configured to: controlling the sample injection valve 33 to be in a first working state according to the received cleaning instruction, and controlling the vacuumizing device 54 to vacuumize the gas path where the quantitative part 52 is located; and controlling the first switching unit 31 to be in the second operation state and the second switching unit 32 to be in the first operation state, so as to purge the first column 11 with the first carrier gas supplied from the first carrier gas inlet line 21, and purge the second column 12 and the gas analyzing unit 40 with the second carrier gas supplied from the second carrier gas inlet line 22.
When the control device 70 receives the cleaning instruction, the sample valve 33, the first switching unit 31, and the second switching unit 32 are switched to the states shown in fig. 1. Referring to fig. 1, at this time, the gas path of the quantitative portion 52 is vacuumized by the vacuum pumping device 54, so as to clean the gas path of the quantitative portion 52; the first carrier gas sequentially flows through the sixth port and the first port of the injection valve 33, the first chromatographic column 11, the fourth port and the third port of the first switching part 31, the separation pipeline 23, the fourth port and the first port of the second switching part 32 and the recovery pipeline 24 to enter the recovery system, so that the sixth port and the first port of the injection valve 33, the first chromatographic column 11, the fourth port and the third port of the first switching part 31, the separation pipeline 23, the fourth port and the first port of the second switching part 32 and the recovery pipeline 24 are cleaned; the second carrier gas flows through the second and first ports of the first switching unit 31, the second chromatographic column 12, the second and third ports of the second switching unit 32, the TCD42, and the PED41 in this order, and enters the recovery system, thereby cleaning the second and first ports of the first switching unit 31, the second and third ports of the second chromatographic column 12, and the second switching unit 32, the TCD42, and the PED 41.
Therefore, the gas path of the gas chromatography device is specially designed, and the cleaning operation of different gas paths of the gas chromatography device can be realized at the same time. Therefore, the gas chromatography device provided by the embodiment of the application is simple in gas path, convenient to switch and convenient to clean.
As will be readily understood by those skilled in the art, when the air path of the quantitative section 52 is evacuated, the control device 70 controls to open the valve 531 of the evacuation line 53 and close the valve 511 of the sample air inlet line 51.
In some embodiments, the control device 70 is further configured to: switching of the sample injection valve 33, the first switching unit 31, and the second switching unit 32 is adjusted and controlled at four times in accordance with the received detection command.
Specifically, at a first time after receiving the detection instruction, the sample injection valve 33 is controlled to be in the first working state, the first switching unit 31 is controlled to be in the first working state or the second working state (either one of the two is selected), and the second switching unit 32 is controlled to be in the first working state or the second working state (either one of the two is selected).
At this stage, the sample gas enters the quantitative section 52. The first carrier gas enters the first separation column 11 and then flows into one of the second separation column 12 and the recovery line 24, and the second carrier gas flows into the other of the second separation column 12 and the recovery line 24.
In some embodiments, after the control device 70 receives the detection command, the sample injection valve 33, the first switching portion 31 and the second switching portion 32 may be switched to the states shown in fig. 1.
At a second time point after receiving the detection command (i.e., after a first predetermined time after the first time point), the second time point is usually a time point (or a time point slightly after) at which the quantitative section 52 is filled with the sample gas. The sample injection valve 33 is controlled to be in the second working state, the first switching part 31 is controlled to be in the first working state, and the second switching part 32 is controlled to be in the first working state or in the second working state (either one of the two is selected).
At this stage, the first carrier gas carries the sample gas in the quantitative section 52 into the first separation column 11, the first separation column 11 separates the hydrogen isotope component and the impurity component in the sample gas, and the first separated hydrogen isotope component and the first carrier gas flow into the second separation column 12; the second carrier gas then flows into the separation line 23.
In some embodiments, after the control device 70 receives the detection command at the second time, the sample injection valve 33, the first switching part 31, and the second switching part 32 may be switched from the state shown in fig. 1 to the state shown in fig. 2.
At a third time after receiving the detection instruction (i.e., after a second preset time after the second time), the third time is generally between the time when the isotope component exits from the first separation column 11 and the time before the impurity component exits from the first separation column 11. The sample injection valve 33 is controlled to be in the second working state, the first switching part 31 is controlled to be in the second working state, and the second switching part 32 is controlled to be in the first working state or the second working state.
At this stage, the hydrogen isotope component carried by the second carrier gas is separated in the second separation column 12, and the impurity component carried by the first carrier gas enters the separation line 23.
At this stage, whether the second switching part 32 is in the first operation state or the second operation state can be determined based on the timing when the impurities enter the gas analysis part 40 from the first chromatographic column 11 and the timing when the hydrogen isotopes enter the gas analysis part 40 from the second chromatographic column 12. In a specific embodiment, the time when the impurity enters the gas analysis portion 40 is earlier than the time when the hydrogen isotope enters the gas analysis portion 40 (and the time difference between the two times is long, and the hydrogen isotope will not flow out of the second separation column 12 until the impurity component is detected after all of the impurity component enters the gas analysis portion 40), the second switching portion 32 is controlled to be in the second operation state, and the impurity component is detected first. Otherwise, if the time when the impurity enters the gas analysis unit 40 is later than the time when the hydrogen isotope enters the gas analysis unit 40, the second switching unit 32 is set to the first operation state, and the hydrogen isotope is detected first.
In some embodiments, after the third time after the control device 70 receives the detection instruction, the sample injection valve 33, the first switching part 31, and the second switching part 32 may be switched from the state shown in fig. 2 to the state shown in fig. 3 or fig. 4. In fig. 3, a gas analyzing section 40 communicates with the second chromatographic column 12 to perform detection analysis of hydrogen isotopes; in fig. 4, the gas analyzing section 40 communicates with the separation line 23 to perform detection analysis of impurities.
Accordingly, at a fourth time (i.e., after a third preset time after the third time) after the detection instruction is received, the fourth time is generally later than the time when the detection of the hydrogen isotope is completed or the detection of the impurity component is completed, i.e., the time when the component that reaches the gas analysis portion 40 first has been detected and the other component has not yet arrived, the sample injection valve 33 is maintained in the second working state, the first switching portion 31 is maintained in the second working state, and only the working state of the second switching portion 32 needs to be controlled to be switched. That is, at the fourth timing, only the operating state of the second switching unit 32 is switched, and another gas that has not been detected is detected. In a specific embodiment, the time when the impurity enters the gas analysis portion 40 is earlier than the time when the hydrogen isotope enters the gas analysis portion 40, the second switching portion 32 may be controlled to be in the second working state at a third time after the detection instruction is received (i.e. after a second preset time after the second time), and the impurity component is detected first; and controlling the second switching part (32) to be in the first working state at a fourth moment after receiving the detection instruction (namely after a third preset time after the third moment), and detecting the hydrogen isotope.
In the embodiment of the present application, after the impurity component and the hydrogen isotope component are detected and analyzed in the gas analyzing section 40, a tritium-containing gas detection chromatogram can be obtained. Fig. 7 and 8 are graphs obtained under laboratory conditions using a gas chromatography apparatus according to an embodiment of the present invention in which the first column 11 is a 2m molecular sieve column and the second column 12 is a 4m × 3.175mm modified alumina column, for hydrogen isotope components and impurity components in two groups. Those skilled in the art will readily understand that deuterium gas can only be used in place of tritium gas in the laboratory for analytical detection of hydrogen-containing isotope gas using a gas chromatography apparatus. FIG. 7 is a chromatogram of trace hydrogen (content 100ppm) and impurity components (both content about 10ppm) in deuterium, and FIG. 8 is a chromatogram of percent hydrogen deuterium component (content about 50%) and trace impurity components. As can be seen from fig. 7 and 8, the gas chromatography device according to the embodiment of the present application has a wide range of measurement ranges and is accurate in measurement.
The gas chromatography analysis device provided by the embodiment of the invention has an optimized gas path layout and control mode, can automatically switch the communication mode of the gas pipeline in the gas chromatography analysis device in a centralized control mode, and provides corresponding gas paths required by different operation processes of the gas chromatography analysis device. The centralized control mode of the invention reuses the gas circuit in the gas chromatography device as much as possible, thereby not only simplifying the gas circuit arrangement in the gas chromatography device, but also reducing the complexity of gas circuit control.
It should also be noted that, in the case of the embodiments of the present invention, features of the embodiments and examples may be combined with each other to obtain a new embodiment without conflict.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and the scope of the present invention is subject to the scope of the claims.
Claims (29)
1. A gas chromatography apparatus, comprising:
a sample introduction part configured to: receiving a quantity of a sample gas carried by a first carrier gas, the sample gas comprising a hydrogen isotope component and an impurity component;
a first chromatographic column (11) communicated with the sample introduction part and used for separating the hydrogen isotope component from the impurity component in the sample gas so as to enable the separated hydrogen isotope component to flow out of the first chromatographic column (11) before the impurity component;
a second chromatographic column (12) for receiving the separated hydrogen isotope component and separating hydrogen isotopes in the hydrogen isotope component;
a separation line (23) for receiving the separated impurity components;
a second carrier gas inlet line (22) for providing a second carrier gas;
a first switching section (31) configured to introduce the second carrier gas into the hydrogen isotope component after the separated hydrogen isotope component flows out of the first chromatography column (11) to carry the hydrogen isotope component with the second carrier gas into the second chromatography column (12) while introducing the separated impurity component into the separation line (23); and
and a gas analysis section (40) for detecting and analyzing the gas component flowing therein.
2. The apparatus of claim 1,
the first switching section (31) is configured to have a first operating state and a second operating state, wherein
When the first switching section (31) is in a first operating state, the second chromatography column (12) is in communication with the first chromatography column (11) and the second carrier gas inlet line (22) is in communication with the separation line (23);
when the first switching part (31) is in a second working state, the second chromatographic column (12) is communicated with the second carrier gas inlet pipeline (22); and the first chromatographic column (11) is communicated with the separation pipeline (23).
3. The apparatus of claim 2,
the first switching section (31) includes a first port, a second port, a third port, and a fourth port; wherein
A first port of the first switching portion (31) communicates with the second chromatography column (12);
a second port of the first switching portion (31) communicates with the second carrier gas intake line (22);
a third port of the first switching portion (31) communicates with the separation line (23);
a fourth port of the first switching portion (31) communicates with the first chromatographic column (11);
when the first switching part (31) is in a first working state, the first port is communicated with the fourth port, and the second port is communicated with the third port;
when the first switching part (31) is in the second working state, the first port is communicated with the second port, and the third port is communicated with the fourth port.
4. The device according to claim 3, wherein the first switching portion (31) is a four-way valve.
5. The apparatus of claim 2, further comprising:
a second switching unit (32) configured to:
introducing the separated hydrogen isotopes into the gas analysis section (40); or
Introducing the separated impurity component into the gas analysis section (40).
6. The apparatus of claim 5, further comprising: a recovery line (24) therein
The second switching section (32) is configured to have a first operating state and a second operating state,
when the second switching section (32) is in a first operating state, the separation line (23) communicates with the recovery line (24), and the second chromatographic column (12) communicates with the gas analyzing section (40);
when the second switching part (32) is in a second working state, the second chromatographic column (12) is communicated with the recovery pipeline (24); and the separation line (23) is communicated with the gas analysis portion (40).
7. The apparatus of claim 6,
the second switch (32) comprises a first port, a second port, a third port, and a fourth port; wherein
A first port of the second switching section (32) and the recovery line (24);
a second port of the second switching portion (32) communicates with the second chromatographic column (12);
a third port of the second switching section (32) communicates with the gas analyzing section (40);
a fourth port of the second switching portion (32) communicates with the separation line (23);
when the second switching part (32) is in a first working state, the first port is communicated with the fourth port, and the second port is communicated with the third port;
when the second switching part (32) is in a second working state, the first port is communicated with the second port, and the third port is communicated with the fourth port.
8. The device according to claim 7, wherein the second switching portion (32) is a four-way valve.
9. The apparatus of claim 5, wherein the sample introduction portion comprises:
a sample inlet line (51) for introducing the sample gas;
a first carrier gas inlet line (21) for providing the first carrier gas;
a quantifying unit (52) for quantifying the sample gas;
an injection valve (33) configured to: -communicating the dosing section (52) selectively with the sample inlet line (51) or with the first carrier gas inlet line (21) and the first chromatography column (11).
10. The apparatus of claim 9,
and a flow regulating piece is arranged on the first carrier gas inlet pipeline (21) and is used for regulating the flow of the first carrier gas.
11. The apparatus of claim 10,
the flow regulating element comprises a damping line (202) and/or an electronic flow controller (201).
12. The apparatus of claim 9,
the injection valve (33) is configured to have a first operating state and a second operating state,
when the sample injection valve (33) is in a first working state, one end of the quantitative part (52) is closed, the other end of the quantitative part is communicated with the sample inlet pipeline (51), and the first carrier gas inlet pipeline (21) is communicated with the first chromatographic column (11);
when the sample injection valve (33) is in a second working state, two ends of the quantitative part (52) are respectively communicated with the first carrier gas inlet pipeline (21) and the first chromatographic column (11), and the sample inlet pipeline (51) is closed.
13. The apparatus of claim 12,
the sample injection valve (33) comprises a first port, a second port, a third port, a fourth port, a fifth port and a sixth port; wherein
A first port of the injection valve (33) is communicated with the first chromatographic column (11);
the second port and the fifth port of the sample injection valve (33) are respectively communicated with two ends of the quantitative part (52);
the third port of the sample injection valve (33) is a closed end;
the fourth port of the sample injection valve (33) is communicated with the sample inlet pipeline (51);
a sixth port of the sample injection valve (33) is communicated with the first carrier gas inlet pipeline (21);
when the sample injection valve (33) is in a first working state, the first port is communicated with the sixth port, the second port is communicated with the third port, and the fourth port is communicated with the fifth port;
when the sample injection valve (33) is in a second working state, the first port is communicated with the second port, the third port is communicated with the fourth port, and the fifth port is communicated with the sixth port.
14. The device according to claim 13, wherein the injection valve (33) is a six-way valve.
15. The apparatus of claim 13, further comprising:
and the air suction pipeline (53) and the sample air inlet pipeline (51) are jointly communicated with the fourth port of the sample injection valve (33).
16. The apparatus of claim 15, further comprising:
an evacuation device (54) in communication with the suction line (53) configured to: when the sample injection valve (33) is in a first working state and the sample inlet pipeline (51) is closed, the gas circuit where the air suction pipeline (53) and the quantitative part (52) are located is controlled to be vacuumized.
17. The apparatus of claim 9, further comprising:
and the pressure sensor (55) is used for detecting the air pressure of the air path where the sample air inlet pipeline (51) and the quantitative part (52) are located when the sample air inlet pipeline (51) is communicated with the quantitative part (52).
18. The apparatus of claim 9, further comprising:
a sealing box (60) filled with a shielding gas;
the quantitative part (52), the sample injection valve (33), the first switching part (31), and the second switching part (32) are arranged in the seal box (60).
19. The apparatus of claim 18, further comprising:
a temperature sensor (61) for detecting the temperature within the seal box (60).
20. The apparatus of claim 18,
the first carrier gas, the second carrier gas and the shielding gas are the same gas.
21. The apparatus of claim 16, further comprising:
a control device (70) configured to: according to the received instructions, the switching of the sample injection valve (33), the first switching part (31) and the second switching part (32) is controlled, and the on-off of the vacuum-pumping device (54) is controlled.
22. The apparatus of claim 21, wherein the control device (70) is further configured to: in accordance with the received washing instruction(s),
controlling the sample injection valve (33) to be in a first working state;
controlling the vacuum-pumping device (54) to pump vacuum to the quantitative part (52);
controlling the first switching part (31) to be in a second working state;
and controlling the second switching part (32) to be in a first working state.
23. The apparatus of claim 21, wherein the control device (70) is further configured to: in accordance with the received detection instruction(s),
controlling the sample injection valve (33) to be in a first working state, controlling the first switching part (31) to be in the first working state or a second working state, and controlling the second switching part (32) to be in the first working state or the second working state;
after the first preset time, controlling the sample injection valve (33) to be in a second working state, controlling the first switching part (31) to be in a first working state, and controlling the second switching part (32) to be in the first working state or in the second working state;
after a second preset time, controlling the sample injection valve (33) to be in a second working state, controlling the first switching part (31) to be in the second working state, and controlling the second switching part (32) to be in the first working state or the second working state;
and after a third preset time, controlling and switching the working state of the second switching part (32).
24. The apparatus of claim 23, wherein the control device (70) is further configured to:
after the second preset time, controlling the second switching part (32) to be in a second working state;
and after the third preset time, controlling the second switching part (32) to be in a first working state.
25. The device according to claim 1, wherein the first chromatography column (11) is a molecular sieve column.
26. The apparatus of claim 1, wherein the second chromatography column (12) is a modified alumina column and the second chromatography column (12) is in a liquid nitrogen environment.
27. Device according to claim 1, characterized in that a damping line (221) is provided on the second carrier gas inlet line (22).
28. Device according to claim 1, characterized in that a damping line (231) is arranged on the separation line (23).
29. The apparatus according to claim 1, wherein the gas analysis section (40) comprises a plasma emission detector (41) and a thermal conductivity detector (42) in series.
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Cited By (1)
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| CN115343391A (en) * | 2022-08-23 | 2022-11-15 | 中国原子能科学研究院 | System and method for chromatographic analysis of isotopic gas components |
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