CN108020612B - Device and method for analyzing content of trace impurities in hydrogen isotope gas and/or helium gas - Google Patents

Abstract

The invention belongs to the technical field of gas chromatographic analysis, and relates to an analysis device and method for the content of trace impurities in hydrogen isotope gas and/or helium gas. The analysis device comprises a three-way pipeline, a first four-way pipeline, a second four-way pipeline, a six-way valve, a first four-way valve, a second four-way valve, a detector, a mechanical pump, a tritium-containing sample gas recovery tank, a tail gas exhaust outlet, a standard gas steel cylinder, a sample gas injection port, a pressure sensor, a pre-separation column and an analysis column. With the analysis device and method of the present invention, trace impurity components H in the gas for hydrogen isotope and/or helium can be obtained ₂ 、O ₂ 、N ₂ 、CO、CH ₄ 、CO ₂ When the content analysis of the impurity components is finished at one time, the sample consumption is small, the analysis time is short, the exhaust emission is small, and the analysis accuracy is high.

Description

Device and method for analyzing trace impurity content in hydrogen isotope gas and/or helium gas

technical field

The invention belongs to the technical field of gas chromatography analysis, and relates to a device and a method for analyzing trace impurity content in hydrogen isotope gas and/or helium gas.

Background technique

Tritium is a radioactive isotope of hydrogen and is a very important strategic energy source material, which is of great significance in other fields such as industry, national defense and scientific research.

In a low-temperature system (around 20K) of liquid hydrogen ( _D2 -DT), any gas other than helium will freeze and accumulate in components such as distillation columns, heat exchangers, connecting pipes, etc. Therefore, it is necessary to accurately monitor the content of trace impurity components in the process gas containing tritium by chromatography, which can ensure the normal operation of the process system.

In the plasma exhaust gas processing system (TEP) of the International Thermonuclear Experimental Reactor (ITER), it is necessary to judge whether the mixed gas of helium and other impurity gases containing tritium products can meet environmental protection and economical requirements after purification. Efficient emission standards.

At present, gas chromatography usually adopts the normal (positive) sampling method for the analysis of the content of different impurity components in the gas. The gas chromatographic analysis using this sample injection method not only requires the sample to be analyzed to be in a micro-positive pressure system, but also requires that the sample flow rate in the analysis be in a continuous steady-state process. The applicable system of normal (positive) sampling method is limited to micro-positive pressure system (negative pressure system is not applicable). The amount of sample lost in the gas chromatographic analysis process using this sampling method is relatively large, and the replacement of the pipeline environment before analysis requires For a long time, these have limited the application of the normal (positive) sampling method in the analysis of hydrogen isotope gas and/or helium gas.

At present, when analyzing the content of trace impurities (H ₂ , O ₂ , N ₂ , CO, CH ₄ , CO ₂ ), gas chromatography adopts a double-needle injection mode, that is, one needle sample injection is aimed at the trace amount of H ₂ in the sample. , O ₂ , N ₂ , CO, CH ₄ impurity component content analysis (using a molecular sieve packed column as the analytical column), another sample injection is aimed at the analysis of the trace amount of CO ₂ impurity component content in the sample (using HayesepD packing column as an analytical column). The gas path of the analysis scheme using this sampling mode is relatively complicated, and compared with the analysis of all impurity components (H ₂ , O ₂ , N ₂ , CO, CH ₄ , CO ₂ ) with single-needle injection, the analysis cycle is prolonged , Increased sample loss and exhaust emissions.

In addition, the molecular sieve packed columns commonly used in gas chromatography analysis (such as 13X column, 5A column) will absorb trace oxygen, which affects the accuracy of trace oxygen component analysis to a certain extent.

Contents of the invention

The primary purpose of the present invention is to provide an analysis device for trace impurity content in hydrogen isotope gas and/or helium, so as to be able to use hydrogen isotope gas and/or trace impurity components in helium H ₂ , O ₂ , N ₂ , When analyzing the contents of CO, CH ₄ , and CO ₂ , the analysis of the content of all impurity components is completed at one time. The sample consumption is small, the analysis time is short, the exhaust emission is small, and the analysis accuracy is high.

To achieve this purpose, in a basic embodiment, the present invention provides an analysis device for trace impurity content in hydrogen isotope gas and/or helium, and the analysis device includes a three-way pipeline, a first four-way pipeline, a second four-way pipeline, and a second four-way pipeline. Through pipeline, six-way valve, first four-way valve, second four-way valve, detector, mechanical pump, tritium-containing sample gas recovery tank, tail gas exhaust port, standard gas cylinder, sample gas inlet, pressure sensor, Pre-separation column, analytical column,

The described mechanical pump used to exhaust the tail gas is connected with one of the three-way pipelines, and the other two pipelines of the three-way pipeline are connected with the tritiated sample gas recovery tank and the three-way pipeline respectively. One of the above-mentioned first four-way pipelines is connected;

The other three pipes in the first four-way pipeline are respectively connected with the exhaust outlet, the calibration gas cylinder, and one of the second four-way pipelines;

The other three pipes in the second four-way pipeline are respectively connected with the sample gas inlet, the pressure sensor, and the six-way valve;

By controlling the opening and closing of the six-way valve, the sample gas or standard gas can be controlled to enter the pre-separation column through the six-way valve for pre-separation;

The pre-separation column is connected with the first four-way valve. By controlling the opening and closing of the first four-way valve, the outlet gas of the pre-separation column can be controlled to pass through the first four-way valve. The valve enters the analytical column for chromatographic analysis;

The analytical column is connected to the second four-way valve, and by controlling the opening and closing of the second four-way valve, the outlet gas of the analytical column can be controlled to pass through the second four-way valve Enter the detector for detection.

In a preferred embodiment, the present invention provides an analysis device for trace impurity content in hydrogen isotope gas and/or helium, wherein said detector is selected from discharge helium ionization detector, pulse discharge helium ionization detector , one of the thermal conductivity detectors.

In a preferred embodiment, the present invention provides an analysis device for trace impurity content in hydrogen isotope gas and/or helium, wherein said pre-separation column has a length of 0.1-2.0m, an internal diameter of 2-5mm, and a built-in 80 - 100-mesh shincarbon filler; the analytical column has a length of 1.5-5.0m, an inner diameter of 2-5mm, and 80-100-mesh shincarbon filler inside.

In a preferred embodiment, the present invention provides an analysis device for trace impurity content in hydrogen isotope gas and/or helium, wherein said analysis device also includes a standard gas sampling valve and a pressure relief valve connected to each other, and they are set On a pipeline of the first four-way pipeline connected to the calibration gas cylinder, the pressure reducing valve is connected to the calibration gas cylinder.

In a preferred embodiment, the present invention provides an analysis device for trace impurity content in hydrogen isotope gas and/or helium, wherein said analysis device also includes a bellows valve, except for said six-way valve, said Except for the connection points on the first four-way valve and the second four-way valve body, the connection points of other pipelines are connected through the bellows valve.

In a preferred embodiment, the present invention provides an analysis device for trace impurity content in hydrogen isotope gas and/or helium, wherein said analysis device also includes a purge gas pipeline connected with said six-way valve , by controlling the opening and closing of the six-way valve, high-purity helium or high-purity deuterium can be controlled to enter the second four-way pipeline through the sweeping gas pipeline.

A second object of the present invention is to provide a method for analyzing the content of trace impurities in hydrogen isotope gas and/or helium using the analysis device as described above, so as to be able to analyze the trace impurities in hydrogen isotope gas and/or helium. When analyzing the contents of H ₂ , O ₂ , N ₂ , CO, CH ₄ , and CO ₂ , the analysis of the content of all impurity components can be completed at one time, with small sample consumption, short analysis time, low exhaust emission and high analysis accuracy. .

To achieve this purpose, in a basic embodiment, the present invention provides a method for analyzing the content of trace impurities in hydrogen isotope gas and/or helium using the analysis device as described above, and the method includes the following steps in sequence:

(1) Replacement of the standard gas and sample gas sampling pipeline environment: Purge the pipelines related to the standard gas and sample gas sampling by introducing gas, and discharge the purged gas through the mechanical pump;

(2) standard curve making: the calibration gas drawn by the calibration gas cylinder is analyzed and detected by the detector through the analysis column with different pressures, and the pressure measurement of the pressure sensor is recorded As a result, a standard curve was drawn according to the detection results of the detector under different injection pressures;

(3) Analysis of trace impurity content in hydrogen isotope gas and/or helium: import sample gas from the sample gas inlet, analyze and detect through the described detector successively through the described analytical column, and Record the pressure measurement results of the pressure sensor, and calculate the content of trace impurities in hydrogen isotope gas and/or helium according to the detection results of the detector, the pressure measurement results and the standard curve, and the trace impurities are _H2 , O ₂ , N ₂ , CO, CH ₄ and CO ₂ .

In a preferred embodiment, the present invention provides a method for analyzing the content of trace impurities in hydrogen isotope gas and/or helium using the analysis device as described above, wherein the method includes the following steps in sequence:

(1) Replacement of standard gas and sample gas sampling pipeline environment: introduce high-purity helium (purity ≥ 99.999%) or high-purity deuterium (purity ≥ 99.999%) through the sweeping gas pipeline for each and standard gas and the pipelines related to sample gas sampling are purged, and the purged gas is discharged through the mechanical pump;

(2) standard curve making: the calibration gas drawn by the calibration gas cylinder is analyzed and detected by the detector through the analysis column with different pressures, and the pressure measurement of the pressure sensor is recorded As a result, a standard curve was drawn according to the detection results of the detector under different injection pressures;

(3) Analysis of trace impurity content in hydrogen isotope gas and/or helium: import sample gas from the sample gas inlet, analyze and detect through the described detector successively through the described analytical column, and Record the pressure measurement results of the pressure sensor, and calculate the content of trace impurities in hydrogen isotope gas and/or helium according to the detection results of the detector, the pressure measurement results and the standard curve, and the trace impurities are _H2 , O ₂ , N ₂ , CO, CH ₄ and CO ₂ .

In a more preferred embodiment, the present invention provides a method for analyzing the content of trace impurities in hydrogen isotope gas and/or helium using the analysis device as described above, wherein the high-purity helium or high-purity deuterium The purging direction of the pump is consistent with the pumping direction of the mechanical pump, which is conducive to quickly and effectively replacing the environment of the clean sample pipeline.

In a preferred embodiment, the present invention provides the method for analyzing the content of trace impurities in hydrogen isotope gas and/or helium using the analytical device as described above, wherein in step (2) and step (3):

When analyzing the content of trace impurities in hydrogen standard gas or tritiated hydrogen, the first four-way valve is in the open state for 0-1.8 minutes, and is in the closed state after 1.8 minutes until the end of the single analysis;

When analyzing the content of trace impurities in helium standard gas or tritiated helium, the first four-way valve is always closed.

In a preferred embodiment, the present invention provides the method for analyzing the content of trace impurities in hydrogen isotope gas and/or helium using the analytical device as described above, wherein in step (3), the hydrogen isotope gas and/or The formula for the content of trace impurities in helium is:

Cv _sample = P ₁ ×A ₂ ×Cv _standard /(P ₂ ×A ₁ ),

in:

Cv _standard and Cv _sample are the volume concentration of standard gas and sample gas respectively, the unit is ppm;

A ₁ and A ₂ are the detector response areas of the standard gas and sample gas components respectively, in mv s;

P ₁ and P ₂ are the injection pressures of calibration gas and sample gas, respectively, in Pa.

The beneficial effects of the present invention are that, using the analysis device and method for trace impurity content in hydrogen isotope gas and/or helium of the present invention, it is possible to analyze trace impurity components _H2 , O in hydrogen isotope gas and/or helium. _2. When analyzing the content of N ₂ , CO, CH ₄ , and CO ₂ , the analysis of the content of all impurity components is completed at one time. The sample consumption is small, the analysis time is short, the tail gas emission is small, and the analysis accuracy is high.

In order to meet the analysis requirements of trace impurity components in hydrogen isotope gas and/or helium, the present invention re-optimizes the traditional gas chromatographic sampling system, which is specifically embodied as follows:

(1) The negative pressure sampling method is adopted to reduce the sample volume required for analysis;

(2) Through the purging of high-purity helium or high-purity deuterium purge gas and the extraction of mechanical pumps, that is, the "one flush and one pump" method quickly and effectively replaces the clean sample pipeline environment, reducing the loss of sample gas and Exhaust emissions;

(3) Use one-needle injection mode instead of double-needle injection mode to complete the one-time analysis of trace impurity components H ₂ , O ₂ , N ₂ , CO, CH ₄ , and CO ₂ , improving analysis efficiency while reducing The amount of loss of samples and the emission of exhaust gas;

(4) Using two shincarbon packed columns to replace the functions of one molecular sieve packed column and one HayesepD packed column avoids the adsorption of oxygen by the molecular sieve packed column and improves the analysis accuracy of trace impurity component O ₂ .

Description of drawings

Fig. 1 is a composition diagram of an exemplary analysis device for trace impurity content in hydrogen isotope gas and/or helium gas according to the present invention.

Fig. 2 is an exemplary relationship diagram between the sampling pressure of different impurity components O ₂ , N ₂ , and CH ₄ and the respective response areas of the components obtained by negative pressure sampling.

Fig. 3 is an exemplary chromatogram of the whole analysis process of different impurity components H ₂ , O ₂ , N ₂ , CO, CH ₄ , and CO ₂ obtained by using the one-needle injection mode.

Detailed ways

The composition of the analysis device of trace impurity content in exemplary hydrogen isotope gas and/or helium of the present invention is shown in Figure 1, comprises three-way pipeline A, the first four-way pipeline B, the second four-way pipeline C, six Through valve D, first four-way valve E, second four-way valve F, detector G, tritium-containing sample gas recovery tank H, tail gas exhaust port I, standard gas cylinder J, sample gas inlet K, pressure sensor L, pre-separation column M, analytical column N, mechanical pump O, first carrier gas pipeline P, second carrier gas pipeline Q, purge gas pipeline R, first vent pipeline S, third carrier gas pipeline T, The second venting pipeline U, pressure display instrument, sampling valve, pressure reducing valve, main exhaust port, bellows valve.

The three ports of the three-way pipeline A are respectively connected to the mechanical pump O intake pipeline A ₁ , the tritiated sample gas recovery pipeline A ₂ (connected to the tritiated sample gas recovery tank H), and one end A ₃ of the first four-way pipeline B. _B1 is connected.

The other three ports of the first four-way pipeline B are respectively connected to the calibration gas sampling pipeline B ₂ (connected to the calibration gas cylinder J), one end B ₃ -C ₁ of the second four-way pipeline C, and the exhaust gas discharge pipeline B ₄ (connected to Exhaust air outlet 1) is connected.

The other three ports of the second four-way pipeline C are respectively connected to the standard gas or tritiated sample gas pressure measuring pipeline C ₂ (connected to the pressure sensor L), the sampling pipeline C ₃ -D ₁ of the six-way valve D, and the tritiated sample gas The sample gas sampling line C ₄ (connected to the sample gas sampling port K) is connected.

When the state of the six-way valve D is closed, the connection status of the six ports is as follows: the sampling line is connected to the D ₁ point of the six-way valve D, the D ₁ point is connected to the D ₂ point, and the D ₂ point is connected to the inlet of the quantitative loop. The first carrier gas pipeline P is connected to point _D3 , point _D3 is connected to point _D4 , point _D4 is connected to the inlet of pre-separation column M, the gas outlet of the quantitative loop is connected to point _D5 , point _D5 The point is connected with the D ₆ point, and the D ₆ point is connected with the purge gas pipeline R.

When the six-way valve D is in the open state, the connection status of the six ports is as follows: the sampling line is connected to the D ₁ point of the six-way valve D, the D ₁ point is connected to the D ₆ point, and the D ₆ point is connected to the purge gas pipeline R The air inlet of the quantitative loop is connected to point D ₂ , point D ₂ is connected to point D ₃ , point D ₃ is connected to the first carrier gas pipeline P, the air inlet of pre-separation column M is connected to point D ₄ , and point D Point ₄ communicates with point D ₅ , and point D ₅ connects with the gas outlet of the quantitative loop.

When the state of the first four-way valve E is closed, the connection state of the four ports is: the gas outlet of the pre-separation column M is connected to the _E1 point of the first four-way valve E, the _E1 point is connected to the _E2 point, and the _E2 point is connected. Point E is connected to the gas inlet of analytical column N, _E3 is connected to the second carrier gas pipeline Q, _E3 is connected to _E4 , and _E4 is connected to the first vent pipeline S.

When the state of the first four-way valve E is open, the connection state of the four ports is: the gas outlet of the pre-separation column M is connected to the _E1 point of the first four-way valve E, the _E1 point is connected to the _E4 point, and the _E4 point is connected. Point is connected to the first venting pipeline S, the gas inlet of the analytical column N is connected to point _E2 , point _E2 is connected to point _E3 , and point _E3 is connected to the second carrier gas pipeline Q.

When the state of the second four-way valve F is closed, the connection status of the four ports is: the gas outlet of the analytical column N is connected to the _F1 point of the second four-way valve F, the _F1 point is connected to the _F2 point, and the _F2 point is connected. It is connected with the gas inlet of the detector G, the point _F3 is connected with the third carrier gas pipeline T, the point _F3 is connected with the point _F4 , and the point _F4 is connected with the second vent pipeline U.

When the second four-way valve F is in the open state, the connection status of the four ports is: the gas outlet of the analytical column N is connected to the _F1 point of the second four-way valve F, the _F1 point is connected to the _F4 point, and the _F4 point is connected. It is connected with the second vent pipeline U, point _F2 is connected with the gas inlet of the detector G, _F2 is connected with _F3 , and _F3 is connected with the third carrier gas pipeline T.

The detector G is one of a discharge helium ionization detector, a pulse discharge helium ionization detector, and a thermal conductivity detector.

The length of the pre-separation column M is 0.1-2.0m, the inner diameter is 2-5mm, and the inner diameter is 80-100 mesh shincarbon packing

The length of the analytical column N is 1.5-5.0m, the inner diameter is 2-5mm, and the inner diameter is 80-100 mesh shincarbon filler.

The pressure measurement value of the pressure sensor L is displayed by the pressure display instrument.

The purge gas pipeline R can introduce high-purity helium or high-purity deuterium.

The calibration gas sampling line _B2 is connected to the calibration gas cylinder J through a calibration gas sampling valve and a pressure reducing valve (not shown in the figure) provided thereon.

The pipeline outlet of the mechanical pump O, the exhaust air outlet I, the outlets of each vent pipeline and the pipeline outlet of the detector G are all led to the total air outlet (not shown in the figure).

Except for the connection points on the valve bodies of the six-way valve D, the first four-way valve E, and the second four-way valve F, the connection points of the other pipelines are all connected by bellows valves.

The operation steps of the exemplary method for analyzing the content of trace impurities in hydrogen isotope gas and/or helium gas using the above exemplary analysis device are as follows. The valve on the tritiated sample gas recovery line A ₂ is only opened when the sample needs to be recovered.

(1) Replacement of standard gas and sample injection pipeline environment

Open the valve of the standard gas cylinder, and then open the pressure reducing valve, standard gas sampling valve and the valve on the exhaust gas discharge pipeline _B4 in sequence, and use standard gas to purge the pressure reducing valve body, standard gas sampling valve and standard gas sampling tube Road B ₂ 5-8min.

Close the valve on the standard gas sampling line B ₂ , close the exhaust gas discharge line B ₄ , the valves on the tritiated sample gas sampling line C ₄ , and the purge gas line R, and open the standard gas or tritiated sample The valve on the gas pressure measurement pipeline _C2 pumps the standard gas and sample injection pipeline environment to less than 10Pa through the mechanical pump O.

Close the valve on the mechanical pump O intake line _A1 , observe the pressure display instrument value on the standard gas or tritium-containing sample gas pressure measuring line _C2 , the reading does not show an upward trend (indicating that the system is well sealed), and open the purge Gas pipeline R valve until high-purity helium enters the pipeline system.

Close the valve R of the purge gas pipeline, open the valve on the intake pipeline _A1 of the mechanical pump O, and start vacuuming until the pressure display value is stable.

Repeat the above steps 2-5 times to reduce the total content of impurity components to be analyzed in the pipeline environment to below 50ppb.

(2) Standard curve creation

Adjust the outlet pressure of the pressure reducing valve to a certain pressure range, control the sampling pressure of the calibration gas through the calibration gas sampling valve (the average sampling pressure of the four sampling points are 54502Pa, 62451Pa, 70284Pa, 77439Pa), and read the calibration gas Or the pressure display instrument value on the tritiated sample gas pressure measuring line C ₂ .

Close the above-mentioned valves, and open the valves on the sampling pipeline C ₃ -D ₁ of the six-way valve D to perform chromatographic analysis. The specific standard curve obtained from the chromatographic analysis is shown in FIG. 2 .

(3) Analysis of trace impurity components in hydrogen isotope gas and/or helium

Replace the pipeline system as in the above step (1), open the valve on the tritiated sample gas sampling line _C4 , and read the pressure display instrument value on the standard gas or the tritiated sample gas pressure measuring line _C2 .

Close the above-mentioned valves, open the valves on the sampling pipeline C ₃ -D ₁ of the six-way valve D to perform chromatographic analysis, and the obtained chromatogram is shown in FIG. 3 . Finally, the obtained chromatographic results are calculated by the following formula to calculate the content of trace impurity components in hydrogen isotope gas and/or helium, which is H ₂ ( _{calculated value of} C=1.52ppm, _{theoretical value of} C=1.47ppm), O ₂ ( _{calculated value of} C _Value = 2.21 ppm, C _Theoretical = 2.28 ppm), _N2 (C _Calcd = 2.43 ppm, C _Theoretical = 2.37 ppm), CO (C _Calcd = 2.35 ppm, C _Theoretical = 2.31 ppm), _CH4 (C _Calcd =2.88ppm, _CTheoretical =2.92ppm), _CO2 ( _Ccalculated =3.83ppm, _CTheoretical =3.76ppm).

Cv _sample = P ₁ ×A ₂ ×Cv _standard /(P ₂ ×A ₁ ),

in:

Cv _standard and Cv _sample are the volume concentration of standard gas and sample gas respectively, the unit is ppm;

A ₁ and A ₂ are the detector response areas of the standard gas and sample gas components respectively, in mv s;

P ₁ and P ₂ are the injection pressures of calibration gas and sample gas, respectively, in Pa.

In addition, the sample is selectively recovered through the tritiated sample gas recovery pipeline _A2 .

In the above method, the sweeping direction of the sweeping gas is consistent with the pumping direction of the mechanical pump O.

In the above method, the temperature of the pre-separation column M and the analytical column N is 60-70°C, the temperature of the detector G is 40-50°C, and the flow rate of the carrier gas at the outlet of the detector G is 40-45mL/min.

In the above method, in step (2) and step (3), when analyzing trace amounts of O ₂ , N ₂ , CO, CH ₄ , and CO ₂ impurity components in hydrogen standard gas or hydrogen isotope gas, the first four-way valve E is on at 0-1.8min, and is off after 1.8min until the end of a single analysis; analyze trace _H2 , _O2 , _N2 , CO, _CH4 , _CO2 in helium standard gas or tritiated helium When the content is high, the first four-way valve E is always in the closed state.

The amount of sample required to complete the above-mentioned trace impurity content analysis is 0.5-2mL, the time is less than 15min, and the exhaust gas emission is 1-3mL.

Obviously, those skilled in the art can make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. Thus, if these modifications and variations of the present invention fall within the scope of the claims of the present invention and equivalent technologies, the present invention also intends to include these modifications and variations. The above-mentioned embodiments or implementations are only examples of the present invention, and the present invention can also be implemented in other specific ways or other specific forms without departing from the gist or essential features of the present invention. Accordingly, the described embodiments should be considered in all respects as illustrative and not restrictive. The scope of the present invention should be described by the appended claims, and any changes equivalent to the intention and scope of the claims should also be included in the scope of the present invention.

Claims (8)

1. The analysis device of trace impurity content in hydrogen isotope gas and/or helium, it is characterized in that: described analysis device comprises three-way pipeline, the first four-way pipeline, the second four-way pipeline, six-way valve, the first Four-way valve, second four-way valve, detector, mechanical pump, tritium-containing sample gas recovery tank, tail gas exhaust port, standard gas cylinder, sample gas inlet, pressure sensor, pre-separation column, analysis column, The described mechanical pump used to exhaust the tail gas is connected with one of the three-way pipelines, and the other two pipelines of the three-way pipeline are connected with the tritiated sample gas recovery tank and the three-way pipeline respectively. One of the above-mentioned first four-way pipelines is connected; The other three pipes in the first four-way pipeline are respectively connected with the exhaust outlet, the calibration gas cylinder, and one of the second four-way pipelines; The other three pipes in the second four-way pipeline are respectively connected with the sample gas inlet, the pressure sensor, and the six-way valve; By controlling the opening and closing of the six-way valve, the sample gas or standard gas can be controlled to enter the pre-separation column through the six-way valve for pre-separation; The pre-separation column is connected with the first four-way valve. By controlling the opening and closing of the first four-way valve, the outlet gas of the pre-separation column can be controlled to pass through the first four-way valve. The valve enters the analytical column for chromatographic analysis; The analytical column is connected to the second four-way valve, and by controlling the opening and closing of the second four-way valve, the outlet gas of the analytical column can be controlled to pass through the second four-way valve Enter the detector for detection; The length of the pre-separation column is 0.1-2.0m, the inner diameter is 2-5mm, and the inner diameter is 80-100 mesh shincarbon packing; the length of the analysis column is 1.5-5.0m, the inner diameter is 2-5mm, and the inner diameter is 80-100 mesh shincarbon filler. 2. The analysis device according to claim 1, wherein the detector is selected from one of a discharge helium ionization detector, a pulse discharge helium ionization detector, and a thermal conductivity detector. 3. The analysis device according to claim 1, characterized in that: the analysis device also includes a calibration gas sampling valve and a pressure reducing valve connected to each other, and they are arranged on the first described connection gas cylinder of the calibration gas. One of the four-way pipelines, so that the pressure reducing valve is connected with the calibration gas cylinder. 4. The analysis device according to claim 1, characterized in that: the analysis device also includes bellows valves, except for the six-way valve, the first four-way valve, and the second four-way valve. Except for the connecting points on the through valve body, the connecting points of other pipelines are all connected through the bellows valve. 5. The analysis device according to claim 1, characterized in that: the analysis device further comprises a purge gas pipeline connected with the six-way valve, by controlling the opening and closing of the six-way valve, High-purity helium or high-purity deuterium can be controlled to enter the second four-way pipeline through the sweeping gas pipeline. 6. Utilize the analysis device described in any one of claim 1-5 to carry out the method for trace impurity content analysis in hydrogen isotope gas and/or helium, it is characterized in that, described method comprises the following steps successively: (1) Replacement of the standard gas and sample gas sampling pipeline environment: Purge the pipelines related to the standard gas and sample gas sampling by introducing gas, and discharge the purged gas through the mechanical pump; The introduced gas is high-purity helium or high-purity deuterium; (2) Standard curve creation: The calibration gas drawn from the calibration gas cylinder passes through the pre-separation column and analysis column at different pressures for analysis and detection by the detector, and records the pressure The pressure measurement results of the sensor are used to draw the standard curve according to the detection results of the detector under different injection pressures; the temperature of the pre-separation column and analytical column is 60-70°C, the temperature of the detector is 40-50°C, and the carrier gas at the detector outlet The flow rate is 40-45mL/min; (3) Analysis of trace impurity content in hydrogen isotope gas and/or helium gas: import sample gas from the sample gas inlet, pass through the pre-separation column, analysis column for analysis and pass through the detector Carry out detection, and record the pressure measurement result of described pressure sensor, calculate the content of trace impurity in hydrogen isotope gas and/or helium according to the detection result of described detector, pressure measurement result and standard curve, described trace The impurities are H ₂ , O ₂ , N ₂ , CO, CH ₄ and CO ₂ ; the temperature of the pre-separation column and analytical column is 60-70°C, the temperature of the detector is 40-50°C, and the flow rate of the carrier gas at the detector outlet is 40-45mL/min. 7. The method according to claim 6, characterized in that: the purging direction of the high-purity helium or high-purity deuterium is consistent with the pumping direction of the mechanical pump. 8. The method according to claim 6 or 7, characterized in that, in step (3), the formula for calculating the content of trace impurities in hydrogen isotope gas and/or helium is: Cv _sample = P ₁ ×A ₂ ×Cv _standard /(P ₂ ×A ₁ ), in: Cv _standard and Cv _sample are the volume concentration of standard gas and sample gas respectively; A ₁ and A ₂ are the detector response areas of calibration gas and sample gas components respectively; P ₁ and P ₂ are the injection pressures of calibration gas and sample gas, respectively.

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