On-line continuous flow analysis and extraction device and method for nitrogen isotope composition in inclusions

Abstract

The present invention belongs to the technical field of determination of nitrogen isotope composition in mineral inclusions, and specifically relates to an online continuous flow analysis and extraction device and method for nitrogen isotope composition in inclusions. In the present invention, two sample channels are respectively connected to the fifth port and the ninth port of the ten-way valve in the ten-way valve, and are used to obtain nitrogen isotopes in the sample; the two sample channels correspond to a nitrogen collection device respectively, and the nitrogen collection device is a first cold trap and a fourth cold trap. The standard gas test channel, the two sample channels, the nitrogen collection device and the sample detection channel are connected through the ten-way valve, and the sample detection channel is used to analyze the nitrogen isotope composition in the sample. The present invention solves the problem of interaction between the components of the traditional thermal explosion method and between the inclusion components and the main mineral, and multi-stage purification of the exploded gas effectively avoids the interference of CO on the determination of N2, improves the accuracy of analysis and testing, and the two-way explosion device is used alternately, and the efficiency of analysis and testing is significantly improved.

Description

Technical Field

[0001] The invention belongs to the technical field of determination of nitrogen isotope composition in mineral inclusions, and in particular relates to an online continuous flow analysis and extraction device and method for nitrogen isotope composition in inclusions. Background Art

[0002] Nitrogen is chemically inactive, and many nitrides have poor thermal stability. In the crust, except for a few nitrate minerals, most nitrogen exists as trace impurities in rocks and minerals. The chemical characteristics of N2 make it more likely to retain its original information during the material exchange process than other fluid substances. The analysis of nitrogen isotopes in inclusions is of great significance for studying the nitrogen cycle and the material exchange process between the crust and the mantle.

[0003] There are currently three main methods for opening inclusions, namely crushing, grinding, and thermal explosion.

[0004] (1) Crushing method: Place the sample into a stainless steel or copper tube with one end sealed and the other end connected to a vacuum valve. Then connect the tube to a vacuum system and evacuate to 10 -3 Pa, then close the valve, remove the tube, and use a press to crush the sample tube to break the mineral sample and open the inclusions. This method cannot break the sample to a particle size below 1mm, so it can only open the inclusions on the fracture surface.

[0005] (2) Grinding method: Put the ore sample into a ball mill for grinding. After grinding, the particle size of the ore sample should be smaller than the diameter of the inclusion so that the inclusion can be opened. The disadvantage of this method is that when the mineral is ground into a very fine powder, the surface area is very large, and gas components will inevitably be adsorbed on its surface.

[0006] (3) Thermal explosion method: The prepared ore sample is placed in a quartz tube and heated to explode. According to the thermal explosion temperature measurement experiment, the optimal particle size of the thermal explosion sample is 0.25-0.5 mm. According to the thermal explosion temperature measurement curve of the sample inclusions, it is determined how many groups of inclusions there are. If the composition of one group of inclusions is to be determined, then the peak explosion temperature of the group of inclusions should be selected as the temperature for opening the inclusions, and the explosion gas should be collected and then analyzed by mass spectrometry.

[0007] The traditional thermal explosion method is to explode the sample at high temperature in a sealed quartz tube, and collect the generated gas after the explosion is complete. When the mineral inclusions are heated and exploded, in addition to releasing nitrogen and volatile nitrogen compounds, they are also accompanied by the release of other volatile compounds, such as H2O, CO2, CH4, H2S, O2 and inert gases. In a sealed high-temperature environment, the components of the inclusions and the components of the inclusions and the main minerals may interact with each other, and this interaction will cause isotope fractionation. Summary of the invention

[0008] The technical problem solved by the present invention is to provide an online continuous flow analysis and extraction device and method for nitrogen isotope composition in inclusions, which solves the problem of interaction between components in traditional thermal explosion method and between inclusion components and main minerals, and effectively avoids the interference of CO on N2 determination by multi-stage purification of the exploded gas, thereby improving the analysis and test accuracy. The two-way explosion device is used alternately, and the analysis and test efficiency is significantly improved.

[0009] The technical solution adopted by the present invention is:

[0010] An online continuous flow analysis and extraction device for nitrogen isotope composition in inclusions comprises a ten-way valve, a standard gas test channel, two sample channels, a nitrogen collection device and a sample detection channel, and is used for testing the standard gas; the two sample channels are respectively connected to a fifth port of the ten-way valve and a ninth port of the ten-way valve in the ten-way valve, and are used for obtaining nitrogen isotopes in the sample; the two sample channels respectively correspond to a nitrogen collection device, and the nitrogen collection devices are a first cold trap and a fourth cold trap; the standard gas test channel, the two sample channels, the nitrogen collection device and the sample detection channel are connected through the ten-way valve, and the sample detection channel is used for analyzing the nitrogen isotope composition in the sample.

[0011] The standard gas test channel includes a first helium gas inlet, a first gas flow meter, a first water trap, a first gas connector, a second water trap, and a first carbon dioxide trap. The first helium gas inlet is connected to the second port of the ten-way valve through a pipeline in sequence through the first gas flow meter, the first water trap, the first gas connector, the second water trap, and the first carbon dioxide trap. A standard gas injector is provided on the first gas connector, and the standard gas injector is inserted into the gas connector with a sealing gasket.

[0012] The two sample channels respectively include a second helium gas inlet, a second gas flow meter, a fourth water trap, a first burst tube, a third water trap, a second cold trap, and a second carbon dioxide trap; the second helium gas inlet is connected to the fifth port of the ten-way valve through a pipeline in sequence through the second gas flow meter, the fourth water trap, the first burst tube, the third water trap, the second cold trap, and the second carbon dioxide trap;

[0013] The third helium gas inlet, the third gas flow meter, the fifth water trap, the second burst tube, the sixth water trap, the third cold trap, and the third carbon dioxide trap are connected to the ninth port of the ten-way valve through a pipeline in sequence through the third gas flow meter, the fifth water trap, the second burst tube, the sixth water trap, the third cold trap, and the third carbon dioxide trap.

[0014] The two ends of the first cold trap are respectively connected to the third port and the sixth port of the ten-way valve; the two ends of the fourth cold trap are respectively connected to the first port and the eighth port of the ten-way valve.

[0015] The sample detection channel includes a reaction tube, a seventh water trap, a fourth carbon dioxide trap, a chromatographic column and a gas isotope mass spectrometer. The gas isotope mass spectrometer is connected to the seventh port of the ten-way valve through a pipeline in sequence through the chromatographic column, the fourth carbon dioxide trap, the seventh water trap, and the reaction tube.

[0016] The first cold trap is placed in the first liquid nitrogen cup, the second cold trap is placed in the second liquid nitrogen cup, the third cold trap is placed in the third liquid nitrogen cup, and the fourth cold trap is placed in the fourth liquid nitrogen cup.

[0017] A first temperature-controlled heating furnace is provided outside the bursting tube, and the first bursting tube is nested in the central groove of the first temperature-controlled heating furnace. A second temperature-controlled heating furnace is provided outside the second bursting tube, and the second bursting tube is nested in the central groove of the second temperature-controlled heating furnace.

[0018] The fourth port of the ten-way valve is connected to the first ventilation through a pipeline via a first single-opening quartz tube; the tenth port of the ten-way valve is connected to the second ventilation through a pipeline via a second single-opening quartz tube.

[0019] The analysis and extraction method of the online continuous flow analysis and extraction device for nitrogen isotope composition in inclusions comprises the following steps:

[0020] Step 1: Standard gas test

[0021] The second port of the ten-way valve is connected to the third port of the ten-way valve, the fourth port of the ten-way valve is connected to the fifth port of the ten-way valve, the sixth port of the ten-way valve is connected to the seventh port of the ten-way valve, the eighth port of the ten-way valve is connected to the ninth port of the ten-way valve, and the tenth port of the ten-way valve is connected to the first port of the ten-way valve, and the first cold trap is inserted into the first liquid nitrogen cup filled with liquid nitrogen, and the flow rate of the first gas flowmeter is adjusted to 30mL / min, and the standard gas injector is inserted into the gas joint through the sealing gasket, and the standard gas is slowly injected into the gas joint;

[0022] The helium in the first helium inlet sequentially passes through the first gas flow meter, the first water trap, the first gas joint, the standard gas in the purge gas joint, and continues to pass through the second water trap, the first carbon dioxide trap, the second port of the ten-way valve, the third port of the ten-way valve, the first cold trap, the sixth port of the ten-way valve, the seventh port of the ten-way valve, the reaction tube, the seventh water trap, the fourth carbon dioxide trap, the chromatographic column, and finally enters the gas isotope mass spectrometer, and the standard gas is analyzed in the gas isotope mass spectrometer;

[0023] Step 2, loading the first burst tube and the second burst tube with samples and heating to remove gas;

[0024] Step 3: High temperature explosion of mineral samples in the second explosion tube

[0025] The fourth cold trap jacket is equipped with a fourth liquid nitrogen cup of liquid nitrogen, the temperature of the second temperature-controlled heating furnace is set to 600°C, the flow rate of the third gas flowmeter is adjusted to 30mL / min, ventilation is carried out for 5 minutes, the heating switch of the second temperature-controlled heating furnace is turned off, and the inclusions in the mineral sample in the second bursting tube are fully burst at high temperature;

[0026] The helium in the third helium inlet passes through the third gas flow meter, the fifth water trap, and the third quick-detachable joint in sequence, enters the second bursting tube, purges the gas burst from the mineral sample, and continues to pass through the fourth quick-detachable joint, the sixth water trap, the third cold trap, the third carbon dioxide trap, the ninth port of the ten-way valve, and the eighth port of the ten-way valve to enter the fourth cold trap. The nitrogen burst from the inclusions in the mineral sample is fully collected by the fourth cold trap, and the unfrozen gas continues to pass through the first port of the ten-way valve, the tenth port of the ten-way valve, and the second single-opening quartz tube, and finally enters the second vent;

[0027] Step 4: Release and detect nitrogen in the fourth cold trap

[0028] Connect the first port of the ten-way valve to the second port of the ten-way valve, connect the third port of the ten-way valve to the fourth port of the ten-way valve, connect the fifth port of the ten-way valve to the sixth port of the ten-way valve, connect the seventh port of the ten-way valve to the eighth port of the ten-way valve, and connect the ninth port of the ten-way valve to the tenth port of the ten-way valve, replace the liquid nitrogen in the fourth liquid nitrogen cup with hot water, and re-cover the fourth cold trap;

[0029] The first helium inlet is ventilated for 10 minutes, and the helium passes through the first gas flow meter, the first water trap, the first gas connector, the second water trap, the first carbon dioxide trap, the second port of the ten-way valve, the first port of the ten-way valve, and enters the fourth cold trap to purge the released nitrogen. The helium continues to pass through the eighth port of the ten-way valve, the seventh port of the ten-way valve, the reaction tube, the seventh water trap, the fourth carbon dioxide trap, and the chromatographic column, and finally enters the gas isotope mass spectrometer for detection;

[0030] Step 5: High temperature explosion of mineral samples in the first explosion tube

[0031] A first liquid nitrogen cup filled with liquid nitrogen is placed on the outer jacket of the first cold trap, the temperature of the first temperature-controlled heating furnace is set to 600° C., the flow rate of the first gas flowmeter is adjusted to 30 mL / min, ventilation is performed for 5 minutes, the first temperature-controlled heating furnace is closed, and the inclusions in the mineral sample in the first bursting tube are fully burst at high temperature;

[0032] The helium in the second helium inlet passes through the first gas flow meter, the fourth water trap, and the second quick detachable joint in sequence, enters the first bursting tube, purges the gas burst from the mineral sample, continues to pass through the first quick detachable joint, the third water trap, the second cold trap, the second carbon dioxide trap, the fifth port of the ten-way valve, and the sixth port of the ten-way valve, and enters the first cold trap. The nitrogen burst from the inclusions in the mineral sample is fully collected by the first cold trap, and the unfrozen gas continues to pass through the third port of the ten-way valve, the fourth port of the ten-way valve, and the first single-opening quartz tube, and finally enters the first ventilation port;

[0033] Step 6: Release and detect nitrogen in the first cold trap

[0034] The second port of the ten-way valve is connected to the third port of the ten-way valve, the fourth port of the ten-way valve is connected to the fifth port of the ten-way valve, the sixth port of the ten-way valve is connected to the seventh port of the ten-way valve, the eighth port of the ten-way valve is connected to the ninth port of the ten-way valve, and the tenth port of the ten-way valve is connected to the first port of the ten-way valve. The liquid nitrogen in the first liquid nitrogen cup is replaced with hot water, and the first cold trap is re-set. The nitrogen in the first cold trap is quickly released by the heat, the flow rate of the first gas flow meter is 30 mL / min, and the ventilation is 10 minutes;

[0035] The helium in the first helium inlet passes through the first gas flow meter, the first water trap, the first gas connector, the second water trap, the first carbon dioxide trap, the second port of the ten-way valve, the third port of the ten-way valve in sequence, enters the first cold trap, purges the released nitrogen, and continues to pass through the sixth port of the ten-way valve, the seventh port of the ten-way valve, the reaction tube, the seventh water trap, the fourth carbon dioxide trap, and the chromatographic column to enter the gas isotope mass spectrometer for detection.

[0036] In the step 2,

[0037] Open the upper cover of the first temperature-controlled heating furnace, open the first quick-detachable joint and the second quick-detachable joint, remove the first bursting tube, load a small amount of 40-60 mesh mineral samples, put the first bursting tube into the central groove of the first temperature-controlled heating furnace, and then connect the two ends of the first bursting tube to the first quick-detachable joint and the second quick-detachable joint;

[0038] The flow rate of the second gas flow meter is adjusted to 50 mL / min, a second liquid nitrogen cup with liquid nitrogen is placed on the second cold trap jacket, and the temperature of the first temperature-controlled heating furnace is set to 100° C.;

[0039] The second helium inlet is ventilated for about 3 minutes. The helium passes through the second gas flow meter, the fourth water trap, the second quick-detachable joint, enters the first burst tube, purges the air in the first burst tube, continues to pass through the first quick-detachable joint, the third water trap, the second cold trap, the second carbon dioxide trap, the fifth port of the ten-way valve, the fourth port of the ten-way valve, the first single-port quartz tube, and finally enters the first ventilation port;

[0040] Adjust the temperature of the first temperature-controlled heating furnace to 200°C and ventilate for about 5 minutes to remove the gas adsorbed on the surface of the mineral sample and the low-temperature secondary inclusions, effectively reducing the interference of other gases on the primary nitrogen inclusions;

[0041] Open the upper cover of the second temperature-controlled heating furnace, open the third quick-detachable joint and the fourth quick-detachable joint, remove the second bursting tube, load a small amount of 40-60 mesh mineral samples, put the second bursting tube into the central groove of the second temperature-controlled heating furnace, and then connect the two ends of the second bursting tube to the third quick-detachable joint and the fourth quick-detachable joint;

[0042] The flow rate of the third gas flow meter is adjusted to 50 mL / min, the third cold trap jacket is equipped with a third liquid nitrogen cup with liquid nitrogen, and the temperature of the third temperature-controlled heating furnace is set to 100° C.;

[0043] The third helium inlet is ventilated for about 3 minutes. The helium passes through the third gas flow meter, the fifth water trap, the third quick-detachable joint, enters the second burst tube, purges the air in the second burst tube, and continues to pass through the fourth quick-detachable joint, the sixth water trap, the third cold trap, the third carbon dioxide trap, the ninth port of the ten-way valve, the eighth port of the ten-way valve, the fourth cold trap, the first port of the ten-way valve, the tenth port of the ten-way valve, the second single-port quartz tube, and finally enters the second ventilation port;

[0044] The temperature of the second temperature-controlled heating furnace was adjusted to 200°C and ventilation was performed for about 5 minutes to remove the gas adsorbed on the surface of the mineral sample and the low-temperature secondary inclusions, effectively reducing the interference of other gases on the primary nitrogen inclusions.

[0045] Compared with the prior art, the present invention has the following beneficial effects:

[0046] (1) The present invention provides an online continuous flow analysis and extraction device and method for the nitrogen isotope composition in inclusions, which adopts a continuous flow sampling system, connects a sample explosion device, a standard gas loading device, a gas purification device, a nitrogen purification and collection device with a stable isotope mass spectrometer, and realizes online heating and explosion of mineral inclusions, online purification and collection of nitrogen gas, and online testing of nitrogen isotope composition.

[0047] (2) The present invention provides an online continuous flow analysis and extraction device and method for nitrogen isotope composition in inclusions. The multi-stage purification device is used to effectively collect nitrogen and effectively remove other interfering gases that may exist in the system. H2O is removed by adsorption through a water trap filled with magnesium perchlorate; CO2 is removed by adsorption through a carbon dioxide trap filled with NaOH; NO2, N2O and other gases are removed by adsorption through a cold trap filled with liquid nitrogen; The liquid nitrogen cold trap of the molecular sieve adsorbs N2, and CO and others can be converted into CO2 through the fillers in the reaction tube, which is further removed by the carbon dioxide trap. Finally, the interfering gas is further separated by the chromatographic column to improve the test accuracy of N2.

[0048] (3) The present invention provides an online continuous flow analysis and extraction device and method for nitrogen isotope composition in inclusions, which adopts a ten-way valve to connect six devices, namely, two sample bursting devices, two gas exhaust devices, one standard gas loading device, and one mass spectrometry analysis device, so as to realize free switching between one standard gas analysis and two sample analysis.

[0049] (4) The present invention provides an online continuous flow analysis and extraction device and method for nitrogen isotope composition in inclusions. The design of separate pipelines of the standard gas loading device and the combustion and explosion device can effectively reduce the contamination of the standard gas by impurity gases. The free switching between the two sample explosion devices can further improve the analysis efficiency of the samples.

[0050] (5) The present invention provides an online continuous flow analysis and extraction device and method for nitrogen isotope composition in inclusions. By using purified He gas as a carrier gas and accurately controlling the carrier gas flow rate with a gas flow meter, the problem of interaction between the various components and between the inclusion components and the main mineral during the explosion process can be effectively avoided. In addition, the carrier gas is used in conjunction with a temperature-controlled heating furnace to quickly remove the generated gas from the high-temperature zone through staged heating, thereby reducing the influence of the gas adsorbed on the surface of the mineral sample and the gas in the secondary inclusions.

[0051] (6) The present invention provides an online continuous flow analysis and extraction device and method for nitrogen isotope composition in inclusions. The sample amount is small and can meet the precise testing requirements. The experiment is simple and convenient, the analysis time for a single sample is about 10 minutes, and the analysis efficiency is high. BRIEF DESCRIPTION OF THE DRAWINGS

[0052] Figure 1 A schematic structural diagram of an embodiment of an on-line continuous flow analysis and extraction device for nitrogen isotope composition in inclusions provided by the present invention;

[0053] Figure 2 A schematic structural diagram of another embodiment of an on-line continuous flow analysis and extraction device for nitrogen isotope composition in inclusions provided by the present invention;

[0054] In the figure, 1 is the first helium inlet, 2 is the first gas flow meter, 3 is the first water trap, 4 is the gas connector, 5 is the second water trap, 6 is the first carbon dioxide trap, 7 is the first cold trap, 8 is the first liquid nitrogen cup, 9 is the second carbon dioxide trap, 10 is the third water trap, 11 is the first quick detachable connector, 12 is the first burst tube, 13 is the first temperature control heater, 14 is the second quick detachable connector, 15 is the fourth water trap, 16 is the second gas flow meter, 17 is the second helium inlet, 18 is the standard gas injector, 19 is the second cold trap, 20 is the second liquid nitrogen cup, 21 is the ten-way valve, 22 is the first single-mouth quartz tube, 23 is the first vent, 24 is the second vent, 25 is the second single-opening quartz tube, 26 is the third helium inlet, 27 is the third gas flow meter, 28 is the fifth water trap, 29 is three quick detachable joints, 30 is a second burst tube, 31 is a second temperature-controlled heater, 32 is a fourth quick detachable joint, 33 is a sixth water trap, 34 is a third cold trap, 35 is a third liquid nitrogen cup, 36 is a third carbon dioxide trap, 37 is a fourth liquid nitrogen cold trap, 38 is a fourth liquid nitrogen cup, 39 is a reaction tube, 40 is a seventh water trap, 41 is a fourth carbon dioxide trap, 42 is a chromatographic column, 43 is a gas isotope mass spectrometer, 2101 is a first port of a ten-way valve, 2102 is a second port of a ten-way valve, 2103 is a third port of a ten-way valve, 2104 is a fourth port of a ten-way valve, 2105 is a fifth port of a ten-way valve, 2106 is a sixth port of a ten-way valve, 2107 is a seventh port of a ten-way valve, 2108 is an eighth port of a ten-way valve, 2109 is a ninth port of a ten-way valve, and 2110 is a tenth port of a ten-way valve. DETAILED DESCRIPTION

[0055] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0056] In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, the terms "first", "second", and "third" are used for descriptive purposes only, and cannot be understood as indicating or implying relative importance.

[0057] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0058] Embodiment 1

[0059] like Figure 1 As shown, an online continuous flow analysis and extraction device for nitrogen isotope composition in a mineral inclusion of the present embodiment comprises a first helium gas inlet 1, a second helium gas inlet 17, a third helium gas inlet 26, a first gas flowmeter 2, a second gas flowmeter 16, a third gas flowmeter 27, a first water trap 3, a second water trap 5, a third water trap 10, a fourth water trap 15, a fifth water trap 28, a sixth water trap 33, a seventh water trap 40, a first carbon dioxide trap 6, a second carbon dioxide trap 9, a third carbon dioxide trap 36, a fourth carbon dioxide trap 41, a first cold trap 7, a second cold trap 19, and a third Cold trap 34, fourth cold trap 37, first liquid nitrogen cup 8, second liquid nitrogen cup 20, third liquid nitrogen cup 35, fourth liquid nitrogen cup 38, first quick detachable joint 11, second quick detachable joint 14, third quick detachable joint 29, fourth quick detachable joint 32, first bursting tube 12, second bursting tube 30, first temperature-controlled heating furnace 13, second temperature-controlled heating furnace 31, first single-opening quartz tube 22, second single-opening quartz tube 25, first vent 23, second vent 24, ten-way valve 21, reaction tube 39, chromatographic column 42, gas isotope mass spectrometer 43;

[0060] The first helium gas inlet 1 is connected to the second port 2102 of the ten-way valve through a pipeline in sequence via the first gas flow meter 2, the first water trap 3, the first gas connector 4, the second water trap 5, and the first carbon dioxide trap 6;

[0061] The second helium gas inlet 17 is connected to the fifth port 2105 of the ten-way valve through a pipeline in sequence through the second gas flow meter 16, the fourth water trap 15, the first burst tube 12, the third water trap 10, the second cold trap 19, and the second carbon dioxide trap 9;

[0062] The third helium inlet 26 is connected to the ninth port 2109 of the ten-way valve through a pipeline in sequence through the third gas flow meter 27, the fifth water trap 28, the second burst tube 30, the sixth water trap 33, the third cold trap 34, and the third carbon dioxide trap 36;

[0063] The two ends of the first cold trap 7 are connected to the third port 2103 of the ten-way valve and the sixth port 2106 of the ten-way valve respectively;

[0064] Two ends of the fourth cold trap 37 are connected to the first port 2101 of the ten-way valve and the eighth port 2108 of the ten-way valve respectively;

[0065] The fourth port 2104 of the ten-way valve is connected to the first vent 23 through a pipeline via the first single-opening quartz tube 22;

[0066] The tenth port 2110 of the ten-way valve is connected to the second vent 24 through a pipeline via a second single-opening quartz tube 25;

[0067] The seventh port 2107 of the ten-way valve is connected to the gas isotope mass spectrometer 43 through a pipeline in sequence through the reaction tube 39, the seventh water trap 40, the fourth carbon dioxide trap 41, and the chromatographic column 42;

[0068] The first cold trap 7 is placed in the first liquid nitrogen cup 8, the second cold trap 19 is placed in the second liquid nitrogen cup 20, the third cold trap 34 is placed in the third liquid nitrogen cup 35, and the fourth cold trap 37 is placed in the fourth liquid nitrogen cup 38;

[0069] A first temperature-controlled heating furnace 13 is provided outside the bursting tube 12, and the first bursting tube 12 is nested in the central groove of the first temperature-controlled heating furnace 13; a second temperature-controlled heating furnace 31 is provided outside the second bursting tube 30, and the second bursting tube 30 is nested in the central groove of the second temperature-controlled heating furnace 31;

[0070] The first gas connector 4 is provided with a sealing gasket, and the standard gas injector 18 is inserted into the gas connector 4 with the sealing gasket;

[0071] The two ends of the first bursting tube 12 are connected to the pipeline through the first quick detachable joint 11 and the second quick detachable joint 14 respectively, and the two ends of the second bursting tube 30 are connected to the pipeline through the third quick detachable joint 29 and the fourth quick detachable joint 32 respectively;

[0072] In this embodiment, the second port 2102 of the ten-way valve is connected to the third port 2103 of the ten-way valve, the fourth port 2104 of the ten-way valve is connected to the fifth port 2105 of the ten-way valve, the sixth port 2106 of the ten-way valve is connected to the seventh port 2107 of the ten-way valve, the eighth port 2108 of the ten-way valve is connected to the ninth port 2109 of the ten-way valve, and the tenth port 2110 of the ten-way valve is connected to the first port 2101 of the ten-way valve.

[0073] In this embodiment, the pipeline is a stainless steel pipe with an outer diameter of 1 / 16 inch.

[0074] In this embodiment, the first burst tube 12 and the second burst tube 30 are both 1 / 4 inch quartz glass tubes.

[0075] In this embodiment, the first cold trap 7 and the fourth cold trap 37 are both 3 / 8 inch stainless steel tubes filled with Molecular sieves can effectively adsorb nitrogen.

[0076] In this embodiment, the second cold trap 19 and the third cold trap 34 are both 1 / 16 inch stainless steel tubes, which can effectively adsorb gases such as CO2 and N2O.

[0077] In this embodiment, the first water well 3, the second water well 5, the third water well 10, the fourth water well 15, the fifth water well 28, the sixth water well 33, and the seventh water well 40 are filled with magnesium perchlorate, which can effectively absorb moisture.

[0078] In this embodiment, the first carbon dioxide trap 6, the second carbon dioxide trap 9, the third carbon dioxide trap 36, and the fourth carbon dioxide trap 41 are filled with sodium hydroxide, which can effectively absorb carbon dioxide gas.

[0079] In this embodiment, the reaction tube 39 is filled with 10 mm quartz wool, 50 mm chromium oxide, 10 mm quartz wool, 100 mm reduced copper, 10 mm quartz wool, 50 mm silver-plated cobalt and cobalt oxide mixture, and 20 mm quartz wool from top to bottom, which can convert CO, CH4, C2H6, etc. into CO2 gas.

[0080] In this embodiment, the standard gas injector 18 is filled with standard gas, and the standard gas can be injected into the gas connector 4 by piercing the sealing gasket of the gas connector 4 with the needle tip.

[0081] In this embodiment, the first temperature-controlled heating furnace 13 and the second temperature-controlled heating furnace 31 can have a maximum temperature of up to 1100°C.

[0082] In this embodiment, the first single-opening quartz tube 22 and the second single-opening quartz tube 25 can only allow air flow in one direction, which can effectively prevent gas backflow.

[0083] In this embodiment, the chromatographic column 42 can effectively separate different types of gases from each other.

[0084] Embodiment 2

[0085] like Figure 2 As shown, the difference between this embodiment and the first embodiment is that:

[0086] The first port 2101 of the ten-way valve is connected to the second port 2102 of the ten-way valve, the third port 2103 of the ten-way valve is connected to the fourth port 2104 of the ten-way valve, the fifth port 2105 of the ten-way valve is connected to the sixth port 2106 of the ten-way valve, the seventh port 2107 of the ten-way valve is connected to the eighth port 2108 of the ten-way valve, and the ninth port 2109 of the ten-way valve is connected to the tenth port 2110 of the ten-way valve.

[0087] An online continuous flow analysis and extraction method for nitrogen isotope composition in mineral inclusions, the method specifically comprising the following steps:

[0088] Step 1: Standard gas test

[0089] Using the device described in Example 1, the first cold trap 7 is inserted into the first liquid nitrogen cup 8 filled with liquid nitrogen, the flow rate of the first gas flowmeter 2 is adjusted to 30 mL / min, the standard gas injector 18 is inserted into the gas connector 4 through the sealing gasket, and the standard gas is slowly injected into the gas connector 4.

[0090] The helium in the first helium inlet 1 passes through the first gas flowmeter 2, the first water trap 3, and the first gas connector 4 in sequence, purges the standard gas in the gas connector 4, and continues to pass through the second water trap 5, the first carbon dioxide trap 6, the second port 2102 of the ten-way valve, the third port 2103 of the ten-way valve, the first cold trap 7, the sixth port 2106 of the ten-way valve, the seventh port 2107 of the ten-way valve, the reaction tube 39, the seventh water trap 40, the fourth carbon dioxide trap 41, and the chromatographic column 42, and finally enters the gas isotope mass spectrometer 43, and the standard gas is analyzed in the gas isotope mass spectrometer 43.

[0091] Step 2: First burst tube sample loading and heating to degas

[0092] Open the upper cover of the first temperature-controlled heating furnace 13, open the first quick-detachable joint 11 and the second quick-detachable joint 14, remove the first bursting tube 12, load a small amount of 40-60 mesh mineral samples, place the first bursting tube 12 into the central groove of the first temperature-controlled heating furnace 13, and then connect the two ends of the first bursting tube 12 to the first quick-detachable joint 11 and the second quick-detachable joint 14.

[0093] The flow rate of the second gas flow meter 16 is adjusted to 50 mL / min, a second liquid nitrogen cup 20 filled with liquid nitrogen is placed on the outer jacket of the second cold trap 19, and the temperature of the first temperature-controlled heating furnace 13 is set to 100°C.

[0094] The second helium inlet 17 is ventilated for about 3 minutes. The helium passes through the second gas flow meter 16, the fourth water trap 15, and the second quick-detachable joint 14 in sequence, enters the first bursting tube 12, purges the air in the first bursting tube 12, and continues to pass through the first quick-detachable joint 11, the third water trap 10, the second cold trap 19, the second carbon dioxide trap 9, the fifth port 2105 of the ten-way valve, the fourth port 2104 of the ten-way valve, and the first single-port quartz tube 22, and finally enters the first ventilation port 23.

[0095] The temperature of the first temperature-controlled heating furnace 13 is adjusted to 200° C. and ventilation is performed for about 5 minutes to remove the gas adsorbed on the surface of the mineral sample and the low-temperature secondary inclusions, effectively reducing the interference of other gases on the primary nitrogen inclusions.

[0096] Step 3: Loading the second burst tube with sample and heating to degas

[0097] Open the upper cover of the second temperature-controlled heating furnace 31, open the third quick-detachable joint 29 and the fourth quick-detachable joint 32, remove the second bursting tube 30, load a small amount of 40-60 mesh mineral samples, place the second bursting tube 30 into the central groove of the second temperature-controlled heating furnace 31, and then connect the two ends of the second bursting tube 30 to the third quick-detachable joint 29 and the fourth quick-detachable joint 32.

[0098] The flow rate of the third gas flow meter 27 is adjusted to 50 mL / min, a third liquid nitrogen cup 35 filled with liquid nitrogen is placed on the outer jacket of the third cold trap 34, and the temperature of the third temperature-controlled heating furnace 31 is set to 100°C.

[0099] The third helium inlet 26 is ventilated for about 3 minutes. The helium passes through the third gas flow meter 27, the fifth water trap 28, and the third quick-detachable joint 29 in sequence, enters the second bursting tube 30, purges the air in the second bursting tube 30, and continues to pass through the fourth quick-detachable joint 32, the sixth water trap 33, the third cold trap 34, the third carbon dioxide trap 36, the ninth port 2109 of the ten-way valve, the eighth port 2108 of the ten-way valve, the fourth cold trap 37, the first port 2101 of the ten-way valve, the tenth port 2110 of the ten-way valve, and the second single-port quartz tube 25, and finally enters the second ventilation port 24.

[0100] The temperature of the second temperature-controlled heating furnace 31 is adjusted to 200° C. and ventilation is performed for about 5 minutes to remove the gas adsorbed on the surface of the mineral sample and the low-temperature secondary inclusions, effectively reducing the interference of other gases on the primary nitrogen inclusions.

[0101] Step 4: High temperature explosion of mineral samples in the second explosion tube

[0102] A fourth liquid nitrogen cup 38 filled with liquid nitrogen is placed on the outer jacket of the fourth cold trap 37, the temperature of the second temperature-controlled heating furnace 31 is set to 600°C, the flow rate of the third gas flowmeter 27 is adjusted to 30mL / min, ventilation is performed for 5 minutes, the heating switch of the second temperature-controlled heating furnace 31 is turned off, and the inclusions in the mineral sample in the second bursting tube 30 are fully burst at high temperature.

[0103] The helium in the third helium inlet 26 passes through the third gas flowmeter 27, the fifth water trap 28, and the third quick-detachable joint 29 in sequence, enters the second bursting tube 30, purges the gas burst out of the mineral sample, continues to pass through the fourth quick-detachable joint 32, the sixth water trap 33, the third cold trap 34, the third carbon dioxide trap 36, the ninth port 2109 of the ten-way valve, and the eighth port 2108 of the ten-way valve, and enters the fourth cold trap 37. The nitrogen burst out of the inclusions in the mineral sample is fully collected by the fourth cold trap 37, and the unfrozen gas continues to pass through the first port 2101 of the ten-way valve, the tenth port 2110 of the ten-way valve, and the second single-opening quartz glass tube 25, and finally enters the second ventilation port 24.

[0104] Step 5: Release and detect nitrogen in the fourth cold trap

[0105] The device described in Example 1 is adjusted to the device described in Example 2, and the liquid nitrogen in the fourth liquid nitrogen cup 38 is replaced with hot water, which is then re-covered outside the fourth cold trap 37 .

[0106] The first helium inlet 1 is ventilated for 10 minutes, and the helium passes through the first gas flowmeter 2, the first water trap 3, the first gas connector 4, the second water trap 5, the first carbon dioxide trap 6, the second port 2102 of the ten-way valve, the first port 2101 of the ten-way valve in sequence, enters the fourth cold trap 37, purges the released nitrogen, continues to pass through the eighth port 2108 of the ten-way valve, the seventh port 2107 of the ten-way valve, the reaction tube 39, the seventh water trap 40, the fourth carbon dioxide trap 41, the chromatographic column 42, and finally enters the gas isotope mass spectrometer 43 for detection.

[0107] During step 5, step 3 and the following step 6 may be performed simultaneously.

[0108] Step 6: High temperature explosion of mineral samples in the first explosion tube

[0109] The first cold trap 7 is covered with a first liquid nitrogen cup 8 filled with liquid nitrogen, the temperature of the first temperature-controlled heating furnace 13 is set to 600° C., the flow rate of the first gas flowmeter 16 is adjusted to 30 mL / min, ventilation is carried out for 5 minutes, and the first temperature-controlled heating furnace 13 is closed. The inclusions in the mineral sample in the first bursting tube 12 are fully burst at high temperature.

[0110] The helium in the second helium inlet 17 passes through the second gas flowmeter 16, the fourth water trap 15, and the second quick detachable joint 14 in sequence, enters the first bursting tube 12, purges the gas burst out of the mineral sample, continues to pass through the first quick detachable joint 11, the third water trap 10, the second cold trap 19, the second carbon dioxide trap 9, the fifth port 2105 of the ten-way valve, and the sixth port 2106 of the ten-way valve, and enters the first cold trap 7. The nitrogen burst out of the inclusions in the mineral sample is fully collected by the first cold trap 7, and the unfrozen gas continues to pass through the third port 2103 of the ten-way valve, the fourth port 2104 of the ten-way valve, and the first single-opening quartz glass tube 22, and finally enters the first ventilation port 23.

[0111] Step 7: Release and detect nitrogen in the first cold trap

[0112] The device described in Example 1 was adjusted back to that described in Example 1, the liquid nitrogen in the first liquid nitrogen cup 8 was replaced with hot water, and the first cold trap 7 was put on again. The nitrogen in the first cold trap 7 was quickly released due to the heat, the flow rate of the first gas flow meter was 30 mL / min, and the ventilation was carried out for 10 minutes.

[0113] The helium in the first helium inlet 1 passes through the first gas flowmeter 2, the first water trap 3, the first gas connector 4, the second water trap 5, the first carbon dioxide trap 6, the second port 2102 of the ten-way valve, and the third port 2103 of the ten-way valve in sequence, enters the first cold trap 7, purges the released nitrogen, and continues to pass through the sixth port 2106 of the ten-way valve, the seventh port 2107 of the ten-way valve, the reaction tube 39, the seventh water trap 40, the fourth carbon dioxide trap 41, and the chromatographic column 42, and enters the gas isotope mass spectrometer 43 for detection.

[0114] During step 7, step 2 and step 4 can be performed simultaneously.

[0115] The sample analysis process can repeat the above steps 5 to 7 in sequence.

[0116] It will be apparent to those skilled in the art that the invention is not limited to the details of the exemplary embodiments described above and that the invention can be implemented in other specific forms without departing from the spirit or essential features of the invention. Therefore, the embodiments should be considered exemplary and non-limiting in all respects, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations falling within the meaning and scope of the equivalent elements of the claims be included in the invention. Any reference numeral in a claim should not be considered as limiting the claim to which it relates.

[0117] In addition, it should be understood that although the present specification is described according to implementation modes, not every implementation mode contains only one independent technical solution. This description of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment may also be appropriately combined to form other implementation modes that can be understood by those skilled in the art.

Claims

1. An on-line continuous flow analysis and extraction device for nitrogen isotope composition in inclusions, characterized in that: The invention comprises a ten-way valve (21), a standard gas test channel, two sample channels, a nitrogen collection device and a sample detection channel, and is used for testing the standard gas; the two sample channels are respectively connected to the fifth port (2105) and the ninth port (2109) of the ten-way valve (21) and are used for obtaining nitrogen isotopes in the sample; the two sample channels respectively correspond to a nitrogen collection device, and the nitrogen collection devices are a first cold trap (7) and a fourth cold trap (37); the standard gas test channel, the two sample channels, the nitrogen collection device and the sample detection channel are connected via the ten-way valve (21); and the sample detection channel is used for analyzing nitrogen isotopes in the sample; The standard gas test channel comprises a first helium gas inlet (1), a first gas flow meter (2), a first water trap (3), a first gas connector (4), a second water trap (5), and a first carbon dioxide trap (6); the first helium gas inlet (1) is connected to the second port (2102) of the ten-way valve via a pipeline in sequence through the first gas flow meter (2), the first water trap (3), the first gas connector (4), the second water trap (5), and the first carbon dioxide trap (6); a sealing gasket is provided on the first gas connector (4), and the standard gas injector (18) is inserted into the first gas connector (4) with the sealing gasket; The two sample channels, one of which comprises a second helium inlet (17), a second gas flow meter (16), a fourth water trap (15), a first burst tube (12), a third water trap (10), a second cold trap (19), and a second carbon dioxide trap (9); the second helium inlet (17) is connected to the fifth port (2105) of the ten-way valve in sequence via a pipeline through the second gas flow meter (16), the fourth water trap (15), the first burst tube (12), the third water trap (10), the second cold trap (19), the second carbon dioxide trap (9), and the fifth port (2105) of the ten-way valve. ); the other sample channel comprises a third helium gas inlet (26), a third gas flow meter (27), a fifth water trap (28), a second burst tube (30), a sixth water trap (33), a third cold trap (34), and a third carbon dioxide trap (36); the third helium gas inlet (26) is connected to the ninth port (2109) of the ten-way valve via a pipeline in sequence through the third gas flow meter (27), the fifth water trap (28), the second burst tube (30), the sixth water trap (33), the third cold trap (34), and the third carbon dioxide trap (36); The two ends of the first cold trap (7) are respectively connected to the third port (2103) of the ten-way valve and the sixth port (2106) of the ten-way valve; the two ends of the fourth cold trap (37) are respectively connected to the first port (2101) of the ten-way valve and the eighth port (2108) of the ten-way valve; The sample detection channel comprises a reaction tube (39), a seventh water trap (40), a fourth carbon dioxide trap (41), a chromatographic column (42) and a gas isotope mass spectrometer (43); the gas isotope mass spectrometer (43) is connected to the seventh port (2107) of the ten-way valve via a pipeline in sequence through the chromatographic column (42), the fourth carbon dioxide trap (41), the seventh water trap (40) and the reaction tube (39); The first cold trap (7) and the fourth cold trap (37) are both filled with 5Å molecular sieves; The first water well (3), the second water well (5), the third water well (10), the fourth water well (15), the fifth water well (28), the sixth water well (33), and the seventh water well (40) are all filled with magnesium perchlorate; The first carbon dioxide trap (6), the second carbon dioxide trap (9), the third carbon dioxide trap (36), and the fourth carbon dioxide trap (41) are all filled with sodium hydroxide; The reaction tube (39) is filled with 10 mm quartz wool, 50 mm chromium oxide, 10 mm quartz wool, 100 mm reduced copper, 10 mm quartz wool, 50 mm silver-plated cobalt and cobalt oxide mixture, and 20 mm quartz wool in order from top to bottom.

2. The on-line continuous flow analysis and extraction device for nitrogen isotope composition in inclusions according to claim 1, characterized in that: The first cold trap (7) is placed in a first liquid nitrogen cup (8), the second cold trap (19) is placed in a second liquid nitrogen cup (20), the third cold trap (34) is placed in a third liquid nitrogen cup (35), and the fourth cold trap (37) is placed in a fourth liquid nitrogen cup (38).

3. The on-line continuous flow analysis and extraction device for nitrogen isotope composition in inclusions according to claim 2, characterized in that: A first temperature-controlled heating furnace (13) is provided outside the first bursting tube (12), and the first bursting tube (12) is nested in a central groove of the first temperature-controlled heating furnace (13); a second temperature-controlled heating furnace (31) is provided outside the second bursting tube (30), and the second bursting tube (30) is nested in a central groove of the second temperature-controlled heating furnace (31).

4. The on-line continuous flow analysis and extraction device for nitrogen isotope composition in inclusions according to claim 3, characterized in that: The fourth port (2104) of the ten-way valve is connected to the first ventilation port (23) through a pipeline via a first single-opening quartz tube (22); the tenth port (2110) of the ten-way valve is connected to the second ventilation port (24) through a pipeline via a second single-opening quartz tube (25).

5. The method for analyzing and extracting the nitrogen isotope composition in inclusions by an online continuous flow analysis and extraction device according to claim 4, characterized in that: The steps include: Step 1: Standard gas test The second port (2102) of the ten-way valve is connected to the third port (2103) of the ten-way valve, the fourth port (2104) of the ten-way valve is connected to the fifth port (2105) of the ten-way valve, the sixth port (2106) of the ten-way valve is connected to the seventh port (2107) of the ten-way valve, the eighth port (2108) of the ten-way valve is connected to the ninth port (2109) of the ten-way valve, and the tenth port (2110) of the ten-way valve is connected to the first port (2101) of the ten-way valve, the first cold trap (7) is inserted into the first liquid nitrogen cup (8) filled with liquid nitrogen, the flow rate of the first gas flow meter (2) is adjusted to 30 mL / min, the standard gas injector (18) is inserted into the first gas connector (4) through the sealing gasket, and the standard gas is slowly injected into the first gas connector (4); The helium in the first helium inlet (1) passes through the first gas flow meter (2), the first water trap (3), and the first gas connector (4) in sequence, purges the standard gas in the first gas connector (4), and continues to pass through the second water trap (5), the first carbon dioxide trap (6), the second port (2102) of the ten-way valve, the third port (2103) of the ten-way valve, the first cold trap (7), the sixth port (2106) of the ten-way valve, the seventh port (2107) of the ten-way valve, the reaction tube (39), the seventh water trap (40), the fourth carbon dioxide trap (41), the chromatographic column (42), and finally enters the gas isotope mass spectrometer (43), and the standard gas is analyzed in the gas isotope mass spectrometer (43); Step 2, loading the first burst tube and the second burst tube with samples and heating to remove gas; Step 3: High temperature explosion of mineral samples in the second explosion tube A fourth liquid nitrogen cup (38) filled with liquid nitrogen is placed on the outer jacket of the fourth cold trap (37), the temperature of the second temperature-controlled heating furnace (31) is set to 600° C., the flow rate of the third gas flow meter (27) is adjusted to 30 mL / min, ventilation is performed for 5 minutes, the heating switch of the second temperature-controlled heating furnace (31) is turned off, and the inclusions in the mineral sample in the second bursting tube (30) are fully burst at high temperature; The helium in the third helium inlet (26) passes through the third gas flow meter (27), the fifth water trap (28), and the third quick-detachable joint (29) in sequence, and enters the second bursting tube (30), purges the gas burst from the mineral sample, and continues to pass through the fourth quick-detachable joint (32), the sixth water trap (33), the third cold trap (34), the third carbon dioxide trap (36), the ninth port (2109) of the ten-way valve, and the eighth port (2108) of the ten-way valve, and enters the fourth cold trap (37). The nitrogen burst from the inclusions in the mineral sample is fully collected by the fourth cold trap (37), and the unfrozen gas continues to pass through the first port (2101) of the ten-way valve, the tenth port (2110) of the ten-way valve, and the second single-opening quartz tube (25), and finally enters the second ventilation port (24); Step 4: Release and detect nitrogen in the fourth cold trap The first port (2101) of the ten-way valve is connected to the second port (2102) of the ten-way valve, the third port (2103) of the ten-way valve is connected to the fourth port (2104) of the ten-way valve, the fifth port (2105) of the ten-way valve is connected to the sixth port (2106) of the ten-way valve, the seventh port (2107) of the ten-way valve is connected to the eighth port (2108) of the ten-way valve, and the ninth port (2109) of the ten-way valve is connected to the tenth port (2110) of the ten-way valve, and the liquid nitrogen in the fourth liquid nitrogen cup (38) is replaced with hot water, and the fourth cold trap (37) is re-installed; The first helium gas inlet (1) is ventilated for 10 minutes, and the helium gas passes through the first gas flow meter (2), the first water trap (3), the first gas connector (4), the second water trap (5), the first carbon dioxide trap (6), the second port (2102) of the ten-way valve, and the first port (2101) of the ten-way valve in sequence, and enters the fourth cold trap (37), where the released nitrogen is purged, and the helium gas continues to pass through the eighth port (2108) of the ten-way valve, the seventh port (2107) of the ten-way valve, the reaction tube (39), the seventh water trap (40), the fourth carbon dioxide trap (41), and the chromatographic column (42), and finally enters the gas isotope mass spectrometer (43) for detection; Step 5: High temperature explosion of mineral samples in the first explosion tube A first liquid nitrogen cup (8) filled with liquid nitrogen is placed on the outer jacket of the first cold trap (7), the temperature of the first temperature-controlled heating furnace (13) is set to 600° C., the flow rate of the second gas flow meter (16) is adjusted to 30 mL / min, ventilation is performed for 5 minutes, the first temperature-controlled heating furnace (13) is closed, and the inclusions in the mineral sample in the first bursting tube (12) are fully burst at high temperature; The helium in the second helium inlet (17) passes through the second gas flow meter (16), the fourth water trap (15), and the second quick-detachable joint (14) in sequence, and enters the first bursting tube (12), purges the gas burst from the mineral sample, and continues to pass through the first quick-detachable joint (11), the third water trap (10), the second cold trap (19), the second carbon dioxide trap (9), the fifth port (2105) of the ten-way valve, and the sixth port (2106) of the ten-way valve, and enters the first cold trap (7). The nitrogen burst from the inclusions in the mineral sample is fully collected by the first cold trap (7), and the unfrozen gas continues to pass through the third port (2103) of the ten-way valve, the fourth port (2104) of the ten-way valve, and the first single-opening quartz tube (22), and finally enters the first ventilation port (23); Step 6: Release and detect nitrogen in the first cold trap The second port (2102) of the ten-way valve is connected to the third port (2103) of the ten-way valve, the fourth port (2104) of the ten-way valve is connected to the fifth port (2105) of the ten-way valve, the sixth port (2106) of the ten-way valve is connected to the seventh port (2107) of the ten-way valve, the eighth port (2108) of the ten-way valve is connected to the ninth port (2109) of the ten-way valve, and the tenth port (2110) of the ten-way valve is connected to the first port (2101) of the ten-way valve, the liquid nitrogen in the first liquid nitrogen cup (8) is replaced with hot water, and the cup is re-installed on the first cold trap (7), the nitrogen in the first cold trap (7) is rapidly released due to the heat, the flow rate of the first gas flow meter is 30 mL / min, and the ventilation is carried out for 10 minutes; The helium gas in the first helium gas inlet (1) passes through the first gas flow meter (2), the first water trap (3), the first gas connector (4), the second water trap (5), the first carbon dioxide trap (6), the second port (2102) of the ten-way valve, the third port (2103) of the ten-way valve, and enters the first cold trap (7). The nitrogen released by the purge continues to pass through the sixth port (2106) of the ten-way valve, the seventh port (2107) of the ten-way valve, the reaction tube (39), the seventh water trap (40), the fourth carbon dioxide trap (41), the chromatographic column (42), and enters the gas isotope mass spectrometer (43) for detection.

6. The method according to claim 5, characterized in that In the step 2, Open the upper cover of the first temperature-controlled heating furnace (13), open the first quick-detachable joint (11) and the second quick-detachable joint (14), remove the first bursting tube (12), load a small amount of 40-60 mesh mineral sample, place the first bursting tube (12) in the central groove of the first temperature-controlled heating furnace (13), and then connect the two ends of the first bursting tube (12) to the first quick-detachable joint (11) and the second quick-detachable joint (14); The flow rate of the second gas flow meter (16) is adjusted to 50 mL / min, a second liquid nitrogen cup (20) filled with liquid nitrogen is placed on the outer jacket of the second cold trap (19), and the temperature of the first temperature-controlled heating furnace (13) is set to 100° C.; The second helium inlet (17) is ventilated for 3 minutes, and the helium passes through the second gas flow meter (16), the fourth water trap (15), and the second quick-detachable joint (14) in sequence, enters the first bursting tube (12), purges the air in the first bursting tube (12), and continues to pass through the first quick-detachable joint (11), the third water trap (10), the second cold trap (19), the second carbon dioxide trap (9), the fifth port (2105) of the ten-way valve, the fourth port (2104) of the ten-way valve, and the first single-opening quartz tube (22), and finally enters the first ventilation port (23); The temperature of the first temperature-controlled heating furnace (13) is adjusted to 200° C. and ventilation is performed for 5 minutes to remove gas adsorbed on the surface of the mineral sample and low-temperature secondary inclusions; Open the upper cover of the second temperature-controlled heating furnace (31), open the third quick-detachable joint (29) and the fourth quick-detachable joint (32), remove the second bursting tube (30), load a small amount of 40-60 mesh mineral sample, place the second bursting tube (30) in the central groove of the second temperature-controlled heating furnace (31), and then connect the two ends of the second bursting tube (30) to the third quick-detachable joint (29) and the fourth quick-detachable joint (32); The flow rate of the third gas flow meter (27) is adjusted to 50 mL / min, a third liquid nitrogen cup (35) filled with liquid nitrogen is placed on the outer jacket of the third cold trap (34), and the temperature of the second temperature-controlled heating furnace (31) is set to 100° C.; The third helium inlet (26) is ventilated for 3 minutes, and the helium passes through the third gas flow meter (27), the fifth water trap (28), and the third quick-detachable joint (29) in sequence, enters the second burst tube (30), purges the air in the second burst tube (30), and continues to pass through the fourth quick-detachable joint (32), the sixth water trap (33), the third cold trap (34), the third carbon dioxide trap (36), the ninth port (2109) of the ten-way valve, the eighth port (2108) of the ten-way valve, the fourth cold trap (37), the first port (2101) of the ten-way valve, the tenth port (2110) of the ten-way valve, and the second single-opening quartz tube (25), and finally enters the second ventilation port (24); The temperature of the second temperature-controlled heating furnace (31) was adjusted to 200°C and ventilation was performed for 5 minutes to remove the gas adsorbed on the surface of the mineral sample and the low-temperature secondary inclusions.

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