Oxidation reaction device for isotope analysis system

Abstract

The invention discloses an oxidation reaction device for an isotope analysis system, and belongs to the technical field of carbon isotope analysis systems.The gas inlet end of the oxidation reaction device is communicated with a gas chromatography, and the gas outlet end of the oxidation reaction device is communicated with an isotope ratio mass spectrometry. A gas inlet end of the heating furnace is communicated with a gas outlet of the gas chromatography, and a gas outlet end of the heating furnace is communicated with the isotope ratio mass spectrum; the oxidizing agent spraying structure is at least partially arranged at the upper end of the inner cavity so as to uniformly spray an oxidizing agent into the inner cavity; the oxidizing agent circulating structure is communicated with the oxidizing agent spraying structure through a first pipeline, and the oxidizing agent circulating structure conveys the oxidizing agent sprayed by the oxidizing agent spraying structure and collected at the bottom of the inner cavity to the oxidizing agent spraying structure again, so that repeated utilization of the oxidizing agent is achieved. According to the invention, by arranging the oxidant spraying structure, an oxidant is uniformly scattered in the heating furnace, so that the oxidation reaction is more sufficient, and the oxidation effect is enhanced.

Description

Technical Field

[0001] The invention belongs to the technical field of isotope analysis systems, and in particular relates to an oxidation reaction device used in isotope analysis systems. Background Art

[0002] As an effective means, stable isotope technology is of great significance for revealing the laws of material evolution in nature. It can provide rich information for studying atoms, molecules and ions in the microscopic world.

[0003] In the existing online carbon isotope test system for specific compounds, the oxidation reaction device is the core component connecting the gas chromatography and the isotope ratio mass spectrometer. The oxidation reaction device mainly includes a heating system, an oxidation reaction system and an interface system, etc. Its function is to oxidize the compounds separated by gas chromatography to generate a gas with a relatively simple molecular structure (such as CO2) through the oxidation reaction device for isotope composition analysis.

[0004] At present, due to the design of the current oxidation device itself, incomplete oxidation reaction will lead to a decrease in system sensitivity and resolution, which to a certain extent restricts the accuracy of the test. Summary of the invention

[0005] In order to solve the above problems, the present invention adopts the following technical solutions:

[0006] An oxidation reaction device for an isotope analysis system, wherein the air inlet end of the oxidation reaction device is connected to a gas chromatograph, and the air outlet end is connected to an isotope ratio mass spectrometer, and the oxidation reaction device comprises:

[0007] A heating furnace, wherein the heating furnace has an inner cavity, an air inlet end of the heating furnace is connected to an air outlet of the gas chromatograph, and an air outlet end of the heating furnace is connected to the isotope ratio mass spectrometer;

[0008] an oxidant spraying structure, wherein the oxidant spraying structure is at least partially disposed at the upper end of the inner cavity to uniformly spray the oxidant in the inner cavity;

[0009] An oxidant circulation structure is connected to the oxidant spraying structure through a first pipe. The oxidant circulation structure transports the oxidant sprayed by the oxidant spraying structure and collected at the bottom of the inner cavity to the oxidant spraying structure again to achieve the reuse of the oxidant.

[0010] Furthermore, a heating rod is arranged in the middle of the heating furnace.

[0011] Furthermore, the outer ring of the heating rod is provided with a spiral guide plate, and the guide plate is used to guide and slow down the oxidant sprayed downward by the oxidant spraying structure and the compound moving upward in the heating furnace.

[0012] Furthermore, a plurality of air holes are arranged on the guide plate.

[0013] Furthermore, the oxidant spraying structure comprises:

[0014] An oxidant storage device, wherein the oxidant storage device is arranged on the top of the heating furnace;

[0015] An air pump, the air pump is arranged at one side of the oxidant storage container, and the air pump is connected to the oxidant storage container through a second pipeline;

[0016] a first solenoid valve, wherein the first solenoid valve is disposed on the second pipeline;

[0017] a spraying dry pipe, wherein a first end of the spraying dry pipe is communicated with the second pipeline, and a second end of the spraying dry pipe penetrates the heating furnace and extends to the inner side of the heating furnace;

[0018] a spray branch pipe, the spray branch pipe being arranged inside the heating furnace and being connected to the second end of the spray main pipe;

[0019] A plurality of nozzles are arranged on the spray branch pipe at intervals.

[0020] Further, the oxidant circulation structure includes:

[0021] An oxidant collecting port, the oxidant collecting port being arranged at the lower end of the heating furnace and being communicated with the inner cavity of the heating furnace;

[0022] a powder delivery pump, wherein the powder delivery pump is disposed at one side of the oxidant collecting port, and the oxidant collecting port, the powder delivery pump and the oxidant storage container are connected through the first pipeline;

[0023] a second solenoid valve, the second solenoid valve being disposed on the first pipeline and located at a side close to the oxidant storage container;

[0024] An oxygen inlet pipe is arranged on a side of the oxidant collecting port away from the powder delivery pump and is communicated with the oxidant collecting port.

[0025] Furthermore, an air outlet pipe is provided at the top of the heating furnace, a dryer is provided at the other end of the air outlet pipe, and the dryer is connected to the isotope ratio mass spectrometer.

[0026] Beneficial effects:

[0027] The present invention arranges an oxidant spraying structure to evenly scatter the oxidant in the heating furnace, so that the oxidation reaction is more complete and the oxidation effect is enhanced.

[0028] The present invention realizes the repeated use of oxidants and saves resources by setting an oxidant circulation structure.

[0029] The present invention can guide the oxidant and block the compound through the spiral guide plate, thereby increasing the reaction time of the two in the heating furnace and enhancing the oxidation effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 The figure is a schematic diagram of the overall structure of an oxidation reaction device of an isotope analysis system of the present invention.

[0031] Among them, 1. gas chromatograph; 2. heating furnace; 3. isotope ratio mass spectrometer; 4. heating rod; 5. guide plate; 6. air pump; 7. first solenoid valve; 8. oxidant storage device; 9. oxidant collection port; 10. powder delivery pump; 11. second solenoid valve; 12. oxygen inlet pipe; 13. dryer; 14. outlet pipe. DETAILED DESCRIPTION

[0032] Example 1

[0033] refer to Figure 1 , an oxidation reaction device for an isotope analysis system, the air inlet end of the oxidation reaction device is connected to a gas chromatograph 1, the air outlet end is connected to an isotope ratio mass spectrometer 3, and the oxidation reaction device comprises:

[0034] A heating furnace 2, wherein the heating furnace 2 has an inner cavity, an air inlet end of the heating furnace 2 is connected to an air outlet of the gas chromatograph 1, and an air outlet end of the heating furnace 2 is connected to an isotope ratio mass spectrometer 3;

[0035] An oxidant spraying structure, wherein the oxidant spraying structure is at least partially disposed at the upper end of the inner cavity, and the oxidant is uniformly sprayed in the inner cavity through the oxidant spraying structure;

[0036] The oxidant circulation structure is connected to the oxidant spraying structure through a first pipe. The oxidant circulation structure transports the oxidant sprayed by the oxidant spraying structure and collected at the bottom of the inner cavity to the oxidant spraying structure again to realize the reuse of the oxidant.

[0037] The present invention arranges an oxidant spraying structure to evenly scatter the oxidant in the heating furnace, so that the oxidation reaction is more complete and the oxidation effect is enhanced.

[0038] In the specific implementation, the single hydrocarbon compounds are separated by gas chromatography 1 column, and the compounds are introduced into the oxidation reaction device in sequence under the drive of He carrier gas (purity ≥ 99.999%) and undergo oxidation reaction to generate CO2, which is introduced into the isotope ratio mass spectrometer 3 under the drive of He carrier gas.

[0039] Example 2

[0040] In order to improve practicality, this embodiment makes further arrangements based on Embodiment 1.

[0041] In this embodiment, a heating rod 4 is arranged in the middle of the heating furnace 2 .

[0042] In this embodiment, the outer ring of the heating rod 4 is provided with a spiral guide plate 5, and the guide plate 5 is used to guide and slow down the oxidant sprayed downward by the oxidant spraying structure and the compound moving upward in the heating furnace 2.

[0043] In specific implementation, the spiral guide plate 5 can not only guide the oxidant, but also block the compound, thereby increasing the reaction time of the two in the heating furnace 2 and enhancing the oxidation effect.

[0044] Preferably, the oxidant is CuO;

[0045] In the specific implementation, during the reaction, the compound needs to be carried out at a temperature greater than 800°C, and the reaction formula is:

[0046] 4CuO→2Cu2O+O2;

[0047] 4CnHm+(4n+m)O2→4nCO2+2mH2O;

[0048] Under high-temperature working conditions, due to the different atomic weights of carbon isotopes 13C and 12C, the difference in the movement rates of molecules with different carbon isotope compositions (such as 12CH4, 13CH4 or 12CO2, 13CO2) can lead to differences in the leakage rates of molecules with different isotope compositions and cause isotope fractionation.

[0049] In this embodiment, the guide plate 5 is provided with a plurality of air holes.

[0050] In this embodiment, the oxidant spraying structure includes:

[0051] The oxidant storage device 8 is arranged on the top of the heating furnace 2;

[0052] An air pump 6, which is disposed on one side of the oxidant storage container 8, and the air pump 6 is connected to the oxidant storage container through a second pipeline;

[0053] A first solenoid valve 7, wherein the first solenoid valve 7 is arranged on the second pipeline;

[0054] A spraying dry pipe, the first end of which is connected to the second pipe, and the second end of which passes through the heating furnace 2 and extends to the inner side of the heating furnace 2;

[0055] A spray branch pipe, which is arranged inside the heating furnace 2 and is connected to the second end of the spray main pipe;

[0056] A plurality of nozzles are arranged on the spray branch pipe at intervals.

[0057] In specific implementation, when the oxidant needs to be sprayed in the heating furnace, the air pump 6 and the first solenoid valve 7 are turned on to drive the CuO powder to be sprayed through the spraying main pipe, the spraying branch pipe and the nozzle and scattered in the inner cavity of the heating furnace 2.

[0058] In this embodiment, the oxidant circulation structure includes:

[0059] The oxidant collecting port 9 is arranged at the lower end of the heating furnace 2 and communicated with the inner cavity of the heating furnace 2;

[0060] In a specific implementation, the bottom of the inner cavity of the heating furnace 2 is funnel-shaped in order to more conveniently collect the oxidant.

[0061] A powder delivery pump 10, which is disposed on one side of the oxidant collecting port 9, and the oxidant collecting port 9, the powder delivery pump 10 and the oxidant storage container 8 are connected via a first pipeline;

[0062] A second solenoid valve 11, which is disposed on the first pipeline and is located on a side close to the oxidant storage container 8;

[0063] The oxygen inlet pipe 12 is arranged at a side of the oxidant collecting port 9 away from the powder delivery pump 10 and is communicated with the oxidant collecting port 9 .

[0064] During specific implementation, a valve is provided on the oxygen inlet pipe 12 .

[0065] In specific implementation, during the operation of the oxidation device, oxygen in CuO is gradually consumed to generate Cu2O, resulting in a decrease in its oxidation ability, and Cu2O is collected through the oxidant collecting port 9, and then oxygen is introduced to perform a 2Cu2O+O2→4CuO reaction to activate the oxidant, and then the second solenoid valve 11 is opened, the first solenoid valve 7 is closed, and the CuO is transported to the oxidant storage container 8 through the powder delivery pump 10 for reuse.

[0066] In this embodiment, an air outlet pipe 14 is disposed at the top of the heating furnace 2 , and a dryer 13 is disposed at the other end of the air outlet pipe 14 . The dryer 13 is connected to the isotope ratio mass spectrometer 3 .

[0067] In a specific implementation, CO2 is driven by He carrier gas, dried by the drying device 14, and then transported to the isotope ratio mass spectrometer 3.

[0068] The above description is only a preferred embodiment of the present invention and does not limit the technical scope of the present invention. Therefore, any slight modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. An oxidation reaction device for an isotope analysis system, wherein the air inlet end of the oxidation reaction device is connected to a gas chromatograph, and the air outlet end is connected to an isotope ratio mass spectrometer, characterized in that: The oxidation reaction device comprises: A heating furnace, wherein the heating furnace has an inner cavity, an air inlet end of the heating furnace is connected to an air outlet of the gas chromatograph, and an air outlet end of the heating furnace is connected to the isotope ratio mass spectrometer; an oxidant spraying structure, wherein the oxidant spraying structure is at least partially disposed at the upper end of the inner cavity to uniformly spray the oxidant in the inner cavity; An oxidant circulation structure is connected to the oxidant spraying structure through a first pipe. The oxidant circulation structure transports the oxidant sprayed by the oxidant spraying structure and collected at the bottom of the inner cavity to the oxidant spraying structure again to achieve the reuse of the oxidant.

2. The oxidation reaction device for isotope analysis system according to claim 1, characterized in that: A heating rod is arranged in the middle of the heating furnace.

3. The oxidation reaction device for isotope analysis system according to claim 2, characterized in that: The outer ring of the heating rod is provided with a spiral guide plate, and the guide plate is used to guide and slow down the oxidant sprayed downward by the oxidant spraying structure and the compound moving upward in the heating furnace.

4. The oxidation reaction device for isotope analysis system according to claim 3, characterized in that: The guide plate is provided with a plurality of air holes.

5. The oxidation reaction device for isotope analysis system according to claim 1, characterized in that: The oxidant spraying structure comprises: An oxidant storage device, wherein the oxidant storage device is arranged on the top of the heating furnace; An air pump, the air pump is arranged at one side of the oxidant storage container, and the air pump is connected to the oxidant storage container through a second pipeline; a first solenoid valve, wherein the first solenoid valve is disposed on the second pipeline; a spraying dry pipe, wherein a first end of the spraying dry pipe is communicated with the second pipeline, and a second end of the spraying dry pipe penetrates the heating furnace and extends to the inner side of the heating furnace; a spray branch pipe, the spray branch pipe being arranged inside the heating furnace and being connected to the second end of the spray main pipe; A plurality of nozzles are arranged on the spray branch pipe at intervals.

6. The oxidation reaction device for isotope analysis system according to claim 5, characterized in that: The oxidant cycle structure includes: An oxidant collecting port, the oxidant collecting port being arranged at the lower end of the heating furnace and being communicated with the inner cavity of the heating furnace; a powder delivery pump, wherein the powder delivery pump is disposed at one side of the oxidant collecting port, and the oxidant collecting port, the powder delivery pump and the oxidant storage container are connected through the first pipeline; a second solenoid valve, the second solenoid valve being disposed on the first pipeline and located at a side close to the oxidant storage container; An oxygen inlet pipe is arranged on a side of the oxidant collecting port away from the powder delivery pump and is communicated with the oxidant collecting port.

7. The oxidation reaction device for isotope analysis system according to claim 1, characterized in that: An air outlet pipe is arranged at the top of the heating furnace, a dryer is arranged at the other end of the air outlet pipe, and the dryer is connected to the isotope ratio mass spectrometer.

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