An accelerator mass spectrometer 14 Graphite sample preparation device for C testing
By designing a graphite sample preparation device including vacuum system, graphite reduction assembly, CO2 purification assembly and sample pretreatment assembly, the problem of 14C sample preparation technology relying on foreign equipment and high cost is solved, and low-cost and efficient graphite samples are achieved. Preparation avoids sample contamination and data loss.
Patent Information
- Application Number
- CN202210683502.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-06-16
- Publication Date
- 2025-02-11
- Estimated Expiration
- 2042-06-16
AI Technical Summary
The existing 14C sample preparation technology relies on foreign commercial instruments or foreign engineers to build it, lacks domestic production, high equipment cost, low vacuum system utilization rate, and samples are easily contaminated during equipment transfer, resulting in the waste of experimental samples and the lack of scientific research data.
A graphite sample preparation device for accelerator mass spectrometer 14C testing is designed, including vacuum system, graphite reduction assembly, CO2 purification assembly and sample pretreatment assembly, to provide and control the vacuum environment through the tee main pipeline and valve system to avoid Sample contamination.
It reduces equipment costs, reduces space occupied, avoids contamination of samples during equipment transfer, and effectively reduces the invalidation of experimental samples and the lack of scientific research data.
Smart Images

Figure CN115078058B_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of graphite preparation, and specifically relates to an accelerator mass spectrometer 14 Graphite sample preparation apparatus for C testing. Background Art
[0002] Currently, radiocarbon isotopes ( 14 C) Accelerator mass spectrometry is widely used in research such as dating and environmental tracing. 14 The abundance of C in nature is about 1.2×10 -10 %, half-life is about 5370±40 years. Natural 14 C is mainly generated by the interaction of thermal neutrons from cosmic rays in the stratosphere with atmospheric nitrogen. 14 C will then be converted back into 14 N. 14 After C is formed, it is easily oxidized to 14 CO2 is then distributed to the atmosphere through atmospheric convection, and undergoes a carbon exchange cycle in the atmosphere-biosphere-hydrosphere through photosynthesis and other processes.
[0003] 14 The widespread use of C detection methods is inseparable from the progress of accelerator mass spectrometry technology. Accelerator mass spectrometry combines accelerator technology, nuclear detection technology and ordinary mass spectrometer technology to directly measure radioactive isotope particles in samples. It has high measurement sensitivity, small sample usage and short measurement time. Accelerator mass spectrometry usually obtains the required data by directly measuring graphite samples. Therefore, the carbon in the sample needs to be reduced to graphite. At the same time, to ensure that the sample is not contaminated by the outside world, the sample preparation needs to be completed under vacuum conditions. This process first converts the C in the carbon-containing sample into CO2 through chemical methods, then purifies the CO2, and then reduces the CO2 to graphite. Currently 14 C sample preparation mainly relies on commercial instruments or is built by foreign engineers. Such instruments have not yet been domestically produced. The manufacturing cost of experimental equipment is high, and the utilization rate of the vacuum system of each equipment is low. Samples are easily contaminated during the transfer process between different equipment, resulting in the scrapping of experimental samples and the loss of scientific research data. Summary of the invention
[0004] Based on the problems mentioned in the above background technology, the present invention provides an accelerator mass spectrometer 14 Graphite sample preparation device for C testing is used to solve the current 14 C Sample preparation mainly relies on foreign commercial instruments or is built by foreign engineers. There is no domestically produced such instrument yet. When preparing graphite samples, each device needs to be equipped with an independent vacuum system, which is costly and has low vacuum system utilization. In addition, samples are easily contaminated during the transfer process between different devices, resulting in the abandonment of experimental samples and the loss of scientific research data.
[0005] The technical solution adopted by the present invention is as follows:
[0006] An accelerator mass spectrometer 14 A graphite sample preparation device for C test comprises a vacuum system, a graphite reduction component, a CO2 purification component and a sample pretreatment component; the vacuum system is connected with the graphite reduction component and the CO2 purification component through a three-way main pipeline, a first main valve is arranged between the vacuum system and the graphite reduction component, a second main valve is arranged between the vacuum system and the CO2 purification component, and a first vacuum gauge is arranged between the first main valve and the second main valve for displaying 14 C. Vacuum degree of graphite sample preparation device; a third main valve is connected between the CO2 purification component and the sample pretreatment component, the vacuum system is used to provide a vacuum preparation environment, the CO2 purification component is used for CO2 purification, and the graphite reduction component includes a plurality of graphite reduction units connected to the three-way main pipeline for CO2 reduction. Through the opening and closing of the first main valve and the second main valve, supplemented by the monitoring of the first vacuum gauge, a set of vacuum system is realized to provide the required vacuum environment for the sample pretreatment component, the CO2 purification component and the graphite reduction component, and the connection between the pretreatment component and the CO2 purification component can prevent the sample from being easily contaminated during the transfer process of different devices.
[0007] On the basis of the above technical solution, the present invention has also made the following improvements:
[0008] Furthermore, the vacuum system includes a vacuum pump and a plate valve, the vacuum pump is connected to the three-way main pipeline through the plate valve, and the low vacuum and high vacuum working environments of the vacuum system are switched by opening and closing the plate valve, wherein the low vacuum is 10 -2 torr, high vacuum is 10 -5 torr.
[0009] Furthermore, the sample pretreatment component includes a connector, a gas sample injection part, a liquid sample injection part and an organic solid sample combustion part, the connector includes a first sub-valve and a first vacuum straight-through joint that are interconnected, the first sub-valve is connected to the CO2 purification component, and the first vacuum straight-through joint is used to connect the gas sample injection part, the liquid sample injection part and the organic solid sample combustion part. According to actual needs, multiple organic solid sample combustion parts can be connected in parallel to achieve batch pretreatment of organic solid samples, or one or three of the gas sample injection part, the liquid sample injection part and the organic solid sample combustion part can be selected and used alternately to achieve pretreatment of different types of samples.
[0010] Furthermore, the gas sample inlet part comprises an aluminum foil sampling bag and an air inlet hose which are interconnected, and the air inlet hose is detachably connected to the first vacuum straight-through connector.
[0011] Further, the liquid sample injection part includes a connecting pipe, on which a first isolation valve and a second vacuum straight-through joint are installed, and the second vacuum straight-through joint is connected to a Y-shaped tube, and the Y-shaped tube is composed of a Y-shaped tube main pipe and a Y-shaped tube side pipe. The Y-shaped tube is connected to the CO2 purification component through the second vacuum straight-through joint.
[0012] Furthermore, the organic solid sample combustion part includes a second isolation valve, an organic solid sample heating tube, a first heating furnace and a first temperature controller, which can realize uniform segmented speed-controlled heating within 1000°C. Under the action of the second isolation valve, the organic solid sample heating tube can be effectively isolated from the vacuum environment during the operation of the first heating furnace, thereby protecting the vacuum system and extending the service life of the vacuum system. The organic solid sample heating tube is detachably connected to the first vacuum straight-through joint, and the second isolation valve is arranged in front of the organic solid sample heating tube. The organic solid sample combustion part is connected to the glass pipeline of the CO2 purification component through the first vacuum straight-through joint, the first sub-valve and the third main valve, and a vacuum environment is provided for the organic solid sample heating tube in the organic solid sample combustion part through the glass pipeline of the CO2 purification component.
[0013] Furthermore, the CO2 purification component has a purification tube, on which a liquid nitrogen cold trap group, a subsidiary tube, a CO2 collection unit, a second vacuum gauge and a water collecting tube are connected, the subsidiary tube is connected to the second main valve, a second sub-valve is installed on the subsidiary tube, a third sub-valve is connected between the purification tube and the second main valve, a closing valve is provided at the end of the purification tube, a third isolation valve is installed at both ends of the connection between the CO2 collection unit and the subsidiary tube and the purification tube, the purification tube is connected to the third main valve through the water collecting tube, and a fourth isolation valve is installed on the water collecting tube.
[0014] Furthermore, the graphite reduction unit includes a three-way reduction tube connected in parallel with the first main valve, a fourth sub-valve is installed on the three-way reduction tube, the other two ends of the three-way reduction tube are respectively connected to a CO2 collector and a heating unit with valves, the sample transfer between the CO2 purification component and the graphite reduction component is carried out by the CO2 collector, a pressure gauge is connected to the heating unit, the heating unit includes an iron reaction tube and a zinc reaction tube connected in parallel, the iron reaction tube and the zinc reaction tube are both equipped with a second heating furnace, the second heating furnace is both equipped with a second temperature controller, and a lifter with a positioning function is installed under the second temperature controller.
[0015] Beneficial effects of the present invention:
[0016] 1. A vacuum system is used to provide the required vacuum environment for the sample pretreatment component, CO2 purification component and graphite reduction component, which reduces the cost and the space occupied by the equipment;
[0017] 2. The samples are not easily contaminated during the transfer between different equipment, which can better avoid the scrapping of experimental samples and the loss of scientific research data. BRIEF DESCRIPTION OF THE DRAWINGS
[0018] The present invention can be further illustrated by the non-limiting examples given in the accompanying drawings;
[0019] Figure 1 An accelerator mass spectrometer according to an embodiment of the present invention 14 C Schematic diagram of the structure of the graphite sample preparation device used for testing;
[0020] Figure 2 It is a structural schematic diagram of a vacuum system in an embodiment of the present invention;
[0021] Figure 3 This is a schematic diagram of the structure of a sample pretreatment component in an embodiment of the present invention;
[0022] Figure 4 This is a schematic diagram of the structure of a CO2 purification component in an embodiment of the present invention;
[0023] Figure 5 This is a schematic diagram of the structure of a graphite reduction assembly in an embodiment of the present invention;
[0024] Figure 6 Schematic diagram of the structure of the lifter in the embodiment of the present invention;
[0025] The main component symbols are described as follows:
[0026] Vacuum system 1, plate valve 1-1, three-way main line 1-2, first vacuum gauge 1-3, vacuum pump 1-4, graphite reduction component 2, first main valve 2-1, pressure gauge 2-2, second temperature controller 2-3, CO2 collector 2-4, iron reaction tube 2-5, fourth sub-valve 2-6, zinc reaction tube 2-7, second heating furnace 2-8, lifter 2-9, CO2 purification component 3, second main valve 3-1, third sub-valve 3-2, second vacuum gauge 3-3, second sub-valve 3-4, third isolation valve 3-5, third main valve 3-6, fourth isolation valve 3-7, water collection pipe 3-8, liquid nitrogen cold trap group 3-9, cold trap 3-9-1, freezing spiral tube 3- 9-2, CO2 collection unit 3-10, CO2 collection tube with valve 3-10-1, closing valve 3-11, sample pretreatment component 4, first sub-valve 4-1, first vacuum straight-through connector 4-2, gas sample injection part 4-3, aluminum foil sampling bag 4-3-1, air intake hose 4-3-2, liquid sample injection part 4-4, first isolation valve 4-4-1, second vacuum straight-through connector 4-4-2, Y-type tube main pipe 4-4-3, Y-type tube side pipe 4-4-4, organic solid sample combustion part 4-5, second isolation valve 4-5-1, organic solid sample heating tube 4-5-2, first heating furnace 4-5-3, first temperature controller 4-5-4. DETAILED DESCRIPTION
[0027] In order to enable those skilled in the art to better understand the present invention, the technical solution of the present invention is further described below in conjunction with the accompanying drawings and embodiments.
[0028] like Figures 1-2 As shown, an accelerator mass spectrometer 14A graphite sample preparation device for C test comprises a vacuum system 1, a graphite reduction component 2, a CO2 purification component 3 and a sample pretreatment component 4; the vacuum system 1 is connected with the graphite reduction component 2 and the CO2 purification component 3 through a three-way main line 1-2, a first main valve 2-1 is arranged between the vacuum system 1 and the graphite reduction component 2, a second main valve 3-1 is arranged between the vacuum system 1 and the CO2 purification component 3, and a first vacuum gauge 1-3 is arranged between the first main valve 2-1 and the second main valve 3-1; a third main valve 3-6 is connected between the CO2 purification component 3 and the sample pretreatment component 4, the vacuum system 1 is used to provide a vacuum preparation environment, the CO2 purification component 3 is used for CO2 purification, the graphite reduction component 2 comprises a plurality of graphite reduction units connected with the three-way main line 1-2 for CO2 reduction, in this embodiment, the number of graphite reduction units is preferably eight groups, and each graphite reduction unit works independently. By opening and closing the first main valve 2-1 and the second main valve 3-1, assisted by monitoring by the first vacuum gauge 1-3, a vacuum system is implemented to provide the required vacuum environment for the sample pretreatment component 4, the CO2 purification component 3 and the graphite reduction component 2.
[0029] Specifically, Figure 2 As shown, the vacuum system 1 includes a vacuum pump 1-4 and a plate valve 1-1. The vacuum pump 1-4 is connected to the three-way main line 1-2 through the plate valve 1-1. The low vacuum and high vacuum working environments of the vacuum system 1 are switched by opening and closing the plate valve 1-1. The low vacuum is 10 -2 torr, high vacuum is 10 -5 torr.
[0030] Specifically, Figure 3 As shown, the sample pretreatment component 4 includes a connector, a gas sample injection part 4-3, a liquid sample injection part 4-4 and an organic solid sample combustion part 4-5, and the connector includes a first sub-valve 4-1 and a first vacuum straight-through connector 4-2 that are interconnected, the first sub-valve 4-1 is connected to the CO2 purification component 3, and the first vacuum straight-through connector 4-2 is used to connect the gas sample injection part 4-3, the liquid sample injection part 4-4 and the organic solid sample combustion part 4-5. According to actual needs, multiple organic solid sample combustion parts 4-5 can be connected in parallel to achieve batch pretreatment of organic solid samples, or one or three of the gas sample injection part 4-3, the liquid sample injection part 4-4 and the organic solid sample combustion part 4-5 can be selected and used alternately to achieve pretreatment of different types of samples.
[0031] like Figure 3As shown, the gas sample inlet portion 4-3 includes an aluminum foil sampling bag 4-3-1 and an air intake hose 4-3-2 which are interconnected, and the air intake hose 4-3-2 is detachably connected to the first vacuum straight-through connector 4-2. The aluminum foil sampling bag 4-3-1 is connected to the CO2 purification component 3 through the air intake hose 4-3-2 and the first vacuum straight-through connector 4-2.
[0032] like Figure 3 As shown, the liquid sample injection part 4-4 includes a connecting pipe, on which a first isolation valve 4-4-1 and a second vacuum straight-through connector 4-4-2 are installed, and the second vacuum straight-through connector 4-4-2 is connected to a Y-shaped tube, and the Y-shaped tube is composed of a Y-shaped tube main pipe 4-4-3 and a Y-shaped tube side pipe 4-4-4. The Y-shaped tube is connected to the CO2 purification component 3 through the second vacuum straight-through connector 4-4-2.
[0033] For the treatment of inorganic carbon in the liquid sample, it is necessary to load the liquid sample to be treated into the Y-tube main pipe 4-4-3, load a certain amount of phosphoric acid into the Y-tube side pipe 4-4-4, connect the Y-tube with the first isolation valve 4-4-1 through the second vacuum straight-through connector 4-4-2, and then connect the liquid sample injection part 4-4 with the CO2 purification component 3 through the first vacuum straight-through connector 4-2. Open the first isolation valve 4-4-1, the first sub-valve 4-1 and the third main valve 3-6, and when the vacuum degree reaches 10 -5 torr, close valves 4-4-1 and 4-1, remove the liquid sample injection part 4-4 from the vacuum system, and properly pour the liquid sample injection part 4-4 to evenly mix the phosphoric acid in the Y-tube side tube 4-4-4 with the liquid sample in the Y-tube main tube 4-4-3, so that a chemical reaction occurs, thereby causing the C in the liquid sample to overflow in the form of CO2. After the reaction is completed, reinstall the liquid sample injection part 4-4 on the system through the first vacuum straight-through connector 4-2, open the third main valve 3-6 and the first sub-valve 4-1, and wait until the vacuum degree reaches 10 -5 torr, open the first isolation valve 4-4-1 to connect with the CO2 purification component 3 to perform purification operation.
[0034] Specifically, Figure 3As shown, the organic solid sample combustion part 4-5 includes a second isolation valve 4-5-1, an organic solid sample heating tube 4-5-2, a first heating furnace 4-5-3 and a first temperature controller 4-5-4. The organic solid sample heating tube 4-5-2 is detachably connected to the first vacuum straight-through connector 4-2, and the second isolation valve 4-5-1 is arranged in front of the organic solid sample heating tube 4-5-2. The organic solid sample combustion part 4-5 is connected to the glass pipeline of the CO2 purification component 3 through the first vacuum straight-through connector 4-2, the first sub-valve 4-1, and the third main valve 3-6, and a vacuum environment is provided for the organic solid sample heating tube 4-5-2 in the organic solid sample combustion part 4-5 through the glass pipeline of the CO2 purification component 3.
[0035] For the treatment of organic solid samples such as collagen, humic acid or wood-like α-cellulose, it is usually necessary to seal the tube first, that is, put the treated organic solid sample and a certain amount of copper oxide into the organic solid sample heating tube 4-5-2, and then connect the vacuum system 1 to evacuate to 10 -5 torr, seal the tube with acetylene flame, heat it with a muffle furnace, and install it into CO2 purification component 3 for purification after cooling. If there is leakage or other errors in the process, the sample needs to be re-prepared.
[0036] In this embodiment, the treated organic sample and a certain amount of copper oxide are placed in the organic solid sample heating tube 4-5-2, plugged with a high temperature resistant filter membrane, and connected to the CO2 purification component 3 through the first vacuum straight-through connector 4-2. -5 torr, close the third main valve 3-6, the first sub-valve 4-1, and the second isolation valve 4-5-1. Open the first heating furnace 4-5-3 and heat directly under the control of the first temperature controller 4-5-4. After the heating is completed, wait for the organic solid sample heating tube 4-5-2 to cool to room temperature, open the third main valve 3-6, the first sub-valve 4-1, and the second isolation valve 4-5-1, and directly introduce the CO2 generated by the calcination of the organic solid sample into the CO2 purification component 3 for purification operation, which can effectively avoid the original organic solid sample heating tube from leaking during heating in the muffle furnace, leaking during sealing, or breaking before purification, resulting in the loss of experimental samples.
[0037] Specifically, Figure 4As shown, the CO2 purification component 3 is a purification tube, and the purification tube is connected with a liquid nitrogen cold trap group 3-9, a sub-tube, a CO2 collection unit 3-10, a second vacuum gauge 3-3 and a water collecting tube 3-8. The sub-tube is connected to the second main valve 3-1, and a second sub-valve 3-4 is installed on the sub-tube. A third sub-valve 3-2 is connected between the purification tube and the second main valve 3-1, and a closing valve 3-11 is provided at the end of the purification tube. The CO2 collection unit 3-10 and both ends of the connection between the sub-tube and the purification tube are installed with a third isolation valve 3-5. The purification tube is connected with the third main valve 3-6 through the water collecting tube 3-8, and a fourth isolation valve 3-7 is installed on the water collecting tube 3-8. Among them, the liquid nitrogen cold trap group 3-9 includes a cold trap 3-9-1 and a freezing spiral tube 3-9-2 which are interconnected, and the freezing spiral tube 3-9-2 is connected to the purification tube; the CO2 collection unit 3-10 also includes a cold trap 3-9-1, and a CO2 collection tube 3-10-1 with a valve is connected between the cold trap 3-9-1 of the CO2 collection unit 3-10 and the purification tube.
[0038] Specifically, Figures 5-6 As shown, the graphite reduction unit includes a three-way reduction tube connected to the first main valve 2-1, a fourth sub-valve 2-6 is installed on the three-way reduction tube, the other two ends of the three-way reduction tube are respectively connected to a CO2 collector 2-4 with a valve and a heating unit, a pressure gauge 2-2 is connected to the heating unit, and the heating unit includes an iron reaction tube 2-5 and a zinc reaction tube 2-7 connected in parallel, and the iron reaction tube 2-5 and the zinc reaction tube 2-7 are both equipped with a second heating furnace 2-8, and the second heating furnace 2-8 is equipped with a second temperature controller 2-3, and a lifter 2-9 with a positioning function is installed below the second temperature controller 2-3. A heating temperature lower than 800°C can be provided as needed. Under the control of the lifter with a positioning function, uniform segmented asynchronous heating can be achieved in the 30cm area of the zinc reaction tube 2-7 and the iron reaction tube 2-5 in the reduction unit.
[0039] Among them, in high vacuum 10 -5 In the torr environment, the following two chemical reactions occur.
[0040]
[0041] Connect the CO2 collector 2-4 storing pure CO2, the zinc reaction tube 2-7 and the iron reaction tube 2-5 to the vacuum system, close the second main valve 3-1, and open the first main valve and the fourth sub-valve 2-6. First, draw a low vacuum to 10 -2 torr, open the plate valve 1-1 to draw a high vacuum. The vacuum degree reaches 10 -5torr, turn on the second heating furnace 2-8 of the heating unit to heat at a predetermined temperature. Remove impurities in the zinc particles and iron powder, and activate them for 30 minutes. Then close the fourth sub-valve 2-6 connected to the vacuum system 1 pipeline, and connect the CO2 collector 2-4, the zinc reaction tube 2-7 and the iron reaction tube 2-5 to conduct gas operation. After completion, raise the second heating furnace 2-8, and enter the reduction heating process according to the predetermined program through the second temperature controller 2-3. The above chemical reaction occurs in the zinc reaction tube 2-7 and the iron reaction tube 2-5, and the reaction pressure change is displayed by the pressure gauge 2-2.
[0042] The accelerator mass spectrometer provided by the present invention is as follows 14 The graphite sample preparation device for C test is introduced in detail. The description of the specific embodiment is only used to help understand the method and core idea of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made to the present invention without departing from the principle of the present invention, and these improvements and modifications also fall within the scope of protection of the claims of the present invention.
Claims
1. An accelerator mass spectrometer 14 C graphite sample preparation device for testing, characterized by: The invention comprises a vacuum system (1), a graphite reduction component (2), a CO2 purification component (3) and a sample pretreatment component (4); the vacuum system (1) is connected to the graphite reduction component (2) and the CO2 purification component (3) through a three-way main pipeline (1-2); a first main valve (2-1) is provided between the vacuum system (1) and the graphite reduction component (2); a second main valve (3-1) is provided between the vacuum system (1) and the CO2 purification component (3); a first vacuum gauge (1-3) is provided between the first main valve (2-1) and the second main valve (3-1); a third main valve (3-6) is connected between the CO2 purification component (3) and the sample pretreatment component (4); the vacuum system (1) The invention is used for providing a vacuum preparation environment. The CO2 purification component (3) is used for CO2 purification. The graphite reduction component (2) comprises a plurality of graphite reduction units connected to the three-way main pipeline (1-2) for CO2 reduction. The graphite reduction unit comprises a three-way reduction tube connected in parallel with the first main valve (2-1). The three-way reduction tube is provided with a fourth sub-valve (2-6). The other two ends of the three-way reduction tube are respectively connected with a CO2 collector (2-4) with a valve and a heating unit. The heating unit is connected with a pressure gauge (2-2). The heating unit comprises an iron reaction tube (2-5) and a zinc reaction tube (2-7) connected in parallel. The iron reaction tube (2-5) and the zinc reaction tube (2-7) are both provided with a second heating The first heating furnace (2-8) and the second heating furnace (2-8) are both equipped with a second temperature controller (2-3), and a lifter (2-9) with a positioning function is installed below the second temperature controller (2-3). The CO2 purification component (3) includes a purification tube, and the purification tube is connected to a liquid nitrogen cold trap group (3-9), an auxiliary pipe, a CO2 collection unit (3-10), a second vacuum gauge (3-3) and a water collection tube (3-8). The liquid nitrogen cold trap group (3-9) includes a cold trap (3-9-1) and a freezing spiral pipe (3-9-2) that are interconnected. The freezing spiral pipe (3-9-2) is connected to the purification tube, and the auxiliary pipe is connected to the second main valve (3-1). The auxiliary pipe is installed with a second sub-valve (3-4). The purification tube is connected to A third sub-valve (3-2) is connected between the second main valves (3-1), a closing valve (3-11) is provided at the end of the purification pipe, a third isolation valve (3-5) is installed at both ends of the CO2 collection unit (3-10) and the connection between the auxiliary pipe and the purification pipe, the purification pipe is connected to the third main valve (3-6) through a water collection pipe (3-8), and a fourth isolation valve (3-7) is installed on the water collection pipe (3-8). The vacuum system (1) comprises a vacuum pump (1-4) and a plate valve (1-1), the vacuum pump (1-4) is connected to the three-way main pipe (1-2) through the plate valve (1-1), and the switching of the low vacuum and high vacuum working environments of the vacuum system (1) is achieved by opening and closing the plate valve (1-1).
2. An accelerator mass spectrometer according to claim 1 14 C graphite sample preparation device for testing, characterized by: The sample pretreatment component (4) comprises a connector, a gas sample injection part (4-3), a liquid sample injection part (4-4) and an organic solid sample combustion part (4-5), wherein the connector comprises a first sub-valve (4-1) and a first vacuum straight-through connector (4-2) which are interconnected, wherein the first sub-valve (4-1) is connected to the CO2 purification component (3), and the first vacuum straight-through connector (4-2) is used to connect the gas sample injection part (4-3), the liquid sample injection part (4-4) and the organic solid sample combustion part (4-5).
3. An accelerator mass spectrometer according to claim 2 14 C graphite sample preparation device for testing, characterized by: The gas sample injection part (4-3) comprises an aluminum foil sampling bag (4-3-1) and an air intake hose (4-3-2) which are interconnected, and the air intake hose (4-3-2) is detachably connected to the first vacuum straight-through connector (4-2).
4. An accelerator mass spectrometer according to claim 2 14 C graphite sample preparation device for testing, characterized by: The liquid sample injection part (4-4) comprises a connecting pipe, on which a first isolation valve (4-4-1) and a second vacuum straight-through joint (4-4-2) are installed, and the second vacuum straight-through joint (4-4-2) is connected to a Y-shaped tube, and the Y-shaped tube consists of a Y-shaped tube main pipe (4-4-3) and a Y-shaped tube side pipe (4-4-4).
5. An accelerator mass spectrometer according to claim 2 14 C graphite sample preparation device for testing, characterized by: The organic solid sample combustion part (4-5) comprises a second isolation valve (4-5-1), an organic solid sample heating tube (4-5-2), a first heating furnace (4-5-3) and a first temperature controller (4-5-4); the organic solid sample heating tube (4-5-2) is detachably connected to the first vacuum straight-through connector (4-2); and the second isolation valve (4-5-1) is arranged in front of the organic solid sample heating tube (4-5-2).
Citation Information
Patent Citations
Device and method for preparing graphite by Zn / Fe flame sealed-tube method
CN110143590A