CN115980378B - Full-automatic multi-station recovery function thermal desorption instrument - Google Patents

Full-automatic multi-station recovery function thermal desorption instrument Download PDF

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Publication number
CN115980378B
CN115980378B CN202310209075.XA CN202310209075A CN115980378B CN 115980378 B CN115980378 B CN 115980378B CN 202310209075 A CN202310209075 A CN 202310209075A CN 115980378 B CN115980378 B CN 115980378B
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sample
recovery
tube
flow controller
mass flow
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CN115980378A (en
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罗利华
韩雷刚
穆培东
燕向晖
郭凯
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Beijing Juxin Zhuifeng Technology Co ltd
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Beijing Juxin Zhuifeng Technology Co ltd
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Abstract

The invention relates to the technical field of sample analysis and discloses a full-automatic multi-station recovery function thermal desorption instrument which comprises a sample tray, sample recovery tubes, sample tubes, a movable module, a low-temperature focusing cold trap, an analysis path mass flow controller, a pre-trap flow distribution recovery path mass flow controller, a sample injection flow distribution recovery path mass flow controller, a six-way valve, an upper needle insertion module and a lower needle insertion module, wherein samples are filled in the sample tubes, the sample recovery tubes and the sample tubes are distributed on the sample tray in an annular shape, and the sample recovery tubes and the sample tubes are arranged perpendicular to the tray surface of the sample tray. The gas circuit adopts the combination of the double electric control six-way valve and the electromagnetic valve, can automatically complete the four processes of primary analysis, secondary low-temperature enrichment, secondary analysis, sample injection and back blowing of the single (double) multi-branch adsorption tube in a programming way, and can independently set the primary analysis temperature, the secondary analysis temperature, the cold trap temperature and the pipeline heating temperature, and better control the processes of sample analysis and the like according to the set split ratio.

Description

Full-automatic multi-station recovery function thermal desorption instrument
Technical Field
The invention relates to the field of sample analysis, in particular to a full-automatic multi-station recovery function thermal desorption instrument.
Background
In the aspect of domestic occupational health, gas which is high in concentration and harmful to human bodies is often analyzed, because the concentration of a sample is high and the sample is possibly harmful to human bodies, when the sample is analyzed by equipment, the accuracy of an experiment result can be ensured, the gas cannot be discharged into the air, the capturing capability of a thermal desorption instrument on the market for the sample is limited, and the recovery of all the samples cannot be ensured even if the thermal desorption instrument has a recovery function.
The existing thermal desorption instrument cannot meet the requirement of a customer for analyzing a high-concentration sample, cannot guarantee the accuracy of experimental data, does not shunt and recycle the sample, cannot prevent toxic samples from being discharged into the air to pollute the air in a laboratory, and causes the influence of sample leakage to influence the health of test staff.
Disclosure of Invention
The invention provides a full-automatic multi-station recovery function thermal desorption instrument, which solves the technical problems that samples cannot be subjected to split recovery in the related art and toxic samples are prevented from being discharged into the air to pollute the air in a laboratory.
The full-automatic multi-station recovery function thermal desorption instrument comprises a sample disk, a sample recovery pipe, sample pipes, a moving module, a low-temperature focusing cold trap, an analytical path mass flow controller, a front-trap split recovery path mass flow controller, a sample split recovery path mass flow controller, a six-way valve, an upper needle insertion module and a lower needle insertion module, wherein the sample pipes are filled with samples, the sample recovery pipe and the sample pipes are distributed on the sample disk in an annular mode, the sample recovery pipe and the sample pipes are perpendicular to the disk surface of the sample disk, the upper needle insertion module and the lower needle insertion module are respectively arranged on two ends of the sample recovery pipe and the sample pipe, the upper needle insertion module and the lower needle insertion module can move towards each other, when the needle ends of the upper needle insertion module and the lower needle insertion module move towards each other, the sample pipes are inserted into the sample pipes, the moving module is positioned on one side of the sample pipes, the end of the moving module is provided with a heating block, the heating block is driven to move towards one side of the sample pipes, the six-way valve is respectively connected with the front-trap split recovery path mass flow controller, the front-split flow controller and the sample pipe split flow controller are connected with the sample recovery path mass flow controller, the front-injection module and the sample injection module are connected with the sample recovery device, the sample injection end of the sample recovery device and the sample recovery device, the sample injection module is connected with the front-station flow control device, the sample recovery device, the sample injection end is connected with the sample recovery port and the sample recovery device, and the sample flow control device;
the moving module drives the heating block to abut against the outer wall of the sample tube to abut against and heat, the analysis path mass flow controller controls the carrier gas to sweep and split the sample heated and separated out in the sample tube, the sample is split into the pre-trap split recovery path mass flow controller, the sample is quantitatively split into the sample recovery tube, the split sample enters the low-temperature focusing cold trap, when the sample is enriched in the low-temperature focusing cold trap, the six-way valve is switched to bypass, the sample enriched in the low-temperature focusing cold trap is switched to the sample injection path, the low-temperature focusing cold trap is heated to enable the enriched sample to escape, the sample split recovery path mass flow controller splits the escaped sample, the sample is quantitatively split into the sample recovery tube, the split sample enters the analysis instrument, the six-way valve is switched from the bypass to an initial state, the carrier gas is introduced to reversely blow and clean the sample tube and the sample recovery tube, the low-temperature focusing cold trap is cooled and switched to an initial state, and the stations of the sample recovery tube and the sample tube are switched on the sample tray.
Further: the feeding and discharging assembly is arranged on one side of the movable module and used for replacing the sample tube and the sample recovery tube after switching stations of the sample recovery tube and the sample tube on the sample tray;
the sample recovery tube and the sample tube comprise a tube body, an upper end cover, a lower end cover and a plastic sealing gasket, wherein both ends of the tube body are sealed through the plastic sealing gasket, and the upper end cover and the lower end cover are used for mounting the tube body part on a sample tray;
the feeding and discharging assembly comprises an end cover dismounting unit and a feeding part, the feeding part is arranged on the bottom side of the end cover dismounting unit, the end cover dismounting unit comprises a connecting seat, a shaft seat, a connecting rod and a transmission shaft, the transmission shaft is vertically arranged on the outer wall of one end of the connecting seat, the shaft seat is sleeved on the shaft end of the transmission shaft, the rod end of the connecting rod is provided with a passive groove, the connecting part is arranged at the bottom end of the connecting seat, the connecting part is used for connecting the shaft seat with the rod end of the connecting rod, the transmission shaft drives the shaft seat to rotate, the shaft seat drives the connecting seat to move back and forth along the vertical direction, the connecting rod is transmitted through the connecting part, the rod end of the connecting rod is connected with a dismounting sheet, the connecting rod drives the upper end cover to rotate and detach from the sample disc through the passive groove, the feeding part replaces the tube and the tube body of the sample recovery tube, and then the upper end cover is rotationally assembled on the tube end of the tube body after replacement, and tube body replacement of the sample recovery tube is achieved.
Further: the device comprises an analysis path mass flow controller, a carrier gas, a purging path pressure stabilizing valve, a blowback valve, an analysis path electromagnetic valve and a standard sample making electromagnetic valve, wherein the purging path pressure stabilizing valve is connected between the analysis path mass flow controller and the carrier gas through pipelines, the purging path pressure stabilizing valve is connected with the blowback valve, the analysis path electromagnetic valve and the standard sample making electromagnetic valve respectively, the analysis path electromagnetic valve is connected with the analysis path mass flow controller, the analysis path mass flow controller is connected to a lower needle inserting module through an electronic pressure sensor, and the lower needle inserting module connected with the electronic pressure sensor is a lower needle inserting module connected with a sample tube.
Further: the upper needle insertion module is connected to the upper needle insertion of the sample tube and is divided into two pipelines, wherein one pipeline is connected to the six-way valve, and the other pipeline is connected to the front-trap diversion-path mass flow controller.
Further: one end of the front shunt path mass flow controller of the trap, which is far away from the six-way valve, is connected with a first tee joint, one end of the first tee joint is connected with an upper needle of the upper needle insertion module, which is connected with a sample recovery tube, the other end of the first tee joint is connected with the shunt flow controller, and one end of the sample recovery tube, which is far away from the tee joint, is connected with a recovery vent through one end of the lower needle insertion module, which is connected with the sample recovery tube.
Further: one end of the standard sample making electromagnetic valve, which is far away from the purging path pressure stabilizing valve, is connected with a needle valve, and the other end of the needle valve is connected to the calibration interface.
Further: one end of the back-blowing valve, which is far away from the purging path pressure stabilizing valve, is connected with a second tee joint, one port of the second tee joint is connected with the emptying valve, and the other port of the second tee joint is connected with the six-way valve.
Further: the low-temperature focusing cold trap is internally provided with a enrichment pipe, one end of the enrichment pipe is connected with the six-way valve, and the other end of the enrichment pipe is connected with the other interface of the six-way valve.
Further: the carrier gas way mass flow controller is connected with a carrier gas way pressure stabilizing valve, the other end of the carrier gas way mass flow controller is connected with one of interfaces of the six-way valve, the interface of the six-way valve is connected with a third tee joint, one end interface of the third tee joint is connected to the column temperature box, the other end interface of the third tee joint is connected with a shunt electromagnetic valve, and the other end of the shunt electromagnetic valve is connected with the shunt flow controller.
Further: the feeding piece comprises a clamping belt, a feeding roller, a driving roller and a support, wherein the feeding roller, the driving roller and a transmission shaft are arranged in the support, the feeding roller, the driving roller and the transmission shaft form a triangular structure, the clamping belt is sleeved on the outer sides of the feeding roller, the driving roller and the transmission shaft, the clamping belt drives the feeding roller to transmit through the driving roller and the transmission shaft, a pipe clamping groove is formed in the clamping belt, and the pipe clamping groove is of an omega-shaped structure.
Further: the both sides of material loading roller are equipped with first convex part and second convex part respectively, and the protrusion height of first convex part is higher than the protrusion height of second convex part.
Further: the shaft seat comprises a lifting part and a transmission tooth part, wherein the lifting part is distributed on the outer edge of the upper end of the transmission tooth part, and the lifting part is of an annular wavy structure.
Further: the feeding and discharging assembly further comprises a feeding top seat and a driving piece, wherein the driving piece is used for driving the feeding top seat to make an L-shaped moving track, and a clamping piece is arranged at the end part of the feeding top seat.
The invention has the beneficial effects that:
the thermal adsorption instrument is provided with a double-ring sample tube and a sample recovery tube, and simultaneously, a gas circuit is combined with a double-electric control six-way valve and an electromagnetic valve, so that four processes of primary analysis, secondary low-temperature enrichment, secondary analysis, sample introduction and back blowing of a single (double) multi-way adsorption tube can be automatically completed in a programming mode, the primary analysis temperature, the secondary analysis temperature, the cold trap temperature and the pipeline heating temperature can be independently set, and according to the set split ratio, the process control such as sample analysis is better, the requirements of customers on analyzing high-concentration samples are met, the accuracy of experimental data is ensured, the samples can be split and recovered, and toxic samples are prevented from being discharged into the air to pollute the indoor air of a laboratory.
Drawings
FIG. 1 is a schematic structural diagram of a thermal desorption instrument with full-automatic multi-station recovery function, which is provided by the invention;
fig. 2 is a schematic diagram of the internal structure of a thermal desorption instrument with full-automatic multi-station recovery function according to the present invention;
FIG. 3 is a side view of a mobile module connecting structure of a thermal desorption instrument with full-automatic multi-station recovery function according to the present invention;
FIG. 4 is a top view of FIG. 3;
FIG. 5 is a schematic diagram of the gas path of a thermal desorption instrument with full-automatic multi-station recovery function according to the present invention;
fig. 6 is a schematic diagram of a loading and unloading assembly of a thermal desorption instrument with full-automatic multi-station recovery function according to the present invention;
fig. 7 is a schematic diagram of the structure of a sample tube and a sample recovery tube of the full-automatic multi-station recovery function thermal desorption instrument;
FIG. 8 is a top view of the feed roll of FIG. 6;
FIG. 9 is a schematic illustration of the connecting rod structure of FIG. 6;
fig. 10 is a schematic view of the axle seat structure of fig. 6.
In the figure: 1. a sample recovery tube; 2. a sample tube; 2a, a tube body; 2b, a plastic packaging gasket; 2c, an upper end cover; 2d, a lower end cover; 3. a sample tray; 4. recovering the road needle; 5. analyzing a path sampling needle; 6. an upper needle inserting module; 7. a six-way valve; 8. a low temperature focusing cold trap; 9. analyzing the road mass flow controller; 10. a pre-trap split recovery path mass flow controller; 11. a sample injection diversion recovery path mass flow controller; 12. an electromagnetic valve group; 13. a heating block; 14. a lower needle inserting module; 15. a mobile module; 16. feeding and discharging components; 161. a driving member; 162. discharging a top seat; 163. a clamping belt; 164. a material injection port; 165. a feeding roller; 1651. a first convex portion; 1652. a second convex portion; 166. an end cover dismounting unit; 1661. a connecting seat; 1662. a shaft seat; 16621. a lifting part; 16622. a transmission tooth portion; 1663. a connecting rod; 16631. a passive slot; 16332. a rod body; 1664. a transmission shaft; 17. a sample transmission line; 18. a power switch; 19. a housing; 20. a pressure gauge; 21. a pressure stabilizing valve group; 22. a rich pipe; 23. a carrier gas path mass flow controller; 24. a blowback valve; 25. a blow-off valve; 26. the gas carrying path pressure stabilizing valve; 27. a sweeping path pressure stabilizing valve; 28. analyzing a path electromagnetic valve; 29. a touch screen; 30. a needle valve; 31. preparing a standard sample electromagnetic valve; 32. an electronic pressure sensor; 33. a pre-trap shunt mass flow controller; 34. a shunt recovery electromagnetic valve in front of the trap; 35. a split flow controller; 36. a shunt electromagnetic valve.
Detailed Description
The subject matter described herein will now be discussed with reference to example embodiments. It is to be understood that these embodiments are merely discussed so that those skilled in the art may better understand and implement the subject matter described herein and that changes may be made in the function and arrangement of the elements discussed without departing from the scope of the disclosure herein. Various examples may omit, replace, or add various procedures or components as desired. In addition, features described with respect to some examples may be combined in other examples as well.
Example 1
Referring to fig. 1-10, a full-automatic multi-station recovery functional thermal desorption instrument comprises a sample tray 3, a sample recovery tube 1, a sample tube 2, a moving module 15, a low-temperature focusing cold trap 8, an analysis path mass flow controller 9, a pre-trap diversion recovery path mass flow controller 10, a sample injection diversion recovery path mass flow controller 11, a six-way valve 7, an upper needle inserting module 6 and a lower needle inserting module 14, wherein samples are filled in the sample tube 2, the sample recovery tube 1 and the sample tube 2 are distributed on the sample tray 3 in an annular shape, the sample recovery tube 1 and the sample tube 2 are arranged perpendicular to the tray surface of the sample tray 3, the upper needle inserting module 6 and the lower needle inserting module 14 are respectively arranged on two ends of the sample recovery tube 1 and the sample tube 2, the upper needle inserting module 6 and the lower needle inserting module 14 can move oppositely or relatively, when the needle ends of the upper needle inserting module 6 and the lower needle inserting module 14 move oppositely, the sample tube 2 and the sample recovery tube 1 are inserted into the needle ends and communicated with the needle ends, the moving module 15 is positioned at one side of the sample tube 2, the end part of the moving module 15 is provided with a heating block 13, the moving module 15 drives the heating block 13 to move towards one side of the sample tube 2, the six-way valve 7 is respectively connected with the analysis path mass flow controller 9, the pre-trap diversion recovery path mass flow controller 10 and the sample injection diversion recovery path mass flow controller 11 through air pipes, the connecting end of the analysis path mass flow controller 9 is connected with carrier gas and the sample tube 2, the connecting end of the pre-trap diversion recovery path mass flow controller 10 is connected with the sample recovery tube 1 and the low-temperature focusing cold trap 8, and the connecting end of the sample injection diversion recovery path mass flow controller 11 is connected with the sample recovery tube 1 and an analysis instrument;
as shown in fig. 1 to 4, the thermal desorption apparatus generally works as follows:
the sample grade on the sample tray 3 consists of an inner ring and an outer ring, the outer ring is a sample tube 2, the inner ring is a diversion recovery tube, a heating block 13 moves forwards to wrap the sample tube 2 on the outer ring of the sample tray 3 when the sample tube 2 is analyzed, at the moment, nitrogen controlled by mass flow passes through the sample tube 2 to blow off the sample to be analyzed from the sample tube 2 after high-temperature analysis, the gaseous sample leaving the sample tube 2 is diverted before entering the low-temperature focusing cold trap 8, and a part of the gaseous sample enters the low-temperature focusing cold trap 8 and the other part of the gaseous sample enters an adsorption tube on the inner ring of the sample tray 3 for recovery according to the set diversion ratio; after the analysis of the sample in the sample tube 2 is finished, the sample enriched in the low-temperature focusing cold trap 8 is heated again, meanwhile, a six-way sample injection valve is switched, the sample is brought into a chromatograph by carrier gas for analysis, the split sample is also subjected to split treatment before entering the chromatograph, the split sample is also recycled into the sample recycling tube 1 of the inner ring through a transmission pipeline, and after the sample injection is finished, nitrogen gas can carry out back flushing cleaning on the low-temperature focusing cold trap 8; after the cleaning is finished, the sample tray 3 is turned to the next station, and the analysis process of the next sample is automatically performed until all the samples are analyzed.
Specifically, the sample recovery tube 1 and the sample tube 2 placed on the sample tray 3 are rotated to specific positions and then respectively move downwards and upwards by the upper needle insertion module 6 and the lower needle insertion module 14, so that the recovery path needle 4 and the analysis path sampling needle 5 are driven to respectively prick the sample recovery tube 1 and the sample tube 2, the moving module 15 drives the heating block 13 to abut against the outer wall of the sample tube 2 and heat the sample, the analysis path mass flow controller 9 controls nitrogen/helium to purge and split the heated and pyrolyzed sample in the sample tube 2, the sample is split into the pre-trap split recovery path mass flow controller 10, the sample is quantitatively split into the sample recovery tube 1, the split sample enters the low-temperature focusing cold trap 8, the sample is enriched in the low-temperature focusing cold trap 8, the six-way valve 7 is switched by a bypass, the sample enriched in the low-temperature focusing cold trap 8 is switched to a sample injection path, the low-temperature focusing cold trap 8 is heated to enable the enriched sample to escape, the sample split the sample is quantitatively split into the sample recovery tube 1, the split sample enters the initial analysis valve 7, the sample is switched to the initial state from the bypass valve 7 to the sample recovery tube 2, and the sample carrier gas is cooled down to the initial stage of the sample recovery tube 2, and the sample recovery tube is cooled down by the carrier gas tube 1, and the sample is cooled down and the initial stage of the sample recovery tube is cooled by the carrier gas tube 1.
It should be noted that, the air circuit is also provided with an electromagnetic valve set 12, and the electromagnetic valve set 12 includes, but is not limited to, an analysis path electromagnetic valve 28, a standard sample preparation electromagnetic valve 31, a pre-trap shunt recovery electromagnetic valve 34 and a shunt electromagnetic valve 36.
It should be noted that, the moving module of the heating block 13 includes but is not limited to a linear pushing member such as an air cylinder, etc., the heating block 13 driving the end portion heats the tube 2a, the heating block 13 is internally provided with a heating member, and the heating member includes but is not limited to a heating wire, a temperature controller, etc., and the heating member is mainly used for heating the tube 2a, so that the internal sample is resolved and escaped.
It should be noted that, a casing 19 is arranged at the outer side of the thermal desorption apparatus, a sample tray 3 is arranged at one side of the casing 19, a pressure stabilizing valve set 21, a pressure gauge 20, a touch screen 29, a power switch 18 and the like are arranged at the outer wall of one side of the casing 19 close to the sample tray 3, one side of the casing 19 is also connected with a sample transmission line 17, and the sample transmission line 17 is connected with an internal feeding and discharging assembly 16;
wherein the valve block 21 includes, but is not limited to, a purge path regulator valve 27 and a carrier gas path regulator valve 26.
The pressure gauge 20 is used for visually reflecting the circulation pressure of the air path, the touch screen 29 is used for displaying a control interface, and the power switch 18 is used for opening and closing electric parts in the equipment.
The complete gas circuit involved in the thermal desorption instrument is shown in fig. 5:
the purging way pressure stabilizing valve 27 is connected between the analysis way mass flow controller 9 and the carrier gas, the purging way pressure stabilizing valve 27 is respectively connected with the blowback valve 24, the analysis way electromagnetic valve 28 and the standard sample preparing electromagnetic valve 31 through pipelines, the analysis way electromagnetic valve 28 is connected with the analysis way mass flow controller 9, the analysis way mass flow controller 9 is connected to the lower needle inserting module 14 through the electronic pressure sensor 32, and the lower needle inserting module 14 connected with the electronic pressure sensor 32 is the lower needle inserting connected with the sample tube 2; the upper needle insertion module 6 is divided into two pipelines, wherein one pipeline is connected to a third port of the six-way valve 7, and the other pipeline is connected to a pre-trap diversion pipeline mass flow controller 33; the end, far away from the six-way valve 7, of the front-trap diversion path mass flow controller 33 is connected with a first tee, one end of the first tee is connected with an upper needle in the upper needle insertion module 6, the other end of the first tee is connected with a diversion flow controller 35, and one end, far away from the tee, of the sample recovery tube 1 is connected to a recovery vent through one end, connected with the sample recovery tube 1, in the lower needle insertion module 14;
one end of the standard sample preparation electromagnetic valve 31, which is far away from the purge path pressure stabilizing valve 27, is connected with a needle valve 30, and the other end of the needle valve 30 is connected to a calibration interface; one end of the back-blowing valve 24, which is far away from the sweeping path pressure stabilizing valve 27, is connected with a second tee joint, one port of the second tee joint is connected with the emptying valve 25, and the other port of the second tee joint is connected with the interface four of the six-way valve 7; the low-temperature focusing cold trap 8 is internally provided with a enrichment pipe 22, one end of the enrichment pipe 22 is connected with the interface two of the six-way valve 7, and the other end of the enrichment pipe 22 is connected with the interface five of the six-way valve 7.
The carrier gas path mass flow controller 23 is connected with a carrier gas path pressure stabilizing valve 26, the other end of the carrier gas path mass flow controller 23 is connected with an interface six of the six-way valve 7, an interface one of the six-way valve 7 is connected with a third tee joint, one end of the third tee joint is connected to the column temperature box, the other end of the third tee joint is connected with a split flow electromagnetic valve 36, and the other end of the split flow electromagnetic valve 36 is connected with a split flow controller 35.
Example two
Referring to fig. 2, 6-10, the thermal desorption apparatus further includes an upper and lower material assembly 16, where the upper and lower material assembly 16 is disposed on one side of the moving module 15, and the upper and lower material assembly 16 is used to replace the sample tube 2 and the sample recovery tube 1 after switching the stations of the sample recovery tube 1 and the sample tube 2 on the sample tray 3;
the sample recovery tube 1 and the sample tube 2 comprise a tube body 2a, an upper end cover 2c, a lower end cover 2d and a plastic sealing gasket 2b, wherein both ends of the tube body 2a are sealed by the plastic sealing gasket 2b, and the upper end cover 2c and the lower end cover 2d are used for partially mounting the tube body 2a on the sample tray 3;
it should be noted that, the plastic sealing gasket 2b is disposed at the upper and lower ends of the tube body 2a, the lower end cap 2d is mounted on the sample tray 3, the tube body 2a is inserted into the lower end cap 2d, and then the upper end cap 2c is sealed to assemble the sample tube 2 and the sample recovery tube 1 to the sample tray 3.
The loading and unloading assembly 16 comprises an end cover dismounting unit 166 and a loading piece, the loading piece is arranged on the bottom side of the end cover dismounting unit 166, the end cover dismounting unit 166 comprises a connecting seat 1661, a shaft seat 1662, a connecting rod 1663 and a transmission shaft 1664, the transmission shaft 1664 is vertically arranged on the outer wall of one end of the connecting seat 1661, the shaft seat 1662 is sleeved on the shaft end of the transmission shaft 1664, the rod end of the connecting rod 1663 is provided with a passive groove 16631, the bottom end of the connecting seat 1661 is provided with a connecting piece, the connecting piece is used for connecting the shaft seat 1662 with the rod end of the connecting rod 1663, the shaft seat 1664 drives the connecting seat 1661 to reciprocate along the vertical direction, the connecting rod 1663 is driven by the connecting piece, the connecting rod 1663 is driven by the passive groove 16631 to do compound motion along the rod direction movement and radial rotation, the dismounting piece drives the upper end cover 2c to rotate and detach from the sample plate 3, the tube 2a of the sample tube 2 and the tube 2a of the sample recycling tube 1 are replaced by the loading piece, and then the sample tube 2a is replaced by the tube 2c after the upper end cover 2c is rotatably assembled to the tube 2a.
The material loading piece includes clamp material area 163, material loading roller 165, driving roller and support, material loading roller 165, driving roller and transmission shaft 1664 are installed in the support, and the triangle structure is constituteed to material loading roller 165, driving roller and transmission shaft 1664, the outside at material loading roller 165, driving roller and transmission shaft 1664 is established to clamp material area 163 cover, clamp material area 163 passes through driving roller and transmission shaft 1664 and drives the transmission of material loading roller 165, be equipped with the pipe clamping groove on the clamp material area 163, the pipe clamping groove is omega type structure, clamp material area 163 passes through the perpendicular centre gripping body 2a of pipe clamping groove.
The loading and unloading assembly 16 further comprises a loading top seat 162 and a driving member 161, wherein the driving member 161 is used for driving the loading top seat 162 to make an L-shaped moving track, and a clamping member is arranged at the end part of the loading top seat 162.
The position of the bracket, which is close to the blanking top seat 162, is provided with a material injection port 164, and the sample transmission line 17 is communicated to the material injection port 164;
wherein the two sides of the feeding roller 165 are respectively provided with a first protrusion 1651 and a second protrusion 1652, the protrusion height of the first protrusion 1651 is higher than that of the second protrusion 1652, namely, when feeding, the clamping belt 163 is jacked up by the first protrusion 1651 and the second protrusion 1652, the clamping groove of the clamping belt 163 is deformed, the tube body 2a is released, the tube body 2a is arranged on the lower end cover 2d, and the assembly of the sample tube 2 positioned at the outer side and the tube body 2a of the sample recovery tube 1 positioned at the inner side is realized by the inconsistent protrusion heights of the first protrusion 1651 and the second protrusion 1652.
As shown in fig. 10, the shaft seat 1662 includes a lifting portion 16621 and a driving tooth portion 16622, the lifting portion 16621 is disposed on an outer edge of an upper end of the driving tooth portion 16622, the lifting portion 16621 is in an annular wavy structure, the lifting portion 16621 drives a portion of the entire shaft seat 1662 to lift up and down, so as to implement an upward pulling action of the upper end cap 2c, and simultaneously cooperates with a passive groove 16631 on the rod body 16332 to move, wherein a groove shape of the passive groove 16631 is shown in fig. 9, the passive groove 16631 is composed of a linear portion and a rotating portion, the linear portion and the rotating portion are disposed at intervals, and the linear portion and the rotating portion are communicated end to end, i.e. when passing through the linear portion, the rod is reciprocally moved, and when passing through the rotating portion, the rod is reciprocally moved, the upper end cap 2c is reciprocally pulled out and is pivotally mounted on the pipe body 2a through the passive groove 16631 in a combined two movement forms, and the driving tooth portion 16622 is used for connecting a connecting piece, including but not limited to a gear set, and a gear of the connecting rod 1663 is provided with a boss, and the boss is disposed in the passive groove 16631.
The feeding and discharging operation of the pipe body 2a is performed by utilizing the feeding and discharging assembly 16 in combination with a thermal desorption instrument, and the specific operation flow is as follows:
the end part of the transmission shaft 1664 is provided with an independent power source, the independent power source drives the feeding roller 165 and the transmission roller to rotate, meanwhile, the clamping belt 163 is transmitted between the feeding roller 165 and the transmission roller, the clamping belt 163 is provided with a pipe body 2a, the pipe body 2a enters a sample through a sample transmission line 17, then a plastic package gasket 2b is sealed, and then the clamping belt enters the positions of the sample pipe 2 and the sample recovery pipe 1;
simultaneously, the transmission shaft 1664 rotates to drive the shaft seat 1662 to rotate, meanwhile, the lifting part 16621 on the shaft seat 1662 drives the whole connecting seat 1661 to move up and down, meanwhile, the transmission tooth part 16622 at the bottom side of the shaft seat 1662 is in abutting connection with the passive groove 16631 of the rod body 16332 through a connecting piece, the rod moves back and forth through the relative motion between the passive groove 16631 and the connecting piece when passing through the straight line part, the rod moves rotationally and reciprocally when passing through the rotating part, the upper end cover 2c is repeatedly pulled out and turned over by combining two motion forms through the passive groove 16631, the upper end cover 2c is mounted on the pipe body 2a in a reciprocating manner, so that an upper end cover 2c is inserted through a disassembly piece, then the upper end of the turnover pull-out pipe body 2a is supported, at this moment, the pipe body 2a is blown back and cleaned, then the pipe body 2a is replaced, the disassembly piece is driven by the passive groove 16631 to move reversely after replacement, the upper end cover 2c is turned over and then pressed into the upper end of the new pipe body 2a, and the pipe body is withdrawn by switching station in cooperation with the station, and the continuous disassembly and assembly of the pipe body 2a can be realized;
after the positions of the sample tube 2 and the sample recovery tube 1 are switched at multiple stations, the sample tube 2 and the sample recovery tube 1 do not need to be assembled, disassembled and replaced in a concentrated mode after the analysis of the sample, the sample input and the assembly marking processes are long, the synchronous obtaining of the results of analysis and detection of multiple groups of samples is not facilitated, and the follow-up sample analysis results have deviation.
The embodiment has been described above with reference to the embodiment, but the embodiment is not limited to the above-described specific implementation, which is only illustrative and not restrictive, and many forms can be made by those of ordinary skill in the art, given the benefit of this disclosure, are within the scope of this embodiment.

Claims (10)

1. The utility model provides a full-automatic multistation retrieves function thermal desorption appearance, a serial communication port, including sample dish (3), sample recovery pipe (1), sample pipe (2), remove module (15), low temperature focus cold trap (8), analyze way mass flow controller (9), before the well reposition of redundant personnel recovery way mass flow controller (10), advance the reposition of redundant personnel recovery way mass flow controller (11), six-way valve (7), go up needle module (6) and lower needle module (14), sample pipe (2) intussuseption is filled with the sample, sample recovery pipe (1), sample pipe (2) all are the annular and distribute on sample dish (3), and sample recovery pipe (1), sample pipe (2) all perpendicular to sample dish (3) quotation setting, go up needle module (6) and lower needle module (14) are located sample recovery pipe (1), on the both ends of sample pipe (2), and go up needle module (6) and lower needle module (14) can move in opposite directions or relatively, insert when needle end of needle module (2) and lower needle module (14) move in opposite directions, sample pipe (1) and sample pipe (15) are equipped with the end of moving between (15) and are located in sample pipe (2) and are retrieved to sample pipe (15), the moving module (15) drives the heating block (13) to move to one side of the sample tube (2), the six-way valve (7) is respectively connected with the analysis path mass flow controller (9), the pre-trap split-flow recovery path mass flow controller (10) and the sample split-flow recovery path mass flow controller (11) through air pipes, the connecting end of the analysis path mass flow controller (9) is connected with carrier gas and the sample tube (2), the connecting end of the pre-trap split-flow recovery path mass flow controller (10) is connected with the sample recovery tube (1) and the low-temperature focusing cold trap (8), and the connecting end of the sample split-flow recovery path mass flow controller (11) is connected with the sample recovery tube (1) and an analytical instrument;
the moving module (15) drives the heating block (13) to abut against the outer wall of the sample tube (2) to heat, the analysis path mass flow controller (9) controls the carrier gas to sweep and split the sample which is heated and separated out in the sample tube (2), the sample is split into the pre-trap split recovery path mass flow controller (10), the sample is quantitatively split into the sample recovery tube (1), the split sample enters the low-temperature focusing cold trap (8), the sample is enriched in the low-temperature focusing cold trap (8), the six-way valve (7) is used for switching the bypass, the sample enriched in the low-temperature focusing cold trap (8) is switched to the sample injection path, the low-temperature focusing cold trap (8) is heated to enable the enriched sample to escape, the sample split recovery path mass flow controller (11) splits the escaped sample, the sample is quantitatively split into the sample recovery tube (1), the split sample enters the analysis instrument, the six-way valve (7) is switched from the bypass to the initial state, the carrier gas is introduced to reversely blow and clean the sample recovery tube (1), the low-temperature focusing cold trap (8) is switched to the initial state, and the sample recovery tube (3) is cooled down, and the sample is cooled down on the sample recovery tube (2).
2. The full-automatic multi-station recovery functional thermal desorption instrument according to claim 1 is characterized by further comprising an upper and lower material assembly (16), wherein the upper and lower material assembly (16) is arranged on one side of the movable module (15), and the upper and lower material assembly (16) is used for replacing the sample tube (2) and the sample recovery tube (1) after switching stations of the sample recovery tube (1) and the sample tube (2) on the sample tray (3);
the sample recovery tube (1) and the sample tube (2) comprise a tube body (2 a), an upper end cover (2 c), a lower end cover (2 d) and a plastic sealing gasket (2 b), wherein both ends of the tube body (2 a) are sealed through the plastic sealing gasket (2 b), and the upper end cover (2 c) and the lower end cover (2 d) are used for partially mounting the tube body (2 a) on the sample disc (3);
the upper and lower material subassembly (16) include end cover dismouting unit (166) and material loading spare, the bottom side of end cover dismouting unit (166) is located to the material loading spare, and end cover dismouting unit (166) are including connecting seat (1661), axle bed (1662), connecting rod (1663) and transmission shaft (1664), transmission shaft (1664) are installed perpendicularly on the one end outer wall of connecting seat (1661), the axle bed (1662) cover is located the axle head of transmission shaft (1664), and the rod end of connecting rod (1663) is equipped with passive groove (16631), the connecting piece is installed to the bottom of connecting seat (1661), the connecting piece is used for axle bed (1662) to be connected with the rod end of connecting rod (1663), transmission shaft (1664) drives axle bed (1662) and rotates, axle bed (1661) along plumb reciprocating movement, connecting rod (1663) are connected with the dismouting piece through the connecting rod, connecting rod (1663) are driven by passive groove (16631) and are along the pole to move and are rotated compound motion along the pole, install and remove sample pipe (2) from the sample pipe (2) and then install and remove sample pipe (2) from the sample pipe (2) and then install end cover (2) and remove sample pipe (2) from the sample pipe (2) The tube body (2 a) of the sample recovery tube (1) is replaced.
3. The full-automatic multi-station recovery function thermal desorption instrument according to claim 1 is characterized in that a purge path pressure stabilizing valve (27) is connected between the analysis path mass flow controller (9) and carrier gas, the purge path pressure stabilizing valve (27) is respectively connected with a back purge valve (24), an analysis path electromagnetic valve (28) and a standard sample preparing electromagnetic valve (31) through pipelines, the analysis path electromagnetic valve (28) is connected with the analysis path mass flow controller (9), the analysis path mass flow controller (9) is connected to a lower needle inserting module (14) through an electronic pressure sensor (32), and the lower needle inserting module (14) connected with the electronic pressure sensor (32) is a lower needle inserting module connected with a sample tube (2).
4. A fully automatic multi-station recovery function thermal desorption apparatus according to claim 3, wherein the upper needle insertion connected to the sample tube (2) in the upper needle insertion module (6) is divided into two pipelines, one of which is connected to the six-way valve (7) and the other of which is connected to the pre-trap split-flow mass flow controller (33).
5. The full-automatic multi-station recovery function thermal desorption instrument according to claim 4, wherein one end of a pre-trap shunt mass flow controller (33) far away from a six-way valve (7) is connected with a first tee, one end of the first tee is connected with an upper needle of an upper needle insertion module (6) connected with a sample recovery tube (1), the other end of the first tee is connected with a shunt flow controller (35), and one end of the sample recovery tube (1) far away from the tee is connected to a recovery vent through one end of a lower needle insertion module (14) connected with the sample recovery tube (1).
6. The full-automatic multi-station recovery function thermal desorption instrument according to claim 5, wherein one end of a standard sample preparation electromagnetic valve (31) far away from a purge path pressure stabilizing valve (27) is connected with a needle valve (30), and the other end of the needle valve (30) is connected to a calibration interface.
7. The full-automatic multi-station recovery function thermal desorption instrument according to claim 6, wherein one end of the back blowing valve (24) far away from the blowing-sweeping-path pressure stabilizing valve (27) is connected with a second tee joint, one port of the second tee joint is connected with the emptying valve (25), and the other port of the second tee joint is connected with the six-way valve (7).
8. The full-automatic multi-station recovery function thermal desorption instrument according to claim 7 is characterized in that a enrichment pipe (22) is arranged in the low-temperature focusing cold trap (8), one end of the enrichment pipe (22) is connected with the six-way valve (7), and the other end of the enrichment pipe (22) is connected with the other interface of the six-way valve (7).
9. The full-automatic multi-station recovery function thermal desorption instrument according to claim 8, wherein a carrier gas path mass flow controller (23) is connected with a carrier gas path pressure stabilizing valve (26), the other end of the carrier gas path mass flow controller (23) is connected with one of interfaces of a six-way valve (7), the interface of the six-way valve (7) is connected with a third tee joint, one end of the third tee joint is connected with a column temperature box, the other end of the third tee joint is connected with a split flow electromagnetic valve (36), and the other end of the split flow electromagnetic valve (36) is connected with a split flow controller (35).
10. The full-automatic multi-station recovery function thermal desorption instrument according to claim 2, wherein the feeding part comprises a clamping belt (163), a feeding roller (165), a driving roller and a support, the feeding roller (165), the driving roller and a driving shaft (1664) are arranged in the support, the feeding roller (165), the driving roller and the driving shaft (1664) form a triangular structure, the clamping belt (163) is sleeved on the outer sides of the feeding roller (165), the driving roller and the driving shaft (1664), the clamping belt (163) drives the feeding roller (165) to drive through the driving roller and the driving shaft (1664), a pipe clamping groove is formed in the clamping belt (163), and the pipe clamping groove is of an omega-shaped structure.
CN202310209075.XA 2023-03-07 2023-03-07 Full-automatic multi-station recovery function thermal desorption instrument Active CN115980378B (en)

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