CN115980378A - Full-automatic multi-station recovery function thermal desorption instrument - Google Patents
Full-automatic multi-station recovery function thermal desorption instrument Download PDFInfo
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- CN115980378A CN115980378A CN202310209075.XA CN202310209075A CN115980378A CN 115980378 A CN115980378 A CN 115980378A CN 202310209075 A CN202310209075 A CN 202310209075A CN 115980378 A CN115980378 A CN 115980378A
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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 moving module, a low-temperature focusing cold trap, an analytical path mass flow controller, a pre-trap shunt recovery path mass flow controller, a sample injection shunt recovery path mass flow controller, a six-way valve, an upper needle inserting module and a lower needle inserting 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 of the invention adopts the combination of the double-electric-control six-way valve and the electromagnetic valve, can automatically complete four processes of primary analysis, secondary low-temperature enrichment, secondary analysis, sample introduction and back flushing of the single (double) circuit multi-branch adsorption tube by programming, the primary analysis temperature, the secondary analysis temperature, the cold trap temperature and the pipeline heating temperature can be independently set, and the processes of sample analysis and the like can be better controlled according to the set split ratio.
Description
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
At present, in the aspect of domestic occupational health, gas which is high in concentration and harmful to human bodies can be analyzed frequently, because the concentration of the sample is high and harmful to the human bodies, the accuracy of an experimental result can be guaranteed when the sample is analyzed by equipment, the gas cannot be discharged into the air, the trapping capacity of a thermal desorption instrument on the market to the sample is limited, and the recovery of all the samples cannot be guaranteed even if the thermal desorption instrument has a recovery function.
The existing thermal desorption instrument can not meet the requirement of analyzing a high-concentration sample by a client, the accuracy of experimental data can not be guaranteed, the sample is not shunted and recovered, the toxic sample can not be prevented from being discharged into the air to pollute the air in a laboratory, and the sample leakage influence is caused to influence the physical health of a tester.
Disclosure of Invention
The invention provides a full-automatic multi-station recovery function thermal desorption instrument, which solves the technical problems that in the related technology, a sample cannot be subjected to shunt recovery, and toxic samples are prevented from being discharged into the air to pollute the air in a laboratory.
The thermal desorption instrument comprises a sample tray, a sample recovery tube, a sample tube, a moving module, a low-temperature focusing cold trap, an analysis path mass flow controller, a trap front shunt recovery path mass flow controller, a sample injection shunt recovery path mass flow controller, a six-way valve, an upper needle module and a lower needle module, wherein samples are filled in the sample tube;
the mobile module drives the heating block to abut against the outer wall of the sample tube to abut against the sample tube for heating, the mass flow controller of the analysis path controls carrier gas to blow and shunt a sample analyzed by heating in the sample tube, the sample is shunted into the mass flow controller of the shunt recovery path before the well, then the sample is quantitatively shunted into the sample recovery tube, the shunted sample enters the low-temperature focusing cold well, when the sample is enriched in the low-temperature focusing cold well, the six-way valve switches a bypass, the sample enriched in the low-temperature focusing cold well is switched to the sample injection path, the low-temperature focusing cold well is heated to enable the enriched sample to escape, the mass flow controller of the sample shunt recovery path shunts the escaped sample, then the sample is quantitatively shunted into the sample recovery tube, the shunted sample enters the analysis instrument, the six-way valve is switched to an initial state from the bypass, the carrier gas is introduced to perform back flushing cleaning on the sample tube and the sample recovery tube, the low-temperature focusing cold well is cooled and switched to the initial state, and stations of the sample recovery tube and the sample tube on the sample tray are switched.
Further: the sample tray is provided with a moving module, a loading and unloading module and a loading and unloading module, wherein the loading and unloading module is arranged on one side of the moving module and used for replacing the sample tubes and the sample recovery tubes after the sample recovery tubes and the sample tubes on the sample tray are switched;
the sample recovery tube and the sample tube respectively comprise a tube body, an upper end cover, a lower end cover and a plastic package gasket, two ends of the tube body are sealed through the plastic package gasket, and the upper end cover and the lower end cover are used for partially installing the tube body on the sample disc;
go up the unloading subassembly and include end cover dismouting unit and material loading spare, the bottom side of end cover dismouting unit is located to the material loading spare, and end cover dismouting unit includes the connecting seat, the axle bed, connecting rod and transmission shaft, the transmission shaft is installed perpendicularly on the one end outer wall of connecting seat, the axle head of transmission shaft is located to the axle bed cover, and the rod end of connecting rod is equipped with passive groove, the connecting piece is installed to the bottom of connecting seat, the connecting piece is used for the rod end of axle bed and connecting rod to be connected, the transmission shaft drives the axle bed and rotates, the axle bed drives the connecting seat along the vertical reciprocating motion, the connecting rod passes through the connecting piece transmission, the rod end of connecting rod is connected with the dismouting piece, the connecting rod drives the connecting rod through passive groove and is along the pole to removal and radial pivoted compound motion, the dismouting piece drives the upper end cover and rotates from the sample tray and tears down, utilize the material loading spare to replace the body of sample cell and sample recovery tube, then with upper end cover spin assembly to the tube after replacing on the tube end, realize the sample cell, the body of sample cell is replaced.
Further: a purging path pressure stabilizing valve is connected between the analysis path mass flow controller and the carrier gas, the purging path pressure stabilizing valve is respectively connected with a back flushing valve, an analysis path electromagnetic valve and a standard sample making electromagnetic valve through pipelines, 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: an upper needle connected to the sample tube in the upper needle module is divided into two pipelines, wherein one pipeline is connected to the six-way valve, and the other pipeline is connected to the mass flow controller of the pre-trap shunt circuit.
Further, the method comprises the following steps: the one end that reposition of redundant personnel way mass flow controller kept away from the six-way valve before the well is connected with first tee bend, and wherein one end of first tee bend is connected to the last acupuncture needle that is connected to sample recovery tube in the last acupuncture needle module, and on the other end of first tee bend was connected with reposition of redundant personnel flow controller, sample recovery tube kept away from the one end of tee bend and was connected to retrieving the drain through the one end of connecting sample recovery tube in the lower acupuncture needle module.
Further: one end of the standard sample making electromagnetic valve, which is far away from the pressure stabilizing valve of the blowing road, is connected with a needle valve, and the other end of the needle valve is connected to the calibration interface.
Further, the method comprises the following steps: one end of the blowback valve, which is far away from the pressure stabilizing valve of the blowing and sweeping circuit, is connected with a second tee joint, one port of the second tee joint is connected with the air release valve, and the other port of the second tee joint is connected with the six-way valve.
Further: an enrichment pipe is arranged in the low-temperature focusing cold trap, 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 connector of the six-way valve.
Further: the carrier gas path mass flow controller is connected with the load gas path pressure stabilizing valve, the other end of the carrier gas path mass flow controller is connected with one interface of the six-way valve, the interface of the six-way valve is connected with a third tee, one end interface of the third tee is connected to the column temperature box, the other end interface of the third tee is connected with the shunt electromagnetic valve, and the other end of the shunt electromagnetic valve is connected with the shunt flow controller.
Further: the material loading spare is including pressing from both sides material area, material loading roller, driving roller and support, and material loading roller, driving roller and transmission shaft are installed in the support, and material loading roller, driving roller and transmission shaft constitution triangle-shaped structure, and the cover of material clamping belt is established in the outside of material loading roller, driving roller and transmission shaft, and the material clamping belt passes through driving roller and transmission shaft and drives the material loading roller transmission, is equipped with the tube clamping groove on the material clamping belt, and the tube clamping groove is omega type structure.
Further, the method comprises the following steps: 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 axle bed includes lift portion and drive tooth portion, and lift portion distributes on drive tooth portion's upper end outer fringe, and lift portion is annular wavy structure.
Further, the method comprises the following steps: go up unloading subassembly still includes unloading footstock and driving piece, and the driving piece is used for driving the unloading footstock and is L type moving trajectory, and the tip of unloading footstock is equipped with the holder.
The invention has the beneficial effects that:
this thermal adsorption appearance is equipped with double-circle sample cell and sample recovery tube, the gas circuit adopts two electric control six-way valve and solenoid valve to combine together simultaneously, can programme automatic completion single (two) way once of many adsorption tubes analytic, secondary low temperature enrichment, the secondary is analytic, advance appearance and four processes of blowback, once analytic temperature, the analytic temperature of secondary, cold trap temperature and pipeline heating temperature can independently set up, according to the split flow ratio that sets up, better with process control such as sample analytic, both satisfy the demand of customer analysis high concentration sample, guarantee the accuracy of experimental data, again can shunt the recovery to the sample, prevent that poisonous sample from discharging and polluting the laboratory air in the air.
Drawings
Fig. 1 is a schematic structural diagram of a full-automatic multi-station recovery function thermal desorption instrument provided by the invention;
fig. 2 is a schematic diagram of an internal structure of a full-automatic multi-station recovery function thermal desorption instrument provided by the invention;
fig. 3 is a side view of a connection structure of a moving module of a full-automatic multi-station recovery function thermal desorption instrument according to the present invention;
FIG. 4 is a top view of FIG. 3;
FIG. 5 is a schematic diagram of a gas path of a full-automatic multi-station recovery function thermal desorption instrument according to the present invention;
fig. 6 is a schematic structural view of a feeding and discharging assembly of the full-automatic multi-station recovery function thermal desorption instrument provided by the invention;
fig. 7 is a schematic structural view of a sample tube and a sample recovery tube of the full-automatic multi-station recovery functional thermal desorption instrument provided by the invention;
FIG. 8 is a top view of the loading roller of FIG. 6;
FIG. 9 is a schematic view 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 pipe body; 2b, plastic packaging a gasket; 2c, an upper end cover; 2d, a lower end cover; 3. a sample tray; 4. recovering the road needle; 5. analyzing the way sampling needle; 6. an upper needle inserting module; 7. a six-way valve; 8. low-temperature focusing cold trap; 9. a resolution path mass flow controller; 10. a shunt recovery path mass flow controller in front of the trap; 11. a sample introduction shunting recovery path mass flow controller; 12. an electromagnetic valve group; 13. a heating block; 14. a lower needle inserting module; 15. a moving module; 16. a feeding and discharging assembly; 161. a drive member; 162. a blanking top seat; 163. clamping the material 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 part; 1663. a connecting rod; 16631. a passive tank; 16332. a rod body; 1664. a drive shaft; 17. a sample transfer line; 18. a power switch; 19. a housing; 20. a pressure gauge; 21. a pressure stabilizing valve bank; 22. an enrichment pipe; 23. a carrier gas line mass flow controller; 24. a blowback valve; 25. an atmospheric valve; 26. a carrier gas path pressure stabilizing valve; 27. a purge circuit pressure maintaining valve; 28. a resolution path electromagnetic valve; 29. a touch screen; 30. a needle valve; 31. manufacturing a standard sample electromagnetic valve; 32. an electronic pressure sensor; 33. a pre-trap shunt path mass flow controller; 34. a shunt recovery electromagnetic valve in front of the trap; 35. a shunt flow controller; 36. a shunt solenoid valve.
Detailed Description
The subject matter described herein will now be discussed with reference to example embodiments. It is to be understood that such embodiments are discussed merely to enable others skilled in the art to better understand and thereby 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. Various examples may omit, substitute, or add various procedures or components as needed. In addition, features described with respect to some examples may also be combined in other examples.
Example one
Referring to fig. 1-10, a fully automatic multi-station recovery function 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, a desorption path mass flow controller 9, a trap front shunting recovery path mass flow controller 10, a sample introduction shunting recovery path mass flow controller 11, a six-way valve 7, an upper needle insertion module 6 and a lower needle insertion module 14, wherein a sample is filled in the sample tube 2, the sample recovery tube 1 and the sample tube 2 are both annularly distributed on the sample tray 3, the sample recovery tube 1 and the sample tube 2 are both arranged perpendicular to the disk surface of the sample tray 3, the upper needle insertion module 6 and the lower needle insertion module 14 are respectively arranged at two ends of the sample recovery tube 1 and the sample tube 2, and the upper needle insertion module 6 and the lower needle insertion module 14 can move towards or relatively, when the needle ends of the upper needle inserting module 6 and the lower needle inserting module 14 move oppositely, the upper needle inserting module is inserted into the sample tube 2 and the sample recovery tube 1 and communicated with the sample tube 2 and the sample recovery tube 1, 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 shunt recovery path mass flow controller 10 and the sample injection shunt recovery path mass flow controller 11 through air pipes, the connecting end of the analysis path mass flow controller 9 is connected with the carrier gas and the sample tube 2, the connecting end of the pre-trap shunt 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 shunt recovery path mass flow controller 11 is connected with the sample recovery tube 1 and the analyzer;
as shown in fig. 1 to 4, the general working flow of the thermal desorption apparatus is as follows:
the sample position on the sample tray 3 is composed of an inner ring and an outer ring, the outer ring is a sample tube 2 position, the inner ring is a shunt recovery tube position, when the sample tube 2 is analyzed, the heating block 13 moves forwards to wrap the sample tube 2 on the outer ring of the sample tray 3, at the moment, nitrogen with the mass flow control passes through the sample tube 2, a sample to be analyzed which is analyzed at a high temperature is blown away from the sample tube 2, a gaseous sample which leaves the sample tube 2 is shunted before entering the low-temperature focusing cold trap 8, and according to the set shunt ratio, one 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; after the sample in the sample tube 2 is analyzed, the sample enriched in the low-temperature focusing cold trap 8 is heated, and meanwhile, the six-way sample injection valve is switched, the sample is brought into a chromatograph by carrier gas for analysis, split flow treatment is carried out before the sample enters the chromatograph, the split flow sample is also recycled into the sample recycling tube 1 of the inner ring through a transmission pipeline, and after sample injection is finished, nitrogen can carry out back flushing cleaning on the low-temperature focusing cold trap 8; after the cleaning is finished, the sample plate 3 is transferred to the next station, and the analysis process of the next sample is automatically carried out until all samples are analyzed.
Specifically, after a sample recovery tube 1 and a sample tube 2 placed on a sample tray 3 are turned to specific positions, an upper needle inserting module 6 and a lower needle inserting module 14 respectively move downwards and upwards to further drive a recovery path needle 4 and a resolution path sampling needle 5 to respectively insert the sample recovery tube 1 and the sample tube 2, a moving module 15 drives a heating block 13 to abut against the outer wall of the sample tube 2 to be heated, a resolution path mass flow controller 9 controls nitrogen/helium to purge and split a sample which is heated and resolved in the sample tube 2, the sample is split into a pre-trap split recovery path mass flow controller 10 and then quantitatively split the sample into the sample recovery tube 1, the split sample enters a low-temperature focusing cold trap 8, when the sample is enriched in the low-temperature focusing cold trap 8, a six-way valve 7 switches a bypass, the sample which is enriched in the low-temperature focusing cold trap 8 is heated to enable the enriched sample to escape, a mass flow controller 11 splits the escaped sample into the sample recovery tube 1 and then quantitatively splits the sample into the sample recovery tube 1, the split sample enters a sample injection path 7 after being split, the sample is switched into an analysis bypass, the sample recovery tube 2, the sample is switched from an initial sample cleaning station and a back-flushing station, and back-flushing device, and the sample cleaning device 2.
It should be added that, the air path is further 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 making electromagnetic valve 31, a pre-trap shunt recovery electromagnetic valve 34, and a shunt electromagnetic valve 36.
It should be added that, the moving module of the heating block 13 includes but is not limited to a cylinder and other linear pushing members, which drive the heating block 13 at the end to heat the tube body 2a, a heating element is disposed in the heating block 13, the heating element includes but is not limited to a heating wire, a temperature controller and other components, and the heating element is mainly used for heating the tube body 2a, so that the sample inside can be analyzed and escaped.
It should be added that, a casing 19 is arranged outside the instrument of the thermal desorption instrument, the sample tray 3 is arranged on 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 on 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 loading and unloading assembly 16;
wherein the surge tank valve group 21 includes, but is not limited to, a purge circuit surge valve 27 and a carrier circuit surge 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 starting and stopping electric components in the equipment.
The complete gas circuit involved in the thermal desorption instrument is shown in fig. 5:
a purging path pressure stabilizing valve 27 is connected between the analysis path mass flow controller 9 and the carrier gas, the purging path pressure stabilizing valve 27 is respectively connected with the back flushing valve 24, the analysis path electromagnetic valve 28 and the standard sample making 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 the lower needle punching module 14 through an electronic pressure sensor 32, and the lower needle punching module 14 connected with the electronic pressure sensor 32 is a lower needle punching connected with the sample tube 2; an upper needle connected to the sample tube 2 in the upper needle module 6 is divided into two pipelines, wherein one pipeline is connected to a third interface of the six-way valve 7, and the other pipeline is connected to a mass flow controller 33 of the pre-trap shunt circuit; one end of the mass flow controller 33 of the trap front shunt path, which is far away from the six-way valve 7, is connected with a first tee joint, one end of the first tee joint is connected with an upper puncture needle connected to the sample recovery tube 1 in the upper puncture needle module 6, the other end of the first tee joint is connected with a shunt flow controller 35, and one end of the sample recovery tube 1, which is far away from the tee joint, is connected to a recovery vent through one end of the lower puncture needle module 14, which is connected with the sample recovery tube 1;
one end of the standard sample making electromagnetic valve 31, which is far away from the purging channel pressure stabilizing valve 27, is connected with a needle valve 30, and the other end of the needle valve 30 is connected with a calibration interface; one end of the blowback valve 24, which is far away from the pressure stabilizing valve 27 of the purging circuit, is connected with a second tee joint, one port of the second tee joint is connected with the blow-down valve 25, and the other port of the second tee joint is connected with the interface four of the six-way valve 7; an enrichment pipe 22 is arranged in the low-temperature focusing cold trap 8, one end of the enrichment pipe 22 is connected with a second connector of the six-way valve 7, and the other end of the enrichment pipe 22 is connected with a fifth connector of the six-way valve 7.
The carrier gas path mass flow controller 23 is connected with the load gas path pressure stabilizing valve 26, the other end of the carrier gas path mass flow controller 23 is connected with a six-way valve 7 interface, the six-way valve 7 interface is connected with a third tee, one end interface of the third tee is connected with the column temperature box, the other end interface of the third tee is connected with a shunt electromagnetic valve 36, and the other end of the shunt electromagnetic valve 36 is connected with a shunt flow controller 35.
Example two
Referring to fig. 2, 6-10, the thermal desorption apparatus further includes a loading and unloading assembly 16, the loading and unloading assembly 16 is disposed on one side of the moving module 15, and the loading and unloading assembly 16 is used for replacing 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 both comprise a tube body 2a, an upper end cover 2c, a lower end cover 2d and a plastic package gasket 2b, two ends of the tube body 2a are sealed by the plastic package gasket 2b, and the upper end cover 2c and the lower end cover 2d are used for partially installing the tube body 2a on the sample tray 3;
it should be added that the plastic package gasket 2b is arranged at the upper end and the lower end of the tube body 2a, the lower end cover 2d is arranged on the sample tray 3, the tube body 2a is inserted into the lower end cover 2d, then the upper end cover 2c is packaged, and the sample tube 2 and the sample recovery tube 1 are assembled on the sample tray 3.
The feeding and discharging assembly 16 comprises an end cover dismounting unit 166 and a feeding piece, the feeding 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 installed 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 connecting part is installed at the bottom end of the connecting seat 1661 and used for connecting the shaft seat 1662 with the rod end of the connecting rod 1663, the transmission shaft 1664 drives the shaft seat 1662 to rotate, the shaft seat 1662 drives the connecting seat 1661 to reciprocate along the vertical direction, the connecting rod 1663 is driven by the connecting part, the rod 1663 is connected with a dismounting piece, the connecting rod 1663 drives the connecting rod 1663 to do a combined motion of rod axial movement and radial rotation along the rod 1663 through the passive groove 16631, the upper end cover 1662 c drives the upper end cover 1663 to rotate and dismount and rotate from the sample disk 3, the sample disk 2a, the tube body of the upper end cover 2c is then, the sample tube is rotatably assembled to replace the sample tube body of the sample recovery tube 2a, and the sample tube is replaced by the sample tube 2a.
The material loading part comprises a material clamping belt 163, a material loading roller 165, a transmission roller and a support, the material loading roller 165, the transmission roller and a transmission shaft 1664 are installed in the support, a triangular structure is formed by the material loading roller 165, the transmission roller and the transmission shaft 1664, the material clamping belt 163 is sleeved on the outer side of the material loading roller 165, the transmission roller and the transmission shaft 1664, the material clamping belt 163 drives the material loading roller 165 to transmit through the transmission roller and the transmission shaft 1664, a pipe clamping groove is formed in the material clamping belt 163 and is of an omega-shaped structure, and the material clamping belt 163 vertically clamps the pipe body 2a through the pipe clamping groove.
The feeding and discharging assembly 16 further comprises a feeding top seat 162 and a driving part 161, the driving part 161 is used for driving the feeding top seat 162 to move in an L-shaped track, and a clamping part is arranged at the end of the feeding top seat 162.
A feeding port 164 is formed in the position, close to the blanking top seat 162, of the support, and the sample transmission line 17 is communicated to the feeding port 164;
first convex portion 1651 and second convex portion 1652 are respectively arranged on two sides of feeding roller 165, the protruding height of first convex portion 1651 is higher than the protruding height of second convex portion 1652, namely when feeding is carried out, material clamping belt 163 is jacked up through first convex portion 1651 and second convex portion 1652, an entrainment groove of material clamping belt 163 is deformed, tube body 2a is released and arranged on lower end cover 2d, and assembling of sample tube 2 located on the outer side and tube body 2a of sample recovery tube 1 located on the inner side is achieved through inconsistency of the protruding heights of first convex portion 1651 and second convex portion 1652.
As shown in fig. 10, the shaft seat 1662 includes a lifting portion 16621 and a transmission tooth portion 16622, the lifting portion 16621 is distributed on an outer edge of an upper end of the transmission tooth portion 16622, the lifting portion 16621 is in an annular wavy structure, the lifting portion 16621 drives the whole shaft seat 1662 to lift up and down, so as to achieve an upward pulling motion of the upper end cover 2c, and simultaneously move in cooperation with a passive slot 16631 on the rod 16332, wherein the slot of the passive slot 16631 is as shown in fig. 9, the passive slot 16631 is composed of a linear portion and a rotary portion, the linear portion and the rotary portion are distributed at intervals, and are connected end to form a closed structure, i.e., the rod moves back and forth when passing through the linear portion, the rod rotates back and forth when passing through the rotary portion, the upper end cover 2c is installed to the tube body 2a in a reversed manner and overturned and pulled out and overturned by the passive slot 16631, the transmission tooth portion 22 is used to connect a connecting element, the connecting element includes, but is not limited to a gear set, and the gear of the connecting rod 1663 has a protruding pillar disposed in the passive slot 16631.
Utilize this last unloading subassembly 16 cooperation thermal desorption appearance to carry out the last unloading operation of body 2a, specific operation flow is as follows:
an independent power source is arranged at the end part of the transmission shaft 1664 and is driven by the independent power source to drive the feeding roller 165 and the transmission roller to rotate, meanwhile, the material clamping belt 163 is driven between the feeding roller 165 and the transmission roller, a pipe body 2a is arranged on the material clamping belt 163, the pipe body 2a enters a sample through the sample transmission line 17, then a plastic package gasket 2b is sealed, and then the sample enters the stations of the sample pipe 2 and the sample recovery pipe 1 along with the material clamping belt;
meanwhile, the transmission shaft 1664 rotates to drive the shaft seat 1662 to rotate, the shaft seat 1662 rotates, the lifting part 16621 on the shaft seat 1662 drives the whole connecting seat 1661 to move up and down, the transmission tooth part 16622 on the bottom side of the shaft seat 1662 abuts against and is connected with the driven groove 16631 of the rod body 16332 through the connecting piece, through the relative motion between the driven groove 16631 and the connecting piece, the rod moves back and forth when passing through the straight line part, the rod rotates to move back and forth when passing through the rotating part, the upper end cover 2c is overturned, pulled out and overturned and installed on the pipe body 2a in a reciprocating way through the driven groove 16631, the upper end cover 2c is inserted through the dismounting piece and then lifted up, the upper end of the overturned and pulled out pipe body 2a is cleaned by back flushing, then the pipe body 2a is replaced, the replaced driven groove 16631 drives the dismounting piece to move reversely, the upper end cover 2c is overturned and then pressed into the upper end of a new pipe body 2a to be dismounted, and matched with the switching of the upper station, and the pipe body 2a can be withdrawn continuously;
the positions of the sample tube 2 and the sample recovery tube 1 are switched at multiple stations, after a sample is analyzed, the sample tube 2 and the sample recovery tube 1 do not need to be assembled, disassembled and replaced in a centralized mode, sample input and assembly marking processes are long, results of analyzing and detecting multiple groups of samples cannot be obtained synchronously, and accordingly subsequent sample analysis results are deviated.
Although the embodiment of the present invention has been described above, the present embodiment is not limited to the above specific embodiments, and the above specific embodiments are only illustrative and not restrictive, and those skilled in the art can make many forms without departing from the spirit of the present embodiment.
Claims (10)
1. A full-automatic multi-station recovery function thermal desorption instrument is characterized by comprising a sample tray (3), sample recovery tubes (1), sample tubes (2), a moving module (15), a low-temperature focusing cold trap (8), a resolution path mass flow controller (9), a trap front shunting recovery path mass flow controller (10), a sample introduction shunting 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 tubes (2), the sample recovery tubes (1) and the sample tubes (2) are distributed on the sample tray (3) in an annular shape, the sample recovery tubes (1) and the sample tubes (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 the sample recovery tubes (1) and two ends of the sample tubes (2), the upper needle inserting module (6) and the lower needle inserting module (14) can move towards each other, the sample tubes (2) and the sample tubes (2) are arranged on two ends, the sample tubes (13) and the sample tubes (2) and the moving module (13) are arranged on one side of the sample tray (2) and the sample tubes (2), the six-way valve (7) is respectively connected with an analysis path mass flow controller (9), a pre-trap shunt recovery path mass flow controller (10) and a sample injection shunt recovery path mass flow controller (11) through air pipes, the connecting end of the analysis path mass flow controller (9) is connected with a carrier gas and a sample pipe (2), the connecting end of the pre-trap shunt recovery path mass flow controller (10) is connected with a sample recovery pipe (1) and a low-temperature focusing cold trap (8), and the connecting end of the sample injection shunt recovery path mass flow controller (11) is connected with the sample recovery pipe (1) and an analysis instrument;
the mobile module (15) drives the heating block (13) to abut against the outer wall of the sample tube (2) to abut against and heat, the analysis path mass flow controller (9) controls carrier gas to blow and shunt a sample analyzed by heating in the sample tube (2), the sample is shunted into the shunt recovery path mass flow controller (10) before the trap, then the sample is quantitatively shunted into the sample recovery tube (1), the shunted sample enters the low-temperature focusing cold trap (8), when the sample is enriched in the low-temperature focusing cold trap (8), the six-way valve (7) switches 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) heats the enriched sample to escape, the sample shunt recovery path mass flow controller (11) shunts the escaped sample, then the sample is quantitatively shunted into the sample recovery tube (1), the shunted sample enters an analysis instrument, the six-way valve (7) is switched to an initial state from the bypass, the carrier gas is introduced to clean the sample tube (2) and the sample recovery tube (1), the low-temperature focusing cold trap (8) is switched to an initial state, and the sample recovery tube (3) and a sample recovery station (2) are reversely blown.
2. The full-automatic multi-station recovery functional thermal desorption instrument according to claim 1, further comprising a feeding and discharging assembly (16), wherein the feeding and discharging assembly (16) is arranged on one side of the moving module (15), and the feeding and discharging assembly (16) is used for replacing the sample tubes (2) and the sample recovery tubes (1) after switching the positions of the sample recovery tubes (1) and the sample tubes (2) on the sample tray (3);
the sample recovery tube (1) and the sample tube (2) respectively comprise a tube body (2 a), an upper end cover (2 c), a lower end cover (2 d) and a plastic package gasket (2 b), two ends of the tube body (2 a) are sealed through the plastic package gasket (2 b), and the upper end cover (2 c) and the lower end cover (2 d) are used for partially installing the tube body (2 a) on the sample tray (3);
go up unloading subassembly (16) and 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 the rod end of axle bed (1662) and connecting rod (1663) to be connected, transmission shaft (1664) drive axle bed (1662) and rotate, axle bed (1662) drive connecting seat (1661) along vertical reciprocating motion, connecting rod (1663) pass through the connecting piece transmission, the rod end of connecting rod (1663) is connected with the dismouting piece, connecting rod (1663) drive connecting rod (1663) through passive groove (16631) and do along the pole to removal and radial pivoted combined motion, the dismouting piece drives upper end cover (2 c) and rotates from sample dish (3) and tears down, utilize the material loading spare to replace body (2 a) of sample tube (2) and sample recovery pipe (1), then with upper end cover (2 c) rotation assembly to after replacing on the pipe end of body (2 a), realize sample tube (2) and the pipe end of body (2 a), realize sample tube (2), the tube body (2 a) of the sample collection tube (1) is replaced.
3. The full-automatic multi-station recovery functional thermal desorption instrument according to claim 1, wherein a purge circuit pressure stabilizing valve (27) is connected between the purge circuit mass flow controller (9) and the carrier gas, the purge circuit pressure stabilizing valve (27) is respectively connected with the blowback valve (24), the purge circuit electromagnetic valve (28) and the standard sample making electromagnetic valve (31) through pipelines, the purge circuit electromagnetic valve (28) is connected with the purge circuit mass flow controller (9), the purge circuit mass flow controller (9) is connected to the lower needle punching module (14) through an electronic pressure sensor (32), and the lower needle punching module (14) connected with the electronic pressure sensor (32) is a lower needle punching connected with the sample tube (2).
4. The full-automatic multi-station recovery function thermal desorption instrument according to claim 3, wherein the upper needle connected to the sample tube (2) in the upper needle module (6) is divided into two pipelines, one of the pipelines is connected to the six-way valve (7), and the other pipeline is connected to the mass flow controller (33) of the pre-trap shunt circuit.
5. The full-automatic multi-station recovery functional thermal desorption instrument according to claim 4, wherein one end of the mass flow controller (33) of the pre-trap shunt path, which is far away from the six-way valve (7), is connected with a first tee joint, one end of the first tee joint is connected with an upper needle connected to the sample recovery tube (1) in the upper needle module (6), the other end of the first tee joint is connected with a shunt flow controller (35), and one end of the sample recovery tube (1), which is far away from the tee joint, is connected to the recovery vent through one end of the lower needle module (14), which is 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 the standard sample preparation solenoid valve (31) 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.
7. The full-automatic multi-station recovery function thermal desorption instrument according to claim 6, wherein one end of the blowback valve (24) far away from the purge circuit pressure maintaining valve (27) is connected with a second tee joint, one port of the second tee joint is connected with the vent 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, wherein a concentration pipe (22) is arranged in the low-temperature focusing cold trap (8), one end of the concentration pipe (22) is connected with the six-way valve (7), and the other end of the concentration pipe (22) is connected with the other connector of the six-way valve (7).
9. The full-automatic multi-station recovery function thermal desorption instrument according to claim 8, wherein the carrier gas path mass flow controller (23) is connected with the load gas path pressure stabilizing valve (26), the other end of the carrier gas path mass flow controller (23) is connected with one interface of the six-way valve (7), the interface of the six-way valve (7) is connected with a third tee, one end interface of the third tee is connected to the column temperature box, the other end interface of the third tee is connected with the shunt electromagnetic valve (36), and the other end of the shunt electromagnetic valve (36) is connected with the shunt flow controller (35).
10. The full-automatic multi-station recovery function thermal desorption instrument according to claim 2, wherein the feeding part comprises a material clamping belt (163), a feeding roller (165), a transmission roller and a support, the feeding roller (165), the transmission roller and a transmission shaft (1664) are installed in the support, the feeding roller (165), the transmission roller and the transmission shaft (1664) form a triangular structure, the material clamping belt (163) is sleeved on the outer sides of the feeding roller (165), the transmission roller and the transmission shaft (1664), the material clamping belt (163) drives the feeding roller (165) to transmit through the transmission roller and the transmission shaft (1664), a pipe clamping groove is formed in the material clamping belt (163), and the pipe clamping groove is of an omega-shaped structure.
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Cited By (1)
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| CN115980378B (en) | 2023-05-26 |
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