Full-automatic specific surface area analyzer auxiliary device and specific surface area analysis system

Abstract

The application discloses a kind of full-automatic specific surface area analyzer auxiliary devices, including automatic sampler, vacuum joint and sample tube locking mechanism, automatic sampler includes drive part, sample rack, drive part drives sample rack and moves horizontally between first position, second position, and lifts between first working position, second working position Action;Vacuum joint is installed at first position, with flexible sealing interface that can be inserted with sample tube and is communicated with vacuum channel and can be sealed;Sample tube locking mechanism is installed at second position, including clamping table with sample tube entrance, flexible locking ring installed on clamping table and locking drive unit, flexible locking ring has sealing mouth for sample tube insertion, and locking drive unit extrudes flexible locking ring relative to clamping table to make flexible locking ring lock sample tube.The application can realize sample tube automatic feeding and locking, and assist specific surface area analyzer to complete full-automatic test.The application also discloses a kind of specific surface area analysis system.

Description

Technical Field

[0001] This invention relates to the field of detection technology, and in particular to fully automated auxiliary equipment and specific surface area analysis system for specific surface area analysis. Background Technology

[0002] The specific surface area analyzer is based on the static volumetric method. It tests the adsorption-desorption process through mass balance equations, static gas equilibrium, and pressure measurement, all conducted at liquid nitrogen temperature. A known amount of gas is introduced into the sample tube, causing a pressure drop, from which the molar mass of the adsorbed gas at adsorption equilibrium is calculated. Using the measured equilibrium adsorption amount, theoretical models are employed to determine the single-point and multi-point BET specific surface area, Langmuir specific surface area, BJH mesopore and macropore volume and area distribution, total pore volume, t-plot micropore volume and surface area, Dubinin-Astakhov micropore distribution, Horvath-Kawazoe micropore distribution, density function theory (DFT), and Monte Carlo (MC) pore size distribution models.

[0003] Before performing surface area analysis on samples in a sample tube using a surface area analyzer, the samples often need to be heated in a vacuum environment. Therefore, when performing surface area analysis, the samples must first be manually taken to the corresponding preparation device for pretreatment, and then taken to the surface area analyzer for specific analysis. In particular, when processing the samples in the surface area analyzer, the sample tubes need to be manually inserted into the analyzer's port and the sample tubes are sealed and positioned by manually tightening the screws. This not only results in low stability of sealing and positioning, but also low work efficiency, making it difficult to achieve truly fully automated surface area analysis.

[0004] Therefore, there is an urgent need for an auxiliary device for a fully automatic specific surface area analyzer and a specific surface area analysis system that can solve the above problems. Summary of the Invention

[0005] The purpose of this invention is to provide an auxiliary device for a fully automatic specific surface area analyzer, which can assist the specific surface area analyzer in forming a fully automatic specific surface area analysis system, and perform automatic feeding, locking and positioning of sample tubes, resulting in high working efficiency.

[0006] To achieve the above objectives, this invention discloses an auxiliary device for a fully automated specific surface area analyzer, comprising an automatic sample feeder, a vacuum connector, a temperature control mechanism, and a sample tube locking mechanism. The device includes a displacement drive unit and a sample holder. The sample holder has one or more sample tube positioning slots for positioning and mounting sample tubes. The temperature control mechanism heats the sample tubes. The displacement drive unit drives the sample holder to move horizontally between a first position and a second position along a first direction, and to move vertically between a first working position and a second working position, wherein the first working position is higher than the second working position. The vacuum connector is installed at the first position and has a flexible connection communicating with the vacuum channel of the vacuum system. A sealing interface is provided, the inlet of which allows the sample tube to be sealed and inserted. A sample tube locking mechanism is installed at the second position, including a clamping platform with a sample tube inlet, a flexible locking ring installed on the clamping platform, and a locking drive unit that squeezes the flexible locking ring from the side away from the clamping platform. The flexible locking ring has a sealing port corresponding to and communicating with the sample tube inlet for the sample tube to be inserted. The sealing port is connected to the sample tube interface of the specific surface area analyzer host. The locking drive unit squeezes or releases the flexible locking ring towards the clamping platform to clamp or release the sample tube.

[0007] Compared with existing technologies, this invention discloses an auxiliary device for a specific surface area analyzer, used to form a fully automated specific surface area analysis system in conjunction with the specific surface area analyzer. This device automatically installs sample tubes at the vacuum station and the specific surface area analysis station for pre-processing and specific surface area analysis. Firstly, the auxiliary device includes an autosampler with a temperature control mechanism, which not only positions and heats the sample tubes but also automatically feeds them to the vacuum station and the specific surface area analysis station. Secondly, the auxiliary device incorporates a sample tube locking mechanism at the specific surface area analyzer. After the sample tube is inserted into the sealing port, a flexible locking ring is directly squeezed to lock the sample tube, simultaneously connecting it to the sample tube interface of the specific surface area analyzer host for specific surface area analysis of the sample within the tube.

[0008] Preferably, the vacuum connector includes a telescopic drive unit and a telescopic drive rod. The end of the telescopic drive rod is provided with the flexible sealing interface. The telescopic drive unit drives the telescopic drive rod to telescopically extend and retract, so that the flexible sealing interface extends downward to the first working position. The telescopic drive rod is provided with a vacuum channel communicating with the vacuum system along its rod body.

[0009] Preferably, the telescopic drive unit is equipped with a first sensor and a solenoid valve for controlling the opening and closing of the vacuum channel. When the flexible sealing interface descends to the second working position, the first sensor controls the solenoid valve to open to start the vacuum operation.

[0010] Preferably, the flexible sealing interface is funnel-shaped and mates with the opening of the sample tube to guide the insertion of the sample tube.

[0011] Preferably, the sample holder is a rotating sample holder that rotates around an axis, and the plurality of sample tube positioning slots are evenly arranged around the axis. The automatic sampler also includes a rotary drive unit that drives the rotating sample holder to rotate around the axis, so that multiple sample tubes can be loaded sequentially.

[0012] Preferably, the displacement driving unit includes a horizontal driving unit and a vertical driving unit. The horizontal driving unit drives the sample holder to move horizontally between a first position and a second position along a first direction. The vertical driving unit drives the sample tube of the sample holder to move up and down, so that the sample tube moves up and down between a first working position and a second working position. The vertical driving unit includes a sample lifting unit and an up-and-down driving unit. The up-and-down driving unit drives the sample holder to move up and down between a first height and a second height. The first height is higher than the second height. The sample lifting unit corresponds to the sample tube positioning groove and includes a sample inlet support plate located at the bottom of the sample tube and supporting the sample tube, and a lifting driving source that drives the sample inlet support plate to move up and down. When the sample holder is at the first height, the lifting driving source drives the sample tube to move up and down between the first working position and the second working position.

[0013] Preferably, the auxiliary device for the fully automated surface area analyzer further includes a control mechanism. The vacuum connector includes a telescopic drive unit and a telescopic drive rod. The end of the telescopic drive rod is provided with the flexible sealing interface. The telescopic drive unit drives the telescopic drive rod to telescopically extend, so that the flexible sealing interface extends downward to the first working position. The telescopic drive rod has a vacuum channel along its body that communicates with the vacuum system. The control mechanism is connected to the automatic sampler, the vacuum connector, and the sample tube locking mechanism. The control mechanism controls the up-and-down drive unit to move, so that the sample holder descends from the first position to a second height to wait for the sample tube. After the sample tube is in place, the control mechanism controls the up-and-down drive unit to move, so that the sample holder rises to the first height to allow the sample tube to be inserted. The tube is inserted and positioned into the sample tube positioning slot; the telescopic drive unit is controlled to move the telescopic drive rod down to the first working position so that the sample tube opening is inserted into the flexible sealing interface; the temperature control mechanism is controlled to heat the bottom of the sample tube; after completing the vacuuming and heating operations, the telescopic drive unit is controlled to reset, and then the horizontal drive unit is controlled to move the sample rack along the first direction to the second position; the sample lifting unit is controlled to move the sample rack up to the first working position so that the sample tube passes through the sample tube inlet and the flexible locking ring in sequence and then extends into the sample tube interface; the locking drive unit is controlled to press the flexible locking ring down against the clamping table to lock the sample tube, ready for the surface area analyzer main unit to work.

[0014] Preferably, the locking drive unit includes a rotary drive unit, a clamping screw, and a clamping nut. The clamping nut is threaded onto the clamping screw and abuts against the flexible locking ring. The rotary drive unit drives the clamping screw to rotate, and the clamping screw drives the clamping nut to move up and down. The clamping nut then drives the flexible locking ring to abut against or release relative to the clamping table.

[0015] Specifically, the rotary drive unit includes a drive source, a rotary drive wheel, a main shaft driven wheel, and a buffer assembly. The first wheel surface of the rotary drive wheel and the second wheel surface of the main shaft driven wheel are opposite each other at a certain distance. Cam beads and protrusions that engage with the rotary drive wheel in the rotation direction are provided on the first wheel surface and the second wheel surface. The buffer assembly provides a buffering elastic force to the main shaft driven wheel relative to the rotary drive wheel, so that the cam beads slide relative to the protrusion under a certain resistance. The drive source drives the rotary drive wheel to rotate, and the rotary drive wheel drives the main shaft driven wheel to rotate through the engagement of the cam beads and the protrusion.

[0016] More specifically, the rotating shaft of the driven wheel is rotatably mounted on a fixed frame, and the rotating shaft of the driving wheel is slidably mounted on the rotating shaft of the driven wheel. The buffer assembly includes a pressing member that presses against the driving wheel from the side of the driving wheel away from the first wheel surface, an elastic mounting seat mounted on the fixed frame, and an elastic member mounted in the elastic mounting seat. The elastic member provides a spring force to the pressing member to press against the driving wheel in the direction of the driven wheel.

[0017] More specifically, the auxiliary device for the fully automatic surface area analyzer also includes an elastic adjustment unit. The elastic mounting base is adjustablely mounted on the fixed frame along the axial direction of the rotation axis, and the elastic adjustment unit adjusts the position of the elastic mounting base along the axial direction of the rotation axis.

[0018] Preferably, the temperature control mechanism is mounted on the sample holder and heats the sample tube.

[0019] More preferably, the temperature control mechanism includes a heating part corresponding to the bottom of the sample tube, a cooling part corresponding to the upper part of the sample tube, and a heat-insulating part located between the heating part and the cooling part. The heating part heats the bottom of the sample tube, the cooling part cools the middle part of the sample tube, and the heat-insulating part wraps around the outer wall of the sample tube to keep the sample tube warm and position it.

[0020] Preferably, the sample tube positioning groove is further provided with a sample tube silicone pad on the groove wall.

[0021] The present invention also discloses a specific surface area analysis system, including a specific surface area analyzer main unit, auxiliary equipment, and a liquid nitrogen lifting mechanism. The auxiliary equipment is a fully automatic specific surface area analyzer auxiliary device as described above. The sample tube interface of the specific surface area analyzer main unit is installed at a second position and located above the first working position. The liquid nitrogen lifting mechanism is installed at a second position and located below the first working position, and is used to support the liquid nitrogen tank and drive the liquid nitrogen tank to lift and lower. Attached Figure Description

[0022] Figure 1 This is a top view of the specific surface area analysis system of the present invention.

[0023] Figure 2 This is a side view of the specific surface area analysis system of the present invention.

[0024] Figure 3 This is a structural diagram of the vacuum connector of the present invention.

[0025] Figure 4a This is a structural diagram of the sample lifting part in the first embodiment of the present invention.

[0026] Figure 4bThis is a structural diagram of the sample lifting part in the second embodiment of the present invention.

[0027] Figure 5 This is a structural diagram of the sample tube locking mechanism of the present invention. Detailed Implementation

[0028] To illustrate the technical content, structural features, objectives, and effects of the present invention in detail, the following description is provided in conjunction with the embodiments and accompanying drawings.

[0029] refer to Figure 1 and Figure 2 The present invention also discloses a specific surface area analysis system 100, including a specific surface area analyzer main unit 200, auxiliary equipment, and a liquid nitrogen lifting mechanism 400. The auxiliary equipment performs a vacuum heating operation on the sample tube 101 and automatically feeds the sample tube 101 into the specific surface area analyzer main unit 200. The sample tube interface of the specific surface area analyzer main unit 200 is installed at the second position 302 and located above the first working position 501. The sample tube interface of the liquid nitrogen lifting mechanism 400 is located at the second position 302 and located below the first working position 501, and is used to support the liquid nitrogen tank 40 and drive the liquid nitrogen tank 40 to lift and lower.

[0030] refer to Figure 2 The auxiliary device includes an autosampler 10, a vacuum connector 20, and a sample tube locking mechanism 30. The autosampler 10 heats the sample tube 101 and delivers it to the vacuum connector 20 and the sample tube locking mechanism 30 respectively.

[0031] refer to Figure 1 and Figure 2 The autosampler 10 includes a horizontal drive unit 121, a vertical drive unit, a sample holder 11, and a temperature control mechanism 14 mounted on the sample holder 11. The sample holder 11 has one or more sample tube positioning slots 111 for positioning and mounting sample tubes 101. The temperature control mechanism 14 is mounted on the sample holder 11 and heats the sample tubes 101. The horizontal drive unit 121 drives the sample holder 11 to move horizontally between a first position 301 and a second position 302 along a first direction. The vertical drive units (122, 123) drive the sample tubes 101 of the sample holder 11 to move up and down, so that the sample tubes 101 move up and down between a first working position 501 and a second working position 502, where the first working position 501 is higher than the second working position 502. Of course, other two-dimensional drive units, such as multi-joint robotic arms, can also be used to replace the horizontal drive unit 121 and the vertical drive unit in this invention.

[0032] The temperature control mechanism 14 may not be installed on the sample holder 11, but may be fixedly set at the first position and may be raised and lowered to detach from or wrap around the sample holder 11, thereby heating the sample in the sample tube 101 on the sample holder 11.

[0033] refer to Figure 2 The vertical drive unit includes a sample lifting unit 13 and an up-and-down drive unit 122. The up-and-down drive unit drives the sample holder 11 to move up and down between a first height 401 and a second height 402, where the first height 401 is higher than the second height 402. (Reference) Figure 4a The sample lifting unit 13 includes a sample inlet support plate 131 located at the bottom of the sample tube 101 and supporting the sample tube 101, and a lifting drive source 361132 that drives the sample inlet support plate 131 to move up and down. When the sample holder 11 is at the first height 401, the lifting drive source 361132 can drive the sample tube 101 to move up and down between the first working position 501 and the second working position 502. In this embodiment, in addition to the sample lifting unit 13, an up and down drive unit 122 is also provided to lift the sample holder 11, so that the sample tube 101 can be automatically loaded onto the sample holder 11.

[0034] The vertical drive unit includes a sample lifting unit 13 corresponding to the sample tube positioning slot 111. This correspondence can be one-to-one or many-to-one. The bottom of each sample tube positioning slot 111 is a sample inlet support plate 131. The correspondence between the sample tube positioning slots 111 and the sample lifting units 13 is determined by the number of sample tube inlets 311 in the sample tube locking mechanism 30, i.e., the number of sample tubes 101 that the sample tube locking mechanism 30 can process at one time. In this embodiment, the sample tube positioning slot 111 horizontally positions the sample tube from the upper middle part of the sample tube 101, and the uppermost edge of the slot wall of the sample tube positioning slot 111 is located above the heating mechanism 14.

[0035] Specifically, in this embodiment, the driving source 361 of the sample lifting part 13 is a pneumatic source, and specifically, the lifting driving source 361132 is a pneumatic cylinder 132 with a return spring 133.

[0036] refer to Figure 4b The sample lifting part 13a in the second embodiment of the present invention is different from the first embodiment. In this embodiment, the driving source 361 of the sample lifting part 13 is an electric source. Specifically, the lifting driving source 361132a is an electric driving source 361 composed of a rotary motor, a lead screw, and a lead screw nut.

[0037] refer to Figure 2The vacuum connector 20 is installed at the first position 301 and has a flexible sealing interface 21 that communicates with the vacuum channel 201 of the vacuum system 300. The inlet of the flexible sealing interface 21 can be used for the sealed insertion of the sample tube 101.

[0038] Continue to refer to Figure 2 The vacuum connector 20 includes a telescopic drive unit 24 and a telescopic drive rod 23. The end of the telescopic drive rod 23 is provided with the flexible sealing interface 21. The telescopic drive unit 24 drives the telescopic drive rod 23 to telescopically extend, so that the flexible sealing interface 21 extends downward to the first working position 501. The telescopic drive rod 23 has a vacuum channel 201 along its body that communicates with the vacuum system 300. The flexible sealing interface 21 is funnel-shaped and mates with the opening of the sample tube 101 to guide the insertion of the sample tube 101.

[0039] In this embodiment, the telescopic drive unit 24 is a telescopic piston cylinder, which includes a piston cylinder and a piston 22 fitted in the piston cylinder. The piston cylinder is connected to an air inlet 241 and an air outlet 242 to control the piston's telescopic movement. A spring 26 is also provided in the piston cylinder to provide a retraction force to the piston, assisting in rapid piston retraction.

[0040] Preferably, the telescopic drive unit 24 is equipped with a first sensor and a solenoid valve that controls the opening and closing of the vacuum channel 201. When the flexible sealing interface 21 descends to the second working position 502, the first sensor controls the solenoid valve to open to start the vacuuming operation. This solution can automatically control the start and end of the vacuuming through the telescopic drive unit 24, realizing linkage control.

[0041] refer to Figure 2 and Figure 5The sample tube locking mechanism 30 is installed at the second position 302 and includes a clamping platform 31 with a sample tube inlet 311, a flexible locking ring 32 installed on the clamping platform 31, and a locking drive unit that squeezes the flexible locking ring 32 from the side away from the clamping platform 31. The flexible locking ring 32 has a sealing port 321 that corresponds to and communicates with the sample tube inlet 311 and allows the sample tube 101 to be inserted. The sealing port 321 communicates with the sample tube interface of the specific surface area analyzer host 200. The locking drive unit can squeeze or release the flexible locking ring 32 towards the clamping platform 31 to clamp or release the sample tube 101. In this embodiment, the flexible locking ring 32 is a rubber ring. Of course, the structure of the flexible locking ring 32 is not limited to this and can also be made of other flexible materials. In this embodiment, the flexible locking ring 32 is in the shape of a corrugated tube. Of course, the structure of the flexible locking ring 32 is not limited to this, and it can also be other structures that can be compressed and bent to reduce the inner diameter.

[0042] refer to Figure 5 The locking drive unit includes a rotary drive unit 36, a clamping screw 34, and a clamping nut 33. The clamping nut 33 is threaded onto the clamping screw 34 and abuts against the flexible locking ring 32. The rotary drive unit 36 ​​drives the clamping screw 34 to rotate, and the clamping screw 34 drives the clamping nut 33 to move up and down. The clamping nut 33 then drives the flexible locking ring 32 to abut against or release relative to the clamping table 31.

[0043] Continue to refer to Figure 5 The rotary drive unit 36 ​​includes a drive source 361, a rotary drive wheel 363, a main shaft driven wheel 364, and a buffer assembly. The first wheel surface of the rotary drive wheel 363 and the second wheel surface of the main shaft driven wheel 364 are opposite each other at a certain distance. Cam beads 3631 and protrusions 3641 that engage with the rotary drive wheel 363 in the rotation direction are provided on the first wheel surface and the second wheel surface. The buffer assembly provides a buffering elastic force to the main shaft driven wheel 364 relative to the rotary drive wheel 363, so that the cam beads 3631 slide relative to the protrusions 3641 under a certain resistance. The drive source 361 drives the rotary drive wheel 363 to rotate. The rotary drive wheel 363 can drive the main shaft driven wheel 364 to rotate through the engagement of the cam beads 3631 and the protrusions 3641. The rotary drive unit 36 ​​further includes a reduction gear set 362, which meshes with the rotary drive wheel 363. The drive source 361 drives the rotary drive wheel 363 to rotate via the reduction gear set 362. The drive source 361 is a rotary motor.

[0044] In this embodiment, the cam bead 3631 is embedded in the first wheel surface of the rotating drive wheel 363, and the protrusion 3641 is integrally formed or fixed to the second wheel surface of the driven wheel 364. The contact surfaces of the cam bead 3631 and the protrusion 3641 are extremely smooth. When the driven wheel 364 encounters external force and cannot rotate, the cam bead 3631 can slip and jump over the protrusion 3641. This not only effectively controls the locking force of the flexible locking ring 32, but also prevents the clamping screw 34 from rotating excessively, which could damage the flexible locking ring 32 or crush or bend the sample tube 101.

[0045] More specifically, the rotating shaft of the driven wheel 364 is rotatably mounted on a fixed frame 360, wherein the rotating shaft of the driven wheel 364 is fixed to the fixed frame 360 ​​via a main shaft mounting seat 365. The rotating shaft of the driving wheel 363 is slidably mounted on the rotating shaft of the driven wheel 364. The buffer assembly includes a pressing member 37 pressing against the driving wheel 363 from the side of the driving wheel 363 away from the first wheel surface, an elastic mounting seat 303 mounted on the fixed frame 360, and an elastic member 35 mounted within the elastic mounting seat 303. The elastic member 35 provides a spring force to the pressing member 37 to press against the driving wheel 363 in the direction of the driven wheel 364. The elastic member 35 provides the pressing spring force to the pressing member 37 through multiple push rods. In this embodiment, the pressing member 37 is a pressure plate.

[0046] More specifically, the rotary drive unit 36 ​​also includes an elastic adjustment unit 38. The elastic mounting seat 303 is axially adjustable on the fixed frame 360 ​​along the rotation axis. The elastic adjustment unit 38 adjusts the position of the elastic mounting seat 303 along the rotation axis, thereby adjusting the tightness of the elastic element 35 to adjust the engagement amplitude between the cam bead 3631 and the protrusion 3641, and finally adjusts the degree of locking of the flexible locking ring 32 to the sample tube 101.

[0047] Of course, the structure of the locking drive unit is not limited to this. It can be an electric piston with high precision and an adjustable pressure relief valve. The electric piston is equipped with a sensor to detect the piston rod pressure and has a solenoid valve on the vent. When the sensor detects that the piston rod thrust is greater than a preset value, it controls the vent to open so as to control the thrust of the electric piston and prevent excessive thrust from damaging the flexible locking ring 32 or the sample tube.

[0048] refer to Figure 2The temperature control mechanism 14 includes a heating part 141 corresponding to the bottom of the sample tube 101, a cooling part 143 corresponding to the upper middle part of the sample tube 101, and a heat-insulating part 142 located between the heating part 141 and the cooling part 143. The heating part 141 heats the bottom of the sample tube 101, the cooling part 143 cools the middle part of the sample tube 101, and the heat-insulating part 142 wraps around the outer wall of the sample tube 101 to keep it warm and position it. The heat-insulating part 142 is a heat-insulating sleeve supported by heat-insulating material, which allows the sample tube 101 to be inserted and positions and insulates it. In this embodiment, an electric heating wire is used as the heating part 141 to heat the bottom of the sample tube 101, and a fan-cooled cooling fan is used as the cooling part 143 to cool the upper middle part of the sample tube 101.

[0049] The sample tube positioning groove 111 has a silicone pad 112 on its wall to wrap around the sample tube 101. The silicone pad 112 wraps around the sample tube 101 and provides a positioning elastic force for the sample tube 101, thereby realizing the automatic clamping of the sample tube positioning groove 111. Of course, the sample tube positioning groove 111 can also be set as an automatic clamping groove with elastic force provided by a spring or as an electrically controlled automatic clamping groove. The silicone pad 112 can also be driven by other cushioning elastic materials, and is not limited to these. In this embodiment, the groove wall of the sample tube positioning groove 111 is located above the sample tube 101, and the bottom of the groove is the sample injection support plate 131. The groove wall of the sample tube positioning groove 111 can only position the sample tube 101 in a horizontal position, while the sample injection support plate 131 positions the sample tube 101 in a vertical position. When the sample injection support plate 131 rises and falls, the sample tube 101 in the sample tube positioning groove 111 rises and falls accordingly.

[0050] The auxiliary device also includes a control mechanism, which is connected to the autosampler 10, the vacuum connector 20, and the sample tube locking mechanism 30, and controls the autosampler 10, the vacuum connector 20, and the sample tube locking mechanism 30 to achieve the preparation and loading of fully automated specific surface area analysis.

[0051] The following describes the process of specific surface area analysis according to the present invention:

[0052] (1) When the work starts, the sample holder 11 is in the first position 301 and at the first height 401.

[0053] (2) The control mechanism controls the up and down drive unit to move so as to drive the sample holder 11 to descend from the first position 301 to the second height 402 and wait for the sample tube 101.

[0054] (3) After the sample tube 101 is in place, the control mechanism controls the upper and lower drive unit to move and drive the sample holder 11 to the first height 401, so that the sample tube 101 is inserted and positioned in the sample tube positioning slot 111. The control mechanism is equipped with parameters such as the number of sample tubes 101 installed, the tag number, and the sample quantity, which facilitates subsequent control.

[0055] (4) The control mechanism controls the telescopic drive unit 24 to move the telescopic drive rod 23 down to the first working position 501, so that the port of the sample tube 101 is inserted into the flexible sealing interface 21. The control mechanism 14 is then controlled to heat the bottom of the sample tube 101. After completing the vacuuming and heating operations, the telescopic drive unit 24 is controlled to reset. The heating operation can be controlled by controlling the heating temperature and heating time, and the vacuuming operation can be controlled by controlling the pressure of the sample tube 101. The specific temperature control and vacuuming control are well known to those skilled in the art and will not be described in detail here.

[0056] (5) The control mechanism controls the horizontal drive unit 121 to move the sample holder 11 along the first direction to the second position 302.

[0057] (6) After the sample holder 11 moves to the second position 302, the control mechanism controls the sample lifting part 13 at the corresponding position to move to drive the sample holder 11 to the first working position 501, so that the sample tube 101 passes through the sample tube inlet 311 and the flexible locking ring 32 in sequence and then extends into the sample tube interface.

[0058] (7) The control mechanism controls the locking drive unit to press down the flexible locking ring 32 against the clamping table 31 to lock the sample tube 101.

[0059] (8) The main unit 200 of the specific surface area analyzer starts automatic testing.

[0060] When it is necessary to immerse the sample tube 101 in liquid nitrogen, in step (8), the up and down drive unit is controlled to move, so as to drive the sample holder 11 to descend from the first position 301 to the second height 402. The sample tube 101, which is locked by the flexible locking ring 32, is released from the sample holder 11, and the sample holder 11 moves along the first direction to the first position 301. Then, the liquid nitrogen lifting mechanism 400 is activated to drive the liquid nitrogen tank 40 to rise until the sample tube is immersed in the liquid nitrogen tank 40, and the specific surface area analyzer host 200 starts automatic testing.

[0061] In this embodiment, the sample tube locking mechanism may have a clamping platform 31 and a flexible locking ring 32, or it may have multiple clamping platforms 31 and multiple flexible locking rings 32. Meanwhile, the surface area analyzer host 200 has multiple corresponding sample tube inlets 311, which can simultaneously position, clamp, and automatically test multiple sample tubes.

[0062] In this embodiment, there may be one vacuum connector 20 or multiple vacuum connectors 20, so that multiple sample tubes 101 can be heated and vacuumed simultaneously, thereby improving operational efficiency.

[0063] The sample holder 11 is a rotating sample holder 11 that rotates around an axis. The plurality of sample tube positioning slots 111 are evenly arranged around the axis. The automatic sample feeder 10 also includes a rotation drive unit 36 ​​that drives the rotating sample holder 11 to rotate around the axis, which can sequentially realize the feeding of multiple sample tubes 101.

[0064] During vacuum heating, the rotary drive unit 36 ​​can be controlled to rotate the rotary sample holder 11 to different positions, so that the sample tubes 101 on the rotary sample holder 11 are aligned with the vacuum connector 20 in turn for vacuuming operations. Similarly, when connected to the specific surface area analyzer main unit 200, the rotary drive unit 36 ​​can rotate the rotary sample holder 11 to different positions, so that the sample tubes 101 on the rotary sample holder 11 are aligned with the sample tube inlet 311 of the sample tube locking mechanism 30 in turn for specific surface area analysis.

[0065] Of course, the specific surface area analysis and vacuuming operation can be performed simultaneously. During operation, after the flexible locking ring 32 presses down against the clamping table 31 in step (7) to lock part of the sample tube 101, the upper and lower driving parts are controlled to move in step (8) to drive the sample rack 11 to descend from the first position 301 to the second height 402. The sample tube 101 locked by the flexible locking ring 32 is released from the sample rack 11. The sample rack 11 carrying the remaining sample tube 101 is controlled to move along the first direction to the first position 301. Then the rotation driving part 36 is controlled to move to the next station to rotate the sample rack 11, thereby rotating the next part of the sample tube 101 to align with the vacuum connector 20. After the previous batch of sample tubes 101 has completed the specific surface area test and the current sample tube 101 has completed heating and vacuuming, step 6 is executed again to complete the specific surface area test of the current batch of sample tubes until the specific surface area test of all sample tubes 101 on the sample rack 11 is completed.

[0066] The above-disclosed embodiments are merely preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. Therefore, any equivalent variations made in accordance with the claims of the present invention are still within the scope of the present invention.

Claims

1. An auxiliary device for a fully automatic specific surface area analyzer, characterized in that: include: An autosampler includes a displacement drive unit and a sample holder. The sample holder has one or more sample tube positioning slots for positioning and mounting sample tubes. The displacement drive unit drives the sample holder to move horizontally between a first position and a second position along a first direction, and to move vertically between a first working position and a second working position. The first working position is higher than the second working position. The temperature control mechanism heats the sample tubes on the sample holder at the first working position; A vacuum connector, installed at the first position, has a flexible sealing interface that communicates with the vacuum channel of the vacuum system, and the inlet of the flexible sealing interface is available for the sample tube to be sealed and inserted. A sample tube locking mechanism, installed at the second position, includes a clamping platform with a sample tube inlet, a flexible locking ring mounted on the clamping platform, and a locking drive unit that squeezes the flexible locking ring from the side away from the clamping platform. The flexible locking ring has a sealing port corresponding to and communicating with the sample tube inlet for insertion of the sample tube. The sealing port is connected to the sample tube interface of the specific surface area analyzer host. The locking drive unit squeezes or releases the flexible locking ring towards the clamping platform to clamp or release the sample tube.

2. The auxiliary device for the fully automatic specific surface area analyzer as described in claim 1, characterized in that: The vacuum connector includes a telescopic drive unit and a telescopic drive rod. The end of the telescopic drive rod is provided with the flexible sealing interface. The telescopic drive unit drives the telescopic drive rod to telescopically extend and retract, so that the flexible sealing interface extends downward to the first working position. The telescopic drive rod is provided with a vacuum channel communicating with the vacuum system along its rod body.

3. The auxiliary device for the fully automatic specific surface area analyzer as described in claim 2, characterized in that: The telescopic drive unit is equipped with a first sensor and a solenoid valve that controls the opening and closing of the vacuum channel. When the flexible sealing interface descends to the second working position, the first sensor controls the solenoid valve to open to start the vacuum operation.

4. The auxiliary device for the fully automatic specific surface area analyzer as described in claim 2, characterized in that: The flexible sealing interface is funnel-shaped and mates with the opening of the sample tube to guide the insertion of the sample tube.

5. The auxiliary device for the fully automatic specific surface area analyzer as described in claim 1, characterized in that: The sample holder is a rotating sample holder that rotates around an axis. The plurality of sample tube positioning slots are evenly arranged around the axis. The autosampler also includes a rotary drive unit that drives the rotating sample holder to rotate around the axis.

6. The auxiliary device for the fully automatic specific surface area analyzer as described in claim 1, characterized in that: The displacement driving unit includes a horizontal driving unit and a vertical driving unit. The horizontal driving unit drives the sample holder to move horizontally between a first position and a second position along a first direction. The vertical driving unit drives the sample tube of the sample holder to move up and down, so that the sample tube moves up and down between a first working position and a second working position. The vertical driving unit includes a sample lifting unit and an up-and-down driving unit. The up-and-down driving unit drives the sample holder to move up and down between a first height and a second height. The first height is higher than the second height. The sample lifting unit corresponds to the sample tube positioning groove and includes a sample inlet support plate located at the bottom of the sample tube and supporting the sample tube, and a lifting driving source that drives the sample inlet support plate to move up and down. When the sample holder is at the first height, the lifting driving source drives the sample tube to move up and down between the first working position and the second working position.

7. The auxiliary device for the fully automatic specific surface area analyzer as described in claim 6, characterized in that: It also includes a control mechanism. The vacuum connector includes a telescopic drive unit and a telescopic drive rod. The end of the telescopic drive rod is provided with the flexible sealing interface. The telescopic drive unit drives the telescopic drive rod to telescopically extend, so that the flexible sealing interface extends downward to the first working position. The telescopic drive rod has a vacuum channel along its body that communicates with the vacuum system. The control mechanism is connected to the automatic sampler, the vacuum connector, and the sample tube locking mechanism. The control mechanism controls the up-and-down drive unit to move, so that the sample holder descends from the first position to a second height to wait for the sample tube. After the sample tube is in place, the control mechanism controls the up-and-down drive unit to move, so that the sample holder rises to the first height, so that the sample tube is inserted and positioned. The sample tube positioning slot is configured as follows: the telescopic drive unit is controlled to move the telescopic drive rod down to the first working position so that the sample tube opening is inserted into the flexible sealing interface; the temperature control mechanism is controlled to heat the bottom of the sample tube; after vacuuming and heating are completed, the telescopic drive unit is controlled to reset, and then the horizontal drive unit is controlled to move the sample rack along the first direction to the second position; the sample lifting unit is controlled to move the sample rack up to the first working position so that the sample tube passes through the sample tube inlet and the flexible locking ring in sequence and then extends into the sample tube interface; the locking drive unit is controlled to press the flexible locking ring down against the clamping table to lock the sample tube, ready for the surface area analyzer main unit to start working.

8. The auxiliary device for the fully automatic specific surface area analyzer as described in claim 1, characterized in that: The locking drive unit includes a rotary drive unit, a clamping screw, and a clamping nut. The clamping nut is threaded onto the clamping screw and abuts against the flexible locking ring. The rotary drive unit drives the clamping screw to rotate, and the clamping screw drives the clamping nut to move up and down. The clamping nut then drives the flexible locking ring to abut against or release relative to the clamping table.

9. The auxiliary device for the fully automatic specific surface area analyzer as described in claim 8, characterized in that: The rotary drive unit includes a drive source, a rotary drive wheel, a main shaft driven wheel, and a buffer assembly. The first wheel surface of the rotary drive wheel and the second wheel surface of the main shaft driven wheel are opposite each other at a certain distance. Cam beads and protrusions that engage with the rotary drive wheel in the rotation direction are provided on the first wheel surface and the second wheel surface. The buffer assembly provides a buffering elastic force to the main shaft driven wheel relative to the rotary drive wheel, so that the cam beads slide relative to the protrusion under a certain resistance. The drive source drives the rotary drive wheel to rotate, and the rotary drive wheel drives the main shaft driven wheel to rotate through the engagement of the cam beads and the protrusion.

10. The auxiliary device for the fully automatic specific surface area analyzer as described in claim 9, characterized in that: The rotating shaft of the driven wheel is rotatably mounted on a fixed frame, and the rotating shaft of the driving wheel is slidably mounted on the rotating shaft of the driven wheel. The buffer assembly includes a pressing member that presses against the driving wheel from the side of the driving wheel away from the first wheel surface, an elastic mounting seat mounted on the fixed frame, and an elastic member mounted in the elastic mounting seat. The elastic member provides a spring force to the pressing member to press against the driving wheel in the direction of the driven wheel.

11. The auxiliary device for the fully automatic specific surface area analyzer as described in claim 10, characterized in that: It also includes an elastic adjustment part, wherein the elastic mounting seat is adjustablely mounted on the fixed frame along the axial direction of the rotation axis, and the elastic adjustment part adjusts the position of the elastic mounting seat along the axial direction of the rotation axis.

12. The auxiliary device for the fully automatic specific surface area analyzer as described in claim 1, characterized in that: The temperature control mechanism is mounted on the sample holder and heats the sample tube.

13. The auxiliary device for the fully automatic specific surface area analyzer as described in claim 12, characterized in that: The temperature control mechanism includes a heating section corresponding to the bottom of the sample tube, a cooling section corresponding to the upper middle part of the sample tube, and a heat-insulating section located between the heating section and the cooling section. The heating section heats the bottom of the sample tube, the cooling section cools the middle part of the sample tube, and the heat-insulating section wraps around the outer wall of the sample tube to keep the sample tube warm and in a fixed position.

14. A specific surface area analysis system, characterized in that: The device includes a specific surface area analyzer main unit, auxiliary equipment, and a liquid nitrogen lifting mechanism. The auxiliary equipment is a fully automatic specific surface area analyzer auxiliary device as described in any one of claims 1-13. The sample tube interface of the specific surface area analyzer main unit is installed at a second position and located above the first working position. The liquid nitrogen lifting mechanism is installed at a second position and located below the first working position, and is used to support the liquid nitrogen tank and drive the liquid nitrogen tank to lift and lower.

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