Physical adsorption instrument sampling device and use method

Abstract

The invention discloses a sample introduction device of a physical adsorption instrument. The sample introduction device comprises a fixed frame, a sample introduction module, a vibration module, a displacement module and a balance, the fixed frame is placed on the balance, and the sample tube with the spherical bottom is fixed on the fixed frame and is vertical to the balance tray; the displacement module is arranged beside the balance, the vibration module comprises an upper part and a lower part, the displacement module is arranged on the lower part of the vibration module, and the upper part of the vibration module is arranged on the displacement module and controlled by the displacement module to realize lifting or translation; and the sample injection module is positioned above the sample tube and is aligned to the orifice of the sample tube, and the sample injection module is mounted on the upper part of the vibration module and vibrates along with the vibration module to realize sample loading. The device is compact in structure, high in practicability, extremely rapid in sample loading and almost free of sample loss, and the scientific research efficiency and quality can be greatly improved; the sample is not rubbed with the sample tube to generate static electricity, lossless sample loading is achieved, and the situation that the sample adheres to the straight tube wall of the sample tube, and consequently the physical adsorption test dead volume is reduced is avoided.

Description

Technical Field

[0001] The present invention relates to the technical field of physical adsorption instrument equipment, and in particular to a physical adsorption instrument sampling device and a use method thereof. Background Art

[0002] Physical adsorption is an excellent method to obtain the physical properties of porous materials such as catalysts, MOFs, COFs, battery materials, biomass carbon, perovskites, etc. It can reflect information on specific surface area, pore size, porosity, pore volume, vapor adsorption, and adsorption heat. However, this requires a detailed understanding of the adsorption process, including the adsorption and phase change of fluids on porous materials and their effects on the adsorption isotherm, which is the basis of surface analysis and pore analysis.

[0003] The pore type and pore size of porous materials such as catalysts, MOFs, COFs, battery materials, biomass carbon, and perovskites will affect the diffusion of guest species into the pores and the configuration of guest species in the pores, thereby affecting the number of effective active sites of the material and ultimately affecting the application performance of the material. When conducting physical adsorption tests on the above-mentioned porous materials, the dead volume of the sample tube is calibrated first. The dead volume calibration affects their specific surface area, pore size, pore type, etc., further affecting the active sites of the material, and ultimately affecting the application performance of the material.

[0004] The sample tube used in the physical adsorption instrument has an open cylindrical straight tube on the top and a round ball tube on the bottom; the diameter of the cylindrical straight tube is 3mm to 5mm, the length is 28 to 30cm; the diameter of the round ball tube is 2cm. During the physical adsorption test, the residual sample on the wall of the cylindrical straight tube affects the calibration of the dead volume of the sample tube, thereby affecting the accuracy of the final result; if the residual sample on the wall of the straight tube has a low density, the sample will be drawn into the internal pipeline of the instrument and contaminate the instrument.

[0005] At present, whether it is a scientific research laboratory or an enterprise laboratory, when loading the sample tube, almost all of them use paper troughs or customized long-diameter glass funnels for manual loading. When using a paper trough to load samples, due to the long straight tube length and small diameter of the sample tube, the paper trough often flips, and a large amount of sample sticks to the wall of the straight tube. The operator will further poke the sample with a soft brush, so that the soft brush will be attached to a large amount of precious sample. If it is a sample with low density and high viscosity, it is often difficult to brush it down. Instead, when it is pulled out, the entire straight tube wall of the sample tube will be stained with the sample. When using a customized glass funnel to load samples, the funnel is made of glass. When the sample passes through, friction will generate static electricity, and the sample will adhere to the glass tube wall, resulting in expensive sample loss. In addition, the aperture of the sample tube is small, and the minimum size of the glass wall is 1mm, so the maximum inner diameter of the glass funnel is 2mm, and the loading speed is particularly slow. It takes about 10 minutes to load an ordinary 0.1 mg sample; when encountering a sample with low density and high viscosity, it takes about 60 minutes to load an ordinary 0.1 mg sample. This method affects the efficiency of scientific research and enterprise experiments. Summary of the invention

[0006] The purpose of the present invention is to overcome the deficiencies of the above-mentioned prior art and to provide a physical adsorption instrument sampling device and a method of use, which can solve the problem of large-scale loss of precious scientific research material samples; greatly shorten the sampling time for samples with low density and high viscosity, and improve scientific research efficiency.

[0007] The present invention is realized through the following technical scheme: a physical adsorption instrument sampling device, comprising a fixing frame, a sampling module, a vibration module, a displacement module and a balance; the fixing frame is placed on the balance, and a sample tube with a spherical bottom is fixed on the fixing frame and is perpendicular to the balance tray; the displacement module is arranged beside the balance, the vibration module comprises an upper part and a lower part, the displacement module is installed on the lower part of the vibration module, and the upper part of the vibration module is installed on the displacement module and is controlled by the displacement module to achieve lifting or translation; the sampling module is located above the sample tube and is aligned with the tube mouth of the sample tube, and the sampling module is installed on the upper part of the vibration module and achieves sampling with the vibration of the vibration module.

[0008] The sample injection module includes a micro-funnel, a retractable sample tube, and a sample tube control structure for controlling the start or stop of the retractable sample tube; the upper end of the retractable sample tube is connected to the outlet at the bottom of the micro-funnel, and the lower end of the retractable sample tube is freely retracted to enter the bottom of the straight tube wall of the sample tube; the sample tube control structure is installed at the lower end of the micro-funnel.

[0009] The micro funnel and the retractable sample receiving tube are both made of non-charged nanomaterials, and the inner wall of the retractable sample receiving tube has a smooth surface, which can prevent the sample from adhering to the surface.

[0010] The upper part of the vibration module includes a support upper chassis, a vibration support, a vibration machine base, a vibration machine and a vibration plate; the lower part of the vibration module includes a vibration-damping foot cup, a support lower chassis and a vibration controller for controlling the operation of the vibration module; one end of the vibration plate is embedded in the micro-funnel, and the bottom of the other end is embedded in the top of one end of the vibration machine, and the bottom of the other end of the vibration machine is installed on the vibration machine base, the bottom of the vibration machine base is fixed to the upper end of the vibration support, and the lower end of the vibration support is fixed to the support upper chassis; the support upper chassis is installed on the displacement module, the displacement module is installed on the support lower chassis, the vibration controller is installed on the upper side of the support lower chassis, and the bottom of the support lower chassis is installed with the vibration-damping foot cup. The vibration-damping foot cup is used to reduce shock.

[0011] There are four vibration brackets, which are evenly distributed at the bottom of the vibration machine; there are four vibration-damping foot cups, which are evenly distributed at the bottom of the chassis under the brackets.

[0012] The displacement module includes a horizontal moving platform and a vertical lifting platform; the horizontal moving platform includes an upper linear guide slide and a lower linear guide slide, the two linear guide slides are vertically assembled into a cross shape, the upper part of the vibration module is mounted on the upper linear guide slide and can slide along it, the upper linear guide slide is mounted on the lower linear guide slide and can slide along it, the lower linear guide slide is mounted on the vertical lifting platform, and the vertical lifting platform is mounted on the lower part of the vibration module. The two linear guide slides are vertically assembled into a cross shape, which can realize the translation of the upper part of the vibration module forward, backward, left and right, and accurately control the displacement.

[0013] The sample tube control structure includes a control component chassis and a control switch, a sample tube controller, a compression spring, and a retractable plate installed on the control component chassis; the control component chassis is connected to the bottom side wall of the micro funnel, the control switch is installed on the sample tube controller and is used to control its on and off, the retractable plate and the compression spring are installed under the sample tube controller, one end of the compression spring is fixed to the sample tube controller, and the other end of the compression spring is fixed to the retractable plate; as the control switch is opened and closed, the retractable plate moves against the retractable sample tube and clamps it under the extension action of the compression spring, or the retractable plate releases the movement of the retractable sample tube and releases its restriction under the compression action of the compression spring. After the control switch is turned on, the sample tube controller releases the restriction on the compression spring, and the compression spring drives the retractable plate to move the retractable sample tube and clamp it so that things cannot fall down; after the control switch is turned off, the sample tube controller drives the compression spring to compress and retract it, thereby releasing the restriction of the retractable plate on the retractable sample tube, and the retractable sample tube is connected to the micro funnel, and the retractable sample tube automatically falls to the bottom of the sample tube.

[0014] The upper linear guide slide and the lower linear guide slide are linear guide slides with the same structure, and the upper linear guide slide includes a first ball screw, a first nut, a first control handle, a first locking clamp for locking the first ball screw, a first supporting structure and a first screw ball seat; the first supporting structure includes a first guide rod and a first positioning plate, the first positioning plate is provided with two pieces, each of which has a hole in the center, and the first screw ball seat is installed in the hole of each first positioning plate, and the two ends of the first ball screw are respectively inserted into the first screw ball seat; one end of the first ball screw extends outward from the outside of the first positioning plate, and the first control handle is installed on the end; the first locking clamp is fixed on the stop cover or bearing cover of the first supporting structure; the first nut is sleeved on the first ball screw; the first supporting structure is installed in the A vertical lifting platform; the lower linear guide slide includes a second ball screw, a second nut, a second control handle, a second locking clamp for locking the second ball screw, a second supporting structure and a second screw ball seat; the second supporting structure includes a second guide rod and a second positioning plate, the second positioning plate is provided with two pieces, each of which has a hole in the center, and the second screw ball seat is installed in the hole of each second positioning plate, and the two ends of the second ball screw are respectively inserted into the second screw ball seat; one end of the second ball screw extends outward from the outside of the second positioning plate, and the second control handle is installed on the end; the second locking clamp is fixed on the stop cover or the bearing cover of the second supporting structure; the second nut is sleeved on the second ball screw; the second supporting structure is installed on the first nut, and the chassis on the bracket is installed on the second nut.

[0015] The vertical lifting platform comprises an upper scissors-type bracket, a lower scissors-type bracket, a bearing, a fixed shaft, an upper fixed plate, a lower fixed plate, a screw and a third control handle installed at the end of the screw; the lower scissors-type brackets are provided on both sides of the lower fixed plate, and the lower scissors-type brackets located on the same side include a fixed lower bracket and a movable lower bracket arranged crosswise, the lower fixed plate is provided with a lower movable groove, the lower end of the fixed lower bracket is hinged to the lower fixed plate through a bearing, and the lower end of the movable lower bracket is movably clamped in the lower movable groove through a bearing and can slide along the lower movable groove; the upper scissors-type brackets are provided on both sides of the upper fixed plate, and the upper scissors-type brackets located on the same side include a fixed upper bracket and a movable upper bracket arranged crosswise, the upper fixed plate is provided with an upper movable groove, and the upper end of the fixed upper bracket is hinged to the upper fixed plate through a bearing On the fixed plate, the lower end of the movable upper bracket is movably clamped in the upper movable groove through a bearing and can slide along the upper movable groove; the lower movable groove is opposite to the upper movable groove; the bearing includes a first bearing and a second bearing, and in the scissors upper bracket and the scissors lower bracket located on the same side, the lower end of the fixed upper bracket is hinged to the upper end of the fixed lower bracket through the first bearing, and the lower end of the movable upper bracket is hinged to the upper end of the movable lower bracket through the second bearing; the two first bearings located on both sides of the vertical lifting platform are connected together through the same fixed shaft, and the two second bearings located on both sides of the vertical lifting platform are connected together through the same fixed shaft; the fixed shaft is provided with a threaded hole, and the two ends of the screw are respectively inserted into the threaded holes of the two fixed shafts.

[0016] A method for using a sample introduction device of a physical adsorption instrument, characterized in that it comprises the following steps:

[0017] Step 1: After the balance is self-calibrated, put it on the fixing frame, return the balance to zero, put the sample tube on the fixing frame, and then read the reading and record it;

[0018] Step 2: Use the handle of the linear guide slide to adjust the left and right displacement and the front and back displacement of the injection module so that the outlet of the injection micro funnel is vertically aligned with the tube opening of the sample tube; start the sample tube control structure to make the retractable sample tube vertically extend into the sample tube, and then control the vertical lifting platform to adjust the height of the retractable sample tube so that it is parallel to the bottom end of the tube wall of the sample tube;

[0019] Step 3: Pour a small amount of sample powder into the micro funnel, start the vibration controller, and turn it off for 3 to 8 seconds. Start the sample tube control structure and retract the retractable sample tube;

[0020] Step 4: Read the balance and write it down.

[0021] Compared with the prior art, the advantages of the present invention are:

[0022] This device provides an ultra-light, almost non-destructive, ultra-fast sample injection device and a method of use. It has a compact structure, high practicality, extremely fast sample injection and almost no sample loss, which can greatly improve scientific research efficiency and quality; it is suitable for sample injection of instruments such as physical adsorption instruments.

[0023] The device is designed with a vibration module, the vibration of which covers the micro-funnel and the retractable sample tube. The sample loading efficiency is very high. It only takes 3 to 8 seconds to load a sample, which can greatly improve scientific research efficiency.

[0024] The micro funnel and retractable sample tube of the device are made of nanometer non-charged materials, which will not cause static electricity generated by friction between the sample and the micro funnel, and precious samples will not adhere to the micro funnel and retractable sample tube, so as to achieve non-destructive loading. It prevents the sample from sticking to the straight tube wall of the physical adsorption instrument sample tube, resulting in a reduction in the dead volume of the physical adsorption test, affecting the accuracy of the test results of the specific surface area, pore size and adsorption heat of porous materials such as catalysts, MOFs, COFs, battery materials, biomass carbon, and perovskites. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 It is a front view of an embodiment of the present invention;

[0026] Figure 2 A side view of an embodiment of the present invention;

[0027] Figure 3 A top view of an embodiment of the present invention;

[0028] Figure 4 This is a schematic diagram of the structure of the sample pipe control structure according to an embodiment of the present invention;

[0029] Figure 5 It is a front view of a horizontal moving platform according to an embodiment of the present invention;

[0030] Figure 6 is a side view of a horizontal moving platform according to an embodiment of the present invention;

[0031] Figure 7 is a top view of a horizontal moving platform according to an embodiment of the present invention;

[0032] Figure 8 This is a front view of a vertical lifting platform according to an embodiment of the present invention;

[0033] Fig. 9 It is a side view of a vertical lifting platform according to an embodiment of the present invention;

[0034] Fig.10 It is a top view of the vertical lifting platform according to an embodiment of the present invention.

[0035] The meanings of the reference numerals in the figure are as follows: 1. vibration-damping foot cup; 2. chassis under the bracket; 3. vibration controller; 4. vertical lifting platform; 41. upper bracket of the scissors fork; 42. bearing; 43. third control handle; 44. lower bracket of the scissors fork; 45. upper fixed plate; 46. lower fixed plate; 47. fixed shaft; 5. horizontal moving platform; 51. upper linear guide slide; 511. first control handle; 512. first locking clamp; 513. first supporting structure; 514. first ball screw; 52. lower linear guide slide Table; 521, second control handle; 522, second locking clamp; 523, second supporting structure; 524, second ball screw; 6, chassis on the bracket; 7, vibration bracket; 8, vibration machine base; 9, vibration machine; 10, vibration plate; 11, micro funnel; 12, sample tube control structure; 121, control switch; 122, sample tube controller; 123, compression spring; 124, retractable plate; 13, retractable sample tube; 14, sample tube; 15, fixed frame; 16, balance. DETAILED DESCRIPTION

[0036] The content of the present invention is further described in detail below in conjunction with the accompanying drawings and specific implementation methods.

[0037] Example

[0038] See also Figures 1 to 10 , which is a physical adsorption instrument sampling device, including a fixed frame 15, a sampling module, a vibration module, a displacement module and a balance 16; the fixed frame 15 is placed on the balance 16, and the sample tube 14 with a spherical bottom is fixed on the fixed frame 15 and perpendicular to the tray of the balance 16; the displacement module is arranged next to the balance 16, the vibration module includes an upper part and a lower part, the displacement module is installed on the lower part of the vibration module, and the upper part of the vibration module is installed on the displacement module and is controlled by the displacement module to achieve lifting or translation; the sampling module is located above the sample tube 14 and is aligned with the tube mouth of the sample tube 14, and the sampling module is installed on the upper part of the vibration module and realizes sampling with the vibration of the vibration module.

[0039] The sampling module includes a micro funnel 11, a retractable sample tube 13, and a sample tube control structure 12 for controlling the start or stop of the retractable sample tube 13; the upper end of the retractable sample tube 13 is connected to the outlet at the bottom of the micro funnel 11, and the lower end of the retractable sample tube 13 is freely retracted to enter the bottom of the straight tube wall of the sample tube 14; the sample tube control structure 12 is installed at the lower end of the micro funnel 11.

[0040] The micro funnel 11 and the retractable sample receiving tube 13 are both made of non-charged nanomaterials, and the inner wall of the retractable sample receiving tube 13 has a smooth surface. The inner wall of the retractable sample receiving tube 13 has a smooth surface, which can prevent the sample from adhering to its surface.

[0041] The upper part of the vibration module includes the upper chassis 6 of the bracket, the vibration bracket 7, the vibration machine base 8, the vibration machine 9 and the vibration plate 10; the lower part of the vibration module includes the vibration-damping foot cup 1, the lower chassis 2 of the bracket and the vibration controller 3 for controlling the operation of the vibration module; one end of the vibration plate 10 is embedded in the micro-funnel 11, and the bottom of the other end is embedded in the top of one end of the vibration machine 9, and the bottom of the other end of the vibration machine 9 is installed on the vibration machine base 8, the bottom of the vibration machine base 8 is fixed to the upper end of the vibration bracket 7, and the lower end of the vibration bracket 7 is fixed to the upper chassis 6 of the bracket; the upper chassis 6 of the bracket is installed on the displacement module, and the displacement module is installed on the lower chassis 2 of the bracket, and the vibration controller 3 is installed on the upper side of the lower chassis 2 of the bracket, and the bottom of the lower chassis 2 of the bracket is installed with a vibration-damping foot cup 1. The vibration-damping foot cup 1 is used to reduce shock.

[0042] There are four vibration brackets 7, which are evenly distributed at the bottom of the vibration machine 9; there are four vibration-damping foot cups 1, which are evenly distributed at the bottom of the chassis 2 under the bracket.

[0043] The displacement module includes a horizontal moving platform 5 and a vertical lifting platform 4; the horizontal moving platform 5 includes an upper linear guide slide 51 and a lower linear guide slide 52, the two linear guide slides are vertically assembled into a cross shape, the upper part of the vibration module is installed on the upper linear guide slide 51 and can slide along it, the upper linear guide slide 51 is installed on the lower linear guide slide 52 and can slide along it, the lower linear guide slide 52 is installed on the vertical lifting platform 4, and the vertical lifting platform 4 is installed on the lower part of the vibration module. The two linear guide slides are vertically assembled into a cross shape, which can realize the translation of the upper part of the vibration module to the front, back, left and right, and accurately control the displacement.

[0044] The sample tube control structure 12 includes a control component chassis and a control switch 121, a sample tube controller 122, a compression spring 123, and a retractable plate 124 installed on the control component chassis; the control component chassis is connected to the bottom side wall of the micro funnel 11, the control switch 121 is installed on the sample tube controller 122 and is used to control its on and off, and a retractable plate 124 and a compression spring 123 are installed under the sample tube controller 122, one end of the compression spring 123 is fixed on the sample tube controller 122, and the other end of the compression spring 123 is fixed on the retractable plate 124; as the control switch 121 is opened and closed, the retractable plate 124 moves against the retractable sample tube 13 under the extension action of the compression spring 123 and clamps it, or the retractable plate 124 releases the retractable sample tube 13 under the compression action of the compression spring 123 and releases its restriction. After the control switch 121 is turned on, the sample tube controller 122 releases the restriction on the compression spring 123, and the compression spring 123 drives the retractable plate 124 to move the retractable sample tube 13 and clamp it so that things cannot fall down; after the control switch 121 is turned off, the sample tube controller 122 drives the compression spring 123 to compress and retract it, thereby releasing the restriction on the retractable plate 124 on the retractable sample tube 13, and the retractable sample tube 13 is connected to the micro funnel 11, and the retractable sample tube 13 automatically falls to the bottom of the sample tube 14.

[0045] The upper linear guide slide 51 and the lower linear guide slide 52 are linear guide slides with the same structure. The upper linear guide slide 51 includes a first ball screw 514, a first nut, a first control handle 511, a first locking clamp 512 for locking the first ball screw 514, a first supporting structure 513 and a first screw ball seat; the first supporting structure 513 includes a first guide rod and a first positioning plate. The first positioning plates are provided with two pieces, each of which has a hole in the center. A first screw ball seat is installed in the hole of each first positioning plate, and the two ends of the first ball screw 514 are respectively inserted into the first screw ball seat; one end of the first ball screw 514 extends outward from the outside of the first positioning plate, and the first control handle 511 is installed on the end; the first locking clamp 512 is fixed on the stop cover or bearing cover of the first supporting structure 513; the first nut is sleeved on the first ball screw 514; the first supporting structure 513 is installed Installed on the vertical lifting platform 4; the lower linear guide slide 52 includes a second ball screw 524, a second nut, a second control handle 521, a second locking clamp 522 for locking the second ball screw 524, a second supporting structure 523 and a second screw ball seat; the second supporting structure 523 includes a second guide rod and a second positioning plate, and the second positioning plate is provided with two pieces, each of which has a hole in the center, and a second screw ball seat is installed in the hole of each second positioning plate, and the two ends of the second ball screw 524 are respectively inserted into the second screw ball seat; one end of the second ball screw 524 extends outward from the outside of the second positioning plate, and the second control handle 521 is installed on the end; the second locking clamp 522 is fixed on the stop cover or bearing cover of the second supporting structure 523; the second nut is sleeved on the second ball screw 524; the second supporting structure 523 is installed on the first nut, and the chassis 6 on the bracket is installed on the second nut. In this embodiment, the ball screw is made of high-precision alloy steel, the nut is made of copper, and the supporting structure is made of cast iron. In this embodiment, the first nut, the second nut, the first screw ball seat, and the second screw ball seat are not shown in the figure. They are all existing equipment and no specific structural analysis is required.

[0046] The vertical lifting platform 4 includes a scissor upper bracket 41, a scissor lower bracket 44, a bearing 42, a fixed shaft 47, an upper fixed plate 45, a lower fixed plate 46, a screw and a third control handle 43 installed at the end of the screw; both sides of the lower fixed plate 46 are provided with scissor lower brackets 44, the scissor lower brackets 44 located on the same side include a fixed lower bracket and a movable lower bracket arranged crosswise, the lower fixed plate 46 is provided with a lower movable groove, the lower end of the fixed lower bracket is hinged to the lower fixed plate 46 through the bearing 42, and the lower end of the movable lower bracket is movably clamped in the lower movable groove through the bearing 42 and can slide along it; both sides of the upper fixed plate 45 are provided with scissor upper brackets 41, the scissor upper brackets 41 located on the same side include a fixed upper bracket and a movable upper bracket arranged crosswise, the upper fixed plate 45 is provided with an upper movable groove, and the upper end of the fixed upper bracket is provided with a movable groove. The end is hinged on the upper fixed plate 45 through a bearing 42, and the lower end of the movable upper bracket is movably clamped in the upper movable groove through the bearing 42 and can slide along it; the lower movable groove is opposite to the upper movable groove; the bearing 42 includes a first bearing and a second bearing, and in the scissor upper bracket 41 and the scissor lower bracket 44 on the same side, the lower end of the fixed upper bracket is hinged to the upper end of the fixed lower bracket through the first bearing, and the lower end of the movable upper bracket is hinged to the upper end of the movable lower bracket through the second bearing; the two first bearings on both sides of the vertical lifting platform 4 are connected together through the same fixed shaft 47, and the two second bearings on both sides of the vertical lifting platform 4 are connected together through the same fixed shaft 47; the fixed shaft 47 is provided with a threaded hole, and the two ends of the screw are respectively inserted into the threaded holes of the two fixed shafts 47. By turning the third control handle 43, the height of the injection module can be accurately adjusted up and down. The thread directions of the threaded holes of the two fixed shafts 47 are opposite. In this embodiment, the first supporting structure 513 is installed on the upper side of the upper fixing plate 45, and the lower fixing plate 46 is installed on the upper side of the lower chassis 2 of the bracket.

[0047] A method for using a sample introduction device of a physical adsorption instrument, characterized in that it comprises the following steps:

[0048] Step 1: After the balance 16 is self-calibrated, it is placed on the fixing frame 15, the balance 16 is reset to zero, and the sample tube 14 is placed on the fixing frame 15, and then the reading is read and recorded;

[0049] Step 2: Use the handle of the linear guide slide to adjust the left-right displacement and the front-back displacement of the sample injection module so that the outlet of the sample injection micro funnel 11 is vertically aligned with the tube mouth of the sample tube 14; start the sample tube control structure 12 to make the retractable sample tube 13 vertically extend into the sample tube 14, and then control the vertical lifting platform 4 to adjust the height of the retractable sample tube 13 so that it is parallel to the bottom end of the tube wall of the sample tube 14;

[0050] Step 3: Pour a small amount of sample powder into the micro funnel 11, start the vibration controller 3, and turn off the vibration controller 3 for 3 to 8 seconds. Start the sample receiving tube control structure 12 and retract the retractable sample receiving tube 13;

[0051] Step 4: Read the 16 reading on the balance and record it.

[0052] Example 1

[0053] (1) After the electronic balance 16 is self-calibrated, it is placed on the fixing frame 15, the balance 16 is reset to zero, and the long-necked spherical sample tube 14 is placed on the fixing frame 15, and then the reading is read, and the reading is recorded as 18.1719 grams;

[0054] (2) adjusting the left-right displacement and the front-back displacement of the sample injection module by the first control handle 511 / the second control handle 521 of the linear guide slide, so that the outlet of the micro-funnel 11 is vertically aligned with the tube mouth of the long-necked spherical sample tube 14; closing the control switch 121 of the sample tube control structure 12, so that the retractable sample tube 13 is vertically extended into the long-necked spherical sample tube 14, and then controlling the third control handle 43 of the vertical lifting platform 4 to adjust the height of the retractable sample tube 13 so that it is parallel to the bottom end of the tube wall of the long-necked spherical sample tube 14;

[0055] (3) Pour a small amount of sample powder into the micro funnel 11, start the vibrator 9, and turn off the vibrator 9 for 3 to 8 seconds. Start the control switch 121 of the sample receiving tube control structure 12 to retract the retractable sample receiving tube 13;

[0056] (4) Read the balance 16 and record 18.2031 grams.

[0057] Example 2

[0058] (1) After the electronic balance 16 is self-calibrated, a weighing paper is placed on it, the balance 16 is reset to zero, a small amount of ultra-light sample powder of a carbon-based lithium battery material is placed with a key, the balance 16 is read, 0.0688 g is recorded, and the weighing paper is taken away.

[0059] The balance 16 is returned to zero, and the holder 15 is placed on the balance 16. The long-necked spherical sample tube 14 is then placed on the holder 15, and then the reading is read, and the reading is recorded as 18.1728 grams;

[0060] (2) adjusting the left-right displacement and the front-back displacement of the sample injection module by the first control handle 511 / the second control handle 521 of the linear guide slide, so that the outlet of the micro-funnel 11 is vertically aligned with the tube mouth of the long-necked spherical sample tube 14; closing the control switch 121 of the sample tube control structure 12, so that the retractable sample tube 13 is vertically extended into the long-necked spherical sample tube 14, and then controlling the third control handle 43 of the vertical lifting platform 4 to adjust the height of the retractable sample tube 13 so that it is parallel to the bottom end of the tube wall of the long-necked spherical sample tube 14;

[0061] (3) Pour a small amount of sample powder into the micro funnel 11, start the vibrator 9, and turn off the vibrator 9 for 3 to 8 seconds. Start the control switch 121 of the sample receiving tube control structure 12 to retract the retractable sample receiving tube 13;

[0062] (4) Read the balance 16 and record 18.2413 grams.

[0063] (5) The error of the sample injection device of this physical adsorption instrument = (18.2413-18.1728) / 0.0688*100% = 99.5%.

[0064] The above detailed description is a specific description of a feasible embodiment of the present invention. The embodiment is not intended to limit the patent scope of the present invention. Any equivalent implementation or modification that does not deviate from the present invention should be included in the patent scope of this case.

Claims

1. A physical adsorption instrument sampling device, characterized in that: The invention comprises a fixing frame, a sampling module, a vibration module, a displacement module and a balance; the fixing frame is placed on the balance, a sample tube with a spherical bottom is fixed on the fixing frame and is perpendicular to the balance tray; the displacement module is arranged beside the balance, the vibration module comprises an upper part and a lower part, the displacement module is mounted on the lower part of the vibration module, the upper part of the vibration module is mounted on the displacement module and is controlled by the displacement module to achieve lifting or translation; the sampling module is located above the sample tube and is aligned with the tube mouth of the sample tube, the sampling module is mounted on the upper part of the vibration module and achieves sample loading as the vibration of the vibration module is achieved.

2. The physical adsorption instrument sampling device according to claim 1, characterized in that: The sample injection module includes a micro-funnel, a retractable sample tube, and a sample tube control structure for controlling the start or stop of the retractable sample tube; the upper end of the retractable sample tube is connected to the outlet at the bottom of the micro-funnel, and the lower end of the retractable sample tube is freely retracted to enter the bottom of the straight tube wall of the sample tube; the sample tube control structure is installed at the lower end of the micro-funnel.

3. The physical adsorption instrument sampling device according to claim 2, characterized in that: The micro funnel and the retractable sample receiving tube are both made of non-charged nano materials, and the inner wall of the retractable sample receiving tube has a smooth surface.

4. The physical adsorption instrument sampling device according to claim 2, characterized in that: The upper part of the vibration module includes a chassis on the bracket, a vibration bracket, a vibration machine base, a vibration machine and a vibration plate; the lower part of the vibration module includes a vibration-damping foot cup, a chassis under the bracket and a vibration controller for controlling the operation of the vibration module; one end of the vibration plate is embedded in the micro-funnel, and the bottom of the other end is embedded in the top of one end of the vibration machine, and the bottom of the other end of the vibration machine is installed on the vibration machine base, the bottom of the vibration machine base is fixed to the upper end of the vibration bracket, and the lower end of the vibration bracket is fixed to the chassis on the bracket; the chassis on the bracket is installed on the displacement module, and the displacement module is installed on the chassis under the bracket, the vibration controller is installed on the upper side of the chassis under the bracket, and the vibration-damping foot cup is installed at the bottom of the chassis under the bracket.

5. The physical adsorption instrument sampling device according to claim 4, characterized in that: There are four vibration brackets, which are evenly distributed at the bottom of the vibration machine; there are four vibration-damping foot cups, which are evenly distributed at the bottom of the chassis under the brackets.

6. The physical adsorption instrument sample introduction device according to claim 4, characterized in that: The displacement module includes a horizontal moving table and a vertical lifting table; the horizontal moving table includes an upper linear guide slide and a lower linear guide slide, and the two linear guide slides are vertically assembled into a cross shape. The upper part of the vibration module is installed on the upper linear guide slide and can slide along it, the upper linear guide slide is installed on the lower linear guide slide and can slide along it, the lower linear guide slide is installed on the vertical lifting table, and the vertical lifting table is installed on the lower part of the vibration module.

7. The physical adsorption instrument sample introduction device according to claim 6, characterized in that: The sample tube control structure includes a control component chassis and a control switch, a sample tube controller, a compression spring, and a retractable plate installed on the control component chassis; the control component chassis is connected to the bottom side wall of the micro funnel, the control switch is installed on the sample tube controller and is used to control its on and off, the retractable plate and the compression spring are installed under the sample tube controller, one end of the compression spring is fixed to the sample tube controller, and the other end of the compression spring is fixed to the retractable plate; as the control switch is opened and closed, the retractable plate moves against the retractable sample tube and clamps it under the extension action of the compression spring, or the retractable plate releases the movement of the retractable sample tube and releases its restriction under the compression action of the compression spring.

8. The physical adsorption instrument sample introduction device according to claim 6, characterized in that: The upper linear guide slide and the lower linear guide slide are linear guide slides with the same structure, and the upper linear guide slide includes a first ball screw, a first nut, a first control handle, a first locking clamp for locking the first ball screw, a first supporting structure and a first screw ball seat; the first supporting structure includes a first guide rod and a first positioning plate, the first positioning plate is provided with two pieces, each of which has a hole in the center, and the first screw ball seat is installed in the hole of each first positioning plate, and the two ends of the first ball screw are respectively inserted into the first screw ball seat; one end of the first ball screw extends outward from the outside of the first positioning plate, and the first control handle is installed on the end; the first locking clamp is fixed on the stop cover or bearing cover of the first supporting structure; the first nut is sleeved on the first ball screw; the first supporting structure is installed in the A vertical lifting platform; the lower linear guide slide includes a second ball screw, a second nut, a second control handle, a second locking clamp for locking the second ball screw, a second supporting structure and a second screw ball seat; the second supporting structure includes a second guide rod and a second positioning plate, the second positioning plate is provided with two pieces, each of which has a hole in the center, and the second screw ball seat is installed in the hole of each second positioning plate, and the two ends of the second ball screw are respectively inserted into the second screw ball seat; one end of the second ball screw extends outward from the outside of the second positioning plate, and the second control handle is installed on the end; the second locking clamp is fixed on the stop cover or the bearing cover of the second supporting structure; the second nut is sleeved on the second ball screw; the second supporting structure is installed on the first nut, and the chassis on the bracket is installed on the second nut.

9. The physical adsorption instrument sample introduction device according to claim 6, characterized in that: The vertical lifting platform comprises an upper scissors-type bracket, a lower scissors-type bracket, a bearing, a fixed shaft, an upper fixed plate, a lower fixed plate, a screw and a third control handle installed at the end of the screw; the lower scissors-type brackets are provided on both sides of the lower fixed plate, and the lower scissors-type brackets located on the same side include a fixed lower bracket and a movable lower bracket arranged crosswise, the lower fixed plate is provided with a lower movable groove, the lower end of the fixed lower bracket is hinged to the lower fixed plate through a bearing, and the lower end of the movable lower bracket is movably clamped in the lower movable groove through a bearing and can slide along it; the upper scissors-type brackets are provided on both sides of the upper fixed plate, and the upper scissors-type brackets located on the same side include a fixed upper bracket and a movable upper bracket arranged crosswise, the upper fixed plate is provided with an upper movable groove, the upper end of the fixed upper bracket is hinged to the upper fixed plate through a bearing, and the lower end of the movable upper bracket is movably clamped in the upper movable groove through a bearing and can slide along it; The lower movable groove is positioned opposite to the upper movable groove; the bearing includes a first bearing and a second bearing, and in the scissors upper bracket and the scissors lower bracket located on the same side, the lower end of the fixed upper bracket is hinged to the upper end of the fixed lower bracket through the first bearing, and the lower end of the movable upper bracket is hinged to the upper end of the movable lower bracket through the second bearing; the two first bearings located on both sides of the vertical lifting platform are connected together through the same fixed shaft, and the two second bearings located on both sides of the vertical lifting platform are connected together through the same fixed shaft; the fixed shaft is provided with a threaded hole, and the two ends of the screw are respectively inserted into the threaded holes of the two fixed shafts.

10. A method for using the physical adsorption instrument sample introduction device according to any one of claims 6 to 9, characterized in that: The steps include: Step 1: After the balance is self-calibrated, put it on the fixing frame, return the balance to zero, put the sample tube on the fixing frame, and then read the reading and record it; Step 2: Use the handle of the linear guide slide to adjust the left and right displacement and the front and back displacement of the injection module so that the outlet of the injection micro funnel is vertically aligned with the tube opening of the sample tube; start the sample tube control structure to make the retractable sample tube vertically extend into the sample tube, and then control the vertical lifting platform to adjust the height of the retractable sample tube so that it is parallel to the bottom end of the tube wall of the sample tube; Step 3: Pour a small amount of sample powder into the micro funnel, start the vibration controller, and turn it off for 3 to 8 seconds. Start the sample tube control structure and retract the retractable sample tube; Step 4: Read the balance and write it down.

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