Pretreatment equipment for solid sample

Abstract

The invention relates to the technical field of chemical analysis, and provides pretreatment equipment for a solid sample, the pretreatment equipment comprises a digestion container, a heating device and a shaking device, the digestion container is provided with a digestion cavity, and the solid sample and a digestion reagent are both contained in the digestion cavity; a heating groove with an upward opening is formed in the heating device; the shaking device comprises a support frame and a vibration mechanism, the digestion container is placed on the support frame, the vibration mechanism is connected with the support frame, and the vibration mechanism drives the support frame to move in the vertical direction, so that the digestion container enters or is separated from the heating tank; and the vibration mechanism drives the support frame to drive the digestion container to oscillate along a direction vertical to the up-down direction. The circumferential wall face and the bottom wall face of the heating groove can both emit heat to heat the digestion container located in the heating groove, the heating uniformity is better, the vibration structure does not need to drive the heating device and the digestion container to vibrate synchronously, and the reliability is improved.

Description

Technical Field

[0001] The present application relates to the technical field of chemical analysis, and in particular to a pre-treatment device for solid samples. Background Art

[0002] This section is intended to provide a background or context to the embodiments of the present application. No description herein is admitted to be prior art by virtue of its inclusion in this section.

[0003] In the radiochemical analysis of transuranic nuclides such as strontium-90, plutonium-238, plutonium-239, and neptunium-237 in solid samples such as soil and marine sediments, the pretreatment process of solid samples such as soil and marine sediments is the front-end process of the entire analysis method. Solid samples are usually digested by acid leaching to achieve pretreatment of solid samples. The operation process is relatively cumbersome and complicated, and the processing time accounts for 1 / 3 of the entire analysis process.

[0004] In the related art, during the acid leaching digestion process of solid samples, the solid samples and the digestion reagent are placed in a beaker, and the beaker is placed on a flat electric heating plate for heating. The flat electric heating plate is used to heat the beaker from the bottom to complete the acid leaching digestion of the solid samples, which results in uneven heating and easy splashing of the solution. Summary of the invention

[0005] In view of this, an embodiment of the present application hopes to provide a solid sample pretreatment device with better heating uniformity.

[0006] The present application provides a solid sample pretreatment device for pretreatment of radiochemical analysis of solid samples, the pretreatment device comprising:

[0007] A digestion container, comprising a digestion cavity, wherein the solid sample and the digestion reagent are both contained in the digestion cavity;

[0008] A heating device, forming a heating tank opening upward;

[0009] The shaking device includes a support frame and a vibration mechanism, the digestion container is placed on the support frame, the vibration mechanism is connected to the support frame, the vibration mechanism drives the support frame to move in the up and down directions, so that the digestion container enters or leaves the heating tank, and when the digestion container is in a state of leaving the heating tank, the vibration mechanism drives the support frame to drive the digestion container to oscillate in a direction perpendicular to the up and down directions.

[0010] In some embodiments, the support frame includes a support plate, the support plate is located above the heating device, the support plate forms a placement hole, and the digestion container is placed in the placement hole.

[0011] In some embodiments, the vibration mechanism includes a power source and a transmission rod, the transmission rod extends in the up-down direction, the upper end of the transmission rod is connected to the support frame, and the lower end of the transmission rod is connected to the power source, and the power source drives the transmission rod to move in the up-down direction and oscillate in a direction perpendicular to the up-down direction.

[0012] In some embodiments, the pretreatment equipment includes a cover assembly and a gripping device, the gripping device includes a clamp, the digestion container has an inlet connected to the digestion chamber, the clamp can grasp or release the cover assembly, and the cover assembly is used to close or open the inlet.

[0013] In some embodiments, the cover assembly includes a mounting frame and a plurality of cover bodies, the number of the digestion containers is multiple, each digestion container corresponds to a cover body, the plurality of cover bodies are all disposed on the mounting frame, and the clamp can grasp or release the mounting frame.

[0014] In some embodiments, the mounting frame is formed with ventilation holes.

[0015] In some embodiments, the mounting frame includes a handle, and the clamp includes two clamping members, the two clamping members can approach each other to grab the handle, and the two clamping members can move away from each other to release the handle.

[0016] In some embodiments, the handle includes a lifting portion, and the clamping member includes a connecting plate and two clamping plates, the two clamping plates are arranged on the connecting plate at intervals along the up and down directions, and the clamping plates of the two clamping members are opposite to each other; the lifting portion enters between the two clamping plates to grab the handle; the lifting portion escapes from the two clamping plates to release the handle.

[0017] In some embodiments, the gripping device includes a lifting mechanism connected to the clamping claw, the clamping claw is located above the handle, and the lifting mechanism drives the clamping claw to move in an up-and-down direction.

[0018] In some embodiments, the pre-treatment equipment includes a liquid adding device, and the liquid adding device is used to inject the digestion reagent into the digestion chamber.

[0019] In some embodiments, the liquid adding device includes a displacement mechanism and a liquid adding nozzle connected to the displacement mechanism, the displacement mechanism drives the liquid adding nozzle to move above the digestion container, and the liquid adding nozzle injects the digestion reagent into the digestion chamber.

[0020] In some embodiments, the displacement mechanism includes a translation structure and a telescopic structure, the telescopic structure connects the translation structure and the liquid adding nozzle, the translation structure drives the telescopic structure and the liquid adding nozzle to move in the left and right direction, and the telescopic structure drives the liquid adding nozzle to move in the front and back direction.

[0021] In some embodiments, the pretreatment equipment includes a collecting device, which is located on one side of the shaking device along the left and right direction. The shifting mechanism drives the liquid adding nozzle to move above the collecting device, and the liquid adding nozzle injects the digestion reagent into the collecting device.

[0022] In some embodiments, the liquid adding device includes a liquid adding pipe, a switching valve and multiple liquid inlet pipes, the switching valve has a liquid outlet and multiple liquid inlets, the liquid adding pipe connects the liquid outlet and the liquid adding nozzle, each of the liquid inlets is connected to one of the liquid inlet pipes, and the switching valve can selectively open or cut off the flow path between the liquid outlet and the liquid inlet.

[0023] In some embodiments, the pre-treatment equipment includes an ultrasonic volume-fixing device, which is disposed on the liquid adding device and is used to emit ultrasonic waves to obtain the height of the liquid level in the digestion chamber.

[0024] In some embodiments, the pre-treatment equipment includes a fume hood, the fume hood includes an operating space, the heating device and the shaking device are both located in the operating space, and the heating device is located below the support frame.

[0025] In the pre-treatment equipment provided by the embodiment of the present application, the circumferential wall and bottom wall of the heating tank can generate heat to heat the digestion container located therein, thereby increasing the heated area of ​​the digestion container. Each part of the digestion container can be more stably maintained at the reaction temperature required for digestion, and the heating uniformity is better, which can reduce the problem of solution splashing caused by uneven heating caused by local heating. The vibration mechanism can drive the support frame to drive the digestion container to move in the up and down directions, so that the digestion container enters or leaves the heating tank, reducing the safety risks caused by manual movement of the digestion container; when the digestion container is in a state of leaving the heating tank, the vibration mechanism drives the support frame to drive the digestion container to oscillate in a direction perpendicular to the up and down direction, which can avoid the interference of the heating tank with the oscillation of the digestion container, and the vibration structure does not need to drive the heating device and the digestion container to vibrate synchronously, thereby improving reliability. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 This is a schematic diagram of the structure of a solid sample pretreatment device in some embodiments of the present application;

[0027] Figure 2 for Figure 1 The enlarged schematic diagram at A in the middle;

[0028] Figure 3 for Figure 1 a schematic diagram of another view of the structure shown;

[0029] Figure 4 for Figure 3 The enlarged schematic diagram of point B in the middle;

[0030] Figure 5 This is a schematic diagram of the structure of the clamp in some embodiments of the present application;

[0031] Figure 6 for Figure 1 A schematic diagram of the structure shown in yet another perspective;

[0032] Figure 7 This is a cross-sectional view at CC.

[0033] Description of Reference Numerals

[0034] 1. Digestion container; 10. First module; 2. Heating device; 2a. Heating tank; 3. Shaking device; 31. Support frame; 311. Support plate; 311a. Placement hole; 32. Vibration mechanism; 321. Transmission rod; 4. Cover assembly; 41. Mounting frame; 41a. Ventilation hole; 411. Handle; 411a. Lifting part; 412. Mounting plate; 42. Cover; 5. Grasping device; 51. Clamping claw; 511. Clamping piece; 5111. Connecting plate; 5112. Card; 511a. Opening mouth; 52. Lifting mechanism; 6. Liquid adding device; 61. Shifting mechanism; 62. Liquid adding nozzle; 63. Switching valve; 64. Liquid pump; 7. Collecting device; 8. Fume hood; 8a. Operating space. DETAILED DESCRIPTION

[0035] The following is a further detailed description of the implementation of the present application in conjunction with the accompanying drawings and examples. The following examples are used to illustrate the present application but cannot be used to limit the scope of the present application.

[0036] The various specific technical features and embodiments described in the specific implementation methods can be combined in any suitable manner without contradiction. For example, different implementation methods can be formed by combining different specific technical features / embodiments. In order to avoid unnecessary repetition, the various possible combinations of the specific technical features / embodiments in this application are no longer described separately. In addition, the terms "first" and "second" are used for descriptive purposes only and cannot be understood as indicating or implying relative importance. The application is further described in detail below in conjunction with the accompanying drawings and specific embodiments.

[0037] It should be noted that the "multiple" in the embodiments of the present application includes two and more than two. Down refers to the direction toward the ground, and up is the direction opposite to down; front is the direction of the pre-processing device toward the operator during normal use, and back is the direction opposite to front; left is the direction of the operator's left hand during normal use of the pre-processing device, and right is the direction opposite to left. The up-down direction, the front-back direction, and the left-right direction together constitute a three-dimensional vertical coordinate system.

[0038] An embodiment of the present application provides a solid sample pretreatment device for pretreatment of solid samples for radiochemical analysis.

[0039] The pretreatment device provided in the embodiment of the present application can be used to digest solid samples, and the solid samples can be solids taken from the natural environment. For example, the solid samples include but are not limited to soil, stones, and marine sediments, etc. The solid samples are taken from the natural environment, and after being digested by the pretreatment device provided in the embodiment of the present application, the digestion products can be used for radiochemical analysis.

[0040] See also Figures 1 to 7 The pretreatment equipment includes a digestion container 1, a heating device 2 and a shaking device 3. The digestion container 1 has a digestion chamber, in which the solid sample and the digestion reagent are placed; the heating device 2 forms a heating tank 2a that opens upward. The shaking device 3 includes a support frame 31 and a vibration mechanism 32. The digestion container 1 is placed on the support frame 31, and the vibration mechanism 32 is connected to the support frame 31. The vibration mechanism 32 drives the support frame 31 to move in the up and down directions, so that the digestion container 1 enters or leaves the heating tank 2a. When the digestion container 1 is in a state of leaving the heating tank 2a, the vibration mechanism 32 drives the support frame 31 to drive the digestion container 1 to oscillate in a direction perpendicular to the up and down directions.

[0041] Specifically, the oscillation direction is perpendicular to the up-down direction, and the oscillation direction may be the front-back direction, the left-right direction, or other directions parallel to the horizontal plane.

[0042] The solid sample and the digestion reagent are both placed in the digestion chamber, and a digestion reaction occurs between the solid sample and the digestion reagent in the digestion chamber, so that the target substance in the solid sample is dissolved.

[0043] Exemplarily, the digestion reagent includes, but is not limited to, at least one of nitric acid, hydrofluoric acid, hydrochloric acid, perchloric acid, sulfuric acid, and hydrogen peroxide.

[0044] The solid sample reacts with a digestion reagent such as an acid and / or an oxidant to destroy the lattice structure and / or organic components in the solid sample, dissolve the target substance in the solid sample, and prepare a solution suitable for radiochemical analysis of radionuclides.

[0045] The type of radionuclides is not limited. For example, the radionuclides include, but are not limited to, transuranic nuclides such as strontium-90, plutonium-238, plutonium-239 or neptunium-237.

[0046] The heating tank 2a is used to place and heat the digestion container 1. The circumferential wall surface and the bottom wall surface of the heating tank 2a can generate heat to heat the digestion container 1 located therein, and the heating uniformity is better. Exemplarily, during the digestion process, the digestion container 1 can be heated by the heating tank 2a so that the solid sample and the digestion reagent are kept at the reaction temperature required for the digestion reaction, thereby promoting the acid leaching digestion of the solid sample. The heating device 2 can also be used to heat the digestion container 1 after digestion to realize the acid removal and evaporation process.

[0047] In some embodiments, the temperature of the heating tank 2a can be controlled within a range of 25°C (degrees Celsius) to 230°C, with a temperature control accuracy of ±1°C, which is beneficial for accurate control of the temperature during the digestion process.

[0048] Exemplarily, the digestion container 1 is placed on the support frame 31. When the digestion container 1 needs to be heated, the vibration mechanism 32 can drive the support frame 31 to move downward, and the support frame 31 drives the digestion container 1 to move downward until the digestion container 1 passes through the upward opening of the heating tank 2a and enters the heating tank 2a. When the digestion container 1 needs to be oscillated, the vibration mechanism 32 can drive the support frame 31 to move upward, and the support frame 31 drives the digestion container 1 to move upward until the digestion container 1 passes through the upward opening of the heating tank 2a and leaves the heating tank 2a. The wall surface of the heating tank 2a will not interfere with the oscillation of the digestion container 1, and the vibration mechanism 32 can drive the support frame 31 to drive the digestion container 1 to oscillate in a direction perpendicular to the up and down direction.

[0049] The digestion container 1 oscillates in a direction perpendicular to the up-down direction, which means that the digestion container 1 may oscillate in a front-to-back direction, a left-to-right direction, or other directions parallel to a horizontal plane.

[0050] The oscillation may be a reciprocating swing of the digestion container 1 so that the digestion container 1 moves in a limited movement space to disperse the solid sample and the digestion reagent to achieve the purpose of shaking.

[0051] In the pre-treatment equipment provided by the embodiment of the present application, the circumferential wall and bottom wall of the heating tank 2a can generate heat to heat the digestion container 1 located therein, thereby increasing the heated area of ​​the digestion container 1. Each part of the digestion container 1 can be more stably maintained at the reaction temperature required for digestion, and the heating uniformity is better, which can reduce the problem of solution splashing caused by uneven heating caused by local heating. The vibration mechanism 32 can drive the support frame 31 to drive the digestion container 1 to move in the up and down directions, so that the digestion container 1 enters or leaves the heating tank 2a, reducing the safety risks caused by manual movement of the digestion container 1; when the digestion container 1 is in a state of leaving the heating tank 2a, the vibration mechanism 32 drives the support frame 31 to drive the digestion container 1 to oscillate in a direction perpendicular to the up and down direction, which can avoid the interference of the heating tank 2a with the oscillation of the digestion container 1, and the vibration structure does not need to drive the heating device 2 and the digestion container 1 to vibrate synchronously, thereby improving reliability.

[0052] For some examples, see Figure 1 , Figure 2 and Figure 7 The number of digestion containers 1 and the number of heating tanks 2a are both multiple, and each heating tank 2a corresponds to a digestion container 1. Such a design can increase the number of solid samples processed in batches and improve processing efficiency.

[0053] In some embodiments, the plurality of digestion containers 1 may be arranged in a matrix. That is, a portion of the plurality of digestion containers 1 are arranged in rows at intervals along the left-right direction, and a plurality of rows of digestion containers 1 are arranged at intervals along the front-back direction. Exemplarily, the number of digestion containers 1 may be 12, and the 12 digestion containers 1 are arranged in a matrix.

[0054] Exemplarily, the plurality of heating slots 2a may be arranged in a matrix. That is, a portion of the plurality of heating slots 2a are arranged in rows at intervals along the left-right direction, and the plurality of rows of heating slots 2a are arranged at intervals along the front-back direction. Exemplarily, the number of the heating slots 2a may be 12, and the 12 heating slots 2a are arranged in a matrix.

[0055] For some examples, see Figure 3 and Figure 4 The pre-treatment equipment includes a fume hood 8, the fume hood 8 includes an operating space 8a, the heating device 2 and the shaking device 3 are both located in the operating space 8a, and the heating device 2 is located below the support frame 31.

[0056] In this embodiment, the heating device 2 is located below the support frame 31, which is convenient for the support frame 31 to move up and down to enter and exit the heating tank 2a. The space above the heating device 2 is open and relatively high, so that the support frame 31 can drive the digestion container 1 to oscillate, and it is also convenient for operators to check the working condition of the shaking device 3. The fume hood 8 can provide an exhaust function, which can exhaust the volatilized digestion reagent and the generated gas from the operating space 8a to improve safety.

[0057] In some embodiments, the pre-treatment equipment includes a fan, an exhaust channel and an exhaust duct, and the side wall of the operation space 8a is formed with an exhaust port, the exhaust channel connects the fan and the exhaust port, and the exhaust duct connects the fan and the external pipeline. The exhaust port is connected to the operation space 8a, and the fan drives the air flow so that the air flow in the operation space 8a is discharged from the fume hood 8 through the exhaust port, the exhaust channel, the fan and the exhaust duct. The exhaust channel and the exhaust duct can collect the acid waste liquid generated by the digestion process; the connection parts of the fan, the exhaust channel and the exhaust duct can be sealed to prevent acid mist from corroding the instrument lines and pipelines.

[0058] In some embodiments, the pre-treatment device includes a cover, and the fume hood 8 has an operation port that opens forward. The operation port is connected to the operation space 8a. The cover is used to selectively open or close the operation port. The operator can take and place the digestion container 1 through the operation port. The fume hood 8 can be in a closed state when in use, and the cover can improve safety.

[0059] The cover can be made of polycarbonate or other materials that are resistant to acid and alkali corrosion.

[0060] For some examples, see Figure 1 and Figure 7 , multiple digestion containers 1 distributed in a matrix form a first module 10, multiple heating tanks 2a distributed in a matrix form a second module, and each first module 10 corresponds to a second module. There are multiple first modules 10 and multiple second modules, and multiple first modules 10 are distributed at intervals along the left and right directions, and multiple second modules are distributed at intervals along the left and right directions. In this way, the size of a single first module 10 and a second module is moderate, which reduces the difficulty of manufacturing and maintenance. Multiple first modules 10 and multiple second modules increase the number of solid samples processed in a single batch, thereby improving efficiency.

[0061] In some embodiments, the wall surface of the heating tank 2a is covered with a Teflon layer, which has the property of being resistant to acid and alkali corrosion.

[0062] In some embodiments, the surface of the heating device 2 may be covered with a Teflon layer.

[0063] Exemplarily, the heating device 2 may include a graphite heating element, which forms a heating groove 2a. The graphite heating element has the characteristic of good heating uniformity, and the circumferential surface and the lower surface of the digestion container 1 may contact the heating groove 2a.

[0064] In some embodiments, the digestion container 1 is detachably placed on the support frame 31. In this way, the operator can remove the digestion container 1 from the support frame 31 to add solid samples to the digestion chamber or clean the digestion container 1, etc.

[0065] For some examples, see Figure 3 and Figure 4 The support frame 31 includes a support plate 311, the support plate 311 is located above the heating device 2, and the support plate 311 forms a placement hole 311a, and the digestion container 1 is placed in the placement hole 311a. Specifically, the placement hole 311a can penetrate the two end surfaces of the support plate 311 in the up and down direction. The support plate 311 has a simple structure, and the digestion container 1 is placed in the placement hole 311a, which is convenient for the digestion container 1 to enter or escape from the heating tank 2a.

[0066] For some examples, see Figures 1 to 4 The vibration mechanism 32 includes a power source and a transmission rod 321. The transmission rod 321 extends in the up-down direction. The upper end of the transmission rod 321 is connected to the support frame 31, and the lower end of the transmission rod 321 is connected to the power source. The power source drives the transmission rod 321 to move in the up-down direction and oscillate in a direction perpendicular to the up-down direction.

[0067] The power source and the transmission rod 321 can be connected through a transmission structure. The power source is used to provide power to drive the transmission rod 321 to move up and down and oscillate in a direction perpendicular to the up and down direction. The power source includes an oscillation motor, which can be used to drive the transmission rod 321 to oscillate in a direction perpendicular to the up and down direction.

[0068] For example, see Figure 1 , four vibration mechanisms 32 can be symmetrically arranged on the support frame 31.

[0069] In this embodiment, the power source is connected to the transmission rod 321, and the transmission rod 321 drives the support frame 31 to move up and down and oscillate in a direction perpendicular to the up and down directions. The transmission rod 321 is a rod-shaped structure extending in the up and down directions, which can increase the amplitude and enhance the oscillation effect.

[0070] In some embodiments, the first modules 10 correspond to the shaking devices 3 one by one. That is, the number of the first modules 10 is the same as the number of the shaking devices 3, and one shaking device 3 is used to match one first module 10.

[0071] In the related art, the leaching process of solid samples requires the use of a large amount of strong acid and oxidant. The acid mist generated by the open heating method of the heating plate will cause corrosion and contamination of the heating plate and other equipment.

[0072] For some examples, see Figures 1 to 5 The pretreatment equipment includes a cover assembly 4 and a gripping device 5, the gripping device 5 includes a clamp 51, the digestion container 1 has an inlet connected to the digestion chamber, the clamp 51 can grasp or release the cover assembly 4, and the cover assembly 4 is used to close or open the inlet.

[0073] The sample inlet can be used to add solid samples and / or digestion reagents, etc. to the digestion chamber.

[0074] Exemplarily, when the injection port needs to be closed, the clamp 51 can grab the cover assembly 4 and close the injection port with the cover assembly 4, and then release the cover assembly 4, so that the cover assembly 4 can be raised and lowered or oscillated together with the digestion container 1. When the injection port needs to be opened, the clamp 51 can grab the cover assembly 4 and remove the cover assembly 4 from the digestion container 1 to open the injection port.

[0075] In this embodiment, the cover assembly 4 closes the sample inlet, reducing the risk of strong acid and / or oxidant overflowing from the digestion chamber and the probability of structural parts being corroded and contaminated. The clamp 51 selectively grasps or releases the cover assembly 4, improving the degree of automation and reducing the risk of manual opening and closing of the cover assembly 4.

[0076] For some examples, see Figures 1 to 5 The cover assembly 4 includes a mounting frame 41 and a plurality of covers 42 . The number of digestion containers 1 is multiple, and each digestion container 1 corresponds to a cover 42 . The plurality of covers 42 are all disposed on the mounting frame 41 , and the clamp 51 can grasp or release the mounting frame 41 .

[0077] Exemplarily, the cover 42 can be detachably connected to the digestion container 1, for example, by snap connection, etc. In some embodiments, the cover 42 can be interference fit with the digestion container 1. In this way, the risk of the cover 42 being separated from the digestion container 1 under a small force can be reduced.

[0078] For example, the cover 42 may be made of PFA material. The cover 42 is resistant to acid and alkali corrosion.

[0079] In this embodiment, multiple digestion containers 1 can increase the number of solid samples processed in a single batch and improve processing efficiency. Multiple covers 42 are all arranged on the mounting frame 41, and the mounting frame 41 drives the multiple covers 42 to move synchronously, reducing the number of clamps 51 and simplifying the structure.

[0080] The fixing method of the cover body 42 and the mounting frame 41 is not limited, and the cover body 42 can be connected to the mounting frame 41 in an undetachable or detachable manner. The undetachable connection includes but is not limited to welding, bonding, etc., and the detachable connection includes but is not limited to snap connection or fastener connection, etc. The fastener includes but is not limited to screws or bolts, etc.

[0081] For some examples, see Figure 2 The mounting frame 41 is formed with a vent hole 41a. Exemplarily, the vent hole 41a can be a through hole. The volatilized digestion reagent in the digestion chamber and the gas generated by the digestion reaction can flow through the vent hole 41a, reducing the risk of the above-mentioned gas accumulating around the digestion container 1.

[0082] For some examples, see Figures 1 to 3 The mounting frame 41 includes a mounting plate 412, which is a flat plate structure, and the vent holes 41a can penetrate both end surfaces of the mounting plate 412 in the up-down direction. The mounting frame 41 has a simple structure and a light weight, so that the clamping claw 51 can grasp it easily.

[0083] For some examples, see Figures 1 to 5 The mounting frame 41 includes a handle 411 , and the clamping claw 51 includes two clamping members 511 . The two clamping members 511 can approach each other to grab the handle 411 , and the two clamping members 511 can move away from each other to release the handle 411 .

[0084] In this embodiment, the two clamping members 511 move relative to each other to grasp or release the handle 411, thereby grasping or releasing the mounting frame 41, which has a simple structure and is easy to implement.

[0085] For some examples, see Figures 1 to 5 The handle 411 includes a lifting portion 411a, and the clamping member 511 includes a connecting plate 5111 and two clamping plates 5112, the two clamping plates 5112 are arranged on the connecting plate 5111 at intervals along the up and down directions, and the clamping plates 5112 of the two clamping members 511 are opposite to each other; the lifting portion 411a enters between the two clamping plates 5112 to grab the handle 411; the lifting portion 411a escapes from the two clamping plates 5112 to release the handle 411.

[0086] That is, when the clamping member 511 grabs the handle 411 , the lifting portion 411 a is located between the two clamping plates 5112 ; when the clamping member 511 releases the handle 411 , the lifting portion 411 a escapes from the two clamping plates 5112 .

[0087] The clamping plates 5112 of the two clamping members 511 are opposite to each other, which means that the clamping plates 5112 of the two clamping members 511 face each other.

[0088] The two clamping plates 5112 have an opening 511 a at one side away from the connecting plate 5111 , and the lifting portion 411 a enters or escapes from between the two clamping plates 5112 through the opening 511 a .

[0089] When the handle 411 needs to be grasped, the two clamping members 511 are close to each other, and the lifting portion 411a enters between the two clamping plates 5112 through the opening 511a to complete the grasping. The two clamping plates 5112 are located on both sides of the lifting portion 411a along the up-down direction, and the two clamping plates 5112 limit the displacement of the lifting portion 411a along the up-down direction, thereby stabilizing the mobile mounting frame 41.

[0090] When the handle 411 needs to be released, the two clamping members 511 move away from each other, and the lifting portion 411 a escapes from between the two clamping plates 5112 through the opening 511 a, thereby completing the release.

[0091] In this embodiment, the handle 411 is grasped and released by the cooperation of the two clamping plates 5112 and the lifting part 411a, and the clamping member 511 has a simple structure and is easy to manufacture. The two clamping plates 5112 can limit the displacement of the lifting part 411a in the up and down directions, reduce the risk of the lifting part 411a falling off from the clamping member 511 due to shaking or impact, and have good reliability.

[0092] For some examples, see Figures 1 to 5 The grasping device 5 includes a lifting mechanism 52 connected to the clamping claw 51, and the clamping claw 51 is located above the handle 411. The lifting mechanism 52 drives the clamping claw 51 to move in the up and down direction.

[0093] Specifically, the two clamping members 511 are disposed on the same lifting mechanism 52 .

[0094] In this embodiment, the clamping jaw 51 is located above the handle 411, and the lifting mechanism 52 drives the clamping jaw 51 to move up and down to make the clamping jaw 51 close to or away from the handle 411. For example, when it is necessary to lift the cover body assembly 4 upward, the lifting mechanism 52 can drive the clamping jaw 51 to descend to the location of the handle 411, and the clamping jaw 51 grabs the handle 411, and the lifting mechanism 52 drives the clamping jaw 51 to rise to complete the action of lifting the cover body assembly 4 upward. When it is necessary to close the sample inlet, the lifting mechanism 52 drives the clamping jaw 51 and the cover body assembly 4 to descend together to close the sample inlet with the cover body assembly 4.

[0095] The specific structure of the lifting mechanism 52 is not limited. For example, the lifting mechanism 52 can adopt a linear motor or a cylinder, etc.

[0096] In some embodiments, the two clamping members 511 may be driven by a motor to move closer to or farther from each other.

[0097] For some examples, see Figures 1 to 3 The pre-treatment equipment includes a liquid adding device 6, which is used to inject a digestion reagent into the digestion chamber.

[0098] In this embodiment, the liquid adding device 6 can automatically inject the digestion reagent into the digestion chamber, reducing manual operations and improving convenience and safety.

[0099] For some examples, see Figures 1 to 3 The liquid adding device 6 includes a displacement mechanism 61 and a liquid adding nozzle 62 connected to the displacement mechanism 61. The displacement mechanism 61 drives the liquid adding nozzle 62 to move to the top of the digestion container 1, and the liquid adding nozzle 62 injects the digestion reagent into the digestion chamber. The displacement mechanism 61 can realize multi-degree-of-freedom movement, so that the liquid adding nozzle 62 moves to the top of any digestion container 1, and the digestion reagent is added to the digestion chamber through the injection port.

[0100] The specific structure of the shifting mechanism 61 is not limited, and the shifting mechanism 61 can be a mechanical arm with multiple joints or other mechanisms.

[0101] In some embodiments, the shifting mechanism 61 includes a translation structure and a telescopic structure. The telescopic structure connects the translation structure and the liquid adding nozzle 62. The translation structure drives the telescopic structure and the liquid adding nozzle 62 to move in the left and right direction, and the telescopic structure drives the liquid adding nozzle 62 to move in the front and back direction.

[0102] In this embodiment, the liquid adding nozzle 62 is driven to move in the left and right direction by the translation structure, and is driven to move in the front and back direction by the telescopic structure, so that the liquid adding nozzle 62 can move in different directions in the horizontal plane. The liquid adding nozzle 62 can be moved to the top of any digestion container 1, and the position of the digestion container 1 can be more diverse.

[0103] The specific structure of the translation structure is not limited. For example, the translation structure can use a motor, a cylinder, etc. as a driving source to drive the telescopic structure and the liquid adding nozzle 62 to move in the left and right directions.

[0104] The specific structure of the telescopic structure is not limited. For example, the telescopic structure can use a motor, a cylinder, etc. as a driving source to drive the liquid adding nozzle 62 to move in the front-to-back direction.

[0105] For some examples, see Figures 1 to 3 The pre-treatment equipment includes a collecting device 7, which is located on one side of the shaking device 3 along the left and right direction. The shifting mechanism 61 drives the liquid adding nozzle 62 to move to the top of the collecting device 7, and the liquid adding nozzle 62 injects the digestion reagent into the collecting device 7.

[0106] The collecting device 7 can collect waste liquid from the liquid filling nozzle 62 or residual liquid in the pipeline, etc.

[0107] Exemplarily, before the liquid adding nozzle 62 adds liquid to the digestion container 1 , there may be residual digestion reagent in the pipeline. The residual digestion reagent can be injected into the collecting device 7 first, and then new digestion reagent can be injected into the digestion container 1 after the residual digestion reagent in the pipeline is removed.

[0108] In this embodiment, the collecting device 7 and the shaking device 3 are arranged in the left-right direction, and the layout is more reasonable, which can avoid the collection device 7 and the shaking device 3 being arranged in the front-back direction to affect the operation of the operator, and can also avoid the collection device 7 and the shaking device 3 being arranged in the up-down direction to cause the movement mode of the shift mechanism 61 to be complicated. The collecting device 7 can be used to collect residual digestion reagents, reduce the influence of residual digestion reagents on the reaction, and improve the accuracy of the analysis results.

[0109] For some examples, see Figures 1 to 3The pretreatment equipment includes a liquid adding pipe, a switching valve 63 and multiple liquid inlet pipes. The switching valve 63 has a liquid outlet and multiple liquid inlets. The liquid adding pipe connects the liquid outlet and the liquid adding nozzle 62. Each liquid inlet is connected to a liquid inlet pipe. The switching valve 63 can selectively open or close the flow path between the liquid outlet and the liquid inlet.

[0110] The liquid inlet pipe is used to communicate with a reagent bottle containing a digestion reagent. Different digestion reagents are contained in different reagent bottles, and multiple liquid inlet pipes can be connected to multiple reagent bottles in a one-to-one correspondence.

[0111] The switching valve 63 can selectively open or close the flow path between the liquid outlet and the liquid inlet, that is, the switching valve 63 can open or close any liquid inlet, the flow path between the opened liquid inlet and the liquid outlet is opened, and the flow path between the closed liquid inlet and the liquid outlet is closed. The switching valve 63 can allow the digestion reagent of any liquid inlet to enter the liquid outlet and enter the digestion chamber through the liquid adding pipe and the liquid adding nozzle 62.

[0112] In this embodiment, multiple liquid inlet pipes can be connected to multiple reagent bottles containing digestion reagents. By controlling the switching valve 63, the digestion reagent in any liquid inlet pipe can enter the digestion chamber, thereby realizing automatic liquid injection of different digestion reagents and improving the degree of automation. The liquid inlet pipes do not affect each other, which to a certain extent avoids cross contamination during the digestion reagent injection process, reduces random errors, and improves the accuracy of the analysis results.

[0113] The type of the switching valve 63 is not limited. The switching valve 63 can be an electrically controlled valve so that the electronic control device can implement control. The liquid inlet of the switching valve 63 can be set according to demand. For example, the number of liquid inlets can be two, three, four or more. The number of liquid inlets and the number of liquid inlet pipes can be the same according to the type of digestion reagent. For example, if there are ten types of digestion reagents, there are ten liquid inlets and ten liquid inlet pipes.

[0114] In some embodiments, both the liquid adding tube and the liquid inlet tube may be made of PFA material. PFA, namely PerfluoroalkoxyAlkane, is a tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer, a perfluoroalkoxy resin.

[0115] For some examples, see Figures 1 to 3 The liquid adding pipe may be provided with a liquid pump 64, and the liquid pump 64 may be used to provide power to drive the flow of the digestion reagent.

[0116] The type of the liquid pump 64 is not limited. By way of example, the liquid pump 64 includes but is not limited to a peristaltic pump.

[0117] In some embodiments, before the digestion process begins, the peristaltic pump can be calibrated using a measuring cylinder to help ensure the accuracy of the amount of digestion reagent added.

[0118] For some examples, see Figures 1 to 3 , the switching valve 63 and the liquid pump 64 can be arranged outside the operation space 8a. For example, the switching valve 63 and the liquid pump 64 are arranged on the left side wall of the fume hood 8. In this way, it is not only convenient to operate the liquid inlet pipe, but also the risk of acid mist contacting the switching valve 63 and the liquid pump 64 can be reduced.

[0119] In some embodiments, the pre-treatment device includes an ultrasonic volume-fixing device, which is disposed on the liquid adding device 6 and is used to emit ultrasonic waves to obtain the height of the liquid level in the digestion chamber.

[0120] The ultrasonic volume setting device can emit ultrasonic waves and determine the height of the liquid level in the digestion chamber through the ultrasonic waves. The control device can control the liquid adding device 6 to add liquid to the digestion chamber to the set liquid level according to the liquid level information.

[0121] In this embodiment, the ultrasonic volume determination device does not contact the solution in the digestion chamber during the process of measuring the height of the liquid level, which can reduce contamination and improve accuracy.

[0122] In some embodiments, the ultrasonic volume determination device includes an ultrasonic generator and an ultrasonic receiver, wherein the ultrasonic generator is used to emit ultrasonic signals and the ultrasonic receiver receives ultrasonic signals. The ultrasonic receiver may be a micro-range low-power ultrasonic sensor. With this device, the volume determination accuracy is better than 1% (50 mL).

[0123] In some embodiments, the pre-treatment device includes a control device, and at least one of the heating device 2, the vibration mechanism 32, the gripping device 5, the displacement mechanism 61 and the ultrasonic volume setting device is electrically connected to the control device. The control device controls at least one of the heating device 2, the vibration mechanism 32, the gripping device 5, the displacement mechanism 61 and the ultrasonic volume setting device.

[0124] Exemplarily, the control device can be arranged outside the fume hood 8, for example, the control device can be arranged on a computer. All operations of the pre-treatment device are controlled by computer software. The software interface can be composed of multiple units, which run independently and complete the steps of establishing, calibrating, flushing, and constant volume of the method for using the pre-treatment device in sequence.

[0125] In this embodiment, the control device controls at least one of the heating device 2, the vibration mechanism 32, the gripping device 5, the displacement mechanism 61 and the ultrasonic volume setting device, thereby improving the degree of automation, reducing manual operation and supervision, and improving safety.

[0126] The following example illustrates the method of using the solid sample pretreatment device in the embodiment of the present application. Taking soil as an example, the solid sample can be weighed into a digestion container 1 for about 30 g of the pretreated soil sample, and 100 μL of Pu-242 (plutonium-242) standard solution (activity concentration is 0.074 Bq / mL, becquerel per microliter) is added as a tracer, and then 70 mL of 8 mol / L (moles per liter) nitric acid is added, shaken for 10 minutes, heated at about 150°C until the solution in the digestion chamber boils, and kept at a constant temperature for 30 minutes. In this way, the soil sample pretreatment is completed. The pre-treated digestion product can be used for radiochemical analysis of radionuclides. For example, the digestion container 1 can be removed from the support frame 31, the solution in the digestion chamber can be cooled and centrifuged, the supernatant can be collected in a 250 mL centrifuge tube, and the residue can be washed once with 40 ml of 8 mol / L nitric acid solution, and the supernatant and the washing solution can be combined. After adjusting the valence state of the combined solution, it is separated and purified by a chromatographic column, and the chemical recovery rate of Pu-242 is measured by an α spectrometer.

[0127] The following is a brief description of the workflow of the pre-treatment equipment, and the use effect of the pre-treatment equipment is verified by 8 soil samples. The specific instructions are as follows:

[0128] A detailed pre-treatment process can be set in the computer software. The basic setting conditions include: the added volume of the digestion reagent, the shaking time of the shaking device 3, the heating speed and reaction temperature of the heating device 2, and the digestion time, etc. Using a graphite heating element, the process of digesting 8 30g soil samples through the pre-treatment device provided in the embodiment of the present application is roughly as follows: open the cover 42, inject the digestion reagent into the digestion chamber, wherein the digestion reagent is 30mL of nitric acid, shake the shaking device 3 for 10 minutes, close the cover 42 after the shaking is completed, and the digestion container 1 is lowered into the heating tank 2a. The heating device 2 is heated to 100°C, the heating speed is full speed, the digestion time is 10min, that is, the constant temperature is 10min, and it is heated again to the reaction temperature of 150°C or 180°C, the heating speed is full speed, the digestion time is 40min, that is, the constant temperature is 40min or 60min, the digestion reaction is completed, and the digestion container 1 rises to be separated from the heating tank 2a. In this way, the digestion pre-treatment of the soil sample is completed. The above different soil samples can use the same or different reaction temperatures and digestion times. Please refer to Table 1 for the pretreatment results.

[0129] Table 1

[0130]

[0131] According to Table 1, the digestion temperature is 150℃~180℃, the digestion time is 40min~60min, and the Pu-242 chemical recovery rate of 30g soil sample digested by the pretreatment equipment provided in the embodiment of the present application is greater than 70%; at the same time, when the temperature is around 150℃, the solution in the digestion chamber is in a slightly boiling state; when the temperature is 180℃, the boiling degree of the solution is more intense. Compared with the heating method using electric heating plates in related technologies, the heating speed and range of the graphite block encircling heating method are faster and more uniform than the electric heating plate heating method, which is more conducive to the digestion of large-volume soil samples.

[0132] In the description of this specification, the description with reference to the terms "an embodiment", "some embodiments" and "exemplary" means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the embodiments of the present application. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art may combine and combine different embodiments or examples described in this specification and the features of different embodiments or examples, unless they are contradictory.

[0133] The various embodiments / implementations provided in this application can be combined with each other without causing any contradiction. The above description is only a preferred embodiment of this application and is not intended to limit this application. For those skilled in the art, this application may have various changes and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of this application shall be included in the protection scope of this application.

Claims

1. A solid sample pretreatment device, characterized in that: Pre-treatment for radiochemical analysis of solid samples, the pre-treatment equipment comprising: A digestion container, comprising a digestion cavity, wherein the solid sample and the digestion reagent are both contained in the digestion cavity; A heating device, forming a heating tank opening upward; The shaking device includes a support frame and a vibration mechanism, the digestion container is placed on the support frame, the vibration mechanism is connected to the support frame, the vibration mechanism drives the support frame to move in the up and down directions, so that the digestion container enters or leaves the heating tank, and when the digestion container is in a state of leaving the heating tank, the vibration mechanism drives the support frame to drive the digestion container to oscillate in a direction perpendicular to the up and down directions.

2. The pre-processing device according to claim 1, characterized in that: The support frame comprises a support plate, the support plate is located above the heating device, the support plate forms a placement hole, and the digestion container is placed in the placement hole.

3. The pre-processing device according to claim 1, characterized in that: The vibration mechanism includes a power source and a transmission rod, the transmission rod extends in the up-down direction, the upper end of the transmission rod is connected to the support frame, and the lower end of the transmission rod is connected to the power source, and the power source drives the transmission rod to move in the up-down direction and oscillate in a direction perpendicular to the up-down direction.

4. The pre-processing equipment according to claim 1, characterized in that: The pre-treatment equipment comprises a cover assembly and a gripping device, wherein the gripping device comprises a clamping claw, the digestion container has an injection port connected to the digestion chamber, the clamping claw can grasp or release the cover assembly, and the cover assembly is used to close or open the injection port.

5. The pre-processing device according to claim 4, characterized in that: The cover assembly includes a mounting frame and a plurality of covers. There are a plurality of digestion containers, each of which corresponds to a cover. The plurality of covers are arranged on the mounting frame, and the clamp can grasp or release the mounting frame.

6. The pre-processing device according to claim 5, characterized in that: The mounting frame is formed with a vent hole.

7. The pre-processing device according to claim 5, characterized in that: The mounting frame comprises a handle, and the clamping claw comprises two clamping members, the two clamping members can approach each other to grab the handle, and the two clamping members can move away from each other to release the handle.

8. The pre-processing device according to claim 7, characterized in that: The handle includes a lifting part, and the clamping member includes a connecting plate and two clamping plates, the two clamping plates are arranged on the connecting plate at intervals along the up and down directions, and the clamping plates of the two clamping members are opposite to each other; the lifting part enters between the two clamping plates to grab the handle; the lifting part escapes from the two clamping plates to release the handle.

9. The pre-processing device according to claim 7, characterized in that: The gripping device comprises a lifting mechanism connected to the clamping claw, the clamping claw is located above the handle, and the lifting mechanism drives the clamping claw to move in the up and down direction.

10. The pre-processing equipment according to claim 1, characterized in that: The pre-treatment equipment comprises a liquid adding device, and the liquid adding device is used to inject the digestion reagent into the digestion chamber.

11. The pre-processing device according to claim 10, characterized in that: The liquid adding device comprises a displacement mechanism and a liquid adding nozzle connected to the displacement mechanism. The displacement mechanism drives the liquid adding nozzle to move above the digestion container, and the liquid adding nozzle injects the digestion reagent into the digestion chamber.

12. The pre-processing device according to claim 11, characterized in that: The displacement mechanism includes a translation structure and a telescopic structure, wherein the telescopic structure connects the translation structure and the liquid adding nozzle, the translation structure drives the telescopic structure and the liquid adding nozzle to move in the left-right direction, and the telescopic structure drives the liquid adding nozzle to move in the front-back direction.

13. The pre-processing device according to claim 11, characterized in that: The pre-treatment equipment includes a collecting device, which is located on one side of the shaking device along the left-right direction. The shifting mechanism drives the liquid adding nozzle to move above the collecting device, and the liquid adding nozzle injects the digestion reagent into the collecting device.

14. The pre-processing device according to claim 11, characterized in that: The liquid adding device includes a liquid adding pipe, a switching valve and multiple liquid inlet pipes, the switching valve has a liquid outlet and multiple liquid inlets, the liquid adding pipe connects the liquid outlet and the liquid adding nozzle, each of the liquid inlets is connected to one of the liquid inlet pipes, and the switching valve can selectively open or cut off the flow path between the liquid outlet and the liquid inlet.

15. The pre-processing device according to claim 10, characterized in that: The pre-treatment equipment comprises an ultrasonic volume-fixing device, which is arranged on the liquid adding device and is used to emit ultrasonic waves to obtain the height of the liquid level in the digestion chamber.

16. The pre-treatment device according to any one of claims 1 to 15, characterized in that: The pre-treatment equipment comprises a fume hood, the fume hood comprises an operating space, the heating device and the shaking device are both located in the operating space, and the heating device is located below the support frame.

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