ICP (Inductively Coupled Plasma) pretreatment digestion system equipment

Abstract

The invention relates to the field of chemical analysis, and discloses ICP (inductively coupled plasma) pretreatment digestion system equipment, which comprises a reagent storage and conveying module, an ICP pretreatment module and an ICP pretreatment module, the digestion module is used for storing a digestion tube and can adjust the digestion temperature; the analysis module is used for determining the digestion degree by measuring the turbidity of the liquid in the digestion tube; the transfer module is used for selectively transferring the digestion tube into the digestion module or the analysis module; the electrical control module is electrically connected with the reagent storage and conveying module, the digestion module, the analysis module and the digestion transfer module respectively. The turbidity of the liquid in the digestion tube is analyzed by arranging the visual camera I, the digestion degree of the digestion sample can be effectively identified, and when the digestion sample is not completely digested, acid can be continuously added for digestion, so that part of insoluble substances are prevented from being remained, and the accuracy of an analysis result is improved.

Description

Technical Field

[0001] The invention relates to the field of chemical analysis, in particular to an ICP pre-treatment digestion system device. Background Art

[0002] In the cutting-edge field of contemporary chemical analysis, inductively coupled plasma (ICP) technology has become the mainstay of elemental analysis of various samples and is widely used in many scientific research and industrial practice scenarios. However, it cannot be ignored that the accuracy of ICP analysis results is to a large extent subject to the quality of sample pretreatment.

[0003] Traditional digestion processes are mostly dominated by manual operations, and operators need to complete a series of complicated steps step by step, such as reagent addition, sample mixing, heating digestion, and cooling. This not only makes the operation process lengthy and cumbersome, and the work efficiency is low, but also due to the inevitable differences in human operations, it is very easy to cause poor uniformity in sample processing, which in turn has a negative impact on the accuracy of the final ICP test results. Furthermore, the digestion process frequently involves corrosive and volatile chemical reagents, which undoubtedly poses a potential risk to the health of operators. In view of this, it is of far-reaching significance and urgent to focus on the research and development of an ICP pretreatment digestion system automation equipment that is highly efficient, highly automated, and low in pollution.

[0004] The patent with publication number CN112326406A discloses a graphite digestion robot and digestion method, including: a frame, a graphite furnace, which is arranged inside the frame and is used to heat the digestion tube; a lifting and oscillating mechanism, which is connected to the frame and is used to carry the digestion tube and can drive the digestion tube close to or away from the graphite furnace; a multi-channel sample adding mechanism, which is arranged on one side of the frame and is used to add reagents to the digestion tube, and the multi-channel sample adding mechanism includes a sample adding drive unit, one end of the sample adding drive unit is connected to a sample adding tube, and the sample adding tube is connected to a pump mechanism. The fully automatic graphite digestion device has a compact structure and a high degree of integration. The liquid adding and heating digestion processes can be automated, which significantly reduces labor costs and improves operation accuracy and safety. At the same time, the device has good corrosion resistance and can work uninterruptedly under high temperature and high corrosion experimental conditions.

[0005] However, after an in-depth study of the patent solution, it was found that it still has several shortcomings that need to be improved. First, this solution lacks the ability to effectively identify the degree of digestion of the digestion sample. In other words, it is impossible to accurately determine whether the digestion sample has been completely digested, which is very likely to cause some insoluble substances to remain, ultimately interfering with the accuracy of the analysis results. Second, a large amount of strong acid reagents will be used in the digestion process, but in the digestion process of this solution, no sealing measures or exhaust treatment are implemented for the digestion tube, causing the acid to easily evaporate to key structural parts such as the sample addition drive part, thereby causing structural corrosion problems. Summary of the invention

[0006] The present invention aims to provide an ICP pretreatment digestion system device to achieve rapid, complete, low-cost and environmentally friendly sample digestion, improve the accuracy and efficiency of ICP analysis, and both the digestion pretreatment and detection processes can be automatically controlled, and the entire experimental process does not require human participation, thereby avoiding various strong acids, especially hydrofluoric acid, from harming the human body;.

[0007] In order to achieve the above object, the technical solution of the present invention is:

[0008] An ICP pre-treatment digestion system device, comprising:

[0009] A reagent storage and delivery module for storing digestion reagents and constant volume reagents and selectively injecting them into the digestion tube;

[0010] A digestion module for storing the digestion tube and capable of adjusting the digestion temperature;

[0011] An analysis module for determining the degree of digestion by measuring the turbidity of the liquid in the digestion tube;

[0012] A transfer module for selectively transferring the digestion tube to the digestion module or the analysis module; and

[0013] An electrical control module electrically connected to the reagent storage and delivery module, the digestion module, the analysis module and the digestion transfer module respectively.

[0014] Furthermore, the analysis module includes:

[0015] An analysis module frame 1, on which a plurality of test tube racks are mounted, and the test tube racks are detachably connected to the digestion tubes; and

[0016] Analysis module frame 2, on which visual camera 1 and visual camera 2 are installed, the visual camera 1 and visual camera 2 are electrically connected to the electrical control module respectively, and are respectively arranged toward one of the test tube racks, the visual camera 1 is used to identify the turbidity of the liquid in the digestion tube, and the visual camera 2 is used to identify the height of the liquid level in the digestion tube.

[0017] Furthermore, the reagent storage and delivery module comprises:

[0018] Reagent storage racks; and

[0019] A plurality of reagent bottles and a pump mechanism are installed on the reagent storage rack, and the pump mechanism is used to inject the liquid in the reagent bottle into the digestion tube on the test tube rack.

[0020] Furthermore, the pump mechanism comprises:

[0021] A peristaltic pump installed on the reagent storage rack and electrically connected to the electrical control module, wherein the input end of the peristaltic pump is connected to one end of a liquid inlet pipe, the other end of the liquid inlet pipe is communicated with the reagent bottle, the output end of the peristaltic pump is connected to one end of a liquid outlet pipe, the other end of the liquid outlet pipe is connected to a sample addition tube, and the reagent bottle, the liquid inlet pipe, the peristaltic pump, the liquid outlet pipe and the sample addition tube are arranged in a one-to-one correspondence;

[0022] a plurality of liquid level sensors installed on the reagent storage rack and electrically connected to the electrical control module, wherein the liquid level sensors monitor the liquid level heights in the reagent bottles one by one; and

[0023] The analysis module frame body 2 is connected to a robotic arm via a horizontal linear module and a vertical linear module, and a plurality of sample adding tubes are mounted on the robotic arm, and the sample adding tubes are located above the test tube rack. The horizontal linear module and the vertical linear module are electrically connected to the electrical control module, respectively, and are used to drive the robotic arm to move in the horizontal direction and the vertical direction, respectively, so as to inject the digestion reagent and the constant volume reagent into the digestion tubes located at the test tube racks at different positions.

[0024] Furthermore, the analysis module also includes:

[0025] A waste liquid barrel installed on the analysis module frame 1, wherein the mechanical arm selectively drives the sample adding tube to move to the top of the waste liquid barrel; and

[0026] A code reader for identifying the identification code on the digestion tube, wherein the code reader is electrically connected to the electrical control module.

[0027] Furthermore, the digestion module comprises:

[0028] a graphite acid-removing instrument electrically connected to the electrical control module, wherein a digestion tube is detachably connected to the graphite acid-removing instrument for adjusting the digestion temperature, and a sealing cover is detachably connected to the top of the instrument; and

[0029] Absorption system used for filtering and absorbing acid mist.

[0030] Furthermore, the transfer module includes:

[0031] a lifting seat electrically connected to the electrical control module; and

[0032] A multi-joint robotic arm, one end of which is connected to the lifting seat and electrically connected to the electrical control module, the multi-joint robotic arm has multiple rotating joints, and the other end of the multi-joint robotic arm is provided with an electric gripper 1, the electric gripper 1 is electrically connected to the electrical control module, and the electric gripper 1 is provided with multiple grippers 1 that can rotate and can move closer to and away from each other.

[0033] Furthermore, it also includes:

[0034] A digestion tube storage rack for storing digestion tubes; and

[0035] The switch cover electric claw is provided with a fixing groove for inserting the lower end of the digestion tube, and an electric clamp 2 detachably connected to the lower end of the digestion tube, and the electric clamp 2 is electrically connected to the electrical control module.

[0036] Furthermore, the sealing cover is detachably connected to the upper end of the second analysis module frame, and a transfer knob is provided at the upper end of the sealing cover, and the transfer knob is detachably connected to the first clamping jaw.

[0037] Furthermore, it also includes a sealing cover arranged around the reagent storage and delivery module, the digestion module, the analysis module and the digestion and transfer module.

[0038] Compared with the prior art, the present invention has at least the following advantages:

[0039] In the present invention, a visual camera is set to analyze the turbidity of the liquid in the digestion tube, so that the digestion degree of the digested sample can be effectively identified. When the digestion is not complete, acid digestion can be continued to avoid the residue of some insoluble substances, thereby improving the accuracy of the analysis result.

[0040] In the present invention, by setting up an absorption system, the volatile strong acid reagents can be neutralized, the sealing cover is used to reduce interference with the outside world, the harmful components in the acid mist are effectively removed, the laboratory air is purified, and the safety of equipment and personnel is guaranteed.

[0041] The present invention realizes automatic digestion of the whole process of ICP pretreatment; automatically judges the digestion result in a visual way, and the automated visual inspection and judgment of the result improve the digestion completion efficiency; solves the problems of time-consuming, labor-intensive and labor-intensive chemical digestion, and modular processing of digestion samples in the same experimental environment improves the efficiency, which has high social applicability value; in addition, the automated and process-based digestion improves the safety of chemical digestion, eliminates the interference of human factors on experimental data, is more reliable, safer and more accurate, and reduces the harm of acid digestion to people to a certain extent; improves the experimental facilities and equipment to ensure that the facilities and equipment used for digestion can work safely, reliably and stably. BRIEF DESCRIPTION OF THE DRAWINGS

[0042] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.

[0043] Figure 1 It is a schematic diagram of the overall structure of the ICP pre-treatment digestion system equipment of the present invention;

[0044] Figure 2 It is a schematic diagram of assembling the analysis module, the transfer module and the switch cover module of the present invention;

[0045] Figure 3 It is a structural schematic diagram of the analysis module of the present invention;

[0046] Figure 4 It is a schematic diagram of the assembly of the reagent storage module and the digestion module of the present invention;

[0047] Figure 5 It is a schematic diagram of the assembly of the digestion module, the analysis module and the transfer module of the present invention;

[0048] Figure 6 It is a schematic diagram of the assembly of the transfer module, the digestion tube storage bracket and the switch cover electric claw of the present invention.

[0049] Figure numerals: 1. Reagent storage and transportation module; 2. Digestion module; 3. Analysis module; 4. Transfer module; 5. Digestion tube storage bracket; 6. Switch cover electric claw; 7. Sealing cover; 8. Digestion tube; 11. Reagent storage rack; 12. Reagent bottle; 13. Peristaltic pump; 14. Liquid level sensor; 15. Horizontal linear module; 16. Vertical linear module; 17. Robotic arm; 18. Sample tube; 21. Graphite acid remover; 22. Sealing cover; 23. Transfer knob; 24. Absorption system; 31. Analysis module rack one; 32. Test tube rack; 33. Waste liquid barrel; 34. Analysis module rack two; 35. Visual camera one; 36. Visual camera two; 37. Code reader; 41. Lifting seat; 42. Multi-joint robotic arm; 43. Electric gripper one; 44. Gripper one; 61. Fixed slot; 62. Electric gripper two. DETAILED DESCRIPTION

[0050] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0051] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0052] Reference Figure 1 The present invention provides an ICP pre-treatment digestion system device, the core of which is to realize the automation and precision operation of sample digestion through the coordinated cooperation of multiple modules. Specifically, the device includes a reagent storage and transportation module 1, a digestion module 2, an analysis module 3, a transfer module 4 and an electrical control module (not shown in the figure). The reagent storage and transportation module 1 is responsible for storing the digestion reagent and the constant volume reagent, and can accurately inject them into the digestion tube 8 as needed; the digestion module 2 is used to store the digestion tube 8, and can accurately adjust the digestion temperature to meet the needs of digestion of different samples; the analysis module 3 determines the degree of digestion by measuring the turbidity of the liquid in the digestion tube 8, and provides a basis for subsequent operations; the transfer module 4 is responsible for selectively transferring the digestion tube 8 to the digestion module 2 or the analysis module 3, so as to realize the smooth flow of samples between different processing links; the electrical control module is preferably a PLC device, and the electrical control module is electrically connected to the above modules respectively, playing a role of unified coordination and control to ensure the orderly operation of the entire equipment.

[0053] Reference Figure 2-3The analysis module 3 is a key component for determining the degree of digestion, and mainly includes an analysis module frame 1 31 , an analysis module frame 2 34 , a waste liquid barrel 33 and a code reader 37 .

[0054] Among them, the analysis module frame 1 31 is the basic support structure of the analysis module 3, and multiple test tube racks 32 are installed on the analysis module frame 1 31. The test tube racks 32 are detachably connected to the digestion tube 8, which is convenient for the rapid replacement of the digestion tube 8 to meet different test stages. The design of the test tube rack 32 fully considers the size and shape of the digestion tube 8, and can ensure that the digestion tube 8 is firmly placed in the test tube rack 32 to avoid shaking during the detection process, thereby ensuring the accuracy of the test results. The second analysis module frame 34 is another basic support structure of the analysis module 3. The second analysis module frame 34 is arranged adjacent to the first analysis module frame 31. The second analysis module frame 34 is equipped with a visual camera 1 35 and a visual camera 2 36. The visual camera 1 35 and the visual camera 2 36 are electrically connected to the electrical control module, respectively, and are respectively arranged toward one of the test tube racks 32. The visual camera 1 35 is used to identify the turbidity of the liquid in the digestion tube 8. After the acid digestion, the visual camera 1 35 can accurately capture the turbidity of the liquid, judge whether the reagent contains undissolved solids, and then judge the progress of the digestion reaction. The visual camera 2 36 is used to identify the height of the liquid level in the digestion tube 8, and is used to ensure that the liquid volume is accurate during the constant volume. Usually, the liquid level is judged when adding pure water to constant volume. The actual judgment accuracy can reach ±0.1ml, avoiding problems such as excessive dilution caused by inaccurate liquid level height.

[0055] The waste liquid bucket 33 is installed on the analysis module frame 1 31 and is used to collect the waste liquid generated during the digestion process. When it is necessary to replace the digestion reagent or perform other operations, the robot arm 17 can drive the sample tube 18 to move above the waste liquid bucket 33 and accurately discharge the waste liquid into the waste liquid bucket 33 to avoid environmental pollution and safety hazards caused by the random discharge of waste liquid.

[0056] The code reader 37 is used to identify the identification code set on the digestion tube 8. Each digestion tube 8 has a unique identification code, which can be a bar code or a two-dimensional code, etc. The code reader 37 is electrically connected to the electrical control module, and can quickly and accurately read the identification code information and transmit it to the electrical control module. The electrical control module accurately controls and manages the corresponding digestion tube 8 according to the identification code information, realizes personalized digestion operations for different samples, and improves the versatility and flexibility of the equipment.

[0057] Reference Figure 4 The reagent storage and delivery module 1 undertakes the important task of storing and delivering digestion reagents and constant volume reagents, and its structure mainly includes a reagent storage frame 11, a reagent bottle 12 and a pump mechanism.

[0058] The reagent storage rack 11 provides a stable storage space for the reagent bottle 12, ensuring that the reagent bottle 12 is firmly placed on the reagent storage rack 11, and facilitating the operator to replenish and replace the reagent. The reagent bottle 12 is used to store digestion reagents and constant volume reagents, and each reagent bottle 12 has a clear label to distinguish different types of reagents. The material selection of the reagent bottle 12 must meet the storage requirements of the chemical reagents, have good corrosion resistance and sealing properties, and ensure the quality and stability of the reagent during storage. The pump mechanism is used to inject the liquid in the reagent bottle 12 into the digestion tube 8 on the test tube rack 32.

[0059] Preferably, the pump mechanism includes a peristaltic pump 13 , a liquid inlet pipe, a liquid outlet pipe, a sample adding pipe 18 and a liquid level sensor 14 .

[0060] Wherein, the peristaltic pump 13 is installed on the reagent storage frame 11 and is electrically connected to the electrical control module. The input end of the peristaltic pump 13 is connected to one end of a liquid inlet pipe (not shown in the figure), and the other end of the liquid inlet pipe is communicated with the reagent bottle 12, so that the liquid in the reagent bottle 12 is introduced into the peristaltic pump 13. The output end of the peristaltic pump 13 is connected to one end of a liquid outlet pipe (not shown in the figure), and the other end of the liquid outlet pipe is connected to a sample adding tube 18. The reagent bottle 12, the liquid inlet pipe, the peristaltic pump 13, the liquid outlet pipe and the sample adding tube 18 are arranged one by one to ensure that each reagent can be accurately injected into the digestion tube 8 through an independent delivery channel. Under the control of the electrical control module, the peristaltic pump 13 can accurately control the delivery speed and delivery amount of the liquid to meet the precise requirements of different digestion operations for the amount of reagents. In a specific embodiment of the present invention, an acid storage area is provided on the reagent storage rack 11, and the acid storage device is provided with a pure water station and four acid and alkali stations. A pure water bucket is placed in the pure water station to achieve constant volume, and other acid and alkali stations can store reagents such as nitric acid, hydrochloric acid, and hydrofluoric acid. A station is reserved for placing an alkali bottle, which can neutralize the residual acid reagent at the pipeline port when the acid bottle is recovered. The acid storage reagent bottle 12 uses a reagent bottle 12 cover equipped with a one-way air filter valve to effectively prevent acid volatilization pollution, and the pipeline joint is made of Teflon material, which can withstand strong acid.

[0061] The liquid level sensor 14 is installed on the reagent storage rack 11 and is electrically connected to the electrical control module. The liquid level sensor 14 monitors the liquid level height in the reagent bottle 12 one by one and feeds back the liquid level information to the electrical control module in real time. The electrical control module promptly reminds the operator to replenish the reagent based on the liquid level information to avoid interruption of the digestion operation due to insufficient reagents and ensure continuous and stable operation of the equipment.

[0062] The sample tube 18 is located above the test tube rack 32 and is connected to the analysis module frame 2 34 through the horizontal linear module 15 and the vertical linear module 16. The horizontal linear module 15 and the vertical linear module 16 are electrically connected to the electrical control module respectively, and both are stepper motors driving the lead screw to achieve linear movement, and are used to drive the mechanical arm 17 to move in the horizontal direction and the vertical direction respectively. In this way, the mechanical arm 17 can accurately move the sample tube 18 to the test tube rack 32 at different positions according to the instructions of the electrical control module, and realize the operation of injecting digestion reagents or constant volume reagents into different digestion tubes 8. The design of the sample tube 18 needs to ensure the smooth transportation and accurate dripping of the liquid to avoid problems such as dripping and clogging.

[0063] The analysis module frame 34 is connected to a robotic arm 17 through a horizontal linear module 15 and a vertical linear module 16. A plurality of sample tubes 18 are installed on the robotic arm 17. The sample tubes 18 are located above the test tube rack 32. The horizontal linear module 15 and the vertical linear module 16 are electrically connected to the electrical control module, respectively, and are used to drive the robotic arm 17 to move in the horizontal direction and the vertical direction, respectively, so as to inject the digestion reagent or the constant volume reagent into the digestion tube 8 located at the test tube rack 32 at different positions.

[0064] Reference Figure 4-5 The digestion module 2 includes a graphite acid remover 21, a sealing cover 22, an absorption system 24 and other structures.

[0065] Among them: the graphite acid-removing instrument 21 is electrically connected to the electrical control module, and a plurality of digestion positions are arranged inside it. The digestion position is detachably connected to the digestion tube 8. Its surface is specially anti-corrosive and heated in three dimensions, which ensures the heating speed, heating efficiency and uniformity, and improves the repeatability of sample pretreatment. The graphite acid-removing instrument 21 adopts advanced heating technology and temperature control system, and can accurately adjust the digestion temperature according to the preset temperature parameters. The temperature is adjustable between room temperature and 250°C. It adopts PID control, and adopts 30-stage gradient heating method during the digestion process to gradually increase the digestion temperature. The sample digestion is more thorough, the temperature accuracy is ±1°C, and the temperature difference between the holes is <0.5°C, providing a stable thermal environment for sample digestion. The top of the instrument is detachably connected with a sealing cover 22. The design of the sealing cover 22 can effectively prevent the overflow of acid mist during the digestion process, while ensuring the pressure stability in the digestion tube 8, and ensuring the smooth progress of the digestion reaction. The sealing cover 22 is detachably connected to the upper end of the second analysis module frame 34 . A transfer knob 23 is disposed on the upper end of the sealing cover 22 . The transfer knob 23 is detachably connected to the first clamping jaw 44 .

[0066] It should be noted that the sealing cover 22 of the present invention can be installed above the graphite acid removal instrument 21 to prevent acid mist from overflowing into the environment and provide a stable digestion temperature for digestion. During the transfer of the digestion tube 8, the sealing cover 22 can be clamped and moved to the top of the analysis module frame 2 34 for temporary storage, so as to facilitate the placement and removal of the digestion tube 8 in the graphite acid removal instrument 21.

[0067] The absorption system 24 is used to filter and absorb the acid mist generated during the digestion process. The acid mist not only corrodes the equipment, but also may cause harm to the health of the operators and the laboratory environment. The absorption system 24 effectively removes harmful components in the acid mist through the principles of physical adsorption and chemical neutralization, purifies the laboratory air, and ensures the safety of equipment and personnel. The absorption system 24 is designed as a closed system, with a vacuum diaphragm pump providing vacuum and operating in a negative pressure state. All acid vapors are absorbed by the alkali solution, eliminating pollution and protecting the safety of the experimenters.

[0068] Referring to 5-6, the transfer module 4 is responsible for the transfer operation of the digestion tube 8 between different modules, and mainly includes a lifting seat 41 and a multi-joint robotic arm 42 and other structures.

[0069] Wherein: the lifting seat 41 is electrically connected to the electrical control module, and can realize vertical lifting movement according to the command. The lifting seat 41 provides a stable support and movement basis for the multi-joint mechanical arm 42, ensuring that the multi-joint mechanical arm 42 can accurately reach the specified height position during the transfer of the digestion tube 8. One end of the multi-joint mechanical arm 42 is connected to the lifting seat 41 and is electrically connected to the electrical control module. The multi-joint mechanical arm 42 has multiple rotating joints, which can realize flexible multi-degree-of-freedom movement and easily cope with various complex transfer paths and posture adjustment requirements. The other end is provided with an electric clamp 43, which is also electrically connected to the electrical control module. The electric clamp 43 is provided with multiple clamps 44 that can rotate and can move closer and farther from each other. These clamps 44 can be accurately clamped according to the size and shape of the digestion tube 8 to ensure the stability and safety of the digestion tube 8 during the transfer process. Through the precise control of the electrical control module, the multi-joint mechanical arm 42 can accurately transfer the digestion tube 8 to the digestion module 2 or the analysis module 3 according to the preset program, so as to realize the efficient flow of samples between different processing links. In addition, the clamping claw 44 can clamp the transfer knob 23 to realize the transfer process of the sealing cover 22.

[0070] In addition, the present invention also includes a digestion tube storage bracket 5, which is used to store unused or digested digestion tubes 8, facilitating the storage and management of the digestion tubes 8. The material of the digestion tube storage bracket 5 should have good corrosion resistance and stability to adapt to the laboratory environment and contact with chemical reagents.

[0071] In addition, the present invention also includes a switch cover electric claw 6, which is provided with a fixing groove 61 for inserting the lower end of the digestion tube 8, and an electric clamp 2 62 detachably connected to the lower end of the digestion tube 8, and the electric clamp 2 62 is electrically connected to the electrical control module.

[0072] In order to improve the sealing performance of the present invention and reduce the diffusion of acid mist and other substances to the surroundings, the present invention is further provided with a sealing cover 7. The sealing cover 7 is arranged around the reagent storage and delivery module 1, the digestion module 2, the analysis module 3 and the digestion transfer module 4.

[0073] The digestion method of the digestion equipment of the present invention is as follows:

[0074] S1. Affix an identification code to the digestion tube 8, add a digestion sample into the digestion tube 8, and then place it on the digestion tube storage bracket 5.

[0075] S2, the electrical control module controls the electric gripper 43 to place the digestion tube 8 on the test tube rack 32 after being identified by the code reader 37, and then controls the peristaltic pump 13 and the mechanical arm 17 to add the digestion reagent into the digestion tube 8. Then, the electric gripper 43 is used to clamp the digestion tube 8 into the graphite acid removal instrument 21, and this operation is repeated to place multiple digestion tubes 8 into the graphite acid removal instrument 21 in sequence.

[0076] S3, the electrical control module controls the electric gripper 43 to install the sealing cover 22 on the graphite acid-removing instrument 21, and then controls the graphite acid-removing instrument 21 to heat and keep warm according to the preset temperature and time.

[0077] S4. The electrical control module controls the electric gripper 43 to remove the sealing cover 22 on the graphite acid removal instrument 21, take out the digestion tube 8, then use the electric gripper 43 to oscillate the digestion tube 8, and place it in the digestion tube storage bracket 5 to cool. Repeat this operation to place multiple digestion tubes 8 into the digestion tube storage bracket 5 in turn.

[0078] S5. The electrical control module controls the electric clamp 43 to clamp the digestion tube 8 onto the test tube rack 32 opposite to the visual camera 35. The visual camera 35 is used to determine the turbidity of the liquid in the digestion tube 8. If the turbidity detection is less than 0.1 NTU, the digestion tube 8 continues the subsequent constant volume operation. If it fails, continue to add acid for digestion, and repeat the operations from S2 to S4.

[0079] S6. The electrical control module controls the electric clamp 43 to clamp the digestion tube 8 on the test tube rack 32 opposite to the visual camera 2 36, controls the peristaltic pump 13 and the robotic arm 17 to add 20 ml of a constant volume reagent, which is water, into the digestion tube 8, and controls the electric clamp 43 to shake the digestion tube 8 for 30 seconds to mix the substances in the digestion tube 8 evenly again, and then places it on the test tube rack 32 opposite to the visual camera 2 36.

[0080] S7, control the peristaltic pump 13 and the robot arm 17 to add a constant volume reagent into the digestion tube 8. In this embodiment, the constant volume reagent is water, which is constant to 50 ml. After the digestion process is completed, let it stand until the solution cools naturally.

[0081] S8, the electrical control module controls the electric clamp 43 to move the digestion tube 8 into the fixing groove 61 of the switch cover electric clamp 6, and uses the electric clamp 2 62 to fix the bottom of the digestion tube 8, and then the electric clamp 43 drives the bottle cap of the digestion tube 8 to rotate and screw into the bottle body of the digestion tube 8, and then the electric clamp 43 puts the digestion tube 8 back on the digestion tube storage bracket 5, and repeats the operations from S6 to S8 until all the digestion tubes 8 are filled to the desired volume.

[0082] In the present invention, by setting a visual camera 35 to analyze the turbidity of the liquid in the digestion tube 8, the digestion degree of the digested sample can be effectively identified. When the digestion is not complete, acid digestion can be continued to avoid the residue of some insoluble substances and improve the accuracy of the analysis results.

[0083] In the present invention, by setting up the absorption system 24, the volatile strong acid reagents can be neutralized, the sealing cover 7 is used to reduce interference with the outside world, and the harmful components in the acid mist are effectively removed, the laboratory air is purified, and the safety of equipment and personnel is guaranteed.

[0084] The present invention realizes automatic digestion of the whole process of ICP pretreatment; automatically judges the digestion result in a visual way, and the automated visual inspection and judgment of the result improve the digestion completion efficiency; solves the problems of time-consuming, labor-intensive and labor-intensive chemical digestion, and modular processing of digestion samples in the same experimental environment improves the efficiency, which has high social applicability value; in addition, the automated and process-based digestion improves the safety of chemical digestion, eliminates the interference of human factors on experimental data, is more reliable, safer and more accurate, and reduces the harm of acid digestion to people to a certain extent; improves the experimental facilities and equipment to ensure that the facilities and equipment used for digestion can work safely, reliably and stably.

[0085] The present invention can be applied to various types of samples, including metals, alloys, geological samples, biological samples, etc.

[0086] In the description of the present invention, it should be understood that the terms "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside" and "outside" etc., indicating orientations or positional relationships, are based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present invention.

[0087] The embodiments described above are only descriptions of the preferred embodiments of the present invention, and are not intended to limit the scope of the present invention. Without departing from the design spirit of the present invention, various modifications and improvements made to the technical solutions of the present invention by ordinary technicians in this field should all fall within the protection scope determined by the claims of the present invention.

Claims

1. An ICP pre-treatment digestion system device, characterized in that: include: A reagent storage and delivery module (1) for storing a digestion reagent and a volume fixing reagent and selectively injecting them into a digestion tube (8); A digestion module (2) for storing the digestion tube (8) and capable of adjusting the digestion temperature; An analysis module (3) for determining the degree of digestion by measuring the turbidity of the liquid in the digestion tube (8); A transfer module (4) for selectively transferring the digestion tube (8) to the digestion module (2) or the analysis module (3); and An electrical control module electrically connected to the reagent storage and delivery module (1), the digestion module (2), the analysis module (3) and the digestion transfer module (4) respectively.

2. The ICP pre-treatment digestion system equipment according to claim 1, characterized in that, The analysis module (3) comprises: An analysis module frame (31), wherein a plurality of test tube racks (32) are mounted on the analysis module frame (31), and the test tube racks (32) are detachably connected to the digestion tubes (8); and The analysis module frame (34) is provided with a visual camera (35) and a visual camera (36) installed on the analysis module frame (34). The visual camera (35) and the visual camera (36) are respectively electrically connected to the electrical control module and are respectively arranged toward one of the test tube racks (32). The visual camera (35) is used to identify the turbidity of the liquid in the digestion tube (8), and the visual camera (36) is used to identify the height of the liquid level in the digestion tube (8).

3. The ICP pre-treatment digestion system equipment according to claim 2, characterized in that, The reagent storage and delivery module (1) comprises: a reagent storage rack (11); and A plurality of reagent bottles (12) and a pump mechanism are installed on the reagent storage rack (11), and the pump mechanism is used to inject the liquid in the reagent bottle (12) into the digestion tube (8) on the test tube rack (32).

4. The ICP pre-treatment digestion system equipment according to claim 3, characterized in that: The pump mechanism comprises: A peristaltic pump (13) installed on the reagent storage rack (11) and electrically connected to the electrical control module, wherein the input end of the peristaltic pump (13) is connected to one end of a liquid inlet pipe, the other end of the liquid inlet pipe is in communication with the reagent bottle (12), the output end of the peristaltic pump (13) is connected to one end of a liquid outlet pipe, the other end of the liquid outlet pipe is connected to a sample addition pipe (18), and the reagent bottle (12), the liquid inlet pipe, the peristaltic pump (13), the liquid outlet pipe and the sample addition pipe (18) are arranged in a one-to-one correspondence; a plurality of liquid level sensors (14) mounted on the reagent storage rack (11) and electrically connected to the electrical control module, wherein the liquid level sensors (14) monitor the liquid level heights in the reagent bottles (12) one by one; and The analysis module frame body 2 (34) is connected to a mechanical arm (17) via a horizontal linear module (15) and a vertical linear module (16). The mechanical arm (17) is provided with a plurality of sample tubes (18) installed thereon. The sample tubes (18) are located above the test tube rack (32). The horizontal linear module (15) and the vertical linear module (16) are respectively electrically connected to the electrical control module and are respectively used to drive the mechanical arm (17) to move in the horizontal direction and the vertical direction, so as to realize the injection of digestion reagent and constant volume reagent into the digestion tubes (8) located at different positions of the test tube rack (32).

5. The ICP pre-treatment digestion system equipment according to claim 4, characterized in that: The analysis module (3) further comprises: A waste liquid bucket (33) is installed on the analysis module frame (31), and the mechanical arm (17) selectively drives the sample adding tube (18) to move above the waste liquid bucket (33); and A code reader (37) for identifying the identification code on the digestion tube (8), wherein the code reader (37) is electrically connected to the electrical control module.

6. The ICP pre-treatment digestion system equipment according to claim 2, characterized in that: The digestion module (2) comprises: a graphite acid-removing instrument (21) electrically connected to the electrical control module, wherein a digestion tube (8) is detachably connected to the graphite acid-removing instrument (21) for adjusting the digestion temperature, and a sealing cover (22) is detachably connected to the top of the graphite acid-removing instrument (21); and An absorption system (24) for filtering and absorbing acid mist.

7. The ICP pre-treatment digestion system equipment according to claim 6, characterized in that: The transfer module (4) comprises: A lifting seat (41) electrically connected to the electrical control module; and A multi-joint robotic arm (42) is connected to the lifting seat (41) at one end and electrically connected to the electrical control module, wherein the multi-joint robotic arm (42) has multiple rotating joints, and an electric clamp (43) is provided at the other end of the multi-joint robotic arm (42), wherein the electric clamp (43) is electrically connected to the electrical control module, and the electric clamp (43) is provided with multiple clamps (44) that can rotate and can move closer to or farther from each other.

8. The ICP pre-treatment digestion system equipment according to claim 7, characterized in that: Also includes: A digestion tube storage bracket (5) for storing the digestion tube (8); and The switch cover electric claw (6) is provided with a fixing groove (61) for inserting the lower end of the digestion tube (8), and an electric clamping claw 2 (62) detachably connected to the lower end of the digestion tube (8), and the electric clamping claw 2 (62) is electrically connected to the electrical control module.

9. The ICP pre-treatment digestion system equipment according to claim 7, characterized in that: The sealing cover (22) is detachably connected to the upper end of the second analysis module frame (34), and a transfer knob (23) is provided at the upper end of the sealing cover (22), and the transfer knob (23) is detachably connected to the first clamp (44).

10. The ICP pre-treatment digestion system equipment according to any one of claims 1 to 9, characterized in that: It also comprises a sealing cover (7) which is arranged around the reagent storage and delivery module (1), the digestion module (2), the analysis module (3) and the digestion and transfer module (4).

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