Impurity detection device and method for preparing high-purity arsenic

Abstract

The invention relates to an impurity detection device and method for high-purity arsenic preparation in the technical field of high-purity arsenic preparation, and the impurity detection device comprises a heating assembly, a waste gas treatment mechanism and an intelligent detector, the waste gas treatment mechanism comprises a fine filter cartridge, a liquid spraying pipe arranged at the upper end of an inner cavity of the fine filter cartridge, a plurality of single filter cartridges vertically arranged in the inner cavity of the fine filter cartridge, a dispersion chamber arranged at the bottom of the inner cavity of the fine filter cartridge, and a transfer pipe communicated with the gas outlet pipe; an adjustable net cover, a regulation and control plate and a regulation and control rope connected with the bottom of the regulation and control plate are arranged in the middle of an inner cavity of each single filter cartridge; a plurality of elastic ribs are distributed on the outer ring of the regulation and control rope in the circumferential direction; the intelligent detector is provided with an analysis module and a regulation and control module, by adopting the structure, when sample impurities are detected, the corresponding reaction purification efficiency can be adjusted according to the amount of harmful gas generated in a detection test, and the purpose of intelligently adjusting the purification effect is achieved.

Description

Technical Field

[0001] The present invention relates to an impurity detection device, and in particular to an impurity detection device and method for high-purity arsenic preparation, which are applied to the technical field of high-purity arsenic preparation. Background Art

[0002] High-purity arsenic is mainly used to prepare semiconductor compounds and high-purity alloys such as gallium arsenide, gallium aluminum arsenide, and indium arsenide. It has increasingly wide applications in the fields of medicine, health, corrosion protection, dyes, etc., especially gallium arsenide, which has a very wide range of applications. In the process of preparing high-purity arsenic, it is necessary to select a quantitative sample to determine its impurity content.

[0003] The invention patent with publication number CN102072833A discloses a sample preparation method for determining impurity elements in high-purity arsenic by ICP-MS, which comprises weighing high-purity arsenic to obtain a mass m of high-purity arsenic, placing all the weighed high-purity arsenic in a quartz tube, introducing oxygen into the quartz tube at 300-350°C, and cooling the quartz tube to room temperature after the high-purity arsenic is oxidized to generate arsenic oxide that is sublimated and removed, taking out the quartz crucible with residues left in the quartz tube; adding electronic grade nitric acid into the quartz crucible, heating it on a heating plate at 150°C until it is completely digested, and then adding a dilute nitric acid solution with a mass percentage concentration of not more than 10% into the crucible to make up the volume, and obtaining the total volume of the fixed volume.

[0004] In the above scheme, when the high-purity arsenic in the quartz tube is heated and oxidized, the formed arsenic oxide has a certain toxicity, which is discharged by ventilation and arsenic discharge (eliminating the interference of matrix As): a silicone plastic hose is used to introduce the quartz tube outlet into a glass container containing an aqueous solution (the plastic hose is inserted 5 mm below the water surface), and oxygen is introduced into the air inlet of the quartz tube. According to the vapor pressure difference, the compound As2O3 of the matrix element As is removed by sublimation at 300-350°C due to its high vapor pressure, while the impurity elements with low vapor pressure remain in the quartz crucible. During the operation, the discharged arsenic oxide gas is absorbed by the aqueous solution. After the gas is introduced, it cannot be fully mixed with the aqueous solution, resulting in poor treatment effect, which affects the health of the experimenters. Summary of the invention

[0005] In view of the above-mentioned prior art, the technical problem to be solved by the present invention is that the exhausted arsenic oxide gas is absorbed by the aqueous solution, and the gas cannot be fully mixed with the aqueous solution after being introduced, resulting in poor treatment effect and affecting the health of the experimenters.

[0006] In order to solve the above problems, the present invention provides an impurity detection device for preparing high-purity arsenic, comprising: A heating assembly, the heating assembly is used to heat a quartz tube containing a sample, one end of the quartz tube is connected to an air inlet pipe and the other end is connected to an air outlet pipe; An exhaust gas treatment mechanism, the exhaust gas treatment mechanism is connected to the output end of the air outlet pipe and is used to treat the gas generated when the sample is heated. The exhaust gas treatment mechanism includes a fine filter cartridge, a liquid sprinkling pipe arranged at the upper end of the inner cavity of the fine filter cartridge, a plurality of single filter cartridges vertically arranged in the inner cavity of the fine filter cartridge, a dispersion chamber arranged at the bottom of the inner cavity of the fine filter cartridge, and a transfer pipe connected to the air outlet pipe. The bottom end of the single filter cartridge is connected to the inner cavity of the dispersion chamber, the output end of the transfer pipe is connected to the inner cavity of the dispersion chamber, a flow rate sensor is installed in the transfer pipe, and an exhaust pipe connected to the upper end of the fine filter cartridge; an adjustable mesh cover, a control plate and a control rope connected to the bottom of the control plate are arranged in the middle of the inner cavity of each single filter cartridge, a plurality of elastic ribs are circumferentially distributed on the outer circle of the control rope, the bottom end of the elastic rib is connected to the inner wall of the single filter cartridge and the top end is abutted against the bottom surface of the control plate, the adjustable mesh cover covers the outer circle of the elastic rib, and a pulling component is arranged at the end of the control rope away from the control plate, which is used to pull the control rope to move vertically; The intelligent detector is arranged on the heating component. The intelligent detector is provided with an analysis module and a control module. The input end of the analysis module is connected to the flow rate sensor signal, the output end of the analysis module is connected to the control module signal, and the output end of the control module is connected to the pulling component signal.

[0007] In the above-mentioned impurity detection device for preparing high-purity arsenic, when detecting sample impurities, the corresponding reaction purification efficiency can be adjusted according to the amount of harmful gas generated during the detection test, thereby achieving the purpose of intelligently adjusting the purification effect.

[0008] As a further improvement of the present application, the transfer pipe is connected to the inner cavity of the dispersion chamber, the bottom of the inner cavity of the dispersion chamber is protruded at a position corresponding to the transfer pipe, and the bottom of the dispersion chamber is connected to a drainage pipe.

[0009] As a further improvement of the present application, the pulling assembly includes a control ring rotatably connected to the bottom of the dispersion chamber, and a driving member installed on the bottom of the dispersion chamber. The output end of the driving member is in contact with the outer ring of the control ring through a roller. The driving member is used to drive the roller to rotate. A control rod corresponding to the control rope is fixed to the outer ring of the control ring. The bottom end of the control rope passes through the dispersion chamber and is fixed to the corresponding control rod. The output end of the control module is signal-connected to the driving member.

[0010] As a further improvement of the present application, a diversion orifice plate fixed to the inner wall of the fine filter cartridge is provided below the shower pipe, and a through hole matching the single filter cartridge is opened on the diversion orifice plate.

[0011] As a further improvement of the present application, a driving member 2 is installed on the top of the fine filter cartridge, and a driving tube connected to the shower tube is fixed to the output end of the driving member 2. The driving member 2 is used to drive the driving tube to rotate. A solenoid valve is installed on the driving tube. The driving tube is connected to a reaction liquid tube, which is used to input the reaction liquid. A purification module is also provided on the intelligent detector. The output end of the purification module is respectively connected to the driving member 2 and the solenoid valve signal, and the input end of the purification module is connected to the analysis module signal.

[0012] As a further improvement of the present application, a pressure measuring chamber is provided at the bottom of the regulating plate, the top of the regulating rope is connected to the pressure measuring chamber, the top of the elastic rib is abutted against the outer circle of the pressure measuring chamber, and a detection chamber connected to the inner cavity of the pressure measuring chamber is opened at the upper end of the regulating plate. The inner cavity of the detection chamber is vertically slidably connected with a piston plate, and a distance sensor corresponding to the piston plate is installed on the top of the detection chamber, and the input end of the analysis module is connected to the distance sensor signal.

[0013] As another improvement of the present application, the inner cavity of the pressure measuring chamber is filled with a pressure measuring solution, the outer wall of the pressure measuring chamber is an elastic abutment surface, and the elastic ribs are an arc-shaped structure.

[0014] As another improved supplement of the present application, an electromagnet is installed on the top of the detection cavity, the piston plate is made of magnet material, the bottom surface of the pressure measuring chamber is in contact with the liquid surface of the pressure measuring solution, and the output end of the control module is connected to the electromagnet signal.

[0015] As another improved supplement of the present application, a primary filter cartridge is arranged between the air outlet pipe and the transfer pipe, reaction liquid is added to the primary filter cartridge, the output end of the air outlet pipe extends into the reaction liquid in the primary filter cartridge, and the input end of the transfer pipe is connected to the top of the inner cavity of the primary filter cartridge.

[0016] A detection method of an impurity detection device for high-purity arsenic preparation, comprising the following steps: S1. Weighing: Weigh 5-10g of sample into a quartz crucible and record the sample weight; S2, heating: adjust the temperature of the heating assembly to between 300-350°C, place the quartz crucible in a quartz tube, one end of the quartz tube is sealed and connected to the air inlet pipe, and the other end is sealed and connected to the air outlet pipe, and place the quartz tube in the heating assembly for heating; S3, arsenic purification: oxygen is introduced into the air inlet pipe, and the gas discharged from the air outlet pipe is introduced into the waste gas treatment mechanism for purification. The gas rate introduced into the transfer pipe is judged by the intelligent detector, and the reaction purification effect of the waste gas treatment mechanism is adjusted. The gas after reaction and purification is discharged through the exhaust pipe and collected; S4, furnace digestion: take out the heated quartz tube, cool it naturally for 12-24 hours, take out the quartz crucible in the quartz tube, add 3-7 ml of electronic grade nitric acid into the quartz crucible, put the crucible with nitric acid on a heating plate at 130-170 ° C and heat it for 40-80 minutes to completely digest the residue in the quartz crucible; S5. Make up the volume: Take out the residual impurity elements in the quartz crucible, and make up the volume to 40-60ml with 5% dilute nitric acid for testing.

[0017] To sum up, when the sample impurities are detected, the generated harmful gases are introduced into the fine filter cartridge through the transfer tube for reaction purification, and the reaction liquid discharged through the sprinkling tube is sprinkled into each single filter cartridge and infiltrated into the surface of the adjustable mesh cover in each single filter cartridge. When the gas passes through the single filter cartridge, it fully reacts with the reaction liquid infiltrated on the adjustable mesh cover, thereby improving the purification effect of the harmful gases, and by setting up an intelligent detector, the analysis module determines the amount of gas entering the dispersion chamber through the flow rate data, and intelligently adjusts the control plate to move up and down, thereby adjusting the surface area of ​​the adjustable mesh cover, and adjusting the reaction effect of the gas and the reaction liquid infiltrated on the adjustable mesh cover. The reaction purification capacity can be adaptively adjusted according to the airflow velocity, thereby improving the purification efficiency of the device, saving the use of reaction liquid, and saving resources. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 This is a schematic diagram of the overall structure of the first and second implementation modes of the present application; Figure 2 Schematic cross-sectional view of the fine filter cartridge of the first and second embodiments of the present application; Figure 3 Schematic cross-sectional view of a single filter cartridge according to the first and second embodiments of the present application; Figure 4 This is a sectional front view of the fine filter cartridge of the first and second embodiments of the present application; Figure 5 This is a schematic diagram of the intelligent detection control principle of the first embodiment of the present application; Figure 6 This is a schematic diagram of the pulling assembly structure of the first and second embodiments of the present application; Figure 7 Schematic cross-sectional views of the adjustable grille and the control panel of the first and second embodiments of the present application; Figure 8 This is a schematic diagram of the intelligent detection control principle of the second implementation mode of this application.

[0019] Description of the numbers in the figure: 1. Heating assembly; 2. Quartz tube; 3. Inlet pipe; 4. Outlet pipe; 5. Primary filter cartridge; 6. Transfer pipe; 7. Fine filter cartridge; 8. Elastic ribs; 9. Drain pipe; 10. Reaction liquid tube; 11. Driver 2; 12. Dispersion chamber; 13. Single filter cartridge; 14. Diverter orifice plate; 15. Intelligent detector; 16. Sprinkling tube; 17. Solenoid valve; 18. Adjustable mesh cover; 19. Control rope; 20. Driver tube; 21. Flow rate sensor; 22. Control board; 23. Pressure measuring chamber; 24. Pressure measuring solution; 25. Detection chamber; 26. Piston plate; 27. Distance sensor; 28. Electromagnet; 29. ​​Control ring; 30. Control rod; 31. Driver 1. DETAILED DESCRIPTION

[0020] Two implementation modes of the present application are described in detail below with reference to the accompanying drawings.

[0021] The first implementation method: Figure 1-Figure 6 An impurity detection device for high-purity arsenic preparation is shown, including a heating component 1, an exhaust gas treatment mechanism, an intelligent detector 15 and a sprinkling tube 16. The heating component 1 is used to heat a quartz tube 2 containing a sample. The heating component 1 is a device for heating experimental samples in the prior art and is a common heating device for people in this field. It has the function of heating the sample to a specified temperature. Its specific structure and working principle have been disclosed, and the technical solution of this application will not be repeated. One end of the quartz tube 2 is connected to an air inlet pipe 3 and the other end is connected to an air outlet pipe 4. A sample of a specified mass is added to a quartz crucible, and then the quartz crucible is placed in the quartz tube 2. The quartz tube 2 is placed on the heating component 1 for heating treatment, and one end of the quartz tube 2 is connected to the air inlet pipe 3 and the other end is connected to the air outlet pipe 4. Oxygen is introduced into the heated sample through the air inlet pipe 3 to oxidize it, and arsenic oxide is discharged through the air outlet pipe 4, thereby eliminating the interference of matrix arsenic on impurity determination.

[0022] It is worth mentioning that see Figure 2-Figure 4The waste gas treatment mechanism is connected to the output end of the air outlet pipe 4 and is used to treat the gas generated when the sample is heated. The waste gas treatment mechanism includes a fine filter cartridge 7, a liquid sprinkling pipe 16 arranged at the upper end of the inner cavity of the fine filter cartridge 7, a plurality of single filter cartridges 13 vertically arranged in the inner cavity of the fine filter cartridge 7, a dispersion chamber 12 arranged at the bottom of the inner cavity of the fine filter cartridge 7, and a transfer pipe 6 connected to the air outlet pipe 4. The bottom end of the single filter cartridge 13 is connected to the inner cavity of the dispersion chamber 12, and the output end of the transfer pipe 6 is connected to the inner cavity of the dispersion chamber 12. The discharged gas to be treated is input into the transfer pipe 6 through the air outlet pipe 4, and is diverted to the plurality of single filter cartridges 13 through the dispersion chamber 12. The gas flows toward the fine filter cartridge 7. The top of the filter cartridge 13 flows, and the shower pipe 16 will spray out the reaction liquid to react with the arsenic oxide. The reaction liquid is an alkaline solution, preferably a calcium hydroxide or magnesium hydroxide solution. A flow rate sensor 21 is installed in the transfer pipe 6. The upper end of the fine filter cartridge 7 is connected to an exhaust pipe. The treated gas is discharged or collected through the exhaust pipe, which reduces the degree of harm of the exhaust gas and improves the safety of the detection process. An adjustable mesh cover 18, a regulating plate 22 and a regulating rope 19 connected to the bottom of the regulating plate 22 are arranged in the middle of the inner cavity of each single filter cartridge 13. A plurality of elastic ribs 8 are distributed circumferentially on the outer circle of the regulating rope 19. The bottom end of the elastic rib 8 is connected to the inner wall of the single filter cartridge 13 and the top end is connected to the regulating plate 22. The bottom surfaces of the plates 22 are in contact with each other, and the adjustable mesh cover 18 covers the outer circle of the elastic ribs 8. The adjustable mesh cover 18 is made of corrosion-resistant fabric, preferably polyester stretch fabric, which has good air permeability, corrosion resistance and elasticity. A pulling assembly is provided at one end of the regulating rope 19 away from the regulating plate 22, which is used to pull the regulating rope 19 to move vertically. The reaction liquid discharged through the shower pipe 16 will fall into each single filter cartridge 13 and fully infiltrate the adjustable mesh cover 18. The gas introduced into the bottom of the single filter cartridge 13 will pass through the adjustable mesh cover 18 infiltrated with the reaction liquid, so that the gas can fully contact and react with the reaction liquid, thereby improving the reaction and purification effect of the gas, and by setting a plurality of elastic ribs The regulating plate 22 is driven up and down by the regulating rope 19. When the regulating plate 22 moves down, the tops of the multiple elastic ribs 8 will close inward, so that the spherical surface area formed by the outer circles of the multiple elastic ribs 8 is reduced, thereby reducing the area of ​​the adjustable mesh cover 18; conversely, when the regulating plate 22 moves up, the tops of the multiple elastic ribs 8 will expand outward, so that the spherical surface area formed by the outer circles of the multiple elastic ribs 8 is increased, thereby increasing the area of ​​the adjustable mesh cover 18. The surface area of ​​the adjustable mesh cover 18 can be adjusted to adjust the corresponding reaction purification effect according to the amount of gas generated during detection, and the adaptive adjustment can achieve a better purification effect, save the use of reaction liquid, and save resources.

[0023] In this embodiment, the intelligent detector 15 is arranged on the heating component 1, and an analysis module and a control module are arranged on the intelligent detector 15. The input end of the analysis module is connected to the flow rate sensor 21 signal, the output end of the analysis module is connected to the control module signal, and the output end of the control module is connected to the pulling component signal. When the gas input through the transfer pipe 6 is reacted and purified by the fine filter cartridge 7, the reaction liquid discharged by the liquid sprinkling pipe 16 is thrown into each single filter cartridge 13, and the surface of the adjustable mesh cover 18 in each single filter cartridge 13 is infiltrated. When the gas passes through the single filter cartridge 13, it is infiltrated with the adjustable mesh cover 18. The reaction liquid reacts fully, and the flow rate sensor 21 is used to detect the flow rate data of the gas entering the transfer pipe 6, and send the flow rate data to the analysis module in real time. The analysis module determines the amount of gas entering the dispersion chamber 12 by analyzing the flow rate data, and sends the corresponding control signal to the control module according to the gas amount. The control module controls the pulling component to control the up and down movement of the control rope 19, thereby controlling the up and down movement of the corresponding control plate 22, adjusting the surface area of ​​the adjustable mesh cover 18, and can adaptably adjust the reaction purification capacity according to the airflow velocity, thereby improving the purification efficiency of the device and saving the use of the reaction liquid.

[0024] It is worth mentioning that see Figure 5 and Figure 6 The pulling assembly includes a control ring 29 rotatably connected to the bottom of the dispersion chamber 12, and a driving member 31 installed at the bottom of the dispersion chamber 12. The output end of the driving member 31 abuts against the outer ring of the control ring 29 through a roller. The driving member 31 is used to drive the roller to rotate. The driving member 31 is preferably an electric motor or a pneumatic motor. The outer ring of the control ring 29 is fixed with a control rod 30 corresponding to the control rope 19. The bottom end of the control rope 19 passes through the dispersion chamber 12 and is fixed to the corresponding control rod 30. The output end of the control module is connected to the driving member 31 signal. When the pulling assembly is adjusted by the control module, the corresponding driving member 31 will be controlled to work. The driving member 31 drives the control ring 29 to rotate forward or reverse through the roller, thereby driving the control rod 30 of the outer ring to swing. The swing of the control rod 30 drives the control rope 19 connected to its end to move, thereby achieving the purpose of pulling the control rope 19 and synchronously controlling the control plate 22 to move up and down.

[0025] In addition, a driving member 11 is installed on the top of the fine filter cartridge 7, and a driving tube 20 connected to the shower tube 16 is fixed at the output end of the driving member 11. The driving member 11 is used to drive the driving tube 20 to rotate. The driving member 11 is preferably an electric motor or a pneumatic motor. A solenoid valve 17 is installed on the driving tube 20. The driving tube 20 is connected to a reaction liquid tube 10. The reaction liquid tube 10 is used to input the reaction liquid. The end of the reaction liquid tube 10 is sleeved with the driving tube 20, and the inner cavities of the two are connected. The reaction liquid is input into the driving tube 20 through the reaction liquid tube 10 and is sprayed out through the shower tube 16. A purification module is also provided on the intelligent detector 15. The output ends of the purification module are respectively connected to the signal of the driving member 11 and the solenoid valve 17. The input end of the purification module is connected with the signal of the analysis module. When the impurity detection starts, the analysis module sends a purification signal to the purification module. The purification module controls the driving member 11 to work and the electromagnetic valve 17 to open. The driving member 11 drives the liquid spraying tube 16 to rotate through the driving tube 20, and evenly sprinkles the reaction liquid into each single filter cartridge 13 to improve the purification effect of harmful gases. When the analysis module determines the air flow velocity through the flow velocity sensor 21, when the flow velocity increases or decreases, it will send a corresponding control signal to increase or decrease the purification effect to the purification module. The purification module will control the corresponding opening degree of the electromagnetic valve 17, so as to cooperate with the adjustment of the surface area of ​​the adjustable mesh cover 18 to adjust the purification effect of harmful gases.

[0026] Preferably, the transfer pipe 6 is connected to the inner cavity of the dispersion chamber 12, and the bottom of the inner cavity of the dispersion chamber 12 is protruding at a position corresponding to the transfer pipe 6. The bottom of the dispersion chamber 12 is connected to a drain pipe 9. The harmful gas is input into the inner cavity of the dispersion chamber 12 through the transfer pipe 6, and is diverted to each single filter cartridge 13 through the dispersion chamber 12. The reacted or unreacted reaction liquid falls into the inner cavity of the dispersion chamber 12 and is discharged and recovered through the drain pipe 9. Since the bottom of the inner cavity of the dispersion chamber 12 is protruding at a position corresponding to the transfer pipe 6, the reaction liquid entering the dispersion chamber 12 can be reduced from flowing into the transfer pipe 6, and the transfer pipe 6 is not easy to be blocked. A diversion orifice plate 14 fixed to the inner wall of the fine filter cartridge 7 is provided below the shower pipe 16, and a through hole matching the single filter cartridge 13 is opened on the diversion orifice plate 14. The reaction liquid discharged through the shower pipe 16 will be diverted to each single filter cartridge 13 through the diversion orifice plate 14, thereby improving the uniformity of the reaction liquid flowing into each single filter cartridge 13.

[0027] In this implementation, see Figure 1 and Figure 2A primary filter cartridge 5 is arranged between the air outlet pipe 4 and the transfer pipe 6, and a reaction liquid is added to the primary filter cartridge 5. The reaction liquid added in the primary filter cartridge 5 is the same as the reaction liquid input into the reaction liquid pipe 10, both of which are alkaline solutions, preferably calcium hydroxide or magnesium hydroxide solution. The output end of the air outlet pipe 4 extends into the reaction liquid of the primary filter cartridge 5, and the input end of the transfer pipe 6 is connected with the top of the inner cavity of the primary filter cartridge 5. The gas entering through the air outlet pipe 4 will first enter the primary filter cartridge 5 to preliminarily react with the reaction liquid. At the same time, it can also reduce the temperature of the gas and reduce the damage to the adjustable mesh cover 18. The gas after the preliminary reaction with the reaction liquid in the primary filter cartridge 5 is input into the transfer pipe 6, and then enters the dispersion chamber 12 in the fine filter cartridge 7, and the gas is finely purified again to improve the purification effect of the gas.

[0028] The second implementation method: Figure 4 , Figure 7-Figure 8 An impurity detection device for high-purity arsenic preparation is shown. Different from the first embodiment, a pressure measuring chamber 23 is provided at the bottom of the regulating plate 22, the top of the regulating rope 19 is connected to the pressure measuring chamber 23, the top of the elastic rib 8 is in contact with the outer ring of the pressure measuring chamber 23, and a detection chamber 25 connected to the inner cavity of the pressure measuring chamber 23 is provided at the upper end of the regulating plate 22. The inner cavity of the detection chamber 25 is vertically slidably connected to a piston plate 26, and a distance sensor 27 corresponding to the piston plate 26 is installed on the top of the detection chamber 25. The input end of the analysis module is connected to the signal of the distance sensor 27. By pulling the regulating rope 19, the pressure measuring chamber 23 will be driven to move, thereby synchronously driving the regulating plate 22 to move up and down. When the ends of the multiple elastic ribs 8 are retracted or expanded, different squeezing pressures will be formed on the outer wall of the pressure measuring chamber 23. When the outer wall of the pressure measuring chamber 23 is squeezed, the gas flow in its inner cavity will change. Since the detection chamber 25 is connected to the inner cavity of the pressure measuring chamber 23, the piston plate 26 will be pushed up and down synchronously, and the distance data from the piston plate 26 is detected by the distance sensor 27. The analysis module determines the position of the piston plate 26 through the distance data fed back by the distance sensor 27, so as to determine the expansion degree of the elastic ribs 8 in the corresponding single filter cartridge 13, thereby accurately determining the expansion area of ​​the adjustable mesh cover 18 on each single filter cartridge 13, and understanding the reaction purification capacity of the adjustable mesh cover 18 at the corresponding single filter cartridge 13.

[0029] In addition, when the surface mesh of the adjustable mesh cover 18 is gradually clogged, the gas entering through the single filter cartridge 13 will form a certain thrust on the adjustable mesh cover 18, thereby changing the force of the top of the elastic rib 8 on the outer circle of the pressure measuring chamber 23, and then changing the distance data detected by the distance sensor 27. The analysis module determines the surface blockage of each adjustable mesh cover 18 according to the detection data of the distance sensor 27, which is convenient for the experimenter to adjust and maintain it in time, clean or replace the adjustable mesh cover 18, so that the device always has a good purification effect and improves the convenience of device maintenance.

[0030] In this embodiment, the inner cavity of the pressure measuring chamber 23 is filled with a pressure measuring solution 24, and the outer wall of the pressure measuring chamber 23 is an elastic abutment surface. The pressure measuring solution 24 can be a liquid with a relatively high concentration. After the elastic abutment surface of the pressure measuring chamber 23 is subjected to force, the pressure measuring solution 24 flows more sensitively and pushes the corresponding piston plate 26 to move, thereby improving the detection accuracy of the distance sensor 27. The elastic ribs 8 are arc-shaped structures, and the elastic ribs 8 with arc-shaped structures can provide better support for the adjustable mesh cover 18, fully stretch the adjustable mesh cover 18 and reduce wrinkles, so that the reaction liquid can fully react with the gas for purification.

[0031] In addition, an electromagnet 28 is installed on the top of the detection cavity 25, and the piston plate 26 is made of magnet material. The bottom surface of the pressure measuring chamber 23 is in contact with the liquid surface of the pressure measuring solution 24. The output end of the control module is connected to the electromagnet 28 signal. By controlling the direction and magnitude of the current passed into the electromagnet 28, the electromagnet 28 can be controlled to generate magnetism of different directions and strengths, thereby controlling the piston plate 26 to approach or move away from the electromagnet 28 and control the distance between the two, thereby adjusting the degree of compression of the pressure measuring solution 24 in the inner cavity of the pressure measuring chamber 23, and further adjusting the position of the top end of the elastic rib 8 located on the outer circle of the pressure measuring chamber 23 to control the expansion or contraction degree of the elastic rib 8. The expansion area of ​​the adjustable mesh cover 18 in each single filter cartridge 13 can be actively adjusted, and the expansion degree of the adjustable mesh cover 18 in each single filter cartridge 13 can be accurately adjusted, thereby adjusting the reaction purification effect of the corresponding single filter cartridge 13, and adaptively adjusting according to the gas flow rate to improve the purification effect of the device.

[0032] A detection method of an impurity detection device for high-purity arsenic preparation, comprising the following steps: S1. Weighing: Weigh 5-10g of sample into a quartz crucible and record the sample weight; S2, heating: adjust the temperature of the heating component 1 to between 300-350°C, place the quartz crucible in the quartz tube 2, one end of the quartz tube 2 is sealed and connected to the air inlet pipe 3, and the other end is sealed and connected to the air outlet pipe 4, and place the quartz tube 2 in the heating component 1 for heating; S3, arsenic purification: oxygen is introduced into the air inlet pipe 3, and the gas discharged from the air outlet pipe 4 is introduced into the waste gas treatment mechanism for purification. The gas rate introduced into the transfer pipe 6 is judged by the intelligent detector 15, and the reaction purification effect of the waste gas treatment mechanism is adjusted. The gas after reaction and purification is discharged through the exhaust pipe and collected; S4, furnace digestion: take out the heated quartz tube 2, cool it naturally for 12-24 hours, take out the quartz crucible in the quartz tube 2, add 3-7 ml of electronic grade nitric acid into the quartz crucible, put the quartz crucible with nitric acid on a heating plate at 130-170 ° C and heat it for 40-80 minutes to completely digest the residue in the quartz crucible; S5. Make up the volume: Take out the residual impurity elements in the quartz crucible, and make up the volume to 40-60ml with 5% dilute nitric acid for testing.

[0033] The fixed volume mixed solution is detected by ICP-MS (inductively coupled plasma mass spectrometer) to obtain the detection value of each element, thereby calculating the corresponding impurity content.

[0034] In view of current practical needs, the above-mentioned implementation mode adopted in this application is not limited to the scope of protection. Various changes made within the knowledge scope of technical personnel in this field without departing from the concept of this application still fall within the scope of protection of the present invention.

Claims

1. An impurity detection device for high-purity arsenic preparation, characterized in that: include: A heating component (1), the heating component (1) being used to heat a quartz tube (2) containing a sample, one end of the quartz tube (2) being connected to an air inlet pipe (3) and the other end of the quartz tube (2) being connected to an air outlet pipe (4); An exhaust gas treatment mechanism, the exhaust gas treatment mechanism is connected to the output end of the exhaust pipe (4) and is used to treat the gas generated when the sample is heated. The exhaust gas treatment mechanism comprises a fine filter cartridge (7), a liquid spraying pipe (16) arranged at the upper end of the inner cavity of the fine filter cartridge (7), a plurality of single filter cartridges (13) vertically arranged in the inner cavity of the fine filter cartridge (7), a dispersion chamber (12) arranged at the bottom of the inner cavity of the fine filter cartridge (7), and a transfer pipe (6) connected to the exhaust pipe (4), the bottom end of the single filter cartridge (13) is connected to the inner cavity of the dispersion chamber (12), the output end of the transfer pipe (6) is connected to the inner cavity of the dispersion chamber (12), and a flow rate sensor is installed in the transfer pipe (6). (21), an exhaust pipe connected to the upper end of the fine filter cartridge (7); an adjustable mesh cover (18), a regulating plate (22) and a regulating rope (19) connected to the bottom of the regulating plate (22) are arranged in the middle of the inner cavity of each single filter cartridge (13); a plurality of elastic ribs (8) are distributed circumferentially around the outer ring of the regulating rope (19); the bottom end of the elastic rib (8) is connected to the inner wall of the single filter cartridge (13) and the top end is in contact with the bottom surface of the regulating plate (22); the adjustable mesh cover (18) covers the outer ring of the elastic rib (8); and a pulling component is arranged at one end of the regulating rope (19) away from the regulating plate (22) for pulling the regulating rope (19) to move vertically; An intelligent detector (15), the intelligent detector (15) being arranged on the heating component (1), the intelligent detector (15) being provided with an analysis module and a control module, the input end of the analysis module being connected to a flow rate sensor (21) signal, the output end of the analysis module being connected to a control module signal, and the output end of the control module being connected to a pulling component signal.

2. The impurity detection device for preparing high-purity arsenic according to claim 1, characterized in that: The transfer pipe (6) is in communication with the inner cavity of the dispersion chamber (12); the bottom of the inner cavity of the dispersion chamber (12) is protruding at a position corresponding to the transfer pipe (6); and the bottom of the dispersion chamber (12) is in communication with a drainage pipe (9).

3. The impurity detection device for preparing high-purity arsenic according to claim 1, characterized in that: The pulling assembly comprises a control ring (29) rotatably connected to the bottom of the dispersion chamber (12), and a driving member (31) installed on the bottom of the dispersion chamber (12); the output end of the driving member (31) is in contact with the outer ring of the control ring (29) through a roller; the driving member (31) is used to drive the roller to rotate; a control rod (30) corresponding to the regulating rope (19) is fixed to the outer ring of the control ring (29); the bottom end of the regulating rope (19) passes through the dispersion chamber (12) and is fixed to the corresponding control rod (30); the output end of the regulating module is signal-connected to the driving member (31).

4. The impurity detection device for preparing high-purity arsenic according to claim 1, characterized in that: A flow distribution orifice plate (14) fixed to the inner wall of the fine filter cartridge (7) is provided below the shower pipe (16), and a through hole matching the single filter cartridge (13) is provided on the flow distribution orifice plate (14).

5. The impurity detection device for preparing high-purity arsenic according to claim 3, characterized in that: A second driving member (11) is installed on the top of the fine filter cartridge (7); a driving tube (20) connected to the shower tube (16) is fixed to the output end of the second driving member (11); the second driving member (11) is used to drive the driving tube (20) to rotate; a solenoid valve (17) is installed on the driving tube (20); a reaction liquid tube (10) is connected to the driving tube (20); the reaction liquid tube (10) is used to input the reaction liquid; a purification module is also provided on the intelligent detector (15); the output end of the purification module is respectively connected to the second driving member (11) and the solenoid valve (17) for signals; and the input end of the purification module is connected to the analysis module for signals.

6. The impurity detection device for preparing high-purity arsenic according to claim 5, characterized in that: A pressure measuring chamber (23) is arranged at the bottom of the regulating plate (22), the top of the regulating rope (19) is connected to the pressure measuring chamber (23), the top of the elastic rib (8) is in contact with the outer ring of the pressure measuring chamber (23), and a detection chamber (25) communicating with the inner cavity of the pressure measuring chamber (23) is provided at the upper end of the regulating plate (22). The inner cavity of the detection chamber (25) is vertically slidably connected to a piston plate (26), and a distance sensor (27) corresponding to the piston plate (26) is installed at the top of the detection chamber (25), and the input end of the analysis module is connected to the distance sensor (27) for signal.

7. The impurity detection device for preparing high-purity arsenic according to claim 6, characterized in that: The inner cavity of the pressure measuring chamber (23) is filled with a pressure measuring solution (24), the outer wall of the pressure measuring chamber (23) is an elastic abutment surface, and the elastic rib (8) is an arc-shaped structure.

8. The impurity detection device for preparing high-purity arsenic according to claim 7, characterized in that: An electromagnet (28) is installed on the top of the detection cavity (25), the piston plate (26) is made of a magnetic material, the bottom surface of the pressure measuring chamber (23) is in contact with the liquid surface of the pressure measuring solution (24), and the output end of the control module is connected to the electromagnet (28) signal.

9. The impurity detection device for preparing high-purity arsenic according to claim 1, characterized in that: A primary filter cartridge (5) is provided between the air outlet pipe (4) and the transfer pipe (6), a reaction liquid is added into the primary filter cartridge (5), an output end of the air outlet pipe (4) extends into the reaction liquid in the primary filter cartridge (5), and an input end of the transfer pipe (6) is in communication with the top of the inner cavity of the primary filter cartridge (5).

10. A detection method for an impurity detection device for preparing high-purity arsenic according to any one of claims 1 to 9, characterized in that: The following steps are involved: S1. Weighing: Weigh 5-10g of sample into a quartz crucible and record the sample weight; S2, heating: adjusting the temperature of the heating component (1) to between 300 and 350°C, placing the quartz crucible in the quartz tube (2), one end of the quartz tube (2) being sealedly connected to the air inlet pipe (3), and the other end of the quartz tube (2) being sealedly connected to the air outlet pipe (4), and placing the quartz tube (2) in the heating component (1) for heating; S3, arsenic exhaust purification: oxygen is introduced into the air inlet pipe (3), and the gas discharged from the air outlet pipe (4) is introduced into the waste gas treatment mechanism for purification. The gas rate introduced into the transfer pipe (6) is determined by the intelligent detector (15), and the reaction purification effect of the waste gas treatment mechanism is adjusted. The gas after reaction purification is discharged through the exhaust pipe and collected; S4, furnace digestion: take out the heated quartz tube (2), cool it naturally for 12-24 hours, take out the quartz crucible in the quartz tube (2), add 3-7 ml of electronic grade nitric acid into the quartz crucible, put the quartz crucible with nitric acid on a heating plate at 130-170° C. and heat it for 40-80 minutes to completely digest the residue in the quartz crucible; S5. Make up the volume: Take out the residual impurity elements in the quartz crucible, and make up the volume to 40-60ml with 5% dilute nitric acid for testing.

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