An impurity detection device and method for preparing high-purity arsenic

Abstract

The present invention relates to an impurity detection device and method for the preparation of high-purity arsenic, which are applied to the technical field of high-purity arsenic preparation. The impurity detection device includes a heating component, an exhaust gas treatment mechanism, and an intelligent detector. The exhaust gas treatment mechanism includes a fine filter cartridge, a liquid spraying 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 communicated with an air outlet pipe. An adjustable mesh cover, a regulation plate, and a regulation rope connected to the bottom of the regulation plate are arranged in the middle of the inner cavity of each single filter cartridge, and a plurality of elastic rib strips are circumferentially distributed on the outer circumference of the regulation rope; an analysis module and a regulation module are arranged on the intelligent detector. With the above structure, when detecting sample impurities, the corresponding reaction purification efficiency can be adjusted according to the amount of harmful gas generated during the detection test, achieving the purpose of intelligent adjustment of the purification effect.

Description

Technical Field

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

[0002] High-purity arsenic is mainly used to prepare semiconductor compounds such as gallium arsenide, gallium aluminum arsenide, indium arsenide, and high-purity alloys, and has been increasingly widely used in the fields of medicine and health, anti-corrosion, dyes, etc. Especially gallium arsenide has quite extensive applications. During the preparation process of high-purity arsenic, it is necessary to select a quantitative sample to measure its impurity content.

[0003] The invention patent with the publication number CN102072833A discloses a sample preparation method for determining impurity elements in high-purity arsenic by ICP-MS method. By weighing high-purity arsenic to obtain the mass m of high-purity arsenic, all the weighed high-purity arsenic is placed in a quartz tube. Under the condition of 300 - 350 °C, oxygen is introduced into the quartz tube. After the high-purity arsenic is oxidized to form arsenic oxide and sublimated and removed, the quartz tube is cooled to room temperature, and a quartz crucible with residues left in the quartz tube is taken out; electronic-grade nitric acid is added into the quartz crucible, and it is heated on a hot plate at 150 °C until it is completely digested, and then a dilute nitric acid solution with a mass percentage concentration of not more than 10% is added into the crucible for volume determination to obtain the total volume of volume determination.

[0004] In the above solution, when heating and oxidizing the high-purity arsenic in the quartz tube, the formed arsenic oxide is somewhat toxic, and it is discharged by the method of discharging arsenic through ventilation (eliminating matrix As interference): at the air outlet of the quartz tube, it is introduced into a glass container filled with an aqueous solution through a silica gel plastic hose (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 sublimes and is removed at 300 - 350 °C due to its large vapor pressure, while the impurity elements with small vapor pressures remain in the quartz crucible. During the operation, the discharged 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 experimental personnel. Summary of the Invention

[0005] Aiming at the above-mentioned prior art, the technical problem to be solved by the present invention is that the discharged 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 experimental personnel.

[0006] To solve the above problems, the present invention provides an impurity detection device for preparing high-purity arsenic, including:

[0007] A heating component, which is used to heat a quartz tube containing a sample. One end of the quartz tube is connected with an air inlet pipe and the other end is connected with an air outlet pipe;

[0008] An exhaust gas treatment mechanism, which 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 spraying 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 communicated with the air outlet pipe. The bottom end of the single filter cartridge is communicated with the inner cavity of the dispersion chamber, the output end of the transfer pipe is communicated with the inner cavity of the dispersion chamber, a flow rate sensor is installed in the transfer pipe, and an exhaust pipe is communicated with the upper end of the fine filter cartridge; in the middle of the inner cavity of each single filter cartridge, an adjustable mesh cover, a regulation plate and a regulation rope connected to the bottom of the regulation plate are arranged. A plurality of elastic rib strips are circumferentially distributed on the outer circle of the regulation rope. The bottom end of the elastic rib strip is connected to the inner wall of the single filter cartridge and the top end abuts against the bottom surface of the regulation plate. The adjustable mesh cover covers the outer circle of the elastic rib strip. One end of the regulation rope far away from the regulation plate is provided with a pulling assembly for pulling the regulation rope to move vertically;

[0009] An intelligent detector is arranged on the heating assembly. The intelligent detector is provided with an analysis module and a regulation module. The input end of the analysis module is signal-connected to the flow rate sensor, the output end of the analysis module is signal-connected to the regulation module, and the output end of the regulation module is signal-connected to the pulling assembly.

[0010] In the above-mentioned impurity detection device for preparing high-purity arsenic, when detecting sample impurities, it can adjust the corresponding reaction purification efficiency according to the amount of harmful gas generated during the detection test, so as to achieve the purpose of intelligent adjustment of the purification effect.

[0011] As a further improvement of the present application, the transfer pipe is communicated with the inner cavity of the dispersion chamber. The bottom of the inner cavity of the dispersion chamber protrudes corresponding to the transfer pipe, and a drain pipe is communicated with the bottom of the dispersion chamber.

[0012] 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 first driving member installed at the bottom of the dispersion chamber. The output end of the first driving member abuts against the outer circle of the control ring through a roller. The first driving member is used to drive the roller to rotate. A control rod corresponding to the regulation rope is fixed on the outer circle of the control ring. The bottom end of the regulation rope penetrates through the dispersion chamber and is fixed to the corresponding control rod. The output end of the regulation module is signal-connected to the first driving member.

[0013] As a further improvement of the present application, a flow splitting orifice plate fixed to the inner wall of the fine filter cartridge is arranged below the liquid spraying pipe, and through holes matching the single filter cartridges are formed on the flow splitting orifice plate.

[0014] As a further improvement of the present application, a second driving member is installed at the top of the fine filter cartridge. A driving pipe communicated with the liquid spraying pipe is fixed at the output end of the second driving member. The second driving member is used to drive the driving pipe to rotate. An electromagnetic valve is installed on the driving pipe. A reaction liquid pipe is communicated with the driving pipe. The reaction liquid pipe is used to input reaction liquid. A purification module is further arranged on the intelligent detector. The output end of the purification module is respectively in signal connection with the second driving member and the electromagnetic valve. The input end of the purification module is in signal connection with the analysis module.

[0015] As a further improvement of the present application, a pressure measuring chamber is arranged at the bottom of the regulation plate. The top of the regulation rope is connected with the pressure measuring chamber. The top end of the elastic rib is abutted against the outer ring of the pressure measuring chamber. A detection chamber communicated with the inner cavity of the pressure measuring chamber is opened at the upper end of the regulation plate. A piston plate is vertically and slidably connected in the inner cavity of the detection chamber. A distance sensor corresponding to the piston plate is installed at the top of the detection chamber. The input end of the analysis module is in signal connection with the distance sensor.

[0016] 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 abutting surface. The elastic rib is of an arc structure.

[0017] As a supplementary improvement of the present application, an electromagnet is installed at the top of the detection chamber. The piston plate is made of a magnetic material. The bottom surface of the pressure measuring chamber is in contact with the liquid level of the pressure measuring solution. The output end of the regulation module is in signal connection with the electromagnet.

[0018] As a supplementary improvement of the present application, a primary filter cartridge is arranged between the air outlet pipe and the transfer pipe. A reaction liquid is added into the primary filter cartridge. The output end of the air outlet pipe extends into the reaction liquid in the primary filter cartridge. The input end of the transfer pipe is communicated with the top of the inner cavity of the primary filter cartridge.

[0019] A detection method for an impurity detection device for high-purity arsenic preparation includes the following steps:

[0020] S1. Weighing: Weigh 5 - 10 g of the sample and place it in a quartz crucible, and record the sample weight;

[0021] S2. Heating: Adjust the temperature of the heating component to between 300 - 350 °C. Place the quartz crucible into the quartz tube. One end of the quartz tube is hermetically connected to the air inlet pipe, and the other end is hermetically connected to the air outlet pipe. Place the quartz tube into the heating component for heating;

[0022] S3. Arsenic removal and purification: Pass oxygen into the air inlet pipe. The gas discharged from the air outlet pipe is introduced into the waste gas treatment mechanism for purification. Judge the gas rate introduced into the transfer pipe through the intelligent detector, and adjust the reaction and purification effect of the waste gas treatment mechanism. The gas after reaction and purification is discharged and collected through the exhaust pipe;

[0023] S4. Furnace discharging and digestion: Take out the heated quartz tube, let it cool 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, place the crucible with added nitric acid on a heating plate at 130 - 170 °C and heat for 40 - 80 minutes to completely digest the residue in the quartz crucible;

[0024] S5. Volume fixing: Take out the residual impurity elements in the quartz crucible, fix the volume to 40 - 60 ml with dilute nitric acid with a mass concentration of 5% for later detection.

[0025] In summary, when detecting the impurities of the sample, the harmful gases generated are introduced into the fine filter cartridge through the transfer pipe for reaction purification. The reaction liquid discharged through the leaching liquid pipe is sprinkled into each single filter cartridge, and the surface of the adjustable mesh cover in each single filter cartridge is wetted. When the gas passes through the single filter cartridge, it reacts fully with the reaction liquid wetted on the adjustable mesh cover, improving the purification effect of the harmful gases. And by setting up an intelligent detector, the analysis module judges the amount of gas entering the dispersion chamber through the flow rate data, and intelligently adjusts the up and down movement of the control board, thereby adjusting the surface area of the adjustable mesh cover and the reaction effect between the gas and the reaction liquid wetted on the adjustable mesh cover. It can adaptively adjust the reaction purification ability according to the gas flow rate, improve the purification efficiency of the device, save the usage amount of the reaction liquid, and save resources. Brief Description of the Drawings

[0026] Figure 1 It is a schematic diagram of the overall structure of the first and second embodiments of the present application;

[0027] Figure 2 It is a schematic cross-sectional view of the fine filter cartridge of the first and second embodiments of the present application;

[0028] Figure 3 It is a schematic cross-sectional view of the single filter cartridge of the first and second embodiments of the present application;

[0029] Figure 4 It is a front view of the schematic cross-section of the fine filter cartridge of the first and second embodiments of the present application;

[0030] Figure 5 It is a schematic diagram of the intelligent detection and control principle of the first embodiment of the present application;

[0031] Figure 6 It is a schematic diagram of the structure of the pulling component of the first and second embodiments of the present application;

[0032] Figure 7 It is a schematic cross-sectional view of the adjustable mesh cover and the control board of the first and second embodiments of the present application;

[0033] Figure 8 It is a schematic diagram of the intelligent detection and control principle of the second embodiment of the present application.

[0034] Description of reference numerals in the figure:

[0035] 1. Heating component; 2. Quartz tube; 3. Inlet pipe; 4. Outlet pipe; 5. Primary filter cartridge; 6. Transfer pipe; 7. Fine filter cartridge; 8. Elastic rib; 9. Drain pipe; 10. Reaction liquid pipe; 11. Second driving member; 12. Dispersion chamber; 13. Single filter cartridge; 14. Flow splitting orifice plate; 15. Intelligent detector; 16. Spraying liquid pipe; 17. Solenoid valve; 18. Adjustable mesh cover; 19. Regulation rope; 20. Driving pipe; 21. Flow rate sensor; 22. Regulation plate; 23. Pressure measurement chamber; 24. Pressure measurement solution; 25. Detection cavity; 26. Piston plate; 27. Distance sensor; 28. Electromagnet; 29. Control ring; 30. Control rod; 31. First driving member. Specific embodiments

[0036] The following describes two embodiments of the present application in detail with reference to the accompanying drawings.

[0037] The first embodiment:

[0038] Figures 1-6 There is shown an impurity detection device for the preparation of high-purity arsenic, including a heating component 1, an exhaust gas treatment mechanism, an intelligent detector 15 and a spraying liquid pipe 16. The heating component 1 is used to heat the quartz tube 2 containing the sample. The heating component 1 is a device for heating experimental samples in the prior art, a common heating device for those skilled in the art, having the function of heating the sample to a specified temperature. Its specific structure and working principle have been disclosed, and the technical solution of the present application will not elaborate on it. One end of the quartz tube 2 is connected to an inlet pipe 3 and the other end is connected to an outlet pipe 4. A specified mass of the sample is added to a quartz crucible, and then the quartz crucible is placed into 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 communicates with the inlet pipe 3 and the other end communicates with the outlet pipe 4. Oxygen is introduced into the heated sample through the inlet pipe 3 to oxidize it, and the arsenic oxide is discharged through the outlet pipe 4 to eliminate the interference of matrix arsenic on the impurity determination.

[0039] It is worth mentioning that, please refer to Figures 2-4, The waste gas treatment mechanism is connected to the output end of the air outlet pipe 4 and is used to treat the gas generated during sample heating. The waste gas treatment mechanism includes 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 communicating with the air outlet pipe 4. The bottom end of the single filter cartridge 13 is communicated with the inner cavity of the dispersion chamber 12, and the output end of the transfer pipe 6 is communicated with the inner cavity of the dispersion chamber 12. The gas to be treated discharged through the air outlet pipe 4 is input into the transfer pipe 6 and is shunted to a plurality of single filter cartridges 13 through the dispersion chamber 12. The gas flows towards the top of the fine filter cartridge 7, and the liquid spraying pipe 16 sprays a reaction liquid to react with arsenic trioxide. The reaction liquid is an alkaline solution, preferably 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 communicated with an exhaust pipe. The treated gas is discharged or collected through the exhaust pipe, reducing the harm degree of the discharged gas and improving the safety of the detection process; in the middle of the inner cavity of each single filter cartridge 13, an adjustable mesh cover 18, a regulation plate 22 and a regulation rope 19 connected to the bottom of the regulation plate 22 are arranged. A plurality of elastic rib strips 8 are circumferentially distributed on the outer circumference of the regulation rope 19. The bottom end of the elastic rib strip 8 is connected to the inner wall of the single filter cartridge 13 and the top end abuts against the bottom surface of the regulation plate 22. The adjustable mesh cover 18 covers the outer circumference of the elastic rib strips 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. One end of the regulation rope 19 far away from the regulation plate 22 is provided with a pulling assembly for pulling the regulation rope 19 to move vertically. The reaction liquid discharged through the liquid spraying pipe 16 will fall into each single filter cartridge 13 and fully wet 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 wetted with the reaction liquid, enabling the gas to fully contact and react with the reaction liquid, improving the reaction and purification effect on the gas. And by arranging a plurality of elastic rib strips 8, the regulation plate 22 is driven to move up and down through the regulation rope 19. When the regulation plate 22 moves down, the tops of the plurality of elastic rib strips 8 will close inward, reducing the spherical surface area formed by the outer circumference of the plurality of elastic rib strips 8, thereby reducing the area of the adjustable mesh cover 18; on the contrary, when the regulation plate 22 moves up, the tops of the plurality of elastic rib strips 8 will expand outward, increasing the spherical surface area formed by the outer circumference of the plurality of elastic rib strips 8, thereby increasing the area of the adjustable mesh cover 18. The surface area of the adjustable mesh cover 18 can be adjusted, and the corresponding reaction purification effect can be adjusted according to the amount of gas generated during detection, and the adjustment is adaptable to achieve a better purification effect, saving the use amount of the reaction liquid and saving resources.

[0040] In this embodiment, the intelligent detector 15 is arranged on the heating component 1. An analysis module and a regulation module are arranged on the intelligent detector 15. The input end of the analysis module is signal-connected to the flow rate sensor 21, the output end of the analysis module is signal-connected to the regulation module, and the output end of the regulation module is signal-connected to the pulling component. When the reaction purification of the gas input through the transfer pipe 6 is carried out by the fine filter cartridge 7, the reaction liquid discharged from the shower pipe 16 is sprinkled into each single filter cartridge 13, and the surface of the adjustable mesh cover 18 in each single filter cartridge 13 is wetted. When the gas passes through the single filter cartridge 13, it fully reacts with the reaction liquid wetted on the adjustable mesh cover 18. 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 judges the amount of gas entering the dispersion chamber 12 by analyzing the flow rate data and sends a corresponding regulation signal to the regulation module according to the amount of gas. The regulation module controls the pulling component to work, controls the regulation rope 19 to move up and down, and thus controls the corresponding regulation plate 22 to move up and down, adjusting the surface area of the adjustable mesh cover 18, so that the reaction purification ability can be adjusted adaptively according to the gas flow rate, improving the purification efficiency of the device and saving the usage amount of the reaction liquid.

[0041] It is worth mentioning that, please refer to Figure 5 and Figure 6 , the pulling component includes a control ring 29 rotatably connected to the bottom of the dispersion chamber 12 and a first driving member 31 installed on the bottom of the dispersion chamber 12. The output end of the first driving member 31 abuts against the outer ring of the control ring 29 through a roller. The first driving member 31 is used to drive the roller to rotate. The first driving member 31 is preferably a motor or a pneumatic motor. A control rod 30 corresponding to the regulation rope 19 is fixed on the outer ring of the control ring 29. The bottom end of the regulation rope 19 penetrates through the dispersion chamber 12 and is fixed to the corresponding control rod 30. The output end of the regulation module is signal-connected to the first driving member 31. When the pulling component is adjusted to work through the regulation module, the corresponding first driving member 31 will be controlled to work. The first driving member 31 drives the control ring 29 to rotate forward or backward through the roller, thereby driving the control rod 30 on the outer ring to swing. The swing of the control rod 30 drives the regulation rope 19 connected to its end to move, so as to achieve the purpose of pulling the regulation rope 19 and synchronously control the regulation plate 22 to move up and down.

[0042] In addition, a second driving member 11 is installed at the top of the fine filter cartridge 7. A driving pipe 20 communicating with the liquid spraying pipe 16 is fixed to the output end of the second driving member 11. The second driving member 11 is used to drive the driving pipe 20 to rotate. The second driving member 11 is preferably a motor or a pneumatic motor. A solenoid valve 17 is installed on the driving pipe 20. A reaction liquid pipe 10 is communicated with the driving pipe 20. The reaction liquid pipe 10 is used to input the reaction liquid. The end of the reaction liquid pipe 10 is sleeved with the driving pipe 20, and the inner cavities of the two are communicated. The reaction liquid is input into the driving pipe 20 through the reaction liquid pipe 10 and sprayed out through the liquid spraying pipe 16. A purification module is further arranged on the intelligent detector 15. The output end of the purification module is respectively in signal connection with the second driving member 11 and the solenoid valve 17. The input end of the purification module is in signal connection with the analysis module. At the beginning of impurity detection, the analysis module sends a purification signal to the purification module. The purification module controls the operation of the second driving member 11 and the opening of the solenoid valve 17. The second driving member 11 drives the liquid spraying pipe 16 to rotate through the driving pipe 20, and evenly sprays the reaction liquid into each single filter cartridge 13, improving the purification effect on harmful gases. When the analysis module judges the air flow velocity through the flow velocity sensor 21, when the flow velocity increases or decreases, a corresponding control signal for increasing or decreasing the purification effect will be sent to the purification module. The purification module will control the opening degree of the corresponding solenoid valve 17, so as to cooperate with adjusting the surface area of the adjustable mesh cover 18 and adjust the purification effect on harmful gases.

[0043] Preferably, the transfer pipe 6 is communicated with the inner cavity of the dispersion chamber 12. A protrusion is arranged at the bottom of the inner cavity of the dispersion chamber 12 corresponding to the transfer pipe 6. A drain pipe 9 is communicated with the bottom of the dispersion chamber 12. The harmful gas is input into the inner cavity of the dispersion chamber 12 through the transfer pipe 6 and is shunted 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 recycled through the drain pipe 9. Since a protrusion is arranged at the bottom of the inner cavity of the dispersion chamber 12 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 easily blocked. A diversion orifice plate 14 fixed to the inner wall of the fine filter cartridge 7 is arranged below the liquid spraying pipe 16. Through holes matching the single filter cartridges 13 are formed in the diversion orifice plate 14. The reaction liquid discharged through the liquid spraying pipe 16 will be diverted to each single filter cartridge 13 through the diversion orifice plate 14, improving the uniformity of the reaction liquid flowing into each single filter cartridge 13.

[0044] In this embodiment, please refer to Figure 1 and Figure 2, 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. The reaction liquid added into the primary filter cartridge 5 is the same as the reaction liquid input into the reaction liquid pipe 10, and both are alkaline solutions, preferably calcium hydroxide or magnesium hydroxide solutions. The output end of the air outlet pipe 4 extends into the reaction liquid in the primary filter cartridge 5. The input end of the transfer pipe 6 is communicated 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, react preliminarily with the reaction liquid, and at the same time can also reduce the temperature of the gas, reducing the damage to the adjustable mesh cover 18. The gas that has reacted preliminarily 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, where the gas is finely purified again to improve the purification effect of the gas.

[0045] The second implementation mode:

[0046] Figure 4 , Figures 7-8 An impurity detection device for preparing high-purity arsenic shown in the figure. Different from the first implementation mode, a pressure measurement chamber 23 is provided at the bottom of the regulation plate 22. The top of the regulation rope 19 is connected to the pressure measurement chamber 23. The top end of the elastic rib 8 abuts against the outer ring of the pressure measurement chamber 23. A detection chamber 25 communicated with the inner cavity of the pressure measurement chamber 23 is opened at the upper end of the regulation plate 22. A piston plate 26 is vertically slidably connected to the inner cavity of the detection chamber 25. A distance sensor 27 corresponding to the piston plate 26 is installed at the top of the detection chamber 25. The input end of the analysis module is signal-connected to the distance sensor 27. By pulling the regulation rope 19, the pressure measurement chamber 23 will be driven to move, thereby synchronously driving the regulation plate 22 to move up and down. When the ends of the plurality of elastic ribs 8 retract or expand, different extrusion forces will be formed on the outer wall of the pressure measurement chamber 23. When the outer wall of the pressure measurement chamber 23 is squeezed, the gas flow in its inner cavity will be changed. Since the detection chamber 25 is communicated with the inner cavity of the pressure measurement chamber 23, the piston plate 26 will be synchronously pushed to move up and down, and the distance data from the piston plate 26 is detected by the distance sensor 27. The analysis module judges the position of the piston plate 26 through the distance data fed back by the distance sensor 27, so as to be able to judge the expansion degree of the elastic rib 8 in the corresponding single filter cartridge 13, and thus accurately judge the unfolded area of the adjustable mesh cover 18 on each single filter cartridge 13, and understand the reaction purification ability of the adjustable mesh cover 18 at the corresponding single filter cartridge 13.

[0047] In addition, when the surface mesh holes of the adjustable mesh cover 18 are gradually blocked, the gas entering through the single filter cartridge 13 will form a certain thrust on the adjustable mesh cover 18, thereby changing the acting force of the top of the elastic rib 8 on the outer ring of the pressure measuring chamber 23. Furthermore, the distance data detected by the distance sensor 27 is changed. The analysis module judges the blockage condition of the surface 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.

[0048] 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 abutting surface. The pressure measuring solution 24 can be a liquid with a relatively high concentration. After the elastic abutting surface of the pressure measuring chamber 23 is stressed, the flow degree of the pressure measuring solution 24 is more sensitive, and it pushes the corresponding piston plate 26 to displace, improving the detection accuracy of the distance sensor 27. The elastic rib 8 is an arc-shaped structure, and the arc-shaped elastic rib 8 can play a good supporting role for the adjustable mesh cover 18, fully stretching the adjustable mesh cover 18 and reducing wrinkles, so that the reaction liquid can fully react with the gas for purification.

[0049] In addition, an electromagnet 28 is installed at the top of the detection chamber 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. The output end of the control module is signal-connected to the electromagnet 28. By controlling the direction and magnitude of the current applied to the electromagnet 28, different directions and intensities of magnetism can be generated by the electromagnet 28, thereby controlling the piston plate 26 to approach or move away from the electromagnet 28 and controlling the distance between the two, so as to adjust the compression degree of the pressure measuring solution 24 in the inner cavity of the pressure measuring chamber 23, further adjusting the position of the top of the elastic rib 8 located on the outer ring of the pressure measuring chamber 23, controlling the expansion or contraction degree of the elastic rib 8, actively adjusting the unfolding area of the adjustable mesh cover 18 in each single filter cartridge 13, accurately adjusting the unfolding degree of the adjustable mesh cover 18 in each single filter cartridge 13, thereby adjusting the reaction purification effect of the corresponding single filter cartridge 13, making an adaptive adjustment according to the gas flow rate, and improving the purification effect of the device.

[0050] A detection method for an impurity detection device for high-purity arsenic preparation includes the following steps:

[0051] S1. Weighing: Weigh 5-10 g of the sample and place it in a quartz crucible, and record the sample weight;

[0052] 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 hermetically connected to the air inlet pipe 3, and the other end is hermetically connected to the air outlet pipe 4. Place the quartz tube 2 in the heating component 1 for heating;

[0053] S3. Arsenic removal and purification: Oxygen is introduced into the intake pipe 3, and the gas discharged from the 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 purification is discharged and collected through the exhaust pipe;

[0054] S4. Furnace removal and digestion: Take out the heated quartz tube 2, naturally cool it 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, and place the quartz crucible with added 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;

[0055] S5. Volume fixing: Take out the residual impurity elements in the quartz crucible, and fix the volume to 40 - 60 ml with dilute nitric acid with a mass concentration of 5% for detection.

[0056] The fixed - volume mixed solution is detected by ICP - MS (Inductively Coupled Plasma Mass Spectrometer) to obtain the detection values of each element, and then the corresponding impurity content is calculated.

[0057] Combined with the current actual requirements, the above - mentioned implementation manner adopted in this application, the protection scope is not limited to this. Within the knowledge scope of those skilled in the art, various changes made without departing from the concept of this application still fall within the protection scope 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) by signal, the output end of the analysis module being connected to a control module by signal, and the output end of the control module being connected to a pulling component by signal; 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).

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: 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).

4. The impurity detection device for preparing high-purity arsenic according to claim 1, 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.

5. The impurity detection device for preparing high-purity arsenic according to claim 4, 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.

6. The impurity detection device for preparing high-purity arsenic according to claim 5, 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.

7. The impurity detection device for preparing high-purity arsenic according to claim 6, 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.

8. 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).

9. A detection method for an impurity detection device for preparing high-purity arsenic according to any one of claims 1 to 8, 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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