Impurity detection device and method for preparing high-purity arsenicTechnical Field
The invention relates to an impurity detection device, in particular to an impurity detection device and method for preparing high-purity arsenic, which are applied to the technical field of preparation of high-purity arsenic.
Background
The high-purity arsenic is mainly used for preparing semiconductor compounds such as gallium arsenide, gallium aluminum arsenide, indium arsenide and the like and high-purity alloys, has more and more wide application in the fields of medicine and health, corrosion resistance, dyes and the like, particularly gallium arsenide, has quite wide application, and in the preparation process of the high-purity arsenic, a quantitative sample is required to be selected for measuring the impurity content of the high-purity arsenic.
The invention patent with publication number CN102072833A discloses a sample preparation method for measuring impurity elements in high-purity arsenic by an ICP-MS method, which comprises the steps of weighing high-purity arsenic, obtaining high-purity arsenic with mass m, placing all the weighed high-purity arsenic in a quartz tube, introducing oxygen into the quartz tube at 300-350 ℃, cooling the quartz tube to normal temperature after the high-purity arsenic is oxidized to form arsenic oxide, sublimating and removing, taking out a quartz crucible with residues left in the quartz tube, adding electronic-grade nitric acid into the quartz crucible, heating on a heating plate at 150 ℃ until the temperature is lower than 10% by mass, and adding dilute nitric acid solution with mass percentage concentration into the crucible for constant volume to obtain the total volume with constant volume.
In the scheme, when high-purity arsenic in a quartz tube is heated and oxidized, the formed arsenic oxide has certain toxicity, and is discharged in a mode of ventilation and arsenic discharge (eliminating matrix As interference), wherein a silica gel plastic hose is used for introducing a glass container containing aqueous solution into an air outlet of the quartz tube (the plastic hose is inserted 5mm below the water surface), oxygen is introduced into an air inlet of the quartz tube, according to the vapor pressure difference, a compound As2O3 of matrix element As is sublimated and removed at the temperature of 300-350 ℃ due to the vapor pressure, impurity elements with low vapor pressure remain in the quartz crucible, and during the operation, discharged arsenic oxide gas is absorbed through the aqueous solution, and cannot be fully mixed with the aqueous solution after the gas is introduced, so that the treatment effect is poor, and the body health of experimental staff is affected.
Disclosure of Invention
Aiming at the prior art, the invention aims to solve the technical problems that the discharged arsenic oxide gas is absorbed by the aqueous solution, and the discharged arsenic oxide gas is not fully mixed with the aqueous solution after being introduced, so that the treatment effect is poor and the physical health of experimental staff is affected.
In order to solve the above problems, the present invention provides an impurity detection device for preparing high purity arsenic, comprising:
The heating component is used for heating the quartz tube filled with the sample, one end of the quartz tube is connected with an air inlet tube, and the other end of the quartz tube is connected with an air outlet tube;
The waste gas treatment mechanism is connected with the output end of the air outlet pipe and is used for treating gas generated when a sample is heated, the waste gas treatment mechanism comprises a fine filter cylinder, a liquid spraying pipe arranged at the upper end of the inner cavity of the fine filter cylinder, a plurality of single filter cylinders vertically arranged at the inner cavity of the fine filter cylinder, a dispersion chamber arranged at the bottom of the inner cavity of the fine filter cylinder, a transfer pipe communicated with the air outlet pipe, the bottom end of the single filter cylinder 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 arranged in the transfer pipe, and an exhaust pipe communicated with the upper end of the fine filter cylinder;
The intelligent detector is arranged on the heating component, an analysis module and a regulation and control module are arranged on the intelligent detector, the input end of the analysis module is connected with the flow rate sensor through signals, the output end of the analysis module is connected with the regulation and control module through signals, and the output end of the regulation and control module is connected with the pulling component through signals.
According to the impurity detection device for preparing high-purity arsenic, when sample impurities are detected, the corresponding reaction purification efficiency can be adjusted according to the harmful gas amount generated in the detection test, and the purpose of intelligently adjusting the purification effect is achieved.
As a further improvement of the application, the transfer pipe is communicated with the inner cavity of the dispersion chamber, the bottom of the inner cavity of the dispersion chamber is arranged in a protruding way at the position corresponding to the transfer pipe, and the bottom of the dispersion chamber is communicated with the liquid discharge pipe.
As a further improvement of the application, the pulling assembly comprises a control ring rotationally connected with the bottom of the dispersion chamber, and a first driving piece installed on the bottom of the dispersion chamber, wherein the output end of the first driving piece is propped against the outer ring of the control ring through a roller, the first driving piece is used for driving the roller to rotate, the outer ring of the control ring is fixedly provided with a control rod corresponding to a regulating rope, the bottom end of the regulating rope penetrates through the dispersion chamber and is fixedly connected with the corresponding control rod, and the output end of the regulating module is in signal connection with the first driving piece.
As a further improvement of the application, a split-flow pore plate fixed with the inner wall of the fine filter cylinder is arranged below the liquid spraying pipe, and a through hole matched with the single filter cylinder is arranged on the split-flow pore plate.
As a further improvement of the application, a second driving piece is arranged at the top of the refined filtering cylinder, a driving pipe communicated with the liquid spraying pipe is fixed at the output end of the second driving piece, the second driving piece is used for driving the driving pipe to rotate, an electromagnetic valve is arranged on the driving pipe, a reaction liquid pipe is communicated with the driving pipe and used for inputting reaction liquid, a purifying module is further arranged on the intelligent detector, the output end of the purifying module is respectively connected with the second driving piece and the electromagnetic valve through signals, and the input end of the purifying module is connected with the analyzing module through signals.
As a further improvement of the application, the bottom of the regulating plate is provided with a pressure measuring chamber, the top of the regulating rope is connected with the pressure measuring chamber, the top of the elastic rib is abutted against the outer ring of the pressure measuring chamber, the upper end of the regulating plate is provided with a detection cavity communicated with the inner cavity of the pressure measuring chamber, the inner cavity of the detection cavity is vertically and slidably connected with a piston plate, the top of the detection cavity is provided with a distance sensor corresponding to the piston plate, and the input end of the analysis module is in signal connection with the distance sensor.
As a further improvement of the application, the inner cavity of the pressure measuring chamber is filled with pressure measuring solution, the outer wall of the pressure measuring chamber is an elastic abutting surface, and the elastic ribs are arc-shaped structures.
In addition to the improvement of the application, an electromagnet is arranged at the top of the detection cavity, the piston plate is made of a magnet material, the bottom surface of the pressure measuring chamber is contacted with the liquid level of the pressure measuring solution, and the output end of the regulating and controlling module is connected with the electromagnet through signals.
As a further improved supplement of the application, a primary filter cylinder is arranged between the air outlet pipe and the transfer pipe, the reaction liquid is added in the primary filter cylinder, the output end of the air outlet pipe extends into the reaction liquid of the primary filter cylinder, and the input end of the transfer pipe is communicated with the top of the inner cavity of the primary filter cylinder.
The detection method of the impurity detection device for preparing the high-purity arsenic comprises the following steps of:
S1, weighing 5-10g of a sample, placing the sample into a quartz crucible, and recording the weight of the sample;
S2, heating, namely adjusting the temperature of the heating component to 300-350 ℃, placing the quartz crucible into a quartz tube, sealing one end of the quartz tube with an air inlet pipe, sealing the other end of the quartz tube with an air outlet pipe, and placing the quartz tube into the heating component for heating;
S3, arsenic removal and purification, namely introducing oxygen into an air inlet pipe, introducing gas exhausted from an air outlet pipe into an exhaust gas treatment mechanism for purification, judging the gas rate introduced into a transfer pipe through an intelligent detector, adjusting the reaction purification effect of the exhaust gas treatment mechanism, and exhausting and collecting the gas after reaction purification through an exhaust pipe;
S4, discharging and digesting, namely taking out the heated quartz tube, naturally cooling for 12-24 hours, taking out the quartz crucible in the quartz tube, adding 3-7ml of electronic grade nitric acid into the quartz crucible, and heating the crucible with the added nitric acid on a heating plate at 130-170 ℃ for 40-80 minutes to completely digest residues in the quartz crucible;
S5, constant volume, namely taking out residual impurity elements in the quartz crucible, and using dilute nitric acid with the mass concentration of 5% to constant volume to 40-60ml for detection.
In summary, when detecting sample impurity, the harmful gas that produces is introduced into the smart cartridge filter through the transfer pipe and reacts and purify, through drenching liquid pipe exhaust reaction liquid and throwing to each single cartridge, and to the adjustable screen panel surface infiltration in each single cartridge, the gas fully reacts with the reaction liquid that infiltrates on the adjustable screen panel when passing through single cartridge, improve the purifying effect to harmful gas, and through setting up intelligent detector, analysis module judges the gas volume that enters into the dispersion chamber through velocity of flow data, intelligent adjustment regulation and control board reciprocates, thereby adjust the surface area of adjustable screen panel, adjust the reaction effect of the reaction liquid that infiltrates on gas and the adjustable screen panel, can be according to the adaptive adjustment reaction purifying capacity of air current velocity, the purification efficiency of device is improved, the use amount of reaction liquid is practiced thrift, and resources are saved.
Drawings
FIG. 1 is a schematic view showing the overall structure of a first and a second embodiment of the present application;
FIG. 2 is a schematic cross-sectional view of a fine filter cartridge according to a first and second embodiment of the present application;
FIG. 3 is a schematic cross-sectional view of a single cartridge of the first and second embodiments of the present application;
fig. 4 is a front cross-sectional view of a cartridge filter cartridge of the first and second embodiments of the present application;
FIG. 5 is a schematic diagram of intelligent detection control according to a first embodiment of the present application;
FIG. 6 is a schematic view of a pulling assembly according to a first and second embodiment of the present application;
FIG. 7 is a schematic cross-sectional view of an adjustable mesh enclosure and a regulator plate according to first and second embodiments of the present application;
Fig. 8 is a schematic diagram of intelligent detection control according to a second embodiment of the present application.
The reference numerals in the figures illustrate:
1. The device comprises a heating component, 2, a quartz tube, 3, an air inlet tube, 4, an air outlet tube, 5, a primary filter tube, 6, a transfer tube, 7, a fine filter tube, 8, an elastic rib, 9, a liquid discharge tube, 10, a reaction liquid tube, 11, a second driving part, 12, a dispersion chamber, 13, a single filter tube, 14, a split orifice plate, 15, an intelligent detector, 16, a liquid spraying tube, 17, an electromagnetic valve, 18, an adjustable net cover, 19, a regulating rope, 20, a driving tube, 21, a flow rate sensor, 22, a regulating plate, 23, a pressure measuring chamber, 24, a pressure measuring solution, 25, a detecting cavity, 26, a piston plate, 27, a distance sensor, 28, an electromagnet, 29, a control ring, 30, a control rod and 31, and a first driving part.
Detailed Description
Two embodiments of the present application will be described in detail with reference to the accompanying drawings.
First embodiment:
Fig. 1-6 show an impurity detection device for preparing high-purity arsenic, which comprises a heating component 1, an exhaust gas treatment mechanism, an intelligent detector 15 and a leaching tube 16, wherein the heating component 1 is used for heating a quartz tube 2 filled with a sample, the heating component 1 is equipment for heating an experimental sample in the prior art, is common heating equipment in the field, has a function of heating the sample to a specified temperature, and has a specific structure and an operating principle, the technical scheme is not repeated, one end of the quartz tube 2 is connected with an air inlet tube 3, the other end of the quartz tube is connected with an air outlet tube 4, the sample with specified mass is added into a quartz crucible, the quartz crucible is placed into the quartz tube 2, the quartz tube 2 is placed onto the heating component 1 for heating treatment, one end of the quartz tube 2 is communicated with the air inlet tube 3, the other end of the quartz tube is communicated with the air outlet tube 4, oxygen is introduced into the heated sample through the air inlet tube 3 for oxidization, arsenic oxide is discharged through the air outlet tube 4, and interference of matrix arsenic on impurity measurement is eliminated.
It should be noted that, referring to fig. 2-4, the exhaust gas treatment mechanism is connected to the output end of the air outlet pipe 4, and is used for treating the gas generated when the sample is heated, the exhaust gas treatment mechanism includes a fine filtration cylinder 7, a shower pipe 16 disposed at the upper end of the inner cavity of the fine filtration cylinder 7, a plurality of single filtration cylinders 13 vertically disposed in the inner cavity of the fine filtration cylinder 7, a dispersion chamber 12 disposed at the bottom of the inner cavity of the fine filtration cylinder 7, and a transfer pipe 6 communicated with the air outlet pipe 4, the bottom end of the single filtration cylinder 13 is communicated with the inner cavity of the dispersion chamber 12, the output end of the transfer pipe 6 is communicated with 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 split into the plurality of single filtration cylinders 13 through the dispersion chamber 12, the gas flows towards the top of the fine filtration cylinder 7, the shower pipe 16 sprays the reaction liquid to react with arsenic oxide, the reaction liquid is 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 filtration cylinder 7 is communicated with the air outlet pipe 6, the treated gas is discharged or collected through the exhaust pipe, the hazard degree is reduced, the safety of the discharged gas is improved; the middle part of the inner cavity of each single filter cylinder 13 is provided with an adjustable mesh enclosure 18, a regulating plate 22 and a regulating rope 19 connected with the bottom of the regulating plate 22, a plurality of elastic ribs 8 are circumferentially distributed on the outer ring of the regulating rope 19, the bottom ends of the elastic ribs 8 are connected with the inner wall of the single filter cylinder 13, the top ends of the elastic ribs are propped against the bottom surface of the regulating plate 22, the adjustable mesh enclosure 18 covers the outer ring of the elastic ribs 8, the adjustable mesh enclosure 18 is made of corrosion-resistant cloth, preferably polyester elastic cloth, has better air permeability, corrosion resistance and elasticity, one end of the regulating rope 19 away from the regulating plate 22 is provided with a pulling component, the adjustable mesh enclosure is used for pulling the regulating ropes 19 to vertically move, reaction liquid discharged through the liquid spraying pipes 16 can fall into each single filter cartridge 13 and fully infiltrate the adjustable mesh enclosure 18, gas introduced from the bottom of each single filter cartridge 13 can pass through the adjustable mesh enclosure 18 infiltrated with the reaction liquid, so that the gas can fully contact and react with the reaction liquid, the reaction and purification effect of the gas are improved, the regulating plate 22 is driven to move up and down through the regulating ropes 19 by the aid of the arrangement of the plurality of elastic ribs 8, the tops of the plurality of elastic ribs 8 can be folded inwards when the regulating plate 22 moves downwards, the spherical surface area of the outer rings of the plurality of elastic ribs 8 is reduced, and therefore the area of the adjustable mesh enclosure 18 is increased, the surface area of the adjustable mesh enclosure 18 can be increased by adjusting the surface area of the plurality of elastic ribs 8, the corresponding reaction purification effect is adjusted according to the quantity of gas generated during detection, the corresponding reaction purification effect is adjusted adaptively, the reaction effect is better purified, the consumption of the reaction liquid is saved, and resources are saved.
In this embodiment, the intelligent detector 15 is disposed on the heating component 1, the intelligent detector 15 is provided with an analysis module and a regulation module, the input end of the analysis module is in signal connection with the flow rate sensor 21, the output end of the analysis module is in signal connection with the regulation module, the output end of the regulation module is in signal connection with the pulling component, when the gas input through the transfer pipe 6 is purified by the fine filtration pipe 7, the reaction liquid discharged by the shower pipe 16 is sprayed into each single filtration cylinder 13 and infiltrates the surface of the adjustable mesh enclosure 18 in each single filtration cylinder 13, the gas fully reacts with the reaction liquid infiltrated on the adjustable mesh enclosure 18 when passing through the single filtration cylinder 13, the flow rate sensor 21 is used for detecting the flow rate data of the gas entering the transfer pipe 6 and sending the flow rate data to the analysis module in real time, the analysis module judges the amount of the 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 the gas, the regulation module is controlled by controlling the pulling component to work, the control rope 19 is controlled to move up and down, thereby the corresponding regulation plate 22 is controlled to move up and down, the surface area of the adjustable mesh enclosure 18 is regulated, the flow rate is adjusted, the flow rate efficiency is adjusted, the reaction purification efficiency is improved, and the reaction liquid consumption is adjusted, and the purification efficiency is improved.
It should be noted that, referring to fig. 5 and 6, the pulling assembly includes a control ring 29 rotatably connected to the bottom of the dispersion chamber 12, a first driving member 31 installed at the bottom of the dispersion chamber 12, where an output end of the first driving member 31 is abutted to an 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 control rope 19 is fixed to the outer ring of the control ring 29, a bottom end of the control rope 19 penetrates through the dispersion chamber 12 and is fixed to the corresponding control rod 30, an output end of the control module is connected with the first driving member 31 in a signal manner, when the pulling assembly is adjusted by the control module, the corresponding driving member 31 is controlled to work, the first driving member 31 drives the control ring 29 to rotate forward or reverse through the roller, so as to drive the control rod 30 of the outer ring to swing, the control rod 30 swings to drive the control rope 19 connected to an end of the control ring to move, thereby achieving the purpose of pulling the control rope 19, and synchronously controlling the control plate 22 to move up and down.
In addition, install driving piece two 11 at the top of cartridge filter 7, driving piece two 11's output is fixed with the driving pipe 20 that is linked together with drenching liquid pipe 16, driving piece two 11 is used for driving pipe 20 and rotates, driving piece two 11 is preferably motor or air motor, install solenoid valve 17 on the driving pipe 20, the intercommunication has reaction liquid pipe 10 on the driving pipe 20, reaction liquid pipe 10 is used for the input reaction liquid, the tip and the driving pipe 20 of reaction liquid pipe 10 cup joint mutually, and both inner chambers are linked together, reaction liquid is through reaction liquid pipe 10 input to in the driving pipe 20, and spray out through drenching liquid pipe 16, still be provided with purification module on the intellectual detector 15, purification module's output respectively with driving piece two 11 and solenoid valve 17 signal connection, purification module's input and analysis module signal connection, at impurity detection start time, analysis module can send the purifying signal for purification module, purification module control driving piece two 11 work and solenoid valve 17 open, driving piece two 11 drive liquid pipe 16 through driving pipe 16 rotates, in every single harmful gas of reaction liquid pipe 10, the even tip, it is to improve to spray in each filter cartridge, the corresponding to the filter cartridge 21, when the flow rate of the corresponding sensor is opened at the corresponding to the flow rate of the analysis module, can be adjusted to the air flow rate, the air flow can be adjusted when the corresponding to the flow rate of the air is reduced, the control effect is adjusted, and the surface can be adjusted, and the purification effect is adjusted, and the surface can be adjusted and the purification is improved.
Preferably, the transfer pipe 6 is communicated with the inner cavity of the dispersion chamber 12, the bottom of the inner cavity of the dispersion chamber 12 is arranged in a protruding manner at the position corresponding to the transfer pipe 6, the bottom of the dispersion chamber 12 is communicated with the drain pipe 9, harmful gas is input into the inner cavity of the dispersion chamber 12 through the transfer pipe 6 and is shunted into each single filter cylinder 13 through the dispersion chamber 12, after reaction or unreacted reaction liquid falls into the inner cavity of the dispersion chamber 12 and is discharged and recycled through the drain pipe 9, as the bottom of the inner cavity of the dispersion chamber 12 is arranged in a protruding manner at the position corresponding to the transfer pipe 6, the reaction liquid entering the dispersion chamber 12 can be reduced to flow into the transfer pipe 6, the transfer pipe 6 is not easy to block, a shunt pore plate 14 fixed with the inner wall of the fine filter cylinder 7 is arranged below the shunt pore plate 14, through holes matched with the single filter cylinders 13 are formed in the shunt pore plate 14, and the reaction liquid discharged through the shunt pore plate 16 into each single filter cylinder 13, so that the uniformity of the reaction liquid flowing into each single filter cylinder 13 is improved.
In this embodiment, referring to fig. 1 and 2, a primary filter cartridge 5 is disposed between an air outlet pipe 4and a transfer pipe 6, a reaction liquid is added in the primary filter cartridge 5, the reaction liquid added in the primary filter cartridge 5 is the same as the reaction liquid input in a reaction liquid pipe 10, and is preferably an alkaline solution, calcium hydroxide or magnesium hydroxide solution, an output end of the air outlet pipe 4 extends into the reaction liquid in the primary filter cartridge 5, an input end of the transfer pipe 6 is communicated with the top of an inner cavity of the primary filter cartridge 5, gas entering through the air outlet pipe 4 can enter the primary filter cartridge 5 to perform primary reaction with the reaction liquid, meanwhile, the temperature of the gas can be reduced, damage to an adjustable mesh enclosure 18 is reduced, and the gas after the primary reaction with the reaction liquid in the primary filter cartridge 5 is input into the transfer pipe 6, so that the gas enters a dispersion chamber 12 in a fine filter cartridge 7 to perform fine purification again, and the purification effect on the gas is improved.
Second embodiment:
The impurity detection device for preparing high-purity arsenic shown in fig. 4 and 7-8 is different from the first embodiment in that the bottom of the regulating plate 22 is provided with a pressure measuring chamber 23, the top of the regulating rope 19 is connected with the pressure measuring chamber 23, the top of the elastic rib 8 is abutted against the outer ring of the pressure measuring chamber 23, the upper end of the regulating plate 22 is provided with a detection cavity 25 communicated with the inner cavity of the pressure measuring chamber 23, the inner cavity of the detection cavity 25 is vertically and slidably connected with a piston plate 26, the top of the detection cavity 25 is provided with a distance sensor 27 corresponding to the piston plate 26, the input end of the analysis module is in signal connection with the distance sensor 27, the regulating rope 19 is pulled to drive the pressure measuring chamber 23 to synchronously drive the regulating plate 22 to move up and down, when the end of the plurality of elastic ribs 8 are retracted or expanded, the outer wall of the pressure measuring chamber 23 is subjected to extrusion, the inner cavity gas flow can be changed when the outer wall of the pressure measuring chamber 23 is extruded, the piston push the piston plate 26 is communicated with the inner cavity of the pressure measuring chamber 23, the piston plate 26 can be synchronously pushed up and down, the distance sensor 27 is correspondingly controlled by the distance sensor 27, the filter cylinder cover 13 can be accurately adjusted by the distance sensor 27, and the filter cylinder 13 can be accurately adjusted by the distance sensor 13 corresponding to the position sensor 13.
In addition, when the surface mesh of adjustable screen panel 18 is blocked gradually, the gas that gets into through single section of thick bamboo 13 can form certain thrust to adjustable screen panel 18 to will change the effort of elastic rib 8 top to the pressure measurement room 23 outer lane, and then change the distance data that distance sensor 27 detected, analysis module judges the surface blocking condition of every adjustable screen panel 18 according to distance sensor 27's detection data, the experimenter of being convenient for in time adjusts the maintenance to it, cleans or changes adjustable screen panel 18, makes the device have better purifying effect all the time, and improves the convenience that the device was maintained.
In this embodiment, the inner cavity of the pressure measuring chamber 23 is filled with the pressure measuring solution 24, the outer wall of the pressure measuring chamber 23 is an elastic abutting surface, the pressure measuring solution 24 can be a liquid with larger concentration, after the elastic abutting surface of the pressure measuring chamber 23 is stressed, the flowing degree of the pressure measuring solution 24 is more sensitive, the corresponding piston plate 26 is pushed to displace, the detection precision of the distance sensor 27 is improved, the elastic ribs 8 are of arc structures, the elastic ribs 8 of the arc structures can play a better supporting role on the adjustable mesh enclosure 18, the adjustable mesh enclosure 18 is completely stretched and wrinkles are reduced, and the reaction liquid is fully reacted with the gas for purification.
In addition, electromagnet 28 is installed at the top of detection chamber 25, piston plate 26 is the magnet material, the bottom surface of pressure measurement room 23 contacts with the liquid level of pressure measurement solution 24, the output of regulation and control module is connected with electromagnet 28 signal, through controlling the electric current direction and the electric current size that lets in electromagnet 28, can control electromagnet 28 produce the magnetism of different directions and different intensity, thereby control piston plate 26 and be close to or keep away from electromagnet 28, and control the distance between the two, thereby adjust the compression degree to pressure measurement solution 24 of pressure measurement room 23 inner chamber, further adjust the position on the top of elastic rib 8 that is located pressure measurement room 23 outer lane, control elastic rib 8 expansion or contraction degree, can initiatively adjust the expansion area of adjustable screen panel 18 in each single section 13, can accurately adjust the expansion degree of adjustable screen panel 18 in each single section 13, thereby adjust the reaction purifying effect of corresponding single section 13, carry out the adaptation adjustment according to the gas velocity, improve the purifying effect of device.
The detection method of the impurity detection device for preparing the high-purity arsenic comprises the following steps of:
S1, weighing 5-10g of a sample, placing the sample into a quartz crucible, and recording the weight of the sample;
s2, heating, namely adjusting the temperature of the heating assembly 1 to 300-350 ℃, placing a quartz crucible into the quartz tube 2, sealing one end of the quartz tube 2 with the air inlet tube 3, sealing the other end with the air outlet tube 4, and placing the quartz tube 2 into the heating assembly 1 for heating;
S3, arsenic removal and purification, namely introducing oxygen into the air inlet pipe 3, introducing gas exhausted from the air outlet pipe 4 into the waste gas treatment mechanism for purification, judging the gas rate introduced into the transfer pipe 6 through the intelligent detector 15, adjusting the reaction purification effect of the waste gas treatment mechanism, and discharging and collecting the gas after reaction purification through the air outlet pipe;
S4, discharging and digesting, namely taking out the heated quartz tube 2, naturally cooling for 12-24 hours, taking out the quartz crucible in the quartz tube 2, adding 3-7ml of electronic grade nitric acid into the quartz crucible, and heating the quartz crucible with the nitric acid on a heating plate at 130-170 ℃ for 40-80 minutes to completely digest residues in the quartz crucible;
S5, constant volume, namely taking out residual impurity elements in the quartz crucible, and using dilute nitric acid with the mass concentration of 5% to constant volume to 40-60ml for detection.
And detecting the mixed solution with the constant volume by ICP-MS (inductively coupled plasma mass spectrometer) to obtain detection values of all elements, thereby calculating the corresponding impurity content.
The present application is not limited to the above-described embodiments, which are adopted in connection with the actual demands, and various changes made by the person skilled in the art without departing from the spirit of the present application are still within the scope of the present application.