Electronic grade potassium fluotantalate sampling detection method

Abstract

The invention discloses an electronic-grade potassium fluotantalate sampling detection method, which relates to the technical field of charging piles, and specifically comprises the following steps: step 1, sample preparation, step 2, instrument setting, and step 3, determination and data analysis. According to the electronic-grade potassium fluotantalate sampling detection method, intermittent and forward and reverse reciprocating stirring of a potassium fluotantalate solution is realized by starting a series of linkage mechanisms driven by a servo motor, and the stirring mode is beneficial to breaking the local concentration gradient in the solution, so that potassium fluotantalate molecules are more uniformly dispersed in a solvent, and the detection accuracy is improved. Therefore, the dissolving speed and efficiency are obviously improved; under the condition that hydrofluoric acid, nitric acid and other acid solutions are added, stirring is beneficial to accelerating chemical reaction, and when potassium fluotantalate reacts with the acids, stirring can ensure full contact between reactants, so that the reaction rate and the conversion rate are increased.

Description

Technical Field

[0001] The invention relates to the technical field of detection equipment, and in particular to a sampling and detection method for electronic-grade potassium tantalate. Background Art

[0002] In the field of electronic materials, electronic grade potassium fluorotantalate is an important raw material, and its purity and uniformity have a crucial impact on the performance of subsequent electronic products. Therefore, sampling and testing of electronic grade potassium fluorotantalate to ensure that its quality meets production requirements is an indispensable part of the production process; At present, the sampling and detection methods of electronic grade potassium fluorotantalate mainly rely on traditional stirring and discharge technology. In terms of stirring, continuous stirring is usually used to mix potassium fluorotantalate solution with ultrapure water and acid solution to promote its dissolution and reaction; However, this continuous stirring method often makes it difficult to break the local concentration gradient in the solution, resulting in uneven dispersion of potassium fluorotantalate molecules in the solvent, thus affecting the dissolution rate and efficiency; and the existing discharge methods lack precise flow and time control, making it difficult to achieve quantitative discharge or specific time interval discharge of acid solutions such as hydrofluoric acid or nitric acid, thus affecting the accuracy and stability of the chemical reaction. Summary of the invention

[0003] In view of the deficiencies in the prior art, the present invention provides a method for sampling and detecting electronic-grade potassium fluorotantalate, which solves the technical problems mentioned in the background technology.

[0004] To achieve the above purpose, the present invention is implemented by the following technical scheme: a method for sampling and detecting electronic grade potassium fluorotantalate, specifically comprising the following steps: Step 1, sample preparation: Weigh the potassium fluorotantalate sample, place it in a beaker on the workbench, add ultrapure water, and then slowly add hydrofluoric acid and nitric acid into the beaker through the hopper, and use the swing rod and the connecting rod to drive the potassium fluorotantalate solution to stir continuously, and heat it through the heating plate on the surface of the workbench to promote the complete dissolution of the sample. After low-temperature heating and dissolution, cool it and add the mixed solution of tartaric acid and boric acid, and then stir it with the swing rod and the connecting rod to obtain the sample solution; Step 2: Instrument settings: Adjust the parameters of the ICP-AES instrument, such as radio frequency power, carrier gas flow rate, and observation height, to ensure that the instrument is in the best working condition. At the same time, select the appropriate analytical spectrum for measurement; Step 3: Determination and data analysis: Introduce the prepared sample solution into the ICP-AES instrument for measurement. The instrument will automatically record the wavelength and intensity of the characteristic light and calculate the calcium and magnesium content in the sample based on these data.

[0005] As a further preferred embodiment of the present technical solution, a support frame is fixedly connected to the top of the workbench, the beaker is placed on the workbench, a movable plate is arranged under the support frame, and the mixing assembly is installed on the movable plate; The mixing assembly includes a servo motor fixedly installed on the top of the movable disk, the output end of the servo motor is fixedly connected to a driving rod, the bottom of the driving rod is provided with a rotating rod connected through a transmission member, the outer wall of the rotating rod is fixedly connected to four groups of positioning rods, the positioning rod is fixedly connected to a fixed disk, the outer wall of the fixed disk is rotatably connected to a swing rod, a row of connecting rods is provided at the bottom of the swing rod, the positioning rod is slidably connected to a movable disk, the outer wall of the movable disk is rotatably connected to an extension rod, and the other end of the extension rod is rotatably connected to the swing rod.

[0006] As a further preferred embodiment of the present technical solution, the transmission member includes a positioning shaft rotatably installed on both sides of the movable disk, a driven wheel is fixedly connected to the top of the positioning shaft, a driving wheel is fixedly connected to the bottom of the driving rod, the driving wheel and the positioning shaft are connected through a synchronous belt, a toggle wheel is fixedly connected to the bottom of the positioning shaft, and a groove wheel that matches the toggle wheel is connected to the fixed rod at the top of the rotating rod.

[0007] As a further preferred embodiment of the present technical solution, a second cylinder is fixedly connected to the inside of the rotating rod, a connecting rod is fixedly connected to the output end of the second cylinder, a sliding rod is fixedly connected to the outer wall of the connecting rod, the sliding rod is slidably installed on the rotating rod in the vertical direction, and the outer end of the sliding rod is fixedly connected to the movable disk.

[0008] As a further preferred embodiment of the present technical solution, the top of the movable disk is fixedly connected to the fixed seat, the top of the fixed seat is rotatably connected to the rotating disk, through holes are provided at the axis of the fixed seat and the rotating disk, and the bottom end of the driving rod passes through the through holes of the rotating disk and the fixed seat, rectangular grooves are provided on both sides of the fixed seat, a clamping block is slidably connected in the rectangular groove, a push rod is fixedly connected to the outer end of the clamping block, and a first damping spring mounted on the push rod is provided in the rectangular groove.

[0009] As a further preferred embodiment of the present technical solution, trapezoidal rods are fixedly connected to both sides of the outer wall of the driving rod, and the specifications of the trapezoidal rods and the clamping blocks are matched, a second damping spring is arranged on the trapezoidal rods, and the other end of the second damping spring is connected to the surface of the rotating disk through a connecting shaft, and a clamping groove matched with the clamping block is opened on the side wall of the rotating disk.

[0010] As a further preferred embodiment of the present technical solution, hoppers are fixedly connected to both sides of the movable disk, an inclined plate is fixedly connected to the inner wall of the hopper, and the other side of the inclined plate and the inner wall of the hopper form a discharge trough, and a liquid sealing plate slidably mounted on the hopper is provided at the bottom of the inclined plate, the inner end of the liquid sealing plate is fixedly connected to one end of the push rod, and a movable frame is fixedly connected to the push rod through a connecting plate.

[0011] As a further preferred embodiment of the present technical solution, a row of knocking rods for knocking the hopper is provided on the movable frame, mounting rods are slidably connected to the bottom of both sides of the movable frame, and the mounting rods are fixedly installed on the movable plate, and a third damping spring is sleeved on the mounting rods, and the third damping spring is located on the outside of the movable frame.

[0012] As a further preferred embodiment of the present technical solution, fixed rods are fixedly connected on both sides of the workbench, cross rods are fixedly connected on the fixed rods, sleeve rods are fixedly connected to the inner ends of the cross rods, and first cylinders fixedly mounted on the support frame are provided on both sides of the movable plate. Compared with the prior art, it has the following beneficial effects: By starting a series of linkage mechanisms driven by a servo motor, intermittent, reciprocating stirring of the potassium fluorotantalate solution is achieved. This stirring method helps to break the local concentration gradient in the solution and make the potassium fluorotantalate molecules more evenly dispersed in the solvent, thereby significantly improving the dissolution speed and efficiency; in the case of adding acid solutions such as hydrofluoric acid and nitric acid, stirring helps to accelerate the chemical reaction. When potassium fluorotantalate reacts with these acids, stirring can ensure sufficient contact between the reactants, thereby improving the reaction rate and conversion rate; intermittent, reciprocating stirring method helps to achieve uniform mixing of the solution and ensure that each part of the potassium fluorotantalate solution has the same composition and properties, which can avoid uneven reaction or precipitation caused by excessively high or low local concentrations, and improve the quality and stability of the reaction; by starting the second cylinder to drive the linkage rod and the sliding rod and other mechanisms, the stirring angle of the swing rod and the connecting rod can be adjusted. The appropriate stirring angle can optimize the fluid dynamics effect, reduce the energy loss during the stirring process, and improve the stirring efficiency. At the same time, the adjustment of the stirring angle also helps to control the reaction rate and reaction uniformity, further improving the reaction efficiency and conversion rate.

[0013] Through the linkage of trapezoidal rods, blocks, push rods and liquid sealing plates, the system can intermittently open and close the discharge chute, thereby accurately controlling the flow of hydrofluoric acid or nitric acid from the hopper to the discharge pipe. This precise control is essential for processes that require quantitative discharge or discharge at specific time intervals, and helps to ensure the accuracy and stability of chemical reactions; when the liquid sealing plate fits tightly on the discharge chute between the inclined plate and the hopper, it can effectively prevent the leakage of hydrofluoric acid or nitric acid and ensure the safety and cleanliness of the working environment; the knocking treatment of the hopper by the knocking rod can vibrate the liquid and the hopper itself, which helps to break the liquid adhesion and deposition caused by long-term standing or low temperature. This knocking treatment is particularly suitable for liquids with a certain viscosity such as hydrofluoric acid and nitric acid, and can promote their smooth flow and avoid problems such as poor flow or blockage. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1It is a schematic diagram of the overall structure of the present invention; Figure 2 It is a schematic diagram of the structure of the moving plate, the hopper and the discharge pipe in the present invention; Figure 3 It is a structural schematic diagram of the driving rod and the fixing seat in the present invention; Figure 4 It is a structural schematic diagram of the transmission member in the present invention; Figure 5 It is a schematic diagram of the structure of the rotating rod, the swinging rod and the connecting rod in the present invention; Figure 6 It is a schematic diagram of the structure of the driving rod, the fixing seat, the rotating disk, the clamping block and the trapezoidal rod in the present invention; Figure 7 It is a schematic diagram of the structure of the fixed seat, the rotating disk, the card slot, the push rod, and the liquid sealing plate in the present invention; Figure 8 It is a schematic diagram of the structure of the hopper, the inclined plate, the liquid sealing plate, the movable frame and the knocking rod in the present invention.

[0015] In the figure: 1, workbench; 2, support frame; 3, beaker; 4, movable plate; 5, mixing assembly; 41, fixed rod; 42, cross bar; 43, sleeve rod; 44, first cylinder; 51, servo motor; 52, driving rod; 53, driving wheel; 54, positioning shaft; 55, driven wheel; 56, synchronous belt; 57, toggle wheel; 58, groove wheel; 59, rotating rod; 510, positioning rod; 511, fixed plate; 512, movable plate; 513, swing rod; 514, extension rod; 515, connecting rod; 51 6. The second cylinder; 517. The connecting rod; 518. The sliding rod; 519. The hopper; 520. The discharge pipe; 521. The tilting plate; 522. The liquid sealing plate; 523. The pushing rod; 524. The fixing seat; 525. The rotating disk; 526. The trapezoidal rod; 527. The slot; 528. The rectangular slot; 529. The block; 530. The first damping spring; 531. The connecting plate; 532. The second damping spring; 533. The mounting rod; 534. The moving frame; 535. The knocking rod; 536. The third damping spring. DETAILED DESCRIPTION

[0016] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the drawings of the specification. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0017] Embodiment 1: Combination Figure 1-Figure 8 As shown, the present invention provides a technical solution: a method for sampling and detecting electronic grade potassium fluorotantalate, which specifically comprises the following steps: Step 1, sample preparation: use a precise electronic balance to weigh a certain amount of potassium fluorotantalate sample, ensure the accuracy of weighing to avoid errors, the sample weight should be determined according to actual needs and the sensitivity of the instrument, place the weighed potassium fluorotantalate sample in the beaker 3 on the workbench 1, add an appropriate amount of ultrapure water, and then slowly add hydrofluoric acid and nitric acid into the beaker 3 through the hopper 519, pay attention to control the addition speed to prevent the reaction from being too violent, heat and dissolve at low temperature, and use the swing rod 513 and the connecting rod 515 to drive the potassium fluorotantalate solution to stir continuously, and heat it through the heating plate on the surface of the workbench 1 to promote the complete dissolution of the sample. During the dissolution process, pay attention to observe the color and transparency of the solution to ensure that the sample is completely dissolved, cool the dissolved solution to room temperature, add an appropriate amount of tartaric acid and boric acid mixed solution to mask other elements that may interfere with the determination, use a volumetric flask to dilute the solution to a certain volume, ensure the concentration of the solution is accurate, and shake the solution to mix it evenly; Step 2, instrument setting: Before the measurement, make sure that the ICP-AES instrument has been preheated to a stable state. The preheating time is determined according to the specific model and instructions of the instrument. Adjust the RF power to ensure stable and efficient excitation of the plasma torch, adjust the carrier gas flow rate to control the shape and stability of the plasma, set the observation height, that is, the distance between the detector and the plasma torch, to obtain the best signal strength, and adjust other relevant parameters as needed, such as nebulizer pressure, pump speed, etc. According to the characteristics of calcium and magnesium elements, select the appropriate analytical spectrum for measurement. The selection of analytical spectrum should take into account interference, sensitivity, linear range and other factors. The best analytical spectrum can be determined by consulting relevant literature or instrument manuals; Step 3, determination and data analysis: Introduce the prepared sample solution into the ICP-AES instrument through the injection system. The instrument will automatically atomize, excite and detect the solution. During the determination process, pay attention to the operating status of the instrument and the signal stability. The instrument will automatically record the wavelength and intensity data of the characteristic light. Use professional data processing software to process and analyze the data. Calculate the content of calcium and magnesium in the sample according to the intensity of the characteristic light. Perform a spike recovery test, that is, add a known concentration of calcium and magnesium standard solution to the sample, and then re-measure. By comparing the difference in the determination results before and after the addition of the spike, the accuracy and reliability of the determination method can be evaluated. Other accuracy test methods can also be used, such as using standard solutions of different concentrations for determination to verify the linear range of the instrument and the accuracy of the determination results. The determination results are presented in the form of a report, including sample name, determination date, determination results, units and other information. Perform quality control on the determination results, including data review, outlier processing, result comparison and other steps to ensure the accuracy and reliability of the determination results. In the sampling and testing of electronic-grade potassium fluorotantalate, a support frame 2 is installed on the top of a workbench 1 by a fixed connection. A beaker 3 is placed on the surface of the workbench 1 for sampling and testing. In order to ensure that the beaker 3 remains stable during the experiment, a clamp can be set on the workbench 1. The clamp can firmly fix the beaker 3 on the workbench 1 according to the needs of the experiment. A movable plate 4 is installed under the support frame 2, so that the entire device has certain flexibility and mobility; The mixing assembly 5 is cleverly mounted on the top of the moving disk 4 to achieve mixing and stirring of the substances in the beaker 3. The core part of the mixing assembly 5 is a servo motor 51, which is fixedly mounted on the top of the moving disk 4. The output end of the servo motor 51 is connected to a driving rod 52, and the bottom of the driving rod 52 is connected to a rotating rod 59 through a transmission member. Four groups of positioning rods 510 are fixedly connected to the outer wall of the rotating rod 59, and these positioning rods 510 are fixedly connected to a fixed disk 511. The outer wall of the fixed disk 511 is rotatably connected to a row of swinging rods 513. A row of connecting rods 515 are arranged at the bottom of the swinging rods 513. These connecting rods 515 can achieve stirring of the substances in the beaker 3. A movable disk 512 is slidably connected to the positioning rod 510, and the outer wall of the movable disk 512 is rotatably connected to the extension rod 514. The other end of the extension rod 514 is rotatably connected to the swing rod 513 to form a linkage mechanism. The transmission member includes a positioning shaft 54 ​​rotatably installed on both sides of the movable disk 4. The top of the positioning shaft 54 ​​is fixedly connected to the driven wheel 55, and the bottom of the driving rod 52 is fixedly connected to the driving wheel 53. The driving wheel 53 and the positioning shaft 54 ​​are connected by a synchronous belt 56. The bottom of the positioning shaft 54 ​​is fixedly connected to the toggle wheel 57, and the top of the rotating rod 59 is fixedly connected to the groove wheel 58 that matches the toggle wheel 57. A second cylinder 516 is fixedly connected to the inside of the rotating rod 59, and the output end of the second cylinder 516 is fixedly connected to the connecting rod 517. The outer wall of the connecting rod 517 is fixedly connected to the sliding rod 518. The sliding rod 518 is slidably installed on the rotating rod 59 in the vertical direction. The outer end of the sliding rod 518 is fixedly connected to the movable disk 512. By turning on the second cylinder 516, the connecting rod 517 can be driven to move up and down. The connecting rod 517 drives the movable disk 512 on the positioning rod 510 to move up and down through the sliding rod 518, so that the swing rod 513 and the connecting rod 515 on the fixed disk 511 are driven to rotate through the movable disk 512 and the extension rod 514. In this way, the stirring angles of the swing rod 513 and the connecting rod 515 can be adjusted to meet the needs of different experiments.

[0018] In the embodiment of the present invention, by starting the servo motor 51, the driving rod 52 can be driven to rotate synchronously, and then the driving rod 52 will drive the driving wheel 53 to rotate at the same speed. The driving wheel 53 is connected to the two driven wheels 55 through the synchronous belt 56, so that the driven wheels 55 can also rotate synchronously. The effect of this synchronous rotation is that the driven wheel 55 can drive the positioning shaft 54 ​​to rotate synchronously, and the rotation of the positioning shaft 54 ​​will drive the toggle wheel 57 to rotate intermittently. The intermittent rotation of the toggle wheel 57 will cause the two toggle wheels 57 to alternately drive the groove wheel 58 to rotate forward and backward. This rotation of the groove wheel 58 will cause the rotating rod 59 to rotate forward and backward intermittently. This movement of the rotating rod 59 will further drive the swing rod 513 and the connecting rod 515, so that they can intermittently and reciprocatingly rotate and stir the potassium fluorotantalate solution in the beaker 3. Mixing, this intermittent rotation of the swing rod 513 and the connecting rod 515 can effectively prevent the reaction from being too violent. Through this intermittent, reciprocating stirring method, the dissolution of potassium tantalate in ultrapure water and acid solution can be more effectively promoted. This stirring method helps to break the local concentration gradient in the solution, so that the potassium tantalate molecules are more evenly dispersed in the solvent, thereby improving the dissolution rate and efficiency. In the case of adding hydrofluoric acid and nitric acid, stirring helps to accelerate the chemical reaction. Potassium tantalate may react with these acids to generate other compounds or ions. Stirring can ensure sufficient contact between the reactants, thereby improving the reaction rate and conversion rate. The intermittent, reciprocating stirring method helps to achieve uniform mixing of the solution, which can ensure that each part of the potassium tantalate solution has the same composition and properties, thereby avoiding uneven reaction or precipitation caused by excessively high or low local concentrations; By starting the second cylinder 516, the connecting rod 517 can be driven to move up and down. The connecting rod 517 drives the movable disk 512 on the positioning rod 510 to move up and down through the sliding rod 518. In this way, the movable disk 512 can cooperate with the extension rod 514 to drive the swing rod 513 and the connecting rod 515 to rotate on the fixed disk 511. In this way, the stirring angle of the swing rod 513 and the connecting rod 515 can be adjusted. Adjusting the stirring angle can ensure that the swing rod 513 and the connecting rod 515 are more fully in contact with the potassium fluorotantalate solution, thereby more effectively mixing the solution. A suitable stirring angle can optimize the fluid dynamics effect, reduce energy loss during stirring, and improve stirring efficiency. Adjustment of the stirring angle helps to control the reaction rate and reaction uniformity of potassium fluorotantalate and the acid solution. By optimizing the stirring angle, sufficient contact between the reactants can be ensured, thereby improving the reaction efficiency and conversion rate. Embodiment 2: Combination Figure 2 , Figure 3 , Figure 6 , Figure 7 , Figure 8 As shown, on the basis of the first embodiment, the top of the movable disk 4 is connected to the fixed seat 524 by a fixed connection, and the top of the fixed seat 524 is connected to the rotating disk 525 by a rotational connection. Through holes are respectively provided at the axial positions of the fixed seat 524 and the rotating disk 525, so that the bottom end of the driving rod 52 can pass through these through holes. A rectangular groove 528 is provided on each side of the fixed seat 524, and a clamping block 529 is slidably connected in these rectangular grooves 528. The outer end of the clamping block 529 is fixedly connected to the push rod 523. At the same time, a first damping spring 530 sleeved on the push rod 523 is also provided in the rectangular groove 528. The outer wall of the driving rod 52 is fixedly connected with trapezoidal rods 526 on both sides. The specifications of these trapezoidal rods 526 are adapted to the clamping blocks 529. The trapezoidal rods 526 are provided with second damping springs 532. The other end of the second damping spring 532 is connected to the surface of the rotating disk 525 through a connecting shaft. The side wall of the rotating disk 525 is provided with a clamping groove 527 adapted to the clamping block 529. The two sides of the movable disk 4 are fixedly connected to the hopper 519, the inner wall of the hopper 519 is fixedly connected to the inclined plate 521, the other side of the inclined plate 521 and the inner wall of the hopper 519 form a discharge trough, the bottom of the inclined plate 521 is provided with a liquid sealing plate 522 slidably mounted on the hopper 519, the inner end of the liquid sealing plate 522 is fixedly connected to one end of the push rod 523, the push rod 523 is fixedly connected to the movable frame 534 through the connecting plate 531, the movable frame 534 is provided with a row of knocking rods 535 for knocking the hopper 519, the bottom of both sides of the movable frame 534 are slidably connected to the mounting rods 533, these mounting rods 533 are fixedly mounted on the movable disk 4, the mounting rods 533 are sleeved with a third damping spring 536, and the third damping spring 536 is located on the outer side of the movable frame 534.

[0019] In the embodiment of the present invention, under the drive of the servo motor 51, the driving rod 52 starts to rotate, thereby driving the trapezoidal rod 526 to rotate synchronously. When the trapezoidal rod 526 does not contact the block 529 during the rotation process, the second damping spring 532 will be stretched as the trapezoidal rod 526 rotates. However, once the trapezoidal rod 526 contacts the block 529, the trapezoidal rod 526 can push the block 529 and the push rod 523 to move outward, while compressing the first damping spring 530. In this way, the block 529 is no longer engaged in the slot 527. As the trapezoidal rod 526 continues to rotate, the trapezoidal rod 526 cooperates with the second damping spring 532 to drive the rotating disk 525 to rotate, so that the slot 527 of the rotating disk 525 can be engaged with the next block 529, thereby realizing a reciprocating driving of the block 529 in the rectangular slot 528. During the reciprocating movement of the block 529, it can drive the push rod 523 and the liquid sealing plate 522 to reciprocate. When the liquid sealing plate 522 moves outward, it can seal the discharge slot between the inclined plate 521 and the hopper 519. When the liquid sealing plate 522 moves inward, the hydrofluoric acid or nitric acid in the hopper 519 can be smoothly put into the discharge pipe 520 and discharged through the discharge pipe 520. The liquid sealing plate 522 performs intermittent reciprocating movement under the action of the block 529 and the push rod 523. By intermittently opening and closing the discharge slot, the flow of hydrofluoric acid or nitric acid from the hopper 519 to the discharge pipe 520 can be accurately controlled. This precise control is crucial for processes that require quantitative discharge or discharge at specific time intervals. When the liquid sealing plate 522 fits tightly on the discharge trough between the inclined plate 521 and the hopper 519, it can effectively prevent the leakage of hydrofluoric acid or nitric acid. At the same time, the push rod 523 drives the movable frame 534 and the knocking rod 535 to move back and forth on the mounting rod 533 through the connecting plate 531 and the third damping spring 536, so that the knocking rod 535 knocks the hopper 519. Since hydrofluoric acid and nitric acid are both liquids and have a certain viscosity, they may adhere to the inner wall of the hopper 519 due to increased viscosity or crystallization after being left still for a long time or at a low temperature, resulting in poor flow. By knocking on the outer wall of the hopper 519, the liquid and the hopper 519 can be vibrated to help break these attachments and deposits, thereby promoting the smooth flow of the liquid. Example 3: Combination Figure 1 As shown, on the basis of the second embodiment, fixed rods 41 are fixedly connected on both sides of the workbench 1, a cross bar 42 is fixedly connected to the fixed rod 41, a sleeve rod 43 is fixedly connected to the inner side of the cross bar 42, and a first cylinder 44 fixedly installed on the support frame 2 is provided on both sides of the movable plate 4.

[0020] In an embodiment of the present invention, by turning on the first cylinder 44, the movable disk 4 can be driven to move downward, and the movable disk 4 drives the mixing assembly 5 to move downward, so that the swing rod 513 and the connecting rod 515 enter the beaker 3, so that the swing rod 513 and the connecting rod 515 stir and mix the potassium fluorotantalate solution in the beaker 3. Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for sampling and detecting electronic grade potassium fluorotantalate, characterized in that: The specific steps include: Step 1, sample preparation: Weigh a potassium fluorotantalate sample, place it in a beaker (3) on a workbench (1), add ultrapure water, then slowly add hydrofluoric acid and nitric acid into the beaker (3) through a hopper (519), and use a swing rod (513) and a connecting rod (515) to drive the potassium fluorotantalate solution to be continuously stirred, and heat it through a heating plate on the surface of the workbench (1) to promote complete dissolution of the sample. After dissolving by low-temperature heating, cool it and add a mixed solution of tartaric acid and boric acid, and then stir it with the swing rod (513) and the connecting rod (515) to obtain a sample solution; Step 2: Instrument settings: Adjust the parameters of the ICP-AES instrument, such as radio frequency power, carrier gas flow rate, and observation height, to ensure that the instrument is in the best working condition. At the same time, select the appropriate analytical spectrum for measurement; Step 3: Determination and data analysis: Introduce the prepared sample solution into the ICP-AES instrument for measurement. The instrument will automatically record the wavelength and intensity of the characteristic light and calculate the calcium and magnesium content in the sample based on these data.

2. The electronic grade potassium fluorotantalate sampling and detection method according to claim 1, characterized in that: A support frame (2) is fixedly connected to the top of the workbench (1), a beaker (3) is placed on the workbench (1), a movable plate (4) is arranged below the support frame (2), and a mixing assembly (5) is mounted on the movable plate (4); The mixing assembly (5) comprises a servo motor (51) fixedly mounted on the top of the movable disk (4); the output end of the servo motor (51) is fixedly connected to a driving rod (52); the bottom of the driving rod (52) is provided with a rotating rod (59) which is connected to the rotating rod (59) through a transmission member; the outer wall of the rotating rod (59) is fixedly connected to four groups of positioning rods (510); the positioning rods (510) are fixedly connected to a fixed disk (511); the outer wall of the fixed disk (511) is rotatably connected to a swing rod (513); a row of connecting rods (515) is provided at the bottom of the swing rod (513); the positioning rod (510) is slidably connected to a movable disk (512); the outer wall of the movable disk (512) is rotatably connected to an extension rod (514); the other end of the extension rod (514) is rotatably connected to the swing rod (513).

3. The electronic grade potassium fluorotantalate sampling and detection method according to claim 2, characterized in that: The transmission member comprises a positioning shaft (54) rotatably mounted on both sides of the moving plate (4); a driven wheel (55) is fixedly connected to the top of the positioning shaft (54); a driving wheel (53) is fixedly connected to the bottom of the driving rod (52); the driving wheel (53) and the positioning shaft (54) are transmission-connected via a synchronous belt (56); a toggle wheel (57) is fixedly connected to the bottom of the positioning shaft (54); and a groove wheel (58) adapted to the toggle wheel (57) is connected to the fixed rod at the top of the rotating rod (59).

4. The electronic grade potassium fluorotantalate sampling and detection method according to claim 3, characterized in that: The rotating rod (59) is fixedly connected to a second cylinder (516) inside, the output end of the second cylinder (516) is fixedly connected to a linkage rod (517), the outer wall of the linkage rod (517) is fixedly connected to a sliding rod (518) around the periphery, the sliding rod (518) is slidably mounted on the rotating rod (59) in a vertical direction, and the outer end of the sliding rod (518) is fixedly connected to the movable disk (512).

5. The electronic grade potassium fluorotantalate sampling and detection method according to claim 4, characterized in that: The top of the movable disk (4) is fixedly connected to a fixed seat (524), and the top of the fixed seat (524) is rotatably connected to a rotating disk (525). A through hole is provided at the axis of the fixed seat (524) and the rotating disk (525), and the bottom end of the driving rod (52) passes through the through holes of the rotating disk (525) and the fixed seat (524). Rectangular grooves (528) are provided on both sides of the fixed seat (524), and a clamping block (529) is slidably connected in the rectangular groove (528). The outer end of the clamping block (529) is fixedly connected to a push rod (523), and a first damping spring (530) sleeved on the push rod (523) is provided in the rectangular groove (528).

6. The electronic grade potassium fluorotantalate sampling and detection method according to claim 5, characterized in that: Trapezoidal rods (526) are fixedly connected to both sides of the outer wall of the driving rod (52), and the specifications of the trapezoidal rods (526) and the clamping block (529) are matched. A second damping spring (532) is arranged on the trapezoidal rod (526), ​​and the other end of the second damping spring (532) is connected to the surface of the rotating disk (525) through a connecting shaft. The side wall of the rotating disk (525) is provided with a clamping groove (527) matched with the clamping block (529).

7. The electronic grade potassium fluorotantalate sampling and detection method according to claim 6, characterized in that: A hopper (519) is fixedly connected to both sides of the movable plate (4), an inclined plate (521) is fixedly connected to the inner wall of the hopper (519), and the other side of the inclined plate (521) and the inner wall of the hopper (519) form a discharge trough, a liquid sealing plate (522) slidably mounted on the hopper (519) is provided at the bottom of the inclined plate (521), the inner side end of the liquid sealing plate (522) is fixedly connected to one end of a push rod (523), and a movable frame (534) is fixedly connected to the push rod (523) via a connecting plate (531).

8. The electronic grade potassium fluorotantalate sampling and detection method according to claim 7, characterized in that: A row of knocking rods (535) for knocking the hopper (519) is provided on the movable frame (534), mounting rods (533) are slidably connected to the bottoms of both sides of the movable frame (534), and the mounting rods (533) are fixedly mounted on the movable plate (4), and a third damping spring (536) is sleeved on the mounting rod (533), and the third damping spring (536) is located outside the movable frame (534).

9. The electronic grade potassium fluorotantalate sampling and detection method according to claim 2, characterized in that: Fixed rods (41) are fixedly connected to both sides of the workbench (1), a cross rod (42) is fixedly connected to the fixed rod (41), a sleeve rod (43) is fixedly connected to the inner end of the cross rod (42), and first cylinders (44) fixedly mounted on the support frame (2) are arranged on both sides of the movable plate (4).

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