Automatic pretreatment equipment and method for fly ash detection

Abstract

The invention discloses automatic pretreatment equipment for fly ash detection. The automatic pretreatment equipment comprises a raw material reagent storage area; a leach liquor preparation area; an extraction bottle functional area; performing suction filtration to determine a functional area; a constant-volume function area is taken separately; and a support frame. The method aims at achieving automation of the pretreatment process for detecting the leachable metal in the fly ash leaching toxicity, the workload of repeated mechanical operation is reduced, analysis errors caused by tedious pretreatment operation are reduced, the detection and analysis work efficiency is improved, and therefore the operation cost of related enterprises and public institutions is reduced. Meanwhile, according to the scheme, through a full-automatic operation process, the processes of automatic preparation of the leaching liquid, automatic split charging of the leaching liquid, automatic filtration / suction filtration of the leaching liquid, automatic determination of the pH value of the leaching filtrate, automatic separation of the leaching filtrate, automatic acid adding before digestion of the filtrate, automatic acid adding and sample reserving of the residual filtrate, automatic volume fixing after digestion of the filtrate and the like are achieved; and no personnel intervention is needed in the normal operation process, the set processing flow is automatically operated, and the automation degree is high.

Description

Technical Field

[0001] The present application relates to the technical field of waste incineration fly ash detection and processing, and in particular to an automated pre-processing device and method for fly ash detection. Background Art

[0002] At present, fly ash from the incineration of domestic waste (hereinafter referred to as fly ash) refers to the bottom ash collected by the flue gas purification system of domestic waste incineration facilities and the bottom ash settled at the bottom of the flue and chimney. At this stage, although waste classification is vigorously promoted, due to the rapid development of the economy and society, the waste entering the incineration facilities is diversified, and it is difficult to accurately distinguish and identify the fly ash after incineration as general waste or hazardous waste by the type of waste. Therefore, fly ash leaching toxicity testing is very necessary; at the same time, fly ash leaching toxicity testing meets the pollution control requirements during its collection, storage, transportation, treatment and disposal.

[0003] In the relevant technology, the detection and analysis process of leaching heavy metals in fly ash leaching toxicity includes the preparation of leaching solution, packaging of leaching solution, flip leaching (more than 18 hours), filtration / suction filtration of leaching solution, pH determination of leaching filtrate, fractionation of leaching filtrate, acid digestion of fractionated filtrate, acidification of remaining filtrate, volume adjustment of digestion solution, preparation of test samples for machine, and detection and analysis of test samples for machine.

[0004] In the entire detection and analysis process, the sample pretreatment process accounts for more than four-fifths of the time, and most of the sample pretreatment process is repetitive mechanical operation. According to research and analysis, the errors made by experimental analysts in the tedious pretreatment operation process are the main source of errors in the final detection and analysis. Summary of the invention

[0005] The purpose of this application is to provide an automated pre-treatment device and method for fly ash detection, so as to solve the problem that in the entire detection and analysis process, the sample pre-treatment process occupies more than four-fifths of the time, and most of the sample pre-treatment process is repetitive mechanical operation. According to research and analysis, the errors of experimental analysts in the tedious pre-treatment operation process are the main source of errors in the final detection and analysis.

[0006] On the one hand, the present application provides an automated pre-treatment device for fly ash detection using the following technical solution:

[0007] An automatic pre-processing device for fly ash detection, comprising:

[0008] The raw material reagent storage area is used to store deionized water for preparing the leaching solution, and is used in conjunction with the reagent module as the raw material reagent area for preparing the leaching solution;

[0009] The extract preparation area is used to stir and mix the added extract preparation raw materials and reagents to achieve homogeneity of the mixed raw materials and reagents and store the prepared extract;

[0010] The extraction bottle functional area is used for dispensing the extraction liquid in the extraction bottle, placing the extraction bottle after flipping the extraction bottle, and serving as a filtration sample area;

[0011] The filtration determination functional area is used for filtering the leaching solution in the filtration sample area, and at the same time, determining the pH value of the leaching solution and collecting the leaching solution, and adding acid to the sample of the filtrate remaining after the fractionation;

[0012] The function area for fractionation and volume determination is used for placing the digestion tube, receiving the extracted leaching liquid, adding acid to the digestion tube, and performing characteristic volume determination after digestion;

[0013] The supporting frame, the extraction bottle functional area, the filtration and determination functional area and the fractionation and volume determination functional area are sequentially arranged on the supporting frame.

[0014] Furthermore, the raw material reagent storage area includes two reagent storage containers, namely a storage barrel and a storage bottle. The storage barrel is used to store deionized water, and the storage bottle cooperates with the reagent module to store glacial acetic acid reagent.

[0015] Furthermore, the storage barrel and the storage bottle are both provided with a one-way ventilation device to prevent the reagents in the storage barrel and the storage bottle from volatilizing and overflowing; the storage barrel and the storage bottle are also both provided with a liquid level monitoring device to monitor the storage conditions of the reagents in the storage barrel and the storage bottle.

[0016] Furthermore, the extract preparation area includes an extract preparation barrel, and a liquid adding pump A and a liquid adding pump B are arranged on one side of the support frame. The two ends of the liquid adding pump A are respectively connected to the storage barrel and the extract preparation barrel through a pipeline flow path, and the two ends of the liquid adding pump B are respectively connected to the storage bottle and the extract preparation barrel through a pipeline flow path. A mixing and homogenizing module is arranged in the extract preparation barrel, and the mixing and homogenizing module is used to mix and stir the prepared solution in the extract preparation barrel. An upper barrel cover is also arranged on the top of the extract preparation barrel, and the upper barrel cover is also provided with a one-way ventilation device.

[0017] Furthermore, the extraction bottle functional area includes an extraction bottle filling module, an extraction liquid filling and adding module and a three-axis A module, the extraction bottle filling module, the extraction liquid filling and adding module and the three-axis A module are respectively arranged on the supporting frame, the extraction bottle filling module is used to place multiple new / unused extraction bottles, the extraction liquid filling and adding module is connected to the extraction liquid preparation barrel to extract and fill the prepared solution in the extraction liquid preparation barrel into the extraction bottle, and the three-axis A module is used to transport the extraction bottle between the extraction bottle functional area to the filtration and determination functional area.

[0018] Furthermore, the filtration measurement functional area includes an extract filtration module and a three-axis B module arranged on the support frame, the extract filtration module includes an extraction bottle station, a filtration head, a rotary dumping module, a filtration module and a double filtration receiving station; the extraction bottle station is used to place the extraction bottle after the flip leaching is completed; the rotary dumping module is used to drive the extraction bottle filled with extract to dump the extract in the extraction bottle into the filtration head; the filtration module cooperates with the filtration head to complete the filtration of the sample liquid in the filtration head; one of the double filtration receiving stations is used to receive the filtrate of the wetting process and use it for the pH value determination of the filtrate, and the other is used to place the filtrate used in the subsequent process, and the three-axis B module is used to transfer the filtration head and the filtration receiving bottle in the filtration measurement functional area between the placement area and the working position area.

[0019] Furthermore, the filtration measurement functional area also includes a filtrate pH measurement module arranged on the support frame, and the filtrate pH measurement module includes a pH meter module, an electrode cleaning station, an electrode dehydration station, a calibration liquid station and an electrode drive rotation device; the pH meter module includes a pH electrode and a module host, and is embedded with automatic calibration and automatic measurement programs that comply with national standards / European standards; the electrode cleaning station is used for cleaning the electrode before and after measurement; the electrode dehydration station is used to remove water droplets adhering to the surface of the electrode after cleaning; the calibration liquid station is used for pH meter calibration to calibrate calibration solutions with different pH values; the electrode drive rotation device is used to drive the electrode to complete the work processes of different stations to realize automatic calibration and automatic measurement of the pH meter.

[0020] Furthermore, the separation and volume determination functional area includes a filtrate receiving bottle management area, a filtrate transfer and distribution module, a pipette tip management area, a digestion tube management area and a three-axis C module, which are respectively arranged on the support frame; the filtrate receiving bottle management area is used to store and place the filtrate receiving bottles; the filtrate transfer and distribution module is used to transfer the filtrate; the pipette tip management area is used to store the pipette tips; the digestion tube management area is used to store the digestion tubes, and the digestion tube management area is also configured with a robotic arm module and a three-axis digestion tube acid addition / volume determination module, which are used to complete the acid addition and dilution and volume determination of the digestion tube respectively; the three-axis C module is used to transfer the filtrate in the suction receiving bottle to the digestion tube in the separation and volume determination functional area.

[0021] Furthermore, the three-axis digestion tube acid addition / constant volume module includes a digestion acid addition module and a constant volume module. The digestion acid addition module adopts two liquid addition channels to complete the digestion acid addition after the digestion tube is taken in the coverage area; the constant volume module adopts an ultrasonic constant volume method, which is composed of an ultrasonic constant volume sensor and a constant volume liquid addition injection pump, combined with a program algorithm, to complete the constant volume / quantitative dilution of the solution in the digestion tube.

[0022] On the other hand, the present application provides an automated pre-processing method for fly ash detection using the following technical solution:

[0023] An automated pre-processing method for fly ash detection comprises the following steps:

[0024] a. Extract preparation process: under the control of the program, according to the set preparation volume and liquid adding speed, use the liquid adding pump A and the liquid adding pump B to accurately add deionized water and glacial acetic acid into the extract preparation barrel, and drive the stirring and mixing at the same time. After the mixed solution is stable, a warning is issued to confirm whether the pH value of the prepared mixed solution meets the requirements (pH = 2.64 ± 0.05);

[0025] b. Extraction liquid filling process: under the control of the control program, according to the set extraction bottle series, the corresponding filling volume and the best filling speed, the extraction liquid filling and adding module is used to fill the prepared extraction liquid in the extraction liquid preparation barrel into the selected extraction bottle;

[0026] c. Leachate filtration / filtrate pH determination / filtrate fractionation / acid addition before digestion / acid addition to retained samples process: After the inverted leaching is completed, the leaching bottle is placed in the leaching bottle management area, and the preparation of related materials and reagents such as the filtration receiving bottle, filtration head, fractionation gun head, fractionation receiving digestion tube, acid addition reagent, cleaning reagent, etc. is completed; the method editing is completed according to the actual leaching bottle sequence; after starting the process, the equipment performs leachate filtration / filtrate pH determination / filtrate fractionation / acid addition before digestion / acid addition to retained samples and other operations in sequence according to the program;

[0027] d. Post-digestion volume determination process: After placing the digested sample in the digestion tube tray, edit the method process, start the volume determination process, use the ultrasonic sensor to detect the sample volume in the digestion tube first, and the built-in algorithm automatically calculates the volume of diluent required to determine the target volume. The volume determination injection pump will then add the exact volume of diluent.

[0028] Compared with the prior art, the beneficial effects of this application are:

[0029] The present application aims to realize the automation of the pretreatment process of fly ash leaching toxicity detection of leachable metals through the development of automated pretreatment equipment for fly ash detection, reduce the workload of repetitive mechanical operations, reduce the analysis errors caused by cumbersome pretreatment operations, improve the efficiency of detection and analysis, and thus reduce the operating costs of related enterprises and institutions.

[0030] At the same time, the solution of the present application realizes the automatic preparation of the extract, automatic packaging of the extract, automatic filtration / filtration of the extract, automatic determination of the pH value of the extract filtrate, automatic separation of the extract filtrate, automatic acid addition before filtrate digestion, automatic acid addition and sampling of the remaining filtrate, and automatic volume setting after filtrate digestion through a fully automatic operation process; and no human intervention is required during normal operation, and the set processing process runs automatically, with a high degree of automation.

[0031] In addition, the use of intelligent robotic arm platforms and sensor monitoring technology can realize intelligent perception in the automated operation process; it can help the inspection department save manpower, requiring only necessary operation and maintenance personnel, and improve work efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 It is a structural schematic diagram of the automated pre-treatment equipment for fly ash detection according to an embodiment of the present application.

[0033] Figure 2 yes Figure 1 main view.

[0034] Figure 3 yes Figure 1 Top view of the .

[0035] Figure 4 It is a flow chart combining the extract preparation process and the extract packaging process of the embodiment of the present application.

[0036] Figure 5 It is a flow chart that separates the extract preparation process and the extract packaging process in the embodiment of the present application.

[0037] Figure 6 It is a flow chart of the leachate filtration / filtrate pH determination / filtrate separation / acid addition before digestion / sample acid addition process of the embodiment of the present application.

[0038] Figure 7 It is a flow chart of the post-digestion volume determination process of an embodiment of the present application.

[0039] Description of reference numerals:

[0040] 1. Raw material and reagent storage area; 11. Storage barrel; 2. Extract preparation area; 21. Extract preparation barrel; 3. Extract bottle functional area; 31. Extract bottle filling module; 32. Extract filling and liquid adding module; 33. Three-axis A module; 4. Filtration and determination functional area; 41. Extract filtration module; 42. Three-axis B module; 43. Filtrate pH determination module; 5. Separation and constant volume functional area; 51. Filtrate receiving bottle management area; 52. Pipette tip management area; 53. Digestion tube management area; 54. Three-axis digestion tube acidification / constant volume module; 55. Three-axis C module; 6. Support frame; 61. Liquid adding pump A; 62. Liquid adding pump B; 63. Extract filling pump; 64. Liquid adding three-way valve; 7. Three-axis sample retention acid addition module; 8. Sample retention acid addition auxiliary function module; 9. Digestion tube acidification / constant volume auxiliary function module. DETAILED DESCRIPTION

[0041] The following is combined with Figure 1-7 This application is described in further detail.

[0042] On the one hand, the present application provides an automated pre-processing device for fly ash detection, referring to Figure 1-Figure 3 In this embodiment, the fly ash detection automatic pre-treatment equipment includes: a raw material reagent storage area 1, an extract preparation area 2, an extract bottle functional area 3, a filtration measurement functional area 4, a separation and volume determination functional area 5 and a support frame 6. Among them, the raw material reagent storage area 1 and the extract preparation area 2 are respectively placed on one side of the support frame 6, and the extract bottle functional area 3, the filtration measurement functional area 4 and the separation and volume determination functional area 5 are respectively installed on the support frame 6 in sequence, so as to carry the extract bottle functional area 3, the filtration measurement functional area 4 and the separation and volume determination functional area 5 at the same time.

[0043] Specifically, the raw material reagent storage area 1 is used to store deionized water for preparing the leaching solution, and is used in conjunction with the reagent module as a raw material reagent area for preparing the leaching solution; and the reagent module is a device for providing glacial acetic acid reagent.

[0044] More specifically, refer to Figure 1-Figure 2 In this embodiment, the raw material reagent storage area 1 includes two specifications of reagent storage containers, which are a storage barrel 11 and a storage bottle. The storage barrel 11 uses a barrel body with a volume of 80L, which is used to store deionized water, and the material of the storage barrel 11 is PE material; the storage bottle uses a bottle body with a volume of 2L, and the storage bottle cooperates with the reagent module so that the reagent module extracts the glacial acetic acid reagent into the storage bottle, so that the storage bottle is used to store glacial acetic acid, and the material of the storage bottle is borosilicate glass material.

[0045] To be specific, the dual raw material reagent reserve container mode is suitable for the preparation of two reagent mixed solutions. The number of reagent reserve containers and the corresponding pipeline flow paths can be increased according to the preparation requirements of the mixed solution; at the same time, the 80L storage barrel 11 is used to store reagents with larger volume usage, while the 2L storage bottle is used to store reagents with smaller volume usage.

[0046] At the same time, a one-way ventilation device is installed on both the storage barrel 11 and the storage bottle; the one-way ventilation device can be used to prevent the reagents in the storage barrel 11 and the storage bottle from volatilizing and overflowing, and can also keep the pressure inside the two containers of the storage barrel 11 and the storage bottle consistent with the atmospheric pressure, so as to ensure the accuracy of liquid addition. In addition, a liquid level monitoring device is also installed on both the storage barrel 11 and the storage bottle; the liquid level monitoring device can monitor the storage status of the reagents in the storage barrel 11 and the storage bottle, so as to remind the operator of the use and storage status of the reagents, so as to replenish the reagents in time, and can also serve as a feedback basis for the realization of the automated process.

[0047] Reference Figure 1-Figure 2 In this embodiment, the extract preparation area 2 is used to stir and mix the added extract preparation raw material reagents to complete the homogenization of the mixed raw material reagents and store the prepared extract; specifically, the extract preparation area 2 includes an extract preparation barrel 21, a liquid adding pump group, a pipeline flow path and a mixing and homogenizing module. Among them, the extract preparation barrel 21 is placed at the front end of the feed of the support frame 6, the specification volume of the extract preparation barrel 21 is 100L, and the material of the storage barrel 11 is PE material; and the top of the extract preparation barrel 21 is also covered with an upper barrel cover, which can be easily removed from the top of the extract preparation barrel 21. At the same time, a one-way ventilation device is also installed on the upper barrel cover. Through the setting of the one-way ventilation device, it can be used to prevent the volatilization and overflow loss of the reagents in the extract preparation barrel 21, and at the same time, the pressure inside the extract preparation barrel 21 can be kept consistent with the atmospheric pressure, thereby ensuring the accuracy of the subsequent liquid addition process.

[0048] The liquid adding pump group includes a liquid adding pump A61 and a liquid adding pump B62, which are respectively installed on one side of the support frame 6 close to the extract preparation barrel 21; specifically, the two ends of the liquid adding pump A61 are respectively connected to the storage barrel 11 and the extract preparation barrel 21 through a pipeline flow path; the two ends of the liquid adding pump B62 are respectively connected to the storage bottle and the extract preparation barrel 21 through a pipeline flow path. When the liquid adding pump A61 and the liquid adding pump B62 are respectively started, the deionized water in the storage barrel 11 and the glacial acetic acid in the storage bottle can be simultaneously extracted into the extract preparation barrel 21 by using the corresponding pipeline flow paths.

[0049] To be specific: for the selection of the liquid adding pump group, the appropriate type is selected according to the liquid adding needs and the type of reagents, such as a valveless ceramic pump, a syringe pump, a peristaltic pump, etc.; and the preparation of the extract in this application uses a valveless ceramic pump (minimum speed ≥1.5L / min, liquid adding error ≤1%) as the liquid adding pump for the 2L storage bottle; a valveless ceramic pump (minimum speed ≥3L / min, liquid adding error ≤1%) is selected as the liquid adding pump for the 80L storage barrel 11, and the parameters such as the liquid adding speed and liquid adding amount of the liquid adding pump support setting.

[0050] At the same time, the mixing and homogenizing module is installed inside the leaching solution preparation barrel 21, and the mixing and homogenizing module includes a paddle stirring mechanical mechanism and a power motor. Among them, the paddle stirring mechanical mechanism is rotatably installed inside the leaching solution preparation barrel 21; the power motor is installed on the top of the leaching solution preparation barrel 21, and the output end of the power motor is interconnected with the paddle stirring mechanical mechanism; when the power motor is started, the output end of the power motor drives the paddle stirring mechanical mechanism to rotate, so that the prepared solution in the leaching solution preparation barrel 21 can be mixed and stirred to complete the mixing and homogenization of the prepared solution. In addition, the stirring intensity and time support setting.

[0051] In addition, refer to Figure 1-Figure 2 In this embodiment, the extraction bottle functional area 3 is located on the side of the support frame 6 close to the extraction liquid preparation barrel 21. The extraction bottle functional area 3 is used for packaging the extraction liquid in the extraction bottle, placing the extraction bottle after flipping the extraction bottle, and serving as a filtration sample area.

[0052] Specifically, the extraction bottle functional area 3 includes an extraction bottle sub-packaging module 31, an extraction liquid sub-packaging and liquid adding module 32, and a three-axis A module 33. The extraction bottle sub-packaging module 31 is installed on the support frame 6, and is used to place a plurality of new / unused extraction bottles, and the extraction bottle sub-packaging module 31 is three extraction bottle sub-packaging trays, and the three extraction bottle sub-packaging trays are respectively configured with 20 workstations, so a total of 60 workstations are designed, and the operator places the new / unused extraction bottles in the corresponding workstations of the extraction bottle sub-packaging trays.

[0053] The extract filling and liquid adding module 32 is installed on the supporting frame 6, and the extract filling and liquid adding module 32 is interconnected with the extract preparation barrel 21, and the extract filling and liquid adding module 32 is composed of an extract filling pump 63, a liquid adding three-way valve 64 and a pipeline; in this way, through the coordinated structure composed of the extract filling pump 63, the liquid adding three-way valve 64 and the pipeline, the equipment program executes the management task, that is, after starting the extract filling pump 63, the extract in the extract preparation barrel 21 can be respectively extracted and filled into the extract bottles in the corresponding workstations, thereby completing the process of filling the extract in the extract bottles.

[0054] Preferably, in the present embodiment, two extract filling pumps 63 are provided, and both extract filling pumps 63 are valveless ceramic pumps; and the specification of one of the valveless ceramic pumps is a minimum speed ≥0.1L / min, and a liquid addition error ≤1%; the specification of the other valveless ceramic pump is a minimum speed ≥3L / min, and a liquid addition error ≤1%; the two together complete the extract filling, thereby meeting the filling requirements of different volumes.

[0055] At the same time, the three-axis A module 33 is also installed on the support frame 6, and the three-axis A module 33 is located between the extraction bottle functional area 3 and the filtration measurement functional area 4; specifically, the three-axis A module 33 takes the functional area corresponding to the horizontal support frame 6 as the X-axis, and is perpendicular to the two parallel X-axes in the same plane as the Y-axis. A mechanical module that can extend downward is configured at the intersection of the X-axis and the Y-axis as the Z-axis, and the end of the Z-axis is also equipped with a clamp adapted to grasp the extraction bottle, so that the extraction bottle can be transferred between the extraction bottle functional area 3 and the filtration measurement functional area 4.

[0056] In addition, refer to Figure 1-Figure 3 In this embodiment, the filtration determination functional area 4 is located in the next process of the leaching bottle functional area 3, and is used for filtering the leaching liquid in the filtration sample area, and at the same time, the pH value of the filtrated leaching liquid is determined and the filtrated leaching liquid is collected, and the sample of the filtrated liquid remaining after the separation is acidified.

[0057] Specifically, the filtration and determination functional area 4 includes a leachate filtration module 41 and a filtrate pH determination module 43. The leachate filtration module 41 and the filtrate pH determination module 43 are respectively installed on the support frame 6, and in the management of the leaching bottle during the leachate filtration process, the operator places the leaching bottle that has completed the flip leaching at the corresponding point, and the equipment program performs the management task, that is, in the filtration and determination functional area 4, the filtration of the leachate and the determination of the filtrate pH are completed with the cooperation of the leachate filtration module 41 and the filtrate pH determination module 43.

[0058] More specifically, the leachate filtration module 41 includes an extraction bottle station, a filtration head, a rotary pouring module, a filtration module and a double filtration receiving station. Among them, the extraction bottle station is used to place the extraction bottle after the flip extraction, and the extraction bottle is the sample bottle; the suction filter head is composed of a solution containing body and two detachable sieve plates, and a filter membrane with a specific pore size and specification is placed in the middle of the sieve plate before the filter head for suction filtration is assembled; and the rotary dumping module is used to drive the extraction bottle filled with the leachate to dump the leachate in the extraction bottle into the suction filter head; the suction filter module is connected to a vacuum pump, and the suction filter module is used in combination with the suction filter head, so as to complete the filtration of the sample liquid in the suction filter head; finally, one of the double suction filter receiving stations is used to receive the filtrate of the wetting process and is used for the determination of the pH value of the filtrate, and has an automatic waste discharge function; the other is used to place the filtrate used in the subsequent process, and the suction filter receiving station is equipped with a suction filter receiving bottle to store the filtrate.

[0059] At the same time, the filtrate pH determination module 43 includes a pH meter module, an electrode cleaning station, an electrode dewatering station, a calibration liquid station, and an electrode drive rotating device. Among them, the pH meter module includes a pH electrode and a module host, and is embedded with an automatic calibration and automatic measurement program that complies with the national standard / European standard; the electrode cleaning station is used for cleaning the electrode before and after measurement, and the cleaning liquid is driven into the electrode by a peristaltic pump, and is discharged through a pipeline after overflow; the electrode dewatering station adopts an air-blowing dewatering method to remove water droplets adhering to the surface of the electrode after cleaning, and reduce the influence of the cleaning liquid on the pH determination; the calibration liquid station is used for calibration of a pH meter that complies with the national standard calibration system, and is designed with 5 positions for placing 5 calibration solutions with different pH values, so that calibration solutions with different pH values ​​can be calibrated; finally, the electrode drive rotating device is used to drive the electrode to complete the workflow of different stations, so that the automatic calibration and automatic determination of the pH meter can be realized.

[0060] And the three-axis B module 42 is installed on the support frame 6, and the three-axis B module 42 is located in the filtration measurement functional area 4; specifically, the three-axis B module 42 takes the horizontal support frame 6 corresponding to the functional area as the X-axis, and the Y-axis perpendicular to the two parallel X-axes in the same plane, and a mechanical module that can be extended downward is configured at the intersection of the X-axis and the Y-axis as the Z-axis. The end of the Z-axis is equipped with a clamp that is compatible with the filtration head and the filtration receiving bottle, so that the filtration head and the filtration receiving bottle in the filtration measurement functional area 4 can be transferred between the placement area and the working area.

[0061] Secondly, refer to Figure 1-Figure 2 In this embodiment, the fractionation and volume determination functional area 5 is located in the next process of the filtration and measurement functional area 4, and is used for the placement area of ​​the digestion tube, for fractionation and reception of the filtration leaching liquid, for acid addition in the digestion tube, and for characteristic volume determination after digestion.

[0062] Specifically, the fractionation and constant volume functional area 5 includes a filtrate receiving bottle management area 51, a filtrate transfer and distribution module, a pipette tip management area 52, and a digestion tube management area 53, which are respectively installed on the support frame 6. Among them, the filtrate receiving bottle management area 51 is designed for 60 stations for storing and placing filtrate receiving bottles; at the same time, an XY two-axis liquid adding mechanical arm module located in the liquid receiving bottle management area is also installed on the support frame 6, and a three-axis sample retention and acid addition module 7 is installed on the XY two-axis liquid adding mechanical arm module. The three-axis sample retention and acid addition module 7 is configured with a peristaltic pump and a pipeline, and the peristaltic pump and the pipeline serve as a Z axis fixed in the depth direction. In this way, through the above-mentioned mutually coordinated structures, the sample retention and acid addition process after the filtrate receiving bottle is separated in the coverage area can be completed.

[0063] At the same time, the filtrate transfer and distribution module is configured with 4 channels, each channel is an independent air displacement pipette pump (ADP), and the filtrate is transferred by a pipette tip, so as to avoid cross contamination. The pipette tip management area 52 is used to store pipette tips, and has an area designed for 60 storage capacities; the digestion tube management area 53 is divided into two placement trays A and B, both of which are designed for 60 stations, for storing digestion tubes of specified specifications; and the digestion tube management area 53 is also equipped with a robotic arm module and a three-axis digestion tube acidification / constant volume module 54, which are used to complete the acidification and dilution constant volume of the digestion tube respectively.

[0064] More specifically, the three-axis digestion tube acid addition / constant volume module 54 is located at the XY two-axis mechanical arm module of the digestion tube placement area of ​​the divided constant volume functional area 5, and the three-axis digestion tube acid addition / constant volume module 54 utilizes a double digestion acid addition channel design, which includes a digestion acid addition module and a constant volume module. Wherein, the digestion acid addition module adopts two liquid addition channels, and the two liquid addition channels are peristaltic pumps. By adopting two peristaltic pumps, the digestion acid addition process after the digestion tube in the coverage area is divided can be completed.

[0065] The constant volume module adopts an ultrasonic constant volume method, and is composed of an ultrasonic constant volume sensor and a constant volume liquid addition injection pump. Preferably, the constant volume liquid addition injection pump is also a constant volume liquid addition channel, and the ultrasonic sensor is used to detect the volume of liquid in the digestion tube. By combining the program algorithm, and then with the cooperation of the ultrasonic sensor and the constant volume liquid addition channel, the constant volume / quantitative dilution of the sample in the digestion tube after the digestion treatment can be achieved.

[0066] At the same time, a three-axis C module 55 is also installed at the rear end of the support frame 6, and the three-axis C module 55 is located between the filtration and measurement functional area 4 and the fractionation and constant volume functional area 5; specifically, the three-axis C module 55 takes the functional area corresponding to the horizontal support frame 6 as the X-axis, and is perpendicular to the two parallel X-axes in the same plane as the Y-axis. A mechanical module that can be extended downward is configured at the intersection of the X-axis and the Y-axis as the Z-axis, and the end of the Z-axis is equipped with a 4-channel air displacement pipette pump (ADP), so that the filtrate in the filtration receiving bottle of the filtration and measurement functional area 4 can be transferred to the digestion tube of the fractionation and constant volume functional area 5.

[0067] Preferably, a sample acid-adding auxiliary function module 8 and a digestion tube acid-adding / constant volume auxiliary function module 9 are also installed on one side of the support frame 6, and the sample acid-adding auxiliary function module 8 and the digestion tube acid-adding / constant volume auxiliary function module 9 are respectively located between the suction filtration determination functional area 4 and the separation and constant volume functional area 5. Specifically, the effect of the sample acid-adding auxiliary function module 8 is: after the filtrate separation is completed, a certain volume of concentrated acid is added to the filtrate receiving bottle so that the filtrate reaches the storage condition. The function of the digestion tube acid-adding / constant volume auxiliary function module 9 is: automatically add a certain volume of concentrated acid to the digestion tube. Before the digestion tube is taken for digestion, a certain volume of concentrated acid needs to be added to the inside, and a certain volume of concentrated acid also needs to be added before constant volume in the digestion tube.

[0068] On the other hand, the present application provides an automated pre-processing method for fly ash detection using the following technical solution:

[0069] An automated pre-processing method for fly ash detection comprises the following steps:

[0070] a. Extract preparation process:

[0071] The extract preparation process is completed between the raw material reagent storage area 1 and the extract preparation area 2. The main operation process is as follows: under the scheduling of the control program, the liquid adding pump A61 and the liquid adding pump B62 are used to accurately add deionized water and glacial acetic acid into the extract preparation barrel 21 according to the set preparation volume and liquid adding speed, and at the same time, the mixed solution in the extract preparation barrel 21 is stirred and mixed by driving the mixing and homogenizing module. After the mixed solution is stable, a warning is issued to confirm whether the pH value of the prepared mixed solution meets the requirements (pH = 2.64 ± 0.05).

[0072] b. Extraction liquid packaging process:

[0073] The extract filling process is completed between the extract preparation area 2 and the extract bottle functional area 3. The main operation process is as follows: under the scheduling of the control program, according to the set filling extract bottle series, the corresponding filling volume and the optimal filling speed, the extract filling and adding module 32 is used to fill the prepared extract in the extract preparation barrel 21 into the selected extract bottle.

[0074] Specifically, the two processes of the extract preparation process and the extract packaging process can be run independently, and the two processes can be run successively. For detailed operation flow chart, refer to Figure 4 and Figure 5 shown.

[0075] c. Leachate filtration / filtrate pH determination / filtrate separation / acid addition before digestion / sample acid addition process:

[0076] The leachate filtration / filtrate pH determination / filtrate fractionation / acid addition before digestion / acid addition to retained samples process is completed in the leaching bottle functional area 3, filtration determination functional area 4 and fractionation and volume determination functional area 5. The main process is as follows: the leaching bottle after flipping leaching is placed in the leaching bottle management area, and the preparation of related materials and reagents such as filtration receiving bottle, filtration head, fractionation gun head, fractionation receiving digestion tube, acid addition reagent, cleaning reagent, etc. is completed; the method editing is completed according to the actual leaching bottle sequence; after starting the process, the equipment performs leachate filtration / filtrate pH determination / filtrate fractionation / acid addition before digestion / acid addition to retained samples and other operations in sequence according to the program;

[0077] Specifically, the leachate filtration / filtrate pH determination / filtrate fractionation / acid addition before digestion / sample acid addition process supports single process operation or automatic operation of all processes. For detailed operation flow chart, refer to Figure 6 shown.

[0078] d. Volume determination process after digestion:

[0079] The post-digestion volume setting process is completed in the volume setting function area 5. The main process is as follows: After placing the digested sample (digestion tube) in the digestion tube tray, edit the method process, start the volume setting process, use the ultrasonic sensor to detect the sample volume in the digestion tube, and the built-in algorithm automatically calculates the volume of diluent required to set the volume to the target volume. The volume setting injection pump will add the exact volume of diluent. For a detailed operation flow chart, please refer to Figure 7 shown.

[0080] The above descriptions are merely embodiments of the present invention and are not intended to limit the patent scope of the present invention. Any equivalent structure or equivalent process transformation made using the contents of the present invention specification and drawings, or directly or indirectly applied in other related technical fields, are also included in the patent protection scope of the present invention.

Claims

1. An automated pre-treatment device for fly ash detection, characterized in that: include: The raw material reagent storage area (1) is used to store deionized water for preparing the leaching solution, and is used in conjunction with the reagent module as a raw material reagent area for preparing the leaching solution; The extract preparation area (2) is used to stir and mix the added extract preparation raw materials and reagents to achieve homogeneity of the mixed raw materials and reagents and to store the prepared extract; The extraction bottle functional area (3) is used for dispensing the extraction liquid in the extraction bottle, placing the extraction bottle after the extraction, and serving as a filtration sample area; The filtration determination functional area (4) is used for filtering the leaching solution in the filtration sample area, and at the same time, determining the pH value of the leaching solution and collecting the leaching solution, and adding acid to the sample of the filtrate remaining after the filtration; The fractionation and volume determination functional area (5) is used for placing the digestion tube, receiving the leached liquid, adding acid to the digestion tube, and performing characteristic volume determination after digestion; A support frame (6), the extraction bottle functional area (3), the filtration and measurement functional area (4) and the fractionation and volume determination functional area (5) are sequentially arranged on the support frame (6).

2. The fly ash detection automated pre-treatment equipment according to claim 1, characterized in that: The raw material reagent storage area (1) comprises two reagent storage containers, namely a storage barrel (11) and a storage bottle. The storage barrel (11) is used to store deionized water, and the storage bottle cooperates with the reagent module to store glacial acetic acid reagent.

3. The fly ash detection automated pre-treatment equipment according to claim 2, characterized in that: The storage barrel (11) and the storage bottle are both provided with a one-way ventilation device for preventing the reagent in the storage barrel (11) and the storage bottle from volatilizing and overflowing; the storage barrel (11) and the storage bottle are also both provided with a liquid level monitoring device for monitoring the storage conditions of the reagent in the storage barrel (11) and the storage bottle.

4. The fly ash detection automated pre-treatment equipment according to claim 1, characterized in that: The extract preparation area (2) comprises an extract preparation barrel (21), and a liquid adding pump A (61) and a liquid adding pump B (62) are arranged on one side of the support frame (6). The two ends of the liquid adding pump A (61) are respectively connected to the storage barrel (11) and the extract preparation barrel (21) through a pipeline flow path, and the two ends of the liquid adding pump B (62) are respectively connected to the storage bottle and the extract preparation barrel (21) through a pipeline flow path. A mixing homogenization module is arranged in the extract preparation barrel (21), and the mixing homogenization module is used to mix and stir the prepared solution in the extract preparation barrel (21). The top of the extract preparation barrel (21) is also provided with an upper barrel cover, and the upper barrel cover is also provided with a one-way ventilation device.

5. The fly ash detection automated pre-treatment equipment according to claim 1, characterized in that: The extraction bottle functional area (3) comprises an extraction bottle filling module (31), an extraction liquid filling and adding module (32) and a three-axis A module (33). The extraction bottle filling module (31), the extraction liquid filling and adding module (32) and the three-axis A module (33) are respectively arranged on the support frame (6). The extraction bottle filling module (31) is used to place a plurality of new / unused extraction bottles. The extraction liquid filling and adding module (32) is connected to the extraction liquid preparation barrel (21) to extract and fill the prepared solution in the extraction liquid preparation barrel (21) into the extraction bottles. The three-axis A module (33) is used to transport the extraction bottles between the extraction bottle functional area (3) and the filtration and determination functional area (4).

6. The fly ash detection automated pre-treatment equipment according to claim 1, characterized in that: The filtration measurement functional area (4) comprises a leachate filtration module (41) and a three-axis B module (42) arranged on the support frame (6); the leachate filtration module (41) comprises a leaching bottle station, a filtration head, a rotary dumping module, a filtration module and a double filtration receiving station; the leaching bottle station is used to place the leaching bottle after the flip leaching is completed; the rotary dumping module is used to drive the leaching bottle containing the leachate to dump the leachate in the leaching bottle into the filtration head; The filtration module cooperates with the filtration head to complete the filtration of the sample liquid in the filtration head; one of the double filtration receiving stations is used to receive the filtrate of the wetting process and is used for the determination of the pH value of the filtrate, and the other is used to place the filtrate used in the subsequent process; the three-axis B module (42) is used to transfer the filtration head and the filtration receiving bottle in the filtration determination functional area (4) between the placement area and the working position area.

7. The fly ash detection automated pre-treatment equipment according to claim 6, characterized in that: The filtration measurement functional area (4) also includes a filtrate pH measurement module (43) arranged on the support frame (6), and the filtrate pH measurement module (43) includes a pH meter module, an electrode cleaning station, an electrode dewatering station, a calibration liquid station, and an electrode drive rotation device; the pH meter module includes a pH electrode and a module host, and is embedded with an automatic calibration and automatic measurement program that complies with national standards / European standards; the electrode cleaning station is used for cleaning the electrode before and after measurement; the electrode dewatering station is used to remove water droplets adhering to the surface of the electrode after cleaning; the calibration liquid station is used for pH meter calibration to calibrate calibration solutions with different pH values; the electrode drive rotation device is used to drive the electrode to complete the work flow of different stations to realize automatic calibration and automatic measurement of the pH meter.

8. The fly ash detection automated pre-treatment equipment according to claim 1, characterized in that: The separation and volume determination functional area (5) comprises a filtrate receiving bottle management area (51), a filtrate transfer and distribution module, a pipette tip management area (52), a digestion tube management area (53) and a three-axis C module (55) which are respectively arranged on the support frame (6); the filtrate receiving bottle management area (51) is used to store and place the filtrate receiving bottle; the filtrate transfer and distribution module is used to transfer the filtrate; the pipette tip management area (52) is used to store the pipette tip; the digestion tube management area (53) is used to store the digestion tube, and the digestion tube management area (53) is also provided with a mechanical arm module and a three-axis digestion tube acid addition / volume determination module (54) to respectively complete the acid addition and dilution and volume determination of the digestion tube; the three-axis C module (55) is used to transfer the filtrate in the suction filtration receiving bottle to the digestion tube of the separation and volume determination functional area (5).

9. The fly ash detection automated pre-treatment equipment according to claim 8, characterized in that: The triaxial digestion tube acid addition / volume constant module (54) comprises a digestion acid addition module and a volume constant module. The digestion acid addition module adopts two liquid addition channels to complete the digestion acid addition after the digestion tube is divided in the coverage area; the volume constant module adopts an ultrasonic volume constant method, and is composed of an ultrasonic volume constant sensor and a volume constant liquid addition injection pump, combined with a program algorithm, to complete the volume constant / quantitative dilution of the solution in the digestion tube.

10. An automated pre-treatment method for fly ash detection, according to an automated pre-treatment device for fly ash detection according to any one of claims 1 to 9, characterized in that: The following steps are involved: a. Extract preparation process: under the control of the control program, according to the set preparation volume and liquid adding speed, deionized water and glacial acetic acid are accurately added into the extract preparation barrel (21) by using the liquid adding pump A (61) and the liquid adding pump B (62), and the mixture is stirred and mixed at the same time. After the mixed solution is stable, a warning is given to confirm whether the pH value of the prepared mixed solution meets the requirement (pH=2.64±0.05); b. Extraction liquid filling process: under the control of the control program, according to the set extraction bottle series, the corresponding filling volume and the optimal filling speed, the extraction liquid filling and adding module (32) is used to fill the prepared extraction liquid in the extraction liquid preparation barrel (21) into the selected extraction bottles; c. Leachate filtration / filtrate pH determination / filtrate fractionation / acid addition before digestion / acid addition to retained samples process: After the inverted leaching is completed, the leaching bottle is placed in the leaching bottle management area, and the preparation of related materials and reagents such as the filtration receiving bottle, filtration head, fractionation gun head, fractionation receiving digestion tube, acid addition reagent, cleaning reagent, etc. is completed; the method editing is completed according to the actual leaching bottle sequence; after starting the process, the equipment performs leachate filtration / filtrate pH determination / filtrate fractionation / acid addition before digestion / acid addition to retained samples and other operations in sequence according to the program; d. Post-digestion volume determination process: After placing the digested sample in the digestion tube tray, edit the method process, start the volume determination process, use the ultrasonic sensor to detect the sample volume in the digestion tube first, and the built-in algorithm automatically calculates the volume of diluent required to determine the target volume. The volume determination injection pump will then add the exact volume of diluent.

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