Pre-treatment device for free silicon dioxide determination

Abstract

The application discloses a free silicon dioxide determination pretreatment device, which comprises a liquid taking unit, a digestion unit, a dilution unit and a filtration unit. The liquid taking unit comprises a liquid taking pipe, the liquid taking pipe is connected with a reagent bottle and a reaction container, reagents in the reagent bottle flow into the reaction container through the liquid taking pipe; the reaction container is arranged in the digestion unit, the digestion unit comprises a temperature control module, the temperature control module is arranged on the side wall of the reaction container to perform heat transfer with the reaction container; the dilution unit is arranged in communication with the digestion unit, so that the solution in the reaction container flows into the dilution unit; the filtration unit is arranged below the dilution unit and is used for receiving the solution discharged from the dilution unit to perform filtration. The technical scheme of the application sets the automatic pretreatment device, so that the experiment process for detecting the free silicon dioxide content in dust by adopting the pyrophosphoric acid method is free from manual operation, and the difficulty of the experiment is reduced.

Description

Technical Field

[0001] This invention relates to the field of dust detection technology, and in particular to a pretreatment device for measuring free silica. Background Technology

[0002] In the production processes of the power and coal industries, occupational hazards mainly include silica dust, coal dust, asbestos dust, and cement dust. These dusts are characterized by high levels of free silica and high dispersion. Free silica is extremely harmful to the human body, causing necrosis of pulmonary macrophages and leading to pulmonary fibrosis, a major cause of pneumoconiosis. Therefore, free silica content is a primary indicator for evaluating the hazard nature of dust. Most national and organizational dust hygiene standards use the amount of free silica in deposited dust as the qualitative measure of dust, and then determine compliance with occupational exposure limits based on these limits.

[0003] Currently, the pyrophosphate method, as specified in GBZ / T192.4-2007 "Determination of Dust in Workplace Air Part 4: Free Silica Content," is used to detect the free silica content in dust. This method has low requirements for instruments and experimental conditions, offering advantages such as low experimental cost. Provided there is no interference from sparingly soluble substances, it is considered a reliable, accurate, and practical method, and is the preferred method for various third-party testing institutions and laboratories. However, the temperature for dissolving dust samples in the pyrophosphate method must be strictly controlled between 245℃ and 250℃. If the temperature is too high, gelation may occur; if the temperature is too low, there is a risk of incomplete reaction. Therefore, continuous stirring is required during the dissolution process to ensure that the dust is uniformly dispersed in the pyrophosphate acid at a uniform temperature.

[0004] Currently, this method mainly relies on manual detection, which is cumbersome, time-consuming, and requires stringent reaction conditions. Furthermore, it demands a high level of skill and meticulousness from the operators. Therefore, there is an urgent need to design a fully automated instrument to address this issue. Summary of the Invention

[0005] The main objective of this invention is to provide a pretreatment device for the determination of free silica, which aims to reduce the experimental difficulty of detecting the free silica content in dust using the pyrophosphate method, and improve the controllability and detection accuracy of the experimental process by adopting an automated approach.

[0006] To achieve the above objectives, the pretreatment device for determining free silica proposed in this invention includes a liquid sampling unit, a digestion unit, a dilution unit, and a filtration unit. The liquid sampling unit includes a sampling tube connected to a reagent bottle and a reaction vessel, through which the reagent in the reagent bottle flows into the reaction vessel. The reaction vessel is located within the digestion unit, which includes a temperature control module disposed on the side wall of the reaction vessel for heat transfer. The dilution unit is connected to the digestion unit to allow the solution in the reaction vessel to flow into the dilution unit. The filtration unit is located below the dilution unit to receive and filter the solution discharged from the dilution unit.

[0007] Optionally, the liquid extraction tube includes a pyrophosphate tube, a hydrochloric acid tube, and a distilled water tube. The liquid extraction unit further includes a switching valve, a liquid extraction pump, and a discharge valve. The switching valve includes a first inlet, a second inlet, a third inlet, and a first outlet. The first inlet is connected to the pyrophosphate tube, the second inlet is connected to the hydrochloric acid tube, and the third inlet is connected to the distilled water tube. The liquid extraction pump is connected to the discharge valve and is used to extract reagents from the pyrophosphate tube, the hydrochloric acid tube, and the distilled water tube respectively, and deliver them to the reaction vessel via the feed pipe. The discharge valve is located at the first outlet and connects the various paths by opening and closing the valve body.

[0008] Optionally, the liquid extraction unit further includes a liquid extraction heating module, which is located in the pipeline where the distilled water pipe is located, and is used to heat the distilled water.

[0009] Optionally, the pretreatment device for determining free silica further includes a support frame, the inside of which is formed a accommodating cavity, and the liquid sampling unit, the digestion unit, the dilution unit and the filtration unit are all disposed in the accommodating cavity;

[0010] The digestion unit also includes a digestion support, which is horizontally mounted on the support frame. The top surface of the digestion support is provided with a receiving groove, and the reaction vessel is located in the receiving groove.

[0011] Optionally, the digestion unit further includes a digestion stirring module, the digestion stirring module comprising:

[0012] A stirring support is provided above the digestion support;

[0013] A first stirring rod is positioned below the stirring support and extends into the reaction vessel to stir the solution within the reaction vessel.

[0014] A first stirring motor is mounted on the stirring bracket and connected to the first stirring rod to drive the first stirring rod to rotate.

[0015] Optionally, the digestion unit further includes a lifting module, which is vertically mounted on the support frame and connected to the stirring bracket and the digestion bracket, so as to drive the stirring bracket to move up and down above the digestion bracket.

[0016] Optionally, the temperature control module includes a digestion heating module and a digestion cooling module. The digestion heating module is disposed on the bottom wall of the receiving tank to heat the reaction vessel, and the digestion cooling module is disposed on the side wall of the receiving tank to cool the reaction vessel.

[0017] And / or, the digestion unit further includes a temperature sensor located below the stirring support and extending into the reaction vessel to measure the temperature of the reaction solution.

[0018] Optionally, the dilution unit includes a dilution cup, the dilution cup being sealed, and the dilution unit further includes:

[0019] An extraction module, comprising an extraction tube and an extraction pump, wherein one end of the extraction tube extends into the chamber of the dilution cup and the other end of the extraction tube extends into the reaction vessel, and the extraction pump is located on the sealing cap of the dilution cup and is used to drive the solution in the reaction vessel to be transferred to the dilution cup through the extraction tube;

[0020] The dilution stirring module includes a second stirring rod and a second stirring motor. The second stirring rod is disposed in the chamber of the dilution cup, and the second stirring motor is disposed in the sealing cap of the dilution cup and connected to the second stirring rod to drive the second stirring rod to rotate.

[0021] Optionally, the dilution unit further includes a dilution support, the top surface of which is provided with a placement position, and the dilution cup is placed in the placement position;

[0022] The dilution unit further includes a dilution heating module, which is located on the side wall of the placement position to heat the dilution cup.

[0023] Optionally, the bottom of the dilution cup is connected to a drain pipe, the lower end of which is connected to the filter unit. The solution in the dilution cup flows into the filter unit through the drain pipe for filtration.

[0024] A shut-off valve is installed on the drain pipe, which is used to control the opening and closing of the drain pipe.

[0025] Optionally, the filtering unit includes:

[0026] funnel;

[0027] A filter support, wherein a funnel groove is formed on the surface of the filter support, and the funnel is placed in the funnel groove;

[0028] Waste liquid tank, which is located below the filter support, and a pH meter is installed in the waste liquid tank.

[0029] Optionally, the filtration unit further includes a filtration heating module, which is disposed on the side wall of the funnel groove to heat the funnel.

[0030] Optionally, the pretreatment device for determining free silica further includes a sliding module, which includes a sliding rod and a sliding seat. The sliding rod includes a left sliding rod and a right sliding rod, which are arranged opposite to each other and are respectively located on the left and right walls of the accommodating cavity and connected to the support frame. One end of the sliding seat is slidably connected to the left sliding rod, and the other end of the sliding seat is slidably connected to the right sliding rod. The digestion unit is located on the sliding seat.

[0031] Optionally, the pretreatment device for determining free silica further includes several sliding modules, with the digestion unit located on a sliding seat of one of the sliding modules and the filtration unit located on a sliding seat of another of the sliding modules.

[0032] This invention proposes a pretreatment device for the determination of free silica, comprising a liquid extraction unit, a digestion unit, a dilution unit, and a filtration unit. The liquid extraction unit includes a liquid extraction tube connected to a reagent bottle and a reaction vessel. Reagent from the reagent bottle flows into the reaction vessel through the liquid extraction tube. The reaction vessel is located within the digestion unit and includes a temperature control module disposed on the side wall of the reaction vessel for heat transfer, ensuring the temperature inside the reaction vessel reaches the required reaction temperature. The dilution unit is connected to the digestion unit, allowing the solution from the reaction vessel to flow into the dilution unit. The filtration unit is located below the dilution unit to collect and filter the solution discharged from the dilution unit. Specifically, the liquid extraction unit adds reagent to the reaction vessel, the digestion unit performs the sample digestion reaction, the dilution unit dilutes the digestion solution, and the filtration unit performs the sample filtration reaction. The technical solution of this invention, by setting up an automated pretreatment device, eliminates the need for manual operation by experimental personnel in the processes of obtaining reaction reagents, performing digestion reactions, and dilution filtration, thereby reducing the difficulty of the experiment and improving the controllability and detection accuracy of the experimental process. Attached Figure Description

[0033] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on the structures shown in these drawings without creative effort.

[0034] Figure 1 This is a schematic diagram of the overall structure of an embodiment of the pretreatment device for determining free silica according to the present invention;

[0035] Figure 2 This is a schematic diagram of the internal structure of the back side of an embodiment of the pretreatment device for measuring free silica of the present invention;

[0036] Figure 3 This is a lower cross-sectional view of the digestion unit of an embodiment of the pretreatment apparatus for determining free silica of the present invention;

[0037] Figure 4 This is a lower perspective view of the digestion unit of an embodiment of the pretreatment apparatus for determining free silica of the present invention;

[0038] Figure 5 This is a top cross-sectional view of the digestion unit in an embodiment of the pretreatment apparatus for determining free silica of the present invention.

[0039] Figure 6 This is a top perspective view of the digestion unit of an embodiment of the pretreatment apparatus for determining free silica of the present invention;

[0040] Figure 7 This is a cross-sectional view of the dilution unit in an embodiment of the pretreatment apparatus for determining free silica according to the present invention.

[0041] Figure 8 This is a perspective view of the dilution unit of an embodiment of the pretreatment apparatus for determining free silica according to the present invention;

[0042] Figure 9 This is a cross-sectional view of the filtration unit of an embodiment of the pretreatment device for measuring free silica of the present invention;

[0043] Figure 10 This is a perspective view of a filter unit located on a sliding module in an embodiment of the pretreatment device for measuring free silica according to the present invention.

[0044] Figure 11 This is a schematic diagram of the workflow of an embodiment of the pretreatment device for measuring free silica according to the present invention.

[0045] Explanation of icon numbers:

[0046]

[0047]

[0048] The realization of the objective, functional features and advantages of the present invention will be further explained in conjunction with the embodiments and with reference to the accompanying drawings. Detailed Implementation

[0049] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0050] It should be noted that all directional indications (such as up, down, left, right, front, back, etc.) in the embodiments of the present invention are only used to explain the relative positional relationship and movement of each component in a certain specific posture (as shown in the figure). If the specific posture changes, the directional indication will also change accordingly.

[0051] Furthermore, the use of terms such as "first" and "second" in this invention is for descriptive purposes only and should not be construed as indicating or implying their relative importance or implicitly specifying the number of technical features indicated. Therefore, a feature defined with "first" or "second" may explicitly or implicitly include at least one of that feature. Additionally, the technical solutions of the various embodiments can be combined with each other, but only on the basis of being achievable by those skilled in the art. When the combination of technical solutions is contradictory or impossible to implement, such a combination of technical solutions should be considered non-existent and not within the scope of protection claimed by this invention.

[0052] Currently, the detection of free silica content in dust uses the pyrophosphate method specified in GBZ / T192.4-2007 "Determination of Dust in Workplace Air Part 4: Free Silica Content". During the experiment, the temperature for dissolving the dust sample in the pyrophosphate method must be strictly controlled between 245℃ and 250℃. If the temperature is too high, it can easily form a gel; if the temperature is too low, there is a risk of incomplete reaction. Therefore, continuous stirring is required during the dissolution process to ensure that the dust is evenly dispersed in the uniformly heated pyrophosphate acid. Currently, this method is mainly performed manually, which is cumbersome, time-consuming, and requires high-level reaction conditions. Furthermore, it demands a high level of skill and meticulousness from the experimental personnel.

[0053] To address the aforementioned issues, this invention proposes a pretreatment device for determining free silica, aiming to reduce the experimental difficulty of detecting free silica content in dust using the pyrophosphate method, and improve the controllability and detection accuracy of the experimental process through automation.

[0054] Reference Figures 1 to 2 The free silica determination pretreatment device 100 proposed in this invention includes a liquid collection unit 1, a digestion unit 2, a dilution unit 3, and a filtration unit 4. The liquid collection unit 1 includes a liquid collection tube 10, which connects a reagent bottle and a reaction container 20. The reagent in the reagent bottle flows into the reaction container 20 through the liquid collection tube 10. The reaction container 20 is located in the digestion unit 2, which includes a temperature control module 21. The temperature control module 21 is located on the side wall of the reaction container 20 to transfer heat with the reaction container 20. The dilution unit 3 is connected to the digestion unit 2 so that the solution in the reaction container 20 flows into the dilution unit 3. The filtration unit 4 is located below the dilution unit 3 to receive the solution discharged from the dilution unit 3 for filtration.

[0055] The liquid extraction unit 1 is used to add reagents to the reaction container 20. One end of the liquid extraction tube 10 is connected to a reagent bottle, and the other end is connected to the reaction container 20, which includes beakers, conical flasks, etc. The digestion unit 2 is used to complete the digestion reaction of the sample, the dilution unit 3 is used to dilute the digestion solution, and the filtration unit 4 is used to complete the filtration reaction of the sample. This invention, by setting up an automated pretreatment device 100, eliminates the need for manual operation by experimental personnel in the processes of obtaining reaction reagents, performing digestion reactions, and dilution and filtration, reducing the difficulty of the experiment and improving the controllability and detection accuracy of the experimental process.

[0056] During the experiment, reagents such as pyrophosphate, distilled water, and hydrochloric acid need to be added. Therefore, the liquid collection tube 10 in this invention includes, but is not limited to, a pyrophosphate tube, a hydrochloric acid tube, and a distilled water tube. The liquid collection unit 1 also includes a switching valve (not shown in the figure), a liquid collection pump 12, and a discharge valve 13. The switching valve includes a first inlet, a second inlet, a third inlet, and a first outlet. The first inlet is connected to the pyrophosphate tube, the second inlet is connected to the hydrochloric acid tube, and the third inlet is connected to the distilled water tube. The liquid collection pump 12 is connected to the switching valve and is used to draw reagents from the pyrophosphate tube, the hydrochloric acid tube, and the distilled water tube respectively, and transport them to the reaction vessel 20 through the feed pipe. The discharge valve 13 is located at the first outlet, and the opening and closing of the valve body realizes the connection of each path.

[0057] It should be noted that, in addition to the pipelines mentioned above, the liquid extraction unit also includes an air pipe. All the different pipelines converge at the switching valve, and then flow into the reaction vessel through the first outlet of the switching valve. The drain valve is located at the first outlet and connected to the liquid extraction pump. The path is connected by opening and closing the valve body.

[0058] Understandably, the concentration of hydrochloric acid can be configured according to actual needs. For example, in one embodiment, the concentration of hydrochloric acid is 0.1 mol / L.

[0059] In the pyrophosphate process, distilled water needs to be added for dilution, and the temperature of the distilled water needs to be controlled between 40°C and 50°C. Therefore, in one embodiment of the present invention, the liquid-taking unit 1 further includes a liquid-taking heating module 14, which is located in the pipeline containing the distilled water and is used to heat the distilled water. The liquid-taking heating module 14 includes a first temperature sensor (not shown in the figure), which is used to monitor the temperature of the distilled water. The distilled water flowing through the liquid-taking heating module 14 is rapidly heated to the set temperature for temperature control.

[0060] Furthermore, the pretreatment device 100 also includes a support frame 6, the interior of which is formed a receiving cavity. The liquid collection unit 1, digestion unit 2, dilution unit 3, and filtration unit 4 are all disposed within the receiving cavity. The support frame 6 is a cuboid frame, with a side plate on one side and openable sides on the remaining sides. The liquid collection unit 1 is disposed on the side plate of the support frame 6, and the digestion unit 2, dilution unit 3, and filtration unit 4 are all disposed within the receiving cavity of the support frame 6. The dilution unit 3 is offset from the digestion unit 2, and the filtration unit 4 is disposed below the dilution unit 3. Thus, the liquid collection unit 1, digestion unit 2, dilution unit 3, and filtration unit 4 are connected as a whole by the support frame 6, which constitutes the frame structure of the pretreatment device of this invention.

[0061] Reference Figures 3 to 4 The digestion unit 2 also includes a digestion support 22, which is horizontally mounted on the support frame 6. The top surface of the digestion support 22 is provided with several spaced-apart receiving tanks 221, and the reaction vessel 20 is located in the receiving tanks 221.

[0062] In one embodiment of the present invention, the digestion unit 2 further includes a sample detector, which is disposed on the bottom wall of the reaction vessel 20 or the inner wall of the receiving tank 221, and is used to determine whether a sample has been placed in the reaction vessel 20 in the receiving tank 221.

[0063] Because constant stirring is required during the digestion reaction, refer to Figure 5 The digestion unit 2 also includes a digestion stirring module 23, which includes a stirring support 231, a first stirring rod 232, and a first stirring motor 233. The stirring support 231 is located above the digestion support 22 and is directly opposite to the digestion support 22. The first stirring rod 232 is located below the stirring support 231 and extends into the reaction container 20 to stir the solution in the reaction container 20. The first stirring motor 233 is located on the stirring support 231 and connected to the first stirring rod 232 to drive the first stirring rod 232 to rotate.

[0064] In one embodiment of the present invention, reference is made to... Figures 5 to 6The digestion unit 2 also includes a lifting module 24, which is vertically mounted on the support frame 6. The lifting module 24 is connected to the stirring bracket 231 and the digestion bracket 22 to drive the stirring bracket 231 to move up and down above the digestion bracket 22.

[0065] The lifting module 24 includes a lifting bracket 241, a lifting rod 242, and a driving device. The lifting bracket 241 is vertically connected to the stirring bracket 231 and the digestion bracket 22. A lifting rod 242 is provided on the side of the lifting bracket 241 facing the stirring bracket 231. The upper end of the lifting rod 242 is connected to the upper end plate of the lifting bracket 241, and the lower end of the lifting bracket 241 is connected to the lower end plate. A lifting hole is provided at the end of the stirring bracket 231, and the lifting rod 242 passes through the lifting hole to achieve a sliding connection between the lifting module 24 and the digestion and stirring module 23. The driving device is connected to the end of the stirring bracket 231 to drive the stirring bracket 231 to slide up and down. It is worth mentioning that the present invention can provide the lifting module 24 at one end of the stirring bracket 231, or it can provide the lifting module 24 at both ends of the stirring bracket 231.

[0066] The principle of the pyrophosphate method for detection is as follows: silicates and metal oxides in dust can dissolve in pyrophosphate heated to 245℃~250℃, while free silica is almost insoluble, thus achieving separation. The separated free silica is then weighed, and its percentage content in the dust is calculated. Therefore, the temperature for dissolving dust samples in the pyrophosphate method must be strictly controlled between 245℃ and 250℃. If the temperature is too high, gelation is likely, and if the temperature is too low, there is a risk of incomplete reaction.

[0067] Therefore, in this invention, the digestion unit 2 includes a temperature control module 21, which is disposed on the side wall of the reaction vessel 20 to transfer heat with the reaction vessel 20. The temperature control module 21 includes a digestion heating module 2 and a digestion cooling module 212. (Refer to...) Figure 3 The digestion heating module 2 is located on the bottom wall of the receiving tank 221 to heat the reaction vessel 20, and the digestion cooling module 212 is located on the side wall of the receiving tank 221 to cool the reaction vessel 20. The digestion heating module 2 is mounted on the digestion support 22 and is used to rapidly heat the sample in the reaction vessel 20 to a set temperature of 245℃~250℃ and maintain the sample at a constant temperature for a set time (15min). The digestion cooling module 212 is mounted on the digestion support 22 and is used to rapidly cool the sample in the beaker to a set temperature of 40℃~50℃.

[0068] In one embodiment, the digestion unit 2 further includes a second temperature sensor 213, which is located below the stirring support 231 and extends into the reaction vessel 20 to measure the temperature of the reaction solution. The second temperature sensor 213 is elongated and is disposed adjacent to the first stirring rod 232. When the stirring support 231 is lowered by the lifting module 24, the second temperature sensor 213 extends into the reaction vessel 20 along with the first stirring rod 232. When the stirring support 231 is raised by the lifting module 24, the second temperature sensor 213 is withdrawn from the reaction vessel 20 along with the first stirring rod 232.

[0069] Because the dilution process requires constant stirring, refer to... Figures 7 to 8 The dilution unit 3 includes a dilution cup 31, which is sealed, with its upper opening sealed by a cap. The dilution unit 3 also includes an extraction module 32 and a dilution stirring module 33. The extraction module 32 includes an extraction tube 321 and an extraction pump 322. One end of the extraction tube 321 extends into the chamber of the dilution cup 31, and the other end extends into the reaction vessel 20. The extraction pump 322 is located on the cap of the dilution cup 31 and is a vacuum pump. Utilizing the principle of vacuum extraction, it drives the solution in the reaction vessel 20 to transfer to the dilution cup 31 through the extraction tube 321.

[0070] In one embodiment of the present invention, the bottom wall of the receiving tank 221 is inclined, and the extraction pipe 321 lands on the lower side, ensuring that the digestion liquid in the reaction vessel 20 can be completely extracted.

[0071] The dilution stirring module 33 includes a second stirring rod 331 and a second stirring motor 332. The second stirring rod 331 is disposed in the chamber of the dilution cup 31, and the second stirring motor 332 is disposed in the sealing cap of the dilution cup 31 and connected to the second stirring rod 331 to drive the second stirring rod 331 to rotate. The second stirring rod 331 adopts a V-shaped design to ensure that the diluent is thoroughly stirred.

[0072] Furthermore, the dilution unit 3 also includes a dilution support 34. The top surface of the dilution support 34 is provided with a plurality of spaced placement positions 341. The placement positions 341 can be arranged in the form of a dilution groove recessed on the top surface of the dilution support 34, or a placement ring or the like. The dilution cup 31 is placed in the placement position 341. The number of placement positions 341 is the same as the number of receiving slots 221 for placing the reaction vessel 20.

[0073] The dilution unit 3 also includes a dilution heating module 35, which is disposed on the side wall of the placement position 341 to heat the dilution cup 31. The dilution heating module 35 is wrapped around the outer side wall of the dilution cup 31 to ensure a constant temperature of the diluted solution.

[0074] It should be noted that the dilution unit 3 also includes a third temperature sensor (not shown in the figure). The third temperature sensor is located on the inner wall of the dilution heating module 35. When the dilution heating module 35 is wrapped around the outer wall of the dilution cup 31, the third temperature sensor is attached to the dilution cup 31 and is used to monitor the temperature of the diluent.

[0075] Reference Figures 7 to 8 A drain pipe 3 is connected to the bottom of the dilution cup 31. The lower end of the drain pipe 3 is connected to the filter unit 4. The solution in the dilution cup 31 flows into the filter unit 4 through the drain pipe 3 for filtration. The drain pipe 3 is preferably a flexible tube, and its lower end extends into the filter unit 4, abutting against the side wall of the filter funnel 41. A shut-off valve 312 is provided on the drain pipe 3. The shut-off valve 312 is used to control the opening and closing of the drain pipe 3, thereby controlling the discharge and stop of the diluent.

[0076] In one embodiment of the present invention, the dilution unit 3 further includes a liquid level detection module, which includes a liquid level probe that extends into the bottom of the dilution cup 31 to monitor the remaining liquid level in the dilution cup 31.

[0077] Reference Figure 9 The filtration unit 4 includes a funnel 41, a filter support 42, and a waste liquid tank 43. The funnel 41 contains filter paper folded into a funnel shape, which is then placed against the inner wall of the funnel 41 and moistened with distilled water. The filter paper separates the reaction products from the reaction liquid, facilitating further processing of the reaction products. The filter support 42 is located below the digestion support 22, and the waste liquid tank 43 is located below the filter support 42. The surface of the filter support 42 has funnel grooves 421, and the funnels 41 are placed in these grooves. The number of funnel grooves 421 matches the number of placement positions 341, and each funnel groove 421 is directly opposite a placement position 341, allowing each funnel 41 to receive the solution discharged from a dilution cup 31 for filtration. During filtration, the filtrate must not exceed 2 / 3 of the filter paper.

[0078] Understandably, to prevent reaction products from adhering to the reaction vessel 20 after the reaction solution is transferred from the reaction vessel 20 to the dilution cup 31, the liquid receiving unit 1 delivers hydrochloric acid to the reaction vessel 20 through a hydrochloric acid tube for rinsing. This transfers all reactants remaining inside the reaction vessel 20 onto the filter paper. Typically, the reaction vessel 20 is rinsed 3-5 times, followed by a thorough rinse with hot distilled water. A pH meter 431 is installed in the waste liquid tank 43. The pH meter 431 is used to monitor the pH value of the filtrate in real time and to determine the endpoint of the rinsing process.

[0079] The filtration unit 4 also includes a filtration heating module 44, which is located on the side wall of the funnel groove 421 to heat the funnel 41. The filtration unit 4 can perform static filtration or vacuum filtration, and maintain a constant temperature during filtration.

[0080] The filtration unit 4 also includes a fourth temperature sensor (not shown in the figure). The fourth temperature sensor is located on the inner wall of the filtration heating module 44. When the filtration heating module 44 is wrapped around the outer wall of the funnel 41, the fourth temperature sensor is attached to the funnel 41 to monitor the temperature of the filtrate in order to ensure constant filtration temperature.

[0081] Understandably, in one embodiment of the present invention, the filtration unit 4 further includes a drain pump 45, which is connected to the waste liquid tank 43 through a drain pipe for discharging the liquid in the waste liquid tank 43.

[0082] Reference Figure 10 The free silica determination pretreatment device 100 also includes a sliding module 5, which includes a sliding rod 51 and a sliding seat 52. The sliding rod 51 includes a left sliding rod 5 and a right sliding rod 512, which are arranged opposite to each other and are respectively located on the left and right walls of the accommodating cavity and connected to the support frame 6. One end of the sliding seat 52 is slidably connected to the left sliding rod 5, and the other end of the sliding seat 52 is also slidably connected to the left sliding rod 5. The digestion unit 2 is located on the sliding seat 52. Thus, the digestion unit 2 is slidably connected to the support frame 6 to achieve horizontal sliding of the digestion unit 2 in the accommodating cavity.

[0083] Furthermore, in one embodiment of the present invention, the free silica determination pretreatment device 100 further includes several sliding modules 5, with the digestion unit 2 located on the sliding seat 52 of one sliding module 5 and the filtering unit 4 located on the sliding seat 52 of another sliding module 5. For example, the sliding module 5 includes an upper sliding module and a lower sliding module, with the lower sliding module located below the upper sliding module. The digestion support 22 of the digestion unit 2 is located on the sliding seat 52 of the upper sliding module, and the filter support 42 of the filtering unit 4 is located on the sliding seat 52 of the lower sliding module, so as to realize the horizontal sliding of the digestion unit 2 and the filtering unit 4 in the accommodating cavity.

[0084] The present invention also proposes a free silica measuring device, which includes a controller electrically connected to the pretreatment device 100 to control the operation of the pretreatment device 100. Since this free silica measuring device adopts all the technical solutions of all the above embodiments, it possesses at least all the beneficial effects brought about by the technical solutions of the above embodiments, which will not be elaborated further here.

[0085] Please refer to the figure. The working steps of the pretreatment device 100 for determining free silica of the present invention are as follows:

[0086] S1: Confirm that 0.1g to 0.2g of sample has been placed in reaction vessel 20;

[0087] S2: Control the liquid taking unit 1 to add 15ml of pyrophosphate into the reaction vessel 20 to obtain a mixed solution;

[0088] S3: Control the digestion heating module 2 to heat the mixture in the reaction vessel 20 to 245℃~250℃, and at the same time start the first stirring motor 233 to drive the first stirring rod 232 to stir for 15 minutes.

[0089] S4: Control the digestion and cooling module 212 to cool the mixture to 40℃~50℃;

[0090] S5: Control the liquid taking unit 1 to add distilled water at 50℃~80℃ to the reaction vessel 20 so that the volume of the mixture is 40ml~45ml, and control the first stirring rod 232 to stir at the same time.

[0091] S6: Control the extraction module 32 to transfer the mixture in the reaction vessel 20 into the dilution cup 31, and control the liquid taking unit 1 to add distilled water at 50℃~80℃ to the reaction vessel 20 again. Control the extraction module 32 to transfer the rinsing liquid in the reaction vessel 20 into the dilution cup 31, so that the volume of the mixture in the dilution cup 31 is 150ml~200ml. At the same time, control the second stirring rod 331 to stir.

[0092] S7: Control the dilution heating module 35 to heat the mixture to boiling;

[0093] S8: Open the shut-off valve 312 to allow the mixture in the reaction vessel 20 to flow into the filter unit 4 in batches for filtration.

[0094] S9: Control the liquid extraction unit 1 to extract hydrochloric acid solution to rinse the reaction vessel 20, and then control the extraction unit to transfer all the cleaning solution in the reaction vessel 20 to the filter unit 4.

[0095] The liquid extraction unit 1 is controlled to draw hot distilled water to rinse the reaction vessel 20, and then the extraction unit is controlled to transfer the cleaning liquid in the reaction vessel 20 to the filtration unit 4.

[0096] S10: Remove the filter paper.

[0097] In this embodiment, the control body of the detection method is a controller, which controls each unit and module. Before step S1, the reaction vessel 20 containing the sample to be tested is manually placed into the sample holder. The sample detector confirms that the reaction vessel 20 contains the sample and sends feedback to the control system for marking. During step S3, the second temperature sensor 213 monitors the temperature of the digestion solution in the reaction vessel 20 in real time. When the temperature fed back by the second temperature sensor 213 reaches 245℃~250℃, it is kept constant for 15 minutes. During step S4, when the temperature fed back by the second temperature sensor 213 reaches the set cooling temperature of 40℃~50℃, the digestion cooling module 212 stops working. During step S4, the liquid extraction pump 12 and the liquid extraction heating module 14 are started. The distilled water obtained reaches the set temperature of 50℃~80℃ after flowing through the liquid extraction heating module 14. The drain valve 13 is started, and the valves corresponding to the marked beakers are opened sequentially, injecting hot distilled water into the reaction vessel 20 through the feed pipe. Step S9 further includes: S91 activating the filter heating module 44 to ensure the liquid in the funnel 41 is kept at a constant temperature within the set temperature, and allowing it to stand for filtration. After step S9, the following steps are also included: S92 the controller calculates the liquid volume in the waste liquid tank 43 based on the discharge volume of the liquid in the funnel 41, and activates the drain pump 45 to discharge the liquid in the waste liquid tank 43.

[0098] In step S9, the liquid extraction unit 1 is controlled to extract distilled water to rinse the reaction vessel 20, and then the extraction unit is controlled to transfer all the cleaning solution in the reaction vessel 20 to the filtration unit 4. The method further includes:

[0099] S93: Observe the pH value of the pH meter 431 installed in the waste liquid tank 43;

[0100] S94: When pH meter 431 reports an acidic pH value, control liquid sampling unit 1 to draw distilled water to rinse reaction vessel 20;

[0101] S95: When pH meter 431 reports no acidic pH value, control liquid sampling unit 1 to stop drawing distilled water.

[0102] In this embodiment, the endpoint of cleaning is determined by observing the detection signal of the pH meter 431, ensuring that all reaction products are transferred to the filter paper and avoiding residue that could affect the accuracy of the detection. Simultaneously, by using the pH meter 431, over-cleaning can be avoided, preventing waste.

[0103] In one implementation, after performing step S1, the following is also included:

[0104] S: Control the upper sliding module 5 to operate, and horizontally move the digestion support 22 to the first sample test position. The lifting module 24 operates to lower the digestion stirring module 23 from the high position to the low position. At this time, the second temperature sensor 213 and the first stirring rod 232 extend into the reaction vessel 20 below the liquid surface.

[0105] S12: Control the operation of the lower sliding module 5 to horizontally move the funnel 41 and waste liquid pool 43 to the test position of the first group of samples.

[0106] After executing S10, the following is also included:

[0107] S101: Control the operation of the lifting module 24 to raise the digestion stirring module 23 and the extraction tube 321 to the high position. The upper sliding module 5 operates to horizontally move the digestion support 22 to the next set of sample test positions. The lifting module 24 operates to lower the digestion stirring module 23 from the high position to the low position. At this time, the second temperature sensor 213 and the first stirring rod 232 extend into the reaction vessel 20 below the liquid surface.

[0108] S102: Control the operation of the lower sliding module 5 to horizontally move the funnel 41 and waste liquid pool 43 to the next group of sample test positions;

[0109] S103: After all tests are completed, control the lifting module 24 to operate, raising the digestion stirring module 23 and the extraction tube 321 to the high position. The upper sliding module 5 and the lower sliding module 5 operate to horizontally move the sample holder and funnel 41 to the initial position.

[0110] This embodiment is applied to situations where multiple sets of samples need to be tested. The sliding module 5 enables the digestion unit 2 and the filtering unit 4 to move quickly to the next set of sample testing positions, thereby improving the efficiency of batch testing.

[0111] The above description is merely a preferred embodiment of the present invention and does not limit the patent scope of the present invention. Any equivalent structural transformations made using the contents of the present invention's specification and drawings under the inventive concept of the present invention, or direct / indirect applications in other related technical fields, are included within the patent protection scope of the present invention.

Claims

1. A pre-treatment device for free silica determination, characterized in that, The device comprises: a liquid taking unit, which comprises a liquid taking pipe connected with a reagent bottle and a reaction container, and the reagent in the reagent bottle flows into the reaction container through the liquid taking pipe; a digestion unit, in which the reaction container is arranged, and the digestion unit comprises a temperature control module arranged on the side wall of the reaction container to perform heat transfer with the reaction container; a dilution unit, which is arranged in communication with the digestion unit to make the solution in the reaction container flow into the dilution unit; a filtration unit, which is arranged below the dilution unit to receive the solution discharged from the dilution unit for filtration; the dilution unit comprises a dilution cup arranged in a sealed manner, and further comprises: an extraction module, which comprises an extraction pipe and an extraction pump, one end of the extraction pipe extends into the cavity of the dilution cup, the other end of the extraction pipe extends into the reaction container, and the extraction pump is arranged on the sealing cover of the dilution cup to drive the solution in the reaction container to be transferred to the dilution cup through the extraction pipe; a dilution stirring module, which comprises a second stirring rod arranged in the cavity of the dilution cup and a second stirring motor arranged on the sealing cover of the dilution cup and connected with the second stirring rod to drive the second stirring rod to rotate.

2. The free silica assay pre-treatment device of claim 1, wherein, The liquid taking pipe comprises a pyrophosphoric acid pipe, a hydrochloric acid pipe and a distilled water pipe, and the liquid taking unit further comprises: a switching valve, which comprises a first inlet, a second inlet, a third inlet and a first outlet, the first inlet is in communication with the pyrophosphoric acid pipe, the second inlet is in communication with the hydrochloric acid pipe, and the third inlet is in communication with the distilled water pipe; a liquid taking pump connected with the switching valve, which is used to extract reagents from the pyrophosphoric acid pipe, the hydrochloric acid pipe and the distilled water pipe respectively and deliver them to the reaction container through the first outlet; a discharge valve arranged at the first outlet to realize the communication of each path by opening and closing the valve body.

3. The free silica assay pre-treatment device of claim 2, wherein, The liquid taking unit further comprises a liquid taking heating module arranged on the pipe line where the distilled water pipe is arranged to heat the distilled water.

4. The free silica assay pretreatment device of claim 1, wherein, The free silicon dioxide determination pretreatment device further comprises a support frame, an accommodating cavity is formed in the inside of the support frame, and the liquid taking unit, the digestion unit, the dilution unit and the filtration unit are arranged in the accommodating cavity; the digestion unit further comprises a digestion support frame horizontally arranged on the support frame, and a containing groove is arranged on the top surface of the digestion support frame, and the reaction container is arranged in the containing groove.

5. The free silica assay pre-treatment device of claim 4, wherein, The digestion unit further comprises a digestion stirring module, which comprises: a stirring support frame arranged above the digestion support frame; a first stirring rod arranged below the stirring support frame and extending into the reaction container to stir the solution in the reaction container; a first stirring motor arranged on the stirring support frame and connected with the first stirring rod to drive the first stirring rod to rotate.

6. The free silica assay pre-treatment device of claim 5, wherein, The digestion unit further comprises a lifting module vertically arranged on the support frame, the lifting module connecting the stirring support and the digestion support to drive the stirring support to lift above the digestion support.

7. The free silica assay pre-treatment device of claim 5, wherein, The temperature control module comprises a digestion heating module arranged on the bottom wall of the accommodating groove to heat the reaction container and a digestion cooling module arranged on the side wall of the accommodating groove to cool the reaction container. The digestion unit further comprises a temperature sensor arranged below the stirring support, the temperature sensor extending into the reaction container to measure the temperature of the reaction solution.

8. The free silica assay pretreatment device of claim 1, wherein, The dilution unit further comprises a dilution support, the top surface of the dilution support being provided with a placement position, and the dilution cup being placed on the placement position. The dilution unit further comprises a dilution heating module arranged on the side wall of the placement position to heat the dilution cup.

9. The free silica assay pretreatment device of claim 1, wherein, The bottom of the dilution cup is connected with a drainage pipe, the lower end of the drainage pipe being connected with the filtration unit, and the solution in the dilution cup flows into the filtration unit through the drainage pipe to be filtered. A stop valve is arranged on the drainage pipe to control the opening and closing of the pipeline of the drainage pipe.

10. The free silica assay pretreatment device of claim 1, wherein, The filtration unit comprises: a funnel; a filtration support, the surface of the filtration support being provided with a funnel groove, and the funnel being placed in the funnel groove; a waste liquid pool arranged below the filtration support, and a pH meter arranged in the waste liquid pool.

11. The free silica assay pre-treatment device of claim 10, wherein, The filtration unit further comprises a filtration heating module arranged on the side wall of the funnel groove to heat the funnel.

12. A pre-treatment device for the determination of free silicon dioxide according to any one of claims 4 to 7, characterized in that The free silicon dioxide determination pretreatment device further comprises a sliding module, the sliding module comprising a sliding rod and a sliding seat, the sliding rod comprising a left sliding rod and a right sliding rod, the left sliding rod and the right sliding rod being oppositely arranged and respectively arranged on the left side wall and the right side wall of the accommodating cavity and connected with the support frame, one end of the sliding seat being slidingly connected with the left sliding rod, and the other end of the sliding seat being slidingly connected with the right sliding rod, and the digestion unit being seated on the sliding seat.

13. The free silica assay pre-treatment device of claim 12, wherein, The free silicon dioxide determination pretreatment device further comprises a plurality of sliding modules, the digestion unit being seated on the sliding seat of one of the sliding modules, and the filtration unit being seated on the sliding seat of another of the sliding modules.

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