High-throughput x-ray diffraction automation pre-treatment device

Abstract

The application discloses a high-flux X diffraction automatic pretreatment device, and technical scheme points are as follows: the device comprises a heating and stirring module, a plurality of stirring stations and ultrasonic stations for placing beakers or centrifuge tubes are arranged on the heating and stirring module, and the heating and stirring module is used for heating and stirring clay samples and liquid media through a mechanical or ultrasonic wave mode; a liquid pumping module is arranged on a three-axis mechanical arm and is used for pumping and discharging supernatant after static setting in the beakers; a quantitative ring pipetting module is arranged on the three-axis mechanical arm and is used for pumping the middle suspension liquid in the beakers into the centrifuge tubes and pumping sample solutions in the centrifuge tubes after centrifugal operation to glass slides. Through the multi-station heating and stirring module, the clay samples can be heated and stirred in batches, the heating and stirring mode can also help the precipitation of clay particles, the mechanical stirring can accelerate the suspension of the clay, and meanwhile, the automatic heating and stirring can realize standardized treatment and inspection and improve the accuracy of clay sample detection.

Description

Technical Field

[0001] This invention relates to clay testing technology, and more specifically, to a high-throughput X-ray diffraction automated pretreatment device. Background Technology

[0002] While methods such as neutron diffraction, electron diffraction, infrared spectroscopy, and Mössbauer spectroscopy can be used to analyze the structure of matter, X-ray diffraction is the most effective and widely used method. Moreover, X-ray diffraction was the first method used by humankind to study the microscopic structure of matter. The applications of X-ray diffraction are extremely broad, and it has now permeated various engineering and technological sciences, including physics, chemistry, earth sciences, and materials science.

[0003] Among them, X-ray diffraction mineral qualitative / quantitative analysis technology is an extremely important and most frequently used research method for the quantitative analysis of mineral components in the three major rock types of sedimentary rocks, igneous rocks, and metamorphic rocks. It is of great significance for oil and gas exploration and development, reservoir evaluation, reservoir stimulation, well logging interpretation, diagenesis and sedimentary environment research.

[0004] According to the current standard SY / T5163-2018 "X-ray Diffraction Analysis Method for Clay Minerals and Common Non-Clay Minerals in Sedimentary Rocks", X-ray diffraction technology can be used to quantitatively analyze mineral components and qualitatively and quantitatively analyze clay minerals in rocks. The testing process mainly includes sample crushing, soaking, extraction, slide preparation, and scanning. However, the suspension of clay minerals during soaking seriously affects the accuracy of the test results. During soaking, the soaking solution of clay minerals needs to be thoroughly stirred to ensure that the clay minerals are suspended to a level that allows for extraction. However, the degree of stirring directly affects the accuracy of the test results. Summary of the Invention

[0005] To address the shortcomings of existing technologies, the present invention aims to provide a high-throughput X-ray diffraction automated pretreatment device.

[0006] The above-mentioned technical objective of the present invention is achieved through the following technical solution: a high-throughput X-ray diffraction automated pretreatment device, comprising: Machine tool; The three-axis robotic arm moves within the machine via a gantry transmission module and is equipped with grippers for lifting and placing beakers or centrifuge tubes to the corresponding positions. The liquid addition module is mounted on a three-axis robotic arm and has at least three independent liquid addition components. The independent liquid addition components are used to add three liquid media into beakers or centrifuge tubes respectively. The liquid media include tap water, distilled water and dilute hydrochloric acid. The heating and stirring module is equipped with several stirring stations and ultrasonic stations for placing beakers or centrifuge tubes, and is used to heat and stir clay samples and liquid media by mechanical or ultrasonic means. The liquid extraction module, mounted on a three-axis robotic arm, is used to extract and discharge the supernatant liquid in a beaker after it has been left to stand. The quantitative loop transfer module, mounted on a three-axis robotic arm, is used to aspirate the middle layer suspension in a beaker into a centrifuge tube and to extract the sample solution from the centrifuge tube after centrifugation into a glass slide. The glass slide heating module is equipped with a storage station for heating glass slides containing sample solutions located in the storage station; The cleaning and pouring module is installed on the machine platform and is used to spray and clean beakers or centrifuge tubes held by grippers. The process involves adding a specific amount of dilute hydrochloric acid to a beaker containing a clay sample via a liquid addition module, stirring and heating the sample in the beaker via a heating and stirring module, then draining the supernatant after heating, stirring, and settling via a liquid extraction module. This process is repeated until the turbidity reaches the required level. The intermediate suspension is then extracted via a quantitative loop transfer module and injected into a centrifuge tube. After centrifugation, the sample solution is transferred to a glass slide via a quantitative loop transfer module, and the slide is heated and prepared via a glass slide heating module.

[0007] The present invention is further configured such that: the heating and stirring module includes an upper seat and a lower seat, the upper seat is provided with a heating module, the heating module is provided with a plurality of cup-holding areas for accommodating beakers, and the lower seat is provided with a plurality of electromagnetic stirring modules corresponding one-to-one with the cup-holding areas, for realizing synchronous or asynchronous heating and stirring of beakers containing clay samples.

[0008] The present invention is further configured such that: a sealing plate is fixedly connected inside the lower seat; the electromagnetic stirring module includes a stirring motor and a magnetic stirring head; and the stirring motor is fixedly connected to the sealing plate through a fixing frame. A magnet holder is fixedly connected to the output end of the stirring motor. The eccentric position of the magnet holder forms several cavities for accommodating magnets, which are used by the stirring motor to drive several magnets to rotate in order to stir the mixture in the beaker.

[0009] The present invention is further configured such that: a temporary storage rack is provided on the machine base on one side of the heating and stirring module, the temporary storage rack is used to place beakers or centrifuge tubes, and a suction head circulation cleaning tank is provided on one side of the temporary storage rack.

[0010] The present invention is further configured such that: the heating and stirring module further includes an ultrasonic module mounted on the machine platform; the ultrasonic module includes a housing; the top surface of the housing is recessed to form an ultrasonic station for placing several centrifuge tubes; an ultrasonic generator is installed inside the housing close to the ultrasonic station; and a test tube rack is detachably connected to the housing.

[0011] The present invention is further configured such that: the cleaning and pouring module includes a beaker cleaning module and a centrifuge tube cleaning module; the machine platform is provided with a pouring area; the pouring area is provided with a filter assembly; the filter assembly is used to trap solid samples on the filter assembly.

[0012] The present invention is further configured such that: the filter assembly includes a waste liquid tank and a retention filter; a horizontal linear sliding module is provided on the machine base; the displacement stroke of the horizontal linear sliding module covers the beaker cleaning module and the filter assembly; and a tilting gripper assembly is connected to the horizontal linear sliding module through a vertical linear sliding module. The tilting gripper assembly is used to hold the beaker to the filter assembly for rotation and tilting, and then move to the beaker cleaning module for rotation and inversion. The inverted beaker is then sprayed and cleaned by the cleaning and tilting module.

[0013] The present invention is further configured such that: the temporary storage rack is provided with at least two placement positions for temporarily storing beakers or centrifuge tubes, the placement positions being used to temporarily store beakers or centrifuge tubes to be cleaned.

[0014] The present invention is further configured such that: the quantitative loop transfer module includes at least two peristaltic pumps, which are used to aspirate the middle layer suspension in the beaker and quantitatively transfer it to the centrifuge tube, and quantitatively aspirate the sample solution to the glass slide after the centrifugation operation is completed.

[0015] In summary, the present invention has the following beneficial effects: This application enables standardized pretreatment of clay samples through equipment. The multi-station heating and stirring module can heat and stir clay samples in batches. The heating and stirring method can also help the clay particles to precipitate. The mechanical stirring can accelerate the suspension of clay, replacing the traditional manual stirring method and freeing up labor. At the same time, the automated heating and stirring can achieve standardized processing and testing, and improve the accuracy of clay sample testing. Secondly, through the liquid extraction module and the liquid addition module, when preparing clay samples, dilute hydrochloric acid and carbonate can be added to fully react, and then distilled water is added in a circulating manner to clean and soak the clay samples. The liquid extraction module also repeatedly extracts the clear liquid from the top layer to reduce the concentration of hydrochloric acid and maintain the accuracy of clay sample preparation. When sampling, selecting to aspirate the suspension in the middle layer can improve the accuracy of clay preparation, avoid the situation where trace amounts of dilute hydrochloric acid remain in the upper liquid, and also avoid large clay particles in the bottom layer, thus improving the reliability of sampling. Furthermore, using a peristaltic pump results in minimal movement when aspirating the liquid, which can also prevent the sample solution from becoming turbid. After sampling, the clay particles were centrifuged to settle, and then the clear liquid was poured out. Distilled water was added again and the mixture was ultrasonically stirred to further reduce the influence of any residual dilute hydrochloric acid in the solution. Then, the sample was heated by a glass slide to simulate air drying, which shortened the slide preparation cycle and facilitated subsequent operations such as the production of high-temperature slides. Attached Figure Description

[0016] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of the present invention and should not be regarded as a limitation on the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0017] Figure 1 The three-dimensional representation of the present invention Figure 1 This is used to indicate the state where the external sheet metal structure of the device is hidden; Figure 2 The three-dimensional representation of the present invention Figure 2 This indicates the state where the truss drive module is hidden; Figure 3 for Figure 2 Enlarged view of point A in the middle; Figure 4 This is a schematic diagram of the truss transmission module in the present invention; Figure 5 This is a partial cross-sectional view of the heating and stirring module in this invention, used to show the internal structure of the heating and stirring module; Figure 6 This is a schematic diagram of the electromagnetic stirring module in this invention; Figure 7 This is a flowchart of Embodiment 2 of the present invention; Figure 8 This is an operation flowchart of Embodiment 2 of the present invention; Figure 9 This is a flowchart of the circulating drainage operation in Embodiment 2 of the present invention; Figure 10 This is a flowchart illustrating the operation of the suspended state in Embodiment 2 of the present invention; Figure 11 This is a flowchart illustrating the clay extraction and clay preparation process in Embodiment 2 of this invention.

[0018] The diagram shows: 1. Machine base; 2. Three-axis robotic arm; 21. Truss transmission module; 22. Gripper; 3. Liquid addition module; 4. Heating and stirring module; 41. Stirring station; 411. Upper seat; 412. Lower seat; 413. Heating module; 414. Electromagnetic stirring module; 415. Magnet holder; 416. Cavity; 42. Ultrasonic station; 421. Box body; 422. Test tube rack; 5. Liquid extraction module; 6. Slide heating module; 7. Cleaning and pouring module; 71. Beaker cleaning module; 72. Pouring area; 73. Horizontal linear sliding module; 74. Pouring gripper assembly; 8. Temporary storage rack. Detailed Implementation

[0019] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, 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 some embodiments of the present invention, and not all embodiments. The components of the embodiments of the present invention described and shown in the accompanying drawings can generally be arranged and designed in various different configurations.

[0020] Therefore, the following detailed description of the embodiments of the invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely to illustrate selected embodiments of the invention. All other embodiments obtained by those skilled in the art based on the embodiments of the invention without inventive effort are within the scope of protection of the invention.

[0021] It should be noted that similar labels and letters in the following figures indicate similar items. Therefore, once an item is defined in one figure, it does not need to be further defined and explained in subsequent figures.

[0022] In the description of this invention, it should be understood that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, or the orientation or positional relationship commonly used when the product of this invention is in use, or the orientation or positional relationship commonly understood by those skilled in the art. They are only used to facilitate the description of this invention and to simplify the description, and are not intended to indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this invention.

[0023] Furthermore, the terms "first," "second," and "third" are used only to distinguish descriptions and should not be interpreted as indicating or implying relative importance.

[0024] In the description of this invention, it should also be noted that, unless otherwise explicitly specified and limited, the terms "set," "install," "connect," and "link" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.

[0025] A high-throughput X-ray diffraction automated pretreatment device, such as Figure 1 , Figure 2 as well as Figure 4 As shown, it includes: Machine tool; The three-axis robotic arm moves within the machine via a gantry transmission module and is equipped with grippers for lifting and placing beakers or centrifuge tubes to the corresponding positions. The liquid addition module is mounted on a three-axis robotic arm and has at least three independent liquid addition components. These components are used to add three different liquid media into beakers or centrifuge tubes, including tap water, distilled water, and dilute hydrochloric acid. In this embodiment, refer to... Figure 1 and Figure 2 As shown, three storage tanks are placed below the machine, used to hold tap water, distilled water, and dilute hydrochloric acid, respectively. Tap water is mainly used for cleaning, supplying the cleaning and pouring module to rinse centrifuge tubes, beakers, and other containers after the experiment. Distilled water is used for circulating liquid addition; after the supernatant is drained, distilled water is added to further heat and stir the clay sample. The dilute hydrochloric acid is mainly used to react with the carbonates in the clay sample during the initial liquid addition. If the reaction is insufficient during subsequent liquid additions, dilute hydrochloric acid can be added again as needed.

[0026] The heating and stirring module is equipped with several stirring stations and ultrasonic stations for placing beakers or centrifuge tubes, and is used to heat and stir clay samples and liquid media by mechanical or ultrasonic means. The liquid extraction module, mounted on a three-axis robotic arm, is used to extract and discharge the supernatant liquid after settling in a beaker. In this embodiment, the range of the supernatant liquid is taken as a 200ml beaker. After the clay sample is heated, stirred, and allowed to settle and separate, the supernatant liquid is extracted from about 20ml below the liquid surface. It should be noted that the accidental extraction of the suspension should be avoided as much as possible when draining the supernatant liquid. In this embodiment, if the 20ml below the liquid surface is clear, it indicates that the operation of adding liquid and extracting the supernatant liquid for drainage is still required. The quantitative loop transfer module, mounted on a three-axis robotic arm, is used to aspirate the intermediate suspension in a beaker into a centrifuge tube. Specifically, the intermediate suspension range refers to the suspension sampled from 40-60 ml above the liquid level. The module also extracts the sample solution from the centrifuge tube after centrifugation and transfers it to a glass slide. The glass slide heating module is equipped with a storage station for heating glass slides containing sample solutions located in the storage station; The cleaning and pouring module is installed on the machine platform and is used to spray and clean beakers or centrifuge tubes held by grippers. In this process, a measured amount of dilute hydrochloric acid is added to a beaker containing a clay sample via a liquid addition module. The sample in the beaker is stirred and heated simultaneously via a heating and stirring module. Specifically, in this embodiment, the heating temperature of the heating and stirring module is set to 80-100℃, preferably 80℃. Then, the supernatant after heating, stirring, and settling is extracted and drained via a liquid extraction module. This process is repeated until the turbidity reaches the standard. The middle suspension is then extracted via a quantitative loop transfer module and injected into a centrifuge tube. After centrifugation, the sample solution is transferred to a glass slide via a quantitative loop transfer module, and the slide is heated and prepared using a glass slide heating module.

[0027] like Figure 5 and Figure 6 As shown, the heating and stirring module includes an upper seat and a lower seat. The upper seat contains a heating module with several cup-holding areas for accommodating beakers. The lower seat contains several electromagnetic stirring modules corresponding to the cup-holding areas, used to synchronously or asynchronously heat and stir the beakers containing clay samples. In this embodiment, a total of four sets of heating and stirring modules are provided, and each heating and stirring module is provided with 25 cup-holding areas and 25 electromagnetic stirring modules. Through the setting of four sets, each with 25 cup-holding areas, the solution in beakers containing clay samples can be heated and stirred. Batch stirring enables high-throughput batch inspection. Specifically, a sealing plate is fixedly connected inside the lower seat. The electromagnetic stirring module includes a stirring motor and a magnetic stirring head. The stirring motor is fixedly connected to the sealing plate via a fixing frame, and a magnetic retainer is fixedly connected to the output end of the stirring motor. The eccentric position of the magnetic retainer forms several cavities for accommodating magnets, which are used by the stirring motor to drive several magnets to rotate to stir the mixture in the beaker. In this embodiment, the magnetic stirring head is placed inside the beaker, and the stirring motor drives the magnetic retainer to rotate.

[0028] like Figure 2 and Figure 3As shown, the machine is equipped with a temporary storage rack located on one side of the heating and stirring module. The temporary storage rack is used to place beakers or centrifuge tubes. A pipette tip circulation cleaning tank is provided on one side of the temporary storage rack. Specifically, in this embodiment, the pipette tip circulation cleaning tank is provided with two chambers, and the side walls of the two chambers adjacent to each other are provided with overflow holes connecting the two chambers. This allows circulating water to flow from the bottom of one chamber to the other chamber through the overflow hole. When cleaning the pipette tip, the pipette tip is immersed in the chamber, and the outer surface of the pipette tip is cleaned by the circulating water. The cleaned circulating water flows to the other chamber through the overflow hole. Therefore, the pipette tip circulation cleaning tank is always kept clean, which can avoid cross-influence caused by the pipette tip when performing operations such as aspirating the upper layer of clear liquid and the middle layer of suspension in each beaker.

[0029] like Figure 1 and Figure 2 As shown, the heating and stirring module also includes an ultrasonic module mounted on the machine platform. The ultrasonic module includes a housing with a recessed top surface forming an ultrasonic station for placing several centrifuge tubes. An ultrasonic generator is installed inside the housing, close to the ultrasonic station. A test tube rack is detachably connected to the housing. Specifically, in this embodiment, the test tube rack is mounted on the housing, water is introduced into the housing, and after the ultrasonic generator is started, the clay sample in the test tubes placed on the test tube rack can be ultrasonically stirred to disperse the clay sample evenly. The test tube rack can also fix the test tubes, so that even when only a small amount of sample remains and the mass is relatively light, the bottom of the test tube can be in contact with water, thereby fully ultrasonically stirring the sample in the test tube.

[0030] The cleaning and tilting module includes a beaker cleaning module and a centrifuge tube cleaning module. The machine base has a tilting area equipped with a filter assembly. The filter assembly is used to trap solid samples. The filter assembly includes a waste liquid tank and a trapping filter. The machine base has a horizontal linear sliding module whose displacement covers both the beaker cleaning module and the filter assembly. A tilting gripper assembly is connected to the horizontal linear sliding module via a vertical linear sliding module. Specifically, the tilting gripper assembly is used to clamp the beaker to the filter assembly for rotational tilting, and then moves to the beaker cleaning module for rotational inversion. The cleaning and tilting module then sprays and cleans the inverted beaker.

[0031] The temporary storage rack has at least two placement positions for temporarily storing beakers or centrifuge tubes. The placement positions are used to temporarily store beakers or centrifuge tubes to be cleaned. The quantitative loop transfer module includes at least two peristaltic pumps. The peristaltic pumps are used to aspirate the middle layer suspension in the beaker and quantitatively transfer it to the centrifuge tube, and quantitatively aspirate the sample solution to the glass slide after the centrifugation operation is completed.

[0032] Example 2, as follows Figure 7-11As shown, the machine simulation slide preparation method using the high-throughput X-ray diffraction automated pretreatment apparatus described in Example 1 includes: Sample preparation: Take a quantitative sample of the crushed clay sample and put it into a beaker. Add 3-10% dilute hydrochloric acid and react until no reaction occurs to remove carbonates. Soak and stir, add distilled water to the beaker, heat the beaker while stirring, and observe the clay suspension. Specifically, observe the clarity of the upper 20ml of solution in the beaker. If the upper layer is clear liquid, perform circulation and drainage. If the upper 20ml of solution contains clay suspension, it indicates that the clay is well suspended, and the middle suspension can be extracted and centrifuged. After circulating the liquid and completing the soaking and stirring operation, the upper clear liquid is extracted and discharged into the waste liquid tank. Then, distilled water is added again, and the soaking and stirring operation is repeated 5-7 times. The suspension of the clay is observed. Manual centrifugation: After the circulation and drainage operation is completed, the middle layer suspension is extracted by standing and dispensed into centrifuge tubes. Several centrifuge tubes containing the middle layer suspension are manually transferred to the centrifuge for centrifugation. After the clay particles settle, the upper waste liquid is poured out. For clay extraction, add 1-5 ml of distilled water to the centrifuge tube after manual centrifugation and mix by sonication. Then, take 0.7-1 ml of the sample using a pipette. Clay slide preparation involves transferring the sample taken by pipette onto a glass slide and then drying it to prepare the slide.

[0033] In this embodiment, 180 ml of 5% dilute hydrochloric acid was added to a beaker containing the clay sample. The mixture was stirred to allow the hydrochloric acid to react with the carbonate components in the clay sample. Optional auxiliary heating was used during stirring to increase the number of collisions between the hydrochloric acid and the hydrogen and carbonate ions in the carbonate, thus ensuring a thorough reaction between the hydrochloric acid and the carbonate. This shortened the time required for acid washing and acidification, and the thorough reaction improved the subsequent suspension effect. After the reaction was complete and the mixture was allowed to stand, the upper waste liquid was drained, followed by soaking and stirring. An appropriate amount of distilled water was added. In this embodiment, a 200 ml beaker was used, and the amount of distilled water added was 180 ml. ml, and stir the mixed solution again at a uniform speed. Heat the beaker to 80-100℃. In this embodiment, heating to 80℃ is selected. Then let it stand for 2 hours, not exceeding 2 hours. Observe the suspension of the mixture in the beaker. When the suspension of the mixture in the beaker does not meet the standard, that is, when the clay is not suspended or the suspension effect is poor, extract the upper waste liquid (the upper waste liquid in this operation is a clear liquid), add an appropriate amount of dilute hydrochloric acid solution, then heat and stir, and then let it stand for 3-10 minutes before observing. By adding dilute hydrochloric acid appropriately, the precipitation of clay particles from carbonate is improved, thereby improving the suspension of clay.

[0034] When the suspension of the mixture in the beaker meets the standard, let it stand and then remove the upper waste liquid (the upper waste liquid in this operation is a clear liquid), and then carry out the operation of circulating and draining the liquid.

[0035] The specific steps of the circulating drainage process include: after completing the soaking and stirring operation, observing the stratification of the suspension in the beaker after standing, extracting the clear upper layer of the stratified suspension and draining it into the waste liquid bucket, then adding distilled water to the beaker again, repeating the soaking and stirring operation, stirring and heating the clay sample in the beaker, then letting it stand for 3-10 minutes to allow stratification, extracting and draining the clear upper layer, and repeating this cycle 5-7 times. Observing the clay suspension and measuring the pH value of the suspension, by adding distilled water and draining the clear upper layer after 5-7 cycles, even if an excess of dilute hydrochloric acid solution is added and there is still residual dilute hydrochloric acid solution after the reaction, the concentration of residual dilute hydrochloric acid in the beaker can be ignored after 5-7 cycles, thus improving the accuracy of slide preparation while ensuring the suspension effect.

[0036] The specific steps of manual centrifugation include: after completing the circulation and drainage operation, let it stand for 2-8 hours, extract 40ml of the middle layer of the suspension from the middle layer of the standing suspension, transfer it to a centrifuge tube, and place it in batches on a centrifuge for centrifugation at a speed of ≥2000r / min. After centrifugation, pour out the waste liquid in the centrifuge tube. Centrifuging the sampled middle layer suspension can cause the clay particles in the suspension to settle, and then pouring out the waste liquid in the centrifuge tube can further reduce the residue of dilute hydrochloric acid.

[0037] The specific steps for clay extraction include: after emptying the waste liquid from several centrifuge tubes that have undergone manual centrifugation, placing the centrifuge tubes in batches into an ultrasonic device, adding 1-5 ml of distilled water to each centrifuge tube, starting the ultrasonic device to ultrasonically stir the mixture in the centrifuge tube, and then taking 0.7-1 ml of sample through a pipette, adding 1-5 ml of distilled water, and ultrasonically stirring, which is beneficial for subsequent sampling and ensures good homogeneity after ultrasonic stirring.

[0038] The specific steps for clay slide preparation include: sequentially extracting the processed clay samples from centrifuge tubes onto glass slides using a pipette, placing the glass slides on a heating stage, setting the temperature of the heating stage to 20-50℃, and simulating air drying.

[0039] In this application, during the sample preparation stage, the pulverized clay is first acid-washed with 3-10% dilute hydrochloric acid, which can effectively remove the carbonate components in the sample. After the reaction is completed, the sample preparation operation is completed. Then, by soaking and stirring, while adding distilled water and stirring, the beaker is heated, which can accelerate the suspension of clay particles. By heating and stirring simultaneously, the suspension time of existing clay particles is shortened. Furthermore, during the soaking and stirring process, the clay suspension was continuously observed. If the suspension effect was poor, dilute hydrochloric acid solution was added to react with the residual carbonates, thereby improving the suspension effect of the clay particles. Then, through the operation of circulating drainage, distilled water was repeatedly added, and heating and stirring were carried out to facilitate the suspension of clay particles. After each settling, the upper waste liquid was extracted to retain the suspended clay particles. With the repeated addition of distilled water, any dilute hydrochloric acid that may remain in the beaker was continuously diluted. After 5-7 cycles, the residual unreacted dilute hydrochloric acid solution in the beaker could be removed, maintaining the accuracy of the clay sample preparation.

[0040] In this application, after completing the circulation and drainage operation, the intermediate suspension located in the middle layer is extracted by allowing it to stand. This can improve the accuracy of clay preparation, avoid the possibility that trace amounts of dilute hydrochloric acid may still remain in the upper liquid, and also avoid the extraction of large-diameter clay particles located at the bottom. On this basis, the extracted intermediate suspension is centrifuged to allow the clay particles to settle, and then the clear liquid at the top is poured off, which can further reduce the influence of the solution medium on the clay sample.

[0041] In the clay extraction and slide preparation steps, 1-5 ml of distilled water is added again and ultrasonically stirred to increase the fluidity of the clay, making sampling easier. Ultrasonic stirring also ensures good uniformity of the sampled clay. Furthermore, during slide preparation, direct heating on the glass slide is used to simulate air drying, which is beneficial for subsequent operations such as making high-temperature slides, avoiding contact between hands and samples, and improving the accuracy of subsequent analysis.

[0042] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A high-throughput X-ray diffraction automated pretreatment device, characterized in that: include: Machine tool; The three-axis robotic arm moves within the machine via a gantry transmission module and is equipped with grippers for lifting and placing beakers or centrifuge tubes to the corresponding positions. The liquid addition module is mounted on a three-axis robotic arm and has at least three independent liquid addition components. The independent liquid addition components are used to add three liquid media into beakers or centrifuge tubes respectively. The liquid media include tap water, distilled water and dilute hydrochloric acid. The heating and stirring module is equipped with several stirring stations and ultrasonic stations for placing beakers or centrifuge tubes, and is used to heat and stir clay samples and liquid media by mechanical or ultrasonic means. The heating and stirring module includes an upper seat and a lower seat. The upper seat is equipped with a heating module and a plurality of cup-holding areas for accommodating beakers. The lower seat is equipped with a plurality of electromagnetic stirring modules corresponding one-to-one with the cup-holding areas, which are used to synchronously or asynchronously heat and stir the beakers containing clay samples. The machine is equipped with a temporary storage rack located on one side of the heating and stirring module. The temporary storage rack is used to place beakers or centrifuge tubes. A suction head circulation cleaning tank is provided on one side of the temporary storage rack. The heating and stirring module also includes an ultrasonic module installed on the machine. The ultrasonic module includes a housing. The top surface of the housing is recessed to form an ultrasonic station for placing several centrifuge tubes. An ultrasonic generator is installed inside the housing close to the ultrasonic station. A test tube rack is detachably connected to the housing. The liquid extraction module, mounted on a three-axis robotic arm, is used to extract and discharge the supernatant liquid in a beaker after it has been left to stand. The quantitative loop transfer module, mounted on a three-axis robotic arm, is used to aspirate the middle layer suspension in a beaker into a centrifuge tube and to extract the sample solution from the centrifuge tube after centrifugation into a glass slide. The glass slide heating module is equipped with a storage station for heating glass slides containing sample solutions located in the storage station; The cleaning and pouring module is installed on the machine platform and is used to spray and clean beakers or centrifuge tubes held by grippers. The process involves adding a specific amount of dilute hydrochloric acid to a beaker containing a clay sample via a liquid addition module, stirring and heating the sample in the beaker via a heating and stirring module, and repeating this process until the turbidity reaches the required level. Then, a quantitative loop transfer module is used to extract the intermediate suspension and inject it into a centrifuge tube. After centrifugation, the sample solution is transferred to a glass slide via a quantitative loop transfer module, and the slide is heated and prepared using a glass slide heating module.

2. The high-throughput X-ray diffraction automated pretreatment device according to claim 1, characterized in that: A sealing plate is fixedly connected inside the lower seat. The electromagnetic stirring module includes a stirring motor and a magnetic stirring head. The stirring motor is fixedly connected to the sealing plate through a fixing frame. A magnet holder is fixedly connected to the output end of the stirring motor. The eccentric position of the magnet holder forms several cavities for accommodating magnets, which are used by the stirring motor to drive several magnets to rotate in order to stir the mixture in the beaker.

3. The high-throughput X-ray diffraction automated pretreatment device according to claim 1, characterized in that: The cleaning and pouring module includes a beaker cleaning module and a centrifuge tube cleaning module. The machine platform is provided with a pouring area, and the pouring area is equipped with a filter assembly. The filter assembly is used to trap solid samples on the filter assembly.

4. The high-throughput X-ray diffraction automated pretreatment device according to claim 3, characterized in that: The filter assembly includes a waste liquid tank and a trapping filter. The machine is equipped with a horizontal linear sliding module. The displacement stroke of the horizontal linear sliding module covers the beaker cleaning module and the filter assembly. A tilting gripper assembly is connected to the horizontal linear sliding module through a vertical linear sliding module. The tilting gripper assembly is used to hold the beaker to the filter assembly for rotation and tilting, and then move to the beaker cleaning module for rotation and inversion. The inverted beaker is then sprayed and cleaned by the cleaning and tilting module.

5. The high-throughput X-ray diffraction automated pretreatment device according to claim 1, characterized in that: The temporary storage rack is provided with at least two placement positions for temporarily storing beakers or centrifuge tubes, which are used to temporarily store beakers or centrifuge tubes to be cleaned.

6. The high-throughput X-ray diffraction automated pretreatment device according to claim 1, characterized in that: The quantitative loop transfer module includes at least two peristaltic pumps, which are used to aspirate the middle layer suspension in the beaker and quantitatively transfer it to the centrifuge tube, and quantitatively aspirate the sample solution to the glass slide after centrifugation.

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