Pretreatment device and experimental instrument for analyzing pesticide components in soil

Abstract

The present invention belongs to the technical field of experimental instruments, and specifically relates to a pretreatment device and an experimental instrument for analyzing pesticide components in soil. The pretreatment device includes a container, a filter assembly is provided in the container, an inlet is provided above the filter assembly, and an outlet is provided below the filter assembly; the filter assembly includes at least one filter plate, a filter hole is provided on the filter plate, a mounting hole is provided at the center of the filter plate, a soft layer is installed in the mounting hole, a mixing device is provided at the soft layer, and a power device for driving the mixing device is provided in the container. The experimental instrument includes a pretreatment device and an analysis device. The present invention is a device for automatically processing soil samples. It does not require sample transfer, does not cause sample loss, is environmentally friendly, does not require multiple replacements of extraction instruments, and saves manual operation.

Description

Technical Field

[0001] The invention belongs to the technical field of experimental instruments, and in particular relates to a pre-treatment device and an experimental instrument for analyzing pesticide components in soil. Background Art

[0002] Crop growth requires the application of pesticides, and the amount of pesticide residues may affect the soil environment or the atmospheric environment. Excessive pesticide residues may also affect the growth of the next crop. Therefore, it is particularly necessary to detect and analyze the content of pesticide components in the soil and determine the soil pesticide residue situation. In the existing technology, the analysis of soil pesticides includes two major steps: soil sample pretreatment and on-machine analysis. Among them, soil sample pretreatment refers to the use of extraction solvents to extract pesticide components in soil samples, and on-machine analysis refers to the use of instruments such as liquid chromatography or gas chromatography for analysis. References include "Shi Yuge, Wang Linlin, Li Yuan, et al. Discussion on pretreatment methods for the detection of 8 organochlorine pesticide residues such as 666 and DDT in soil [J]. Arid Environmental Monitoring, 2022(003):036", "Liu Xi, Shi Yuge, Li Yuan, et al. Determination of organochlorine pesticide residues in soil and sediments by rapid solvent extraction-gas chromatography / mass spectrometry [J]. Fujian Analysis and Testing, 2023, 32(3):37-42".

[0003] Instruments such as liquid chromatographs or gas chromatographs are precision analytical instruments. In addition to pesticides, soil samples also contain impurities such as sand, clay, microorganisms, and fertilizer molecules, all of which will affect and interfere with the test results. Therefore, soil sample pretreatment is an important part of determining the accuracy of soil pesticide residue analysis results.

[0004] In existing technology, operators use extraction instruments such as beakers and funnels to extract pesticides from soil. The extracted material is transferred to a sample bottle, and then analyzed for specific components using instruments such as liquid chromatography or gas chromatography. This extraction process sometimes requires multiple steps and sample transfers, resulting in sample loss and hindering the detection of trace pesticides. Furthermore, these extraction instruments require manual mixing, resulting in low extraction efficiency. Summary of the Invention

[0005] In order to solve the above-mentioned technical problems of "sample loss and low extraction rate", the present invention provides a pretreatment device and experimental instrument for analyzing pesticide components in soil. The pretreatment device is an automated process for processing soil samples, which does not require sample transfer and does not cause sample loss. It is environmentally friendly and does not require multiple replacements of extraction instruments, saving manual operations. The experimental instrument includes a pretreatment device and an analysis device to analyze pesticide components.

[0006] The object of the present invention is to provide a pretreatment device for analyzing pesticide components in soil, comprising a container, a filter assembly disposed in the container, a sample inlet disposed above the filter assembly, and a sample outlet disposed below the filter assembly;

[0007] The filter assembly includes at least one filter plate having a filter hole formed therein. A mounting hole is formed at the center of the filter plate. A soft layer is mounted within the mounting hole. A mixing device is mounted within the soft layer. The mixing device is an elastic member that can move up and down and left and right. A power device for driving the mixing device is located within the container. The mixing device is used to mix the material and accelerate the dissolution of the pesticide component in the extraction reagent.

[0008] Preferably, the number of filter plates is a positive integer ≥ 2, and they are distributed from top to bottom within the container, with the diameters of the filter holes on the filter plates decreasing sequentially from top to bottom. Mixing devices are provided between adjacent soft layers and between the soft layers and the top inner wall of the container, and the power device is provided on the top inner wall of the container. The greater the number of filter plates, the better the filtration effect.

[0009] Preferably, the elastic member is a spring that can move up, down, left, and right.

[0010] Preferably, the elastic member is a zigzag structure formed by connecting a plurality of elastic rods end to end.

[0011] Preferably, in order to enhance the mixing and extraction effect, the mixing device is zigzag-shaped with an asymmetric width.

[0012] Preferably, the mounting hole is set to be circular with a diameter of 3cm to 5cm, or the mounting hole is set to be rectangular or square with a size of 3cm to 5cm in length and 3cm to 5cm in width.

[0013] Preferably, the power device is a rotary motor, a telescopic motor or a vibration motor.

[0014] The present invention also provides an experimental instrument for analyzing pesticide components in soil, comprising the pretreatment device described in any one of the above items, and an analysis device for detecting pesticide components, wherein the analysis device comprises a sample loading port, and the sample outlet of the pretreatment device is connected to the sample loading port.

[0015] Preferably, the sample outlet is connected to one end of a delivery tube, the other end of the delivery tube is connected to a sample loading port of an analysis device, and a peristaltic pump is provided on the delivery tube.

[0016] Preferably, the analysis device is a liquid chromatograph, a gas chromatograph, a mass spectrometer, a gas chromatography-mass spectrometer or a thin layer chromatograph.

[0017] Compared with the prior art, the present invention has the following beneficial effects:

[0018] In the present invention, the mixing device is an elastic member that can move up and down, left and right, and can drive the soft layer to move up and down, left and right. Only a single power device is needed to drive the topmost mixing device, which can then drive all other mixing devices and the soft layer to form a mixed whole. A soil sample and extraction reagent are added to the container through the sampling port. First, the soil sample is located above the topmost filter plate. The pesticide in the soil sample dissolves in the extraction reagent, and impurities of different particle sizes are gradually filtered from top to bottom. The power device controls the movement of the mixing device to achieve mixing. Finally, the sample discharged from the sampling port enters the analysis device for analysis of the pesticide composition.

[0019] In the present invention, the materials above and below the filter plate are not mixed and are filtered in an orderly manner. A solid treatment agent such as a color remover is arranged above the filter plate to reduce impurities in the liquid discharged from the sample outlet, thereby reducing the interference of these impurities on the final analysis results.

[0020] The pretreatment device of the present invention automates the process of processing soil samples, does not need to transfer samples, does not cause sample loss, is environmentally friendly, does not require multiple replacements of extraction instruments, and saves manual operations. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 This is a structural perspective view of the pre-treatment device for analyzing pesticide components in soil according to the present invention.

[0022] Figure 2 This is a longitudinal cross-sectional view of the experimental instrument for analyzing pesticide components in soil according to the present invention.

[0023] Figure 3 This is a diagram showing the usage status of the pretreatment device for analyzing pesticide components in soil according to the present invention. DETAILED DESCRIPTION

[0024] In order to enable those skilled in the art to better understand and implement the technical solution of the present invention, the present invention is further described below with reference to specific embodiments and drawings.

[0025] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like to indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.

[0026] The terms "first" and "second" are used for descriptive purposes only and should not be understood to indicate or imply relative importance or implicitly specify the number of the technical features indicated. Therefore, features specified as "first" or "second" may explicitly or implicitly include one or more of such features; and in the description of the present invention, unless otherwise specified, "plurality" means two or more.

[0027] Beakers and funnels are common containers for extraction and separation operations, and are also common containers for extracting pesticide components from soil samples. The general procedure is to place the soil sample in a beaker, add the extraction reagent, manually mix it with a glass rod, and then filter it through a funnel placed with filter paper to collect the filtrate. Although most solid impurities are filtered out at this time, colored substances or small-sized solid particles may still exist in the filtrate. These colored substances may also interfere with the extraction results, so sometimes a secondary filtration or color removal operation is required before the sample is collected in a sample bottle and analyzed using liquid chromatography or other detection instruments. The above process requires multiple sample transfers, resulting in sample loss and waste, and is not environmentally friendly. The multiple replacement of extraction instruments and manual operation methods are also time-consuming and labor-intensive, and the degree of automation is low.

[0028] Based on the above reasons, the present invention provides an experimental instrument for analyzing pesticide components in soil to solve the problems that "the extraction operation of beakers and funnels sometimes needs to be carried out multiple times and samples need to be transferred, resulting in sample loss, which is not conducive to the detection of trace pesticides, and these extraction instruments require manual mixing and low extraction efficiency."

[0029] The invention of the present invention is as follows: The experimental instrument for analyzing the pesticide components in soil includes two parts: a pre-treatment device and an analysis device 8. The analysis device 8 is an instrument capable of detecting compound components such as a liquid chromatograph, a gas chromatograph, a mass spectrometer, a gas chromatograph-mass spectrometer, or a thin-layer chromatography instrument in the prior art. The structure of the pre-treatment device is shown in FIG. Figures 1 to 3, including a container 1, which is hollow and used to hold soil samples and extraction reagents; a filter assembly is provided in the container 1, and the filter assembly is a filter plate 2. When the number of filter plates 2 is ≥2, these filter plates 2 are distributed from top to bottom, and the spacing between them can be equal or unequal. According to the order from top to bottom, the diameters of the filter holes 21 on the filter plates 2 decrease successively; a mounting hole is provided at the center of the filter plate 2, and a soft layer 3 is installed in the mounting hole. The soft layer 3 can be prepared from a material with a filtering effect or a material without a filtering effect; a mixing device 4 is provided between the two upper and lower adjacent soft layers 3, and a mixing device 4 is also provided between the soft layer 3 and the top wall of the container 1. The mixing device 4 is an elastic member that can move up and down and left and right. A power device 5 for driving the mixing device 4 is provided in the container 1; the container 1 is provided with an inlet 11 above the uppermost filter plate 2, and the container 1 is provided with an outlet 12 below the lowermost filter plate 2. The soil sample and the extraction reagent are added to the container 1 from the inlet 11, first located above the uppermost filter plate 2, and then gradually fall. The pesticide in the soil sample is dissolved in the extraction reagent, and impurities of different particle sizes are gradually filtered out from top to bottom. The power device 5 is used to control the movement of the mixing device 4 to play a mixing role. Finally, the sample discharged from the outlet 12 enters the analysis device 8 to analyze the pesticide components.

[0030] The present invention includes the following embodiments.

[0031] Example 1

[0032] An experimental instrument for analyzing pesticide components in soil includes a pretreatment device and an analysis device 8. The analysis device 8 is a liquid chromatograph, gas chromatograph, mass spectrometer, gas chromatography-mass spectrometry (GC-MS) or thin-layer chromatography instrument in the prior art, which is used to detect compound components. These existing analysis devices 8 all have a sample loading port, and the pretreatment device is connected to the sample loading port.

[0033] The structure of the pre-processing device is shown in Figure 1 , comprising a container 1, a filter plate 2, a soft layer 3, a mixing device 4, and a power device 5. Container 1 is hollow and is used to accommodate a soil sample and an extraction reagent. Preferably, container 1 is made of a transparent material to facilitate observation of the mixing of the soil sample and the extraction reagent. Container 1 is cylindrical or cubic in shape, with a horizontal bottom surface, making it convenient to place on a laboratory bench. Preferably, a shelf is provided at the bottom of container 1 for placing container 1 to facilitate sampling from the sample outlet 12 of container 1.

[0034] Continue to refer to Figure 1A filter assembly is provided in the container 1, and the filter assembly includes multiple layers of filter plates 2, such as 2 to 3 layers of filter plates 2. The filter plates 2 are provided with filter holes 21, and these filter plates 2 all have a filtering function. These layers of filter plates 2 are distributed from top to bottom in the container 1, and the spacing between adjacent filter plates 2 may be equal or unequal. Measured in order from top to bottom, the diameters of the filter holes 21 on these filter plates 2 decrease successively, and the diameters of the filter holes 21 on the same filter plate 2 are equal. There is no strict limit on the thickness of the filter plate 2, and those skilled in the art can set it according to their needs, such as setting the thickness of the filter plate 2 to 0.5 cm to 2 cm.

[0035] A mounting hole is provided at the center of the filter plate 2. The mounting hole is circular with a diameter of 3cm to 5cm, or rectangular or square with a length of 3cm to 5cm and a width of 3cm to 5cm. A soft layer 3 is installed in the mounting hole. The soft layer 3 is made of a soft material, such as a non-woven fabric or a filter mesh. These soft materials are flexible and can deform and move with the movement of the mixing device 4. These soft materials also have a filtering effect and can filter impurities. It should be noted that if the soft layer 3 is configured as a filter mesh, the filter mesh's pore diameter should be the same as the diameter of the filter hole 21 on the filter plate 2 where it is located to ensure the same filtration level.

[0036] A mixing device 4 is provided between each pair of adjacent soft layers 3, and between each soft layer 3 and the inner top wall of the container 1. The mixing device 4 is an elastic member that can move up and down, left and right. For example, the mixing device 4 can be a spring that can move up and down, left and right, or it can be a zigzag structure formed by multiple elastic rods connected end to end. The function of the mixing device 4 is to mix the materials and accelerate the dissolution of the pesticide components in the extraction reagent. For example, organophosphorus pesticide residues such as triazophos, methamidophos, and parathion are extracted using acetone or an acetone-containing extraction solution; benzyl ammonium chloride residues are extracted using ethyl acetate.

[0037] In order to enhance the mixing and extraction effect, the mixing device 4 is a zigzag shape with asymmetric width, see Figures 1 and 2 , that is, the lengths of the zigzag endpoints protruding to the left and right are unequal and irregular. When mixing, the irregular shape of the mixing device 4 contacts materials at different sites, that is, it can mix materials at different sites. When the shape of the mixing device 4 is irregular, the disturbance it produces on the materials is also irregular, reducing the generation of vortices. Since the position of the vortex will cause a large amount of air to be brought in, affecting the mixing of pesticide molecules in the liquid with the extraction reagent, the present invention adopts an irregular mixing device 4 structure to reduce the generation of vortices, accelerate the extraction of pesticide components, and improve extraction efficiency.

[0038] Because the soft layer 3 is movable, when the mixing device 4 moves, it drives the soft layer 3 up, down, left, and right. Only one power device 5 is needed to drive the topmost mixing device 4, which in turn drives all other mixing devices 4 and the soft layer 3 to form a mixed whole. To prevent the materials above and below the filter plate 2 from mixing and filtering in an orderly manner, a solid treatment agent such as a color remover is placed above the filter plate 2 to reduce impurities in the liquid discharged from the sample outlet 12, thereby reducing the interference of these impurities on the final analysis results.

[0039] A power unit 5 is provided within the container 1 for driving the mixing device 4. The power unit 5 can be a rotary motor, a telescopic motor, or a vibrating motor. For example, the power unit 5 includes a mounting portion and a power output portion. The mounting portion is mounted on the top wall of the container 1. The power output portion is connected to the top of the uppermost mixing device 4, and the bottom of the mixing device 4 is connected to the adjacent soft layer below it. Because the present invention provides a flexible mixing device 4 and a soft soft layer 3, the power unit 5 can produce a mixing effect as long as it can drive the mixing device 4.

[0040] The container 1 is provided with an inlet 11 above the uppermost filter plate 2, and a sample outlet 12 below the lowermost filter plate 2. The soil sample and the extraction reagent are added to the container 1 from the inlet 11, first located above the uppermost filter plate 2, and then continue to flow downward. During the flow, the pesticide in the soil sample dissolves in the extraction reagent, and impurities of different particle sizes are gradually filtered out from top to bottom. The power device 5 is used to control the activity of the mixing device 4 to play a mixing role. Finally, the sample discharged from the sample outlet 12 enters the analysis device 8 to analyze the pesticide components.

[0041] In order to facilitate the connection between the pretreatment device and the analysis device 8, one end of the delivery tube 6 is connected to the sample outlet 12, and the other end of the delivery tube 6 is connected to the sample loading port of the analysis device 8. A peristaltic pump 7 is provided on the delivery tube 6, and the peristaltic pump 7 is used to drive the sample injection.

[0042] It should be noted that the component connection relationships not specifically mentioned in the present invention are all assumed to adopt the existing technology. Since they do not involve the invention point and are widely used in the existing technology, the structural connection relationships are not described in detail.

[0043] It should be noted that when numerical ranges are mentioned in the present invention, it should be understood that both endpoints of each numerical range and any value between the two endpoints may be selected. Since the steps and methods used are the same as those in the embodiments, the present invention describes preferred embodiments to avoid redundancy. Although preferred embodiments of the present invention have been described, those skilled in the art may make additional changes and modifications to these embodiments once they understand the basic inventive concepts, and such changes and modifications fall within the scope of the present invention.

[0044] Obviously, those skilled in the art can make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. If these modifications and variations of the present invention fall within the scope of the equivalent technology of the present invention, the present invention is also intended to include these modifications and variations.

Claims

1. A pre-treatment device for analyzing pesticide components in soil, characterized in that: The invention comprises a container (1), wherein a filter assembly is provided in the container (1), a sample inlet (11) is provided on the upper side of the filter assembly, and a sample outlet (12) is provided on the lower side of the filter assembly; The filter assembly comprises at least one filter plate (2), the filter plate (2) being provided with a filter hole (21), a mounting hole being provided at the center of the filter plate (2), a soft layer (3) being installed in the mounting hole, a mixing device (4) being provided at the soft layer (3), the mixing device (4) being an elastic member capable of moving up and down and left and right, and a power device (5) for driving the mixing device (4) to move is provided in the container (1); The elastic member is a zigzag structure formed by connecting a plurality of elastic rods end to end; The mixing device (4) is zigzag-shaped with an asymmetric width; The number of the filter plates (2) is a positive integer ≥ 2, and they are distributed from top to bottom in the container (1), and the diameters of the filter holes (21) on the filter plates (2) decrease in order from top to bottom; The mixing device (4) is provided between adjacent soft layers (3) and between the soft layer (3) and the top inner wall of the container (1), and the power device (5) is provided at the top inner wall of the container (1).

2. The pretreatment device for analyzing pesticide components in soil according to claim 1, characterized in that: The mounting hole is circular with a diameter of 3cm~5cm; or the mounting hole is set to be rectangular with a size of 3cm~5cm in length and 3cm~5cm in width.

3. The pre-treatment device for analyzing pesticide components in soil according to claim 1, characterized in that: The power device (5) is a rotating motor, a telescopic motor or a vibrating motor.

4. An experimental instrument for analyzing pesticide components in soil, characterized in that: The method comprises the pretreatment device according to any one of claims 1 to 3, and further comprises an analysis device (8) for detecting pesticide components, wherein the analysis device (8) comprises a sample loading port, and a sample outlet (12) of the pretreatment device is connected to the sample loading port.

5. The experimental instrument for analyzing pesticide components in soil according to claim 4, characterized in that: The sample outlet (12) is connected to one end of a delivery tube (6), the other end of the delivery tube (6) is connected to a sample loading port of the analysis device (8), and a peristaltic pump (7) is provided on the delivery tube (6).

6. The experimental instrument for analyzing pesticide components in soil according to claim 5, characterized in that: The analysis device (8) is a liquid chromatograph, a gas chromatograph, a mass spectrometer, a gas chromatography-mass spectrometry (GC-MS) or a thin layer chromatograph.

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