Heavy metal element spectrum determination auxiliary device

Abstract

The invention relates to the technical field of spectral analysis assistance, in particular to a heavy metal element spectral measurement assisting device which comprises a preparation cylinder, a solvent groove and a sample groove are formed in the two sides of the top of the preparation cylinder respectively, a partition plate is fixedly connected into the preparation cylinder, a driving assembly is arranged at the top of the preparation cylinder, and the driving assembly is in signal connection with a control system; a stirring assembly is fixedly connected to the bottom of the driving assembly, a temperature control assembly is further arranged in the mixing cavity, siphons are symmetrically and fixedly connected to the side wall of the mixing cavity, and one end of each siphon extends to the bottom face of the mixing cavity while the other end extends into the filtering cavity; according to the present invention, by designing the intelligent control of the temperature of the mixing environment and the solvent feeding amount, and by using the siphon principle to control the amount of the sample dissolving liquid, the accurate concentration of the sample before the determination is ensured, and the accuracy of the subsequent heavy metal element spectrum determination of the sample is improved; and an accurate and efficient measurement process is realized.

Description

Technical Field

[0001] The present invention relates to the technical field of spectral analysis assistance, and particularly to an auxiliary device for spectral determination of heavy metal elements. Background Art

[0002] The spectral determination of heavy metal elements plays a crucial role in multiple key fields, such as environmental pollution monitoring, food safety assurance, and chemical engineering. However, these elements often exist in diverse chemical forms in samples, covering various forms such as organic matter-bound states and inorganic salts. To accurately determine these elements, a prerequisite is to effectively release them from the complex sample matrix and convert them into a form suitable for spectral analysis. This process, namely the pretreatment of samples, aims to break the organic structure in the samples, promote the conversion of heavy metal elements into inorganic forms, and minimize or eliminate other components that may interfere with spectral determination.

[0003] Current sample pretreatment technologies have significant shortcomings in precisely controlling the treatment environment, which is mainly reflected in the rough management of multiple key links such as environmental temperature, solvent dosage, and collection of the mixed solution. This lack of control precision may not only weaken the pretreatment effect, resulting in insufficient release or improper conversion of heavy metal elements into the ideal analytical form, but also introduce additional interfering factors, directly disturbing the accuracy of subsequent spectral determination.

[0004] Therefore, it is necessary to propose an auxiliary device that can combine existing heavy metal element sample pretreatment technologies to precisely control key parameters of the treatment environment, ensuring that heavy metal elements can be efficiently and accurately released from the complex sample matrix and converted into an ideal form suitable for spectral analysis. Summary of the Invention

[0005] To solve the above problems, the present invention provides an auxiliary device for spectral determination of heavy metal elements. By designing to intelligently control the temperature and solvent dosage of the mixing environment and using the siphon principle to control the amount of sample dissolution solution, the accuracy of the sample concentration before determination is ensured, the accuracy of subsequent spectral determination of heavy metal elements in the sample is improved, and an accurate and efficient determination process is achieved.

[0006] To achieve the above object, the technical solution of the present invention is as follows: An auxiliary device for spectral determination of heavy metal elements, including a preparation cylinder body. On both sides of the top of the preparation cylinder body, a solvent tank and a sample tank are respectively provided. A partition is fixedly connected inside the preparation cylinder body, and the partition divides the interior of the preparation cylinder body from top to bottom into a mixing chamber and a filtering chamber. Both the solvent tank and the sample tank are communicated with the mixing chamber. A driving component for providing rotational drive is provided at the top of the preparation cylinder body, and the driving component is signal-connected to a control system for intelligently controlling the preparation environment; The bottom of the driving component is fixedly connected with a stirring component for converting rotation into a stirring action. A temperature control component for regulating the stirring and mixing temperature is also arranged in the mixing cavity. The temperature control component is signal-connected to the control system. The side walls of the mixing cavity are symmetrically and fixedly connected with siphons. One end of each siphon extends to the bottom surface of the mixing cavity, and the other end of each siphon penetrates through the side wall of the preparation cylinder and extends into the filtering cavity. A filtering component for filtering the stirred sample is arranged in the filtering cavity, and a liquid outlet is opened at the bottom of the filtering cavity.

[0007] The technical principle of the above solution is as follows: By designing the preparation cylinder as the main part of the whole device, the mixing and filtering of the sample can be continuously completed in one device; Through the design of the solvent tank and the sample tank, they are respectively used for putting the eutectic solvent and the sample to be measured. By designing the siphon and using the siphon principle, when the liquid in the mixing cavity reaches a certain height, the liquid will automatically flow into the filtering cavity, so as to control the amount of the mixed liquid. By signal-connecting the intelligent system, the control of environmental temperature, solvent dosage, and mixing time parameters can be realized.

[0008] The following beneficial effects can be obtained by adopting the above solution: 1. In this solution, through the designed cylinder structure with an internal mixing cavity and a filtering cavity, the efficient and sufficient mixing of the sample and the solvent in the mixing cavity can be realized. Moreover, after the mixing is completed, the mixture can be finely filtered and separated through the filtering cavity, effectively removing insoluble impurities, providing a clear, pure and high-quality sample solution for the spectral determination step of heavy metal elements, reducing the measurement error caused by sample contamination or impurity interference, and improving the accuracy and sensitivity of subsequent spectral analysis.

[0009] 2. In this solution, the driving component and the intelligent control system are integrated, so that the environmental parameters in the mixing process of the sample can be controlled. Through the preset program, the system can automatically adjust the mixing time, mixing rate and stirring intensity parameters to ensure that each mixing can reach the ideal uniformity and stability. It not only improves the efficiency of sample processing, but also further ensures the consistency of sample quality by reducing the interference of human factors, laying a solid foundation for subsequent precise analysis.

[0010] 3. In this solution, the design of the siphon uses the siphon principle to realize the automatic control of the amount of the mixed liquid, which not only simplifies the operation process, but also fundamentally avoids the error that may occur during manual measurement, so as to ensure the accuracy of the sample amount in the subsequent spectral determination step.

[0011] Furthermore, pressure sensors are arranged on both the solvent tank and the sample tank, and electric control valves are arranged at the communication parts between the solvent tank and the sample tank and the mixing cavity. A number of electric control valves and pressure sensors are all signal-connected to the control system.

[0012] Beneficial effects: The pressure sensor can monitor the pressure changes in the solvent tank and the sample tank in real time and convert them into mass data. By setting a preset mass range, the control system can accurately judge whether the dosing amounts of the solvent and the sample meet the requirements. When the dosing amount reaches the preset range, the control system will send a signal to the corresponding electromagnetic valve to open it, allowing the solvent or the sample to enter the mixing chamber. This precise control of the dosing amount ensures the consistency of the experimental conditions each time, improving the accuracy and repeatability of the experiment.

[0013] Furthermore, the inner sidewall of the mixing chamber is designed as a vertical arc structure.

[0014] Beneficial effects: The arc-shaped wall surface can guide the fluid to generate vortices and turbulence, enhancing the mixing effect, which helps to ensure that the solvent and the sample are fully and evenly mixed in the mixing chamber, providing a high-quality sample solution for subsequent spectroscopic determination. In addition, compared with traditional right-angle or flat structures, the vertical arc structure can reduce the resistance of the fluid in the mixing chamber. When the fluid flows through the arc-shaped wall surface, its flow direction can transition more smoothly, reducing the fluid resistance caused by right-angle or sudden change structures and reducing the probability of the mixed liquid adhering to the wall.

[0015] Furthermore, the driving assembly includes a driving box fixedly connected to the top surface of the preparation cylinder. A servo motor is fixedly connected to the inner top wall of the driving box. The output shaft of the servo motor penetrates through the bottom wall of the driving box and the top wall of the preparation cylinder and extends into the mixing chamber. The stirring assembly includes a rotating cylinder coaxially and fixedly connected to the output shaft of the servo motor. A plurality of stirring blades integrally formed with the rotating cylinder are fixedly connected to the side wall of the rotating cylinder along its circumference.

[0016] Beneficial effects: The servo motor has the characteristics of high precision and high torque output, which can ensure that the rotating cylinder and the stirring blades rotate at a stable speed and force. Through the signal transmission drive of the control system, it can achieve precise and stable rotational power output, realizing an accurate mixing process, ensuring that the solvent and the sample can be fully mixed in the mixing chamber, and improving the mixing uniformity and efficiency.

[0017] Furthermore, the temperature control assembly includes a plurality of electric heating plates located in the mixing chamber. The electric heating plates are fixedly connected to the inner sidewall of the preparation cylinder. The electric heating plates are all signal-connected to the control system. A temperature sensor fixedly connected to the inner top wall of the preparation cylinder is also provided in the mixing chamber. The temperature sensor is signal-connected to the control system.

[0018] Beneficial effects: The combined use of the electric heating plates and the temperature sensor enables the control system to monitor the temperature in the mixing chamber in real time and automatically adjust it according to the preset temperature range, ensuring the temperature stability during the mixing process and avoiding problems such as uneven mixing or sample deterioration caused by temperature changes.

[0019] Furthermore, the filtering component includes a filter membrane, which is located below the partition plate and is detachably connected to the inner wall of the preparation cylinder through a buckle.

[0020] Beneficial effects: As the core component of the filtering component, the filter membrane can effectively intercept insoluble substances such as solid particles and impurities in the mixed liquid, ensuring that the filtered sample solution is clear and transparent, and providing high-quality samples for subsequent spectral determination.

[0021] Furthermore, the filtering cavity is a conical structure with the cone tip facing downwards, and a spiral groove is provided on the side wall of the filtering cavity, and the spiral groove is opened on the inner side wall of the preparation cylinder.

[0022] Beneficial effects: The conical filtering cavity can utilize the design with the cone tip facing downwards to guide the mixed liquid to flow down naturally along the conical surface and smoothly enter the spiral groove; the design of the spiral groove not only increases the contact area between the mixed liquid and the filter membrane, but also promotes the uniform distribution of the mixed liquid, thereby improving the filtering efficiency and replacing the operation of shaking evenly.

[0023] Furthermore, the solvent tank is used to put the deep eutectic solvent, and the deep eutectic solvent is a mixed solvent of maleic acid and choline chloride heated and stirred in a molar ratio of 1:1 - 1:2.

[0024] Beneficial effects: Due to its low melting point, the deep eutectic solvent can achieve good dissolution performance at a relatively low temperature. This makes the sample easier to be dissolved and dispersed during the mixing process, thereby improving the mixing uniformity and efficiency. As a dicarboxylic acid, maleic acid has two strongly polar carboxylic acid groups, and the carboxylic acid groups can form coordination bonds with metal ions or organic molecules containing oxygen or nitrogen, enhancing the dissolution ability for metal oxides or polar compounds, and can promote the hydrolysis of certain chemical bonds in the target sample in a weakly acidic environment with a pH of 2 - 3, improving the extraction efficiency; while choline chloride as a quaternary ammonium salt, the quaternary ammonium cation binds to negatively charged molecules through electrostatic interaction, destroying their aggregated structure and enhancing the dispersibility, and the hygroscopicity of choline chloride can reduce solvent volatilization and extend the service life. The combination of maleic acid and choline chloride can interact with certain components in the target sample, thereby enhancing the extraction ability for the sample, which is of great significance for improving the sensitivity and accuracy of spectral determination.

[0025] Furthermore, the solvent tank and the sample tank are both detachably connected with tank covers, and sealing rings are sleeved on the edges of the tank covers.

[0026] Beneficial effects: The design of the tank cover can effectively seal the solvent tank and the sample tank, preventing the solvent and the sample from volatilizing during mixing or storage, thereby ensuring the accuracy and stability of the experiment.

[0027] Furthermore, the control system includes a pressure acquisition and analysis module, a temperature acquisition and analysis module, and a driving module; The pressure acquisition and analysis module is used to acquire pressure data through pressure sensors respectively located on the solvent tank and the sample tank, convert the pressure data into mass data, and determine the masses placed in the solvent tank and the sample tank respectively. When the mass data of the eutectic solvent placed in the solvent tank is 1.42 - 1.50 g, a signal for driving the corresponding electromagnetic valve is sent to the driving module. When the mass data of the sample tank is 0.10 - 0.12 g, a signal for driving the corresponding electromagnetic valve is sent to the driving module; The temperature acquisition and analysis module is used to acquire the temperature data in the mixing chamber through a temperature sensor and determine the temperature data. When the temperature in the mixing chamber collected is lower than 68 °C, a signal for starting the heating plate is sent to the driving module. When the temperature in the mixing chamber collected is higher than 70 °C, a driving signal for stopping the heating plate is sent to the driving module; The driving module is used to receive the driving signals transmitted by each module, and transmit signals to several electromagnetic valves and the heating plate according to the driving signals. Then, when both side electromagnetic valves are opened, a signal is transmitted to the servo motor to make the servo motor rotate at a rotation rate of 600 rpm, and the rotation time is recorded. When the rotation time reaches 45 min, a stop signal is sent to the servo motor.

[0028] Advantageous effects: The pressure acquisition and analysis module can accurately acquire pressure data and convert it into mass data, ensuring that the mass of the eutectic solvent placed in the solvent tank is between 1.42 - 1.50 g, and the mass of the sample in the sample tank is between 0.10 - 0.12 g, thus improving the accuracy and repeatability of the experiment; The temperature acquisition and analysis module monitors the temperature in the mixing chamber in real time through the temperature sensor, ensuring the temperature stability during the mixing process and avoiding experimental errors caused by temperature changes; The automatic control mechanism also reduces the direct intervention of operators, further reducing the risk of experimental failure.

[0029] Furthermore, the folding inflection point of the siphon tube is located at the volume height of 5 mL in the mixing chamber.

[0030] Advantageous effects: Setting the folding inflection point of the siphon tube at the volume height of 5 mL in the mixing chamber can ensure that only the mixed liquid with this specific volume will be pumped out during the siphon process, helping to avoid the influence of excessive or insufficient volume of the mixed liquid on the experimental results and improving the accuracy and reliability of the experiment.

[0031] Additional aspects and advantages of the present invention will be given in part in the following description, become apparent in part from the following description, or be understood through the practice of the present invention. Description of the Drawings

[0032] Figure 1Schematic diagram of the overall structure of an embodiment of the auxiliary device for the spectroscopic determination of heavy metal elements of the present invention; Figure 2 Axonometric sectional view of an embodiment of the auxiliary device for the spectroscopic determination of heavy metal elements of the present invention; Figure 3 Schematic diagram of the connection of the siphon tube in an embodiment of the auxiliary device for the spectroscopic determination of heavy metal elements of the present invention; Figure 4 For an embodiment of the auxiliary device for the spectroscopic determination of heavy metal elements of the present invention Figure 2 Enlarged schematic diagram of part A with respect to the sample tank or solvent tank in the present invention.

[0033] Reference numerals in the accompanying drawings of the specification include: 1, preparation cylinder; 101, mixing chamber; 102, filtration chamber; 2, solvent tank; 3, sample tank; 4, partition board; 5, siphon tube; 6, liquid outlet; 7, pressure sensor; 8, electric control valve; 9, driving box body; 10, servo motor; 11, rotating cylinder; 12, stirring blade; 13, electric heating plate; 14, temperature sensor; 15, filter membrane; 16, spiral groove; 17, groove cover. Detailed implementation manners

[0034] Next, the technical solutions of the present invention will be clearly and completely described in conjunction with the accompanying drawings. Obviously, the described embodiments are part of the embodiments of the present invention, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0035] In the description of the present invention, it should be noted that the orientation or positional relationship indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. is based on the orientation or positional relationship shown in the accompanying drawings. It is 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 construed as a limitation of the present invention. In addition, the terms "first", "second", "third" are only used for descriptive purposes and cannot be construed as indicating or implying relative importance.

[0036] In the description of the present invention, it should be noted that unless otherwise clearly specified and limited, the terms "installed", "connected", "connected" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, and it can be the internal communication of two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific situations.

[0037] The following is a further detailed description through specific embodiments: Example 1: As shown in the Figure 1 , Figure 2 , Figure 3 and Figure 4 figures: An auxiliary device for spectral determination of heavy metal elements, including a preparation cylinder body 1. A partition plate 4 is welded inside the preparation cylinder body 1. The partition plate 4 divides the inside of the preparation cylinder body 1 into a mixing chamber 101 and a filtering chamber 102 from top to bottom. Solvent tanks 2 and sample tanks 3 communicating with the mixing chamber 101 are respectively arranged on both sides of the top of the preparation cylinder body 1. The solvent tank 2 is used for putting eutectic solvents. The eutectic solvent is a mixed solvent obtained by heating and stirring maleic acid (hydrogen bond donor, HBD) and choline chloride (hydrogen bond acceptor, HBA) in a molar ratio of 1:1 - 1:2. For the design of 1:1 molar ratio, the hydrogen bond donor and acceptor are strictly matched to form a dense hydrogen bond network, which can reduce the melting point to the lowest, but the synthesized eutectic solvent has a higher viscosity and is suitable for static extraction. As the proportion of choline chloride increases, the excessive choline chloride provides more hydrogen bond acceptors, reduces the viscosity of the system, and improves the fluidity, making it suitable for dynamic mixing or microfluidic systems.

[0038] Experiment 1: Verify the influence of different molar ratios on the extraction efficiency of the eutectic solvent after mixing Experimental steps: 1. Heat and mix maleic acid and choline chloride in molar ratios of 1:1, 1:1.5, and 1:2 to form eutectic solvents.

[0039] 2. Measure the extraction rate of polyphenols and the solubility of lipids of eutectic solvents with different molar ratios respectively.

[0040] Experimental data: Table 1: Eutectic solvents with different molar ratios Experimental conclusion: By expanding the molar ratio of maleic acid to choline chloride to the range of 1:1 to 1:2, the eutectic solvent not only maintains the advantage of low melting point but also realizes the efficient dissolution and selective extraction of diverse target components. This design not only improves the mixing uniformity and spectral detection accuracy but also can adapt to different application scenarios (such as static extraction or dynamic mixing) by adjusting the molar ratio, significantly enhancing the flexibility and economy of the system.

[0041] In addition, since the carboxylic acid group HBD has a better extraction effect on heavy metal cations in bamboo leaf litter than the alcohol group HBD, maleic acid is selected as the HBD raw material for the eutectic solvent.

[0042] Regarding the design of the molar ratio of HBD to HBA, when the molar ratio of HBD increases, the solid components of the eutectic solution form a liquid eutectic at a higher temperature, resulting in the inability of the eutectic solution to form a stable homogeneous liquid at 80 °C. Therefore, a molar ratio of 1:1 is selected as the optimal ratio for extracting heavy metal elements from samples using the eutectic solution.

[0043] On the top surface of the preparation cylinder body 1, a driving box body 9 is welded. On the inner top wall of the driving box body 9, a servo motor 10 is fixedly connected by screws. The servo motor 10 is signal-connected to a control system for intelligently regulating the preparation environment. The output shaft of the servo motor 10 passes through the bottom wall of the driving box body 9 and the top wall of the preparation cylinder body 1 and extends into the mixing cavity 101. And the output shaft of the servo motor 10 is coaxially and fixedly connected with a rotating cylinder 11 through a coupling. Along the circumferential direction of the side wall of the rotating cylinder 11, a number of stirring blades 12 integrally formed with the rotating cylinder 11 are fixedly connected; the operator only needs to input the driving program into the control system, and then can send accurate driving signals to the servo motor 10 through the control system to ensure that the servo motor 10 can always maintain a constant stirring rate during the stirring and mixing process; the design of the constant control of the stirring rate can ensure that the materials in all parts of the mixing cavity 101 can be fully stirred and mixed. In addition, the control of this stirring rate can also effectively reduce the irregular movement of the liquid droplets in the mixing cavity 101, reduce the influence of factors such as gravity, shear force or turbulence on the liquid droplets, resulting in residual mixed liquid hanging on the inner wall of the mixing cavity 101, thereby affecting the uniformity of sample mixing and causing changes in the sample concentration of the final mixed sample, thus increasing the randomness of the spectral measurement results.

[0044] During the stirring and mixing process of the eutectic solvent and the sample to be measured, temperature control can ensure that the collision frequency and energy distribution between reactant molecules are in the best state, thereby accelerating the release and extraction process of the target analyte from the sample matrix; therefore, it is designed that a number of electric heating plates 13 fixedly connected to the inner side wall of the preparation cylinder body 1 through a snap mechanism are arranged in the mixing cavity 101. The electric heating plates 13 are all signal-connected to the control system, and a temperature sensor 14 fixedly connected to the inner top wall of the preparation cylinder body 1 by screws is also arranged in the mixing cavity 101. The temperature sensor 14 is signal-connected to the control system. Since the change in temperature may affect the interaction forces between the eutectic solvent and heavy metal elements, such as hydrogen bonds, ionic bonds, etc., precise temperature control is designed to optimize these interaction forces, thereby improving the selectivity of extraction.

[0045] Specifically, due to the relatively high viscosity ratio of the deep eutectic solvent, after heating and stirring the sample to be measured and the deep eutectic solvent, ultrapure water is added to reduce the viscosity of the system, promote the complete dissolution of the deep eutectic solvent, ensure that all reaction components can be evenly distributed, and avoid experimental errors caused by too high or too low local concentrations. Since the samples to be measured and the deep eutectic solvent are both added in fixed amounts, the amount of ultrapure water added is also added in a fixed amount; therefore, specifically as Figure 3 shown, siphon tubes 5 are symmetrically welded to the side wall of the mixing chamber 101. One end of each siphon tube 5 extends to the bottom surface of the mixing chamber 101, and the other end of each siphon tube 5 penetrates through the side wall of the preparation cylinder 1 and extends into the filtration chamber 102. The folding inflection point of the siphon tube 5 is located at the 5 mL volume height of the mixing chamber 101. When the liquid in the mixing chamber 101 reaches the 5 mL volume height where the folding inflection point of the siphon tube 5 is located, due to the siphon effect, the liquid will automatically rise along the siphon tube 5 and flow into the filtration chamber 102. This design uses the siphon principle to control the final mixing amount of ultrapure water, deep eutectic solvent, and the sample to be measured to ensure the accuracy of subsequent spectral measurements.

[0046] Experiment 2: Verify the automatic control function of the siphon tube 5 for the volume of the mixed liquid Experimental steps: 1. Inject liquids with different volumes (3 mL, 5 mL, 7 mL) into the mixing chamber 101, and observe whether the siphon tube 5 triggers liquid transfer only at 5 mL.

[0047] 2. Measure the volume of the liquid received by the filtration chamber 102.

[0048] Experimental data: Collect the liquid volume error when the siphon is triggered; Table 2: Verification of the siphon function Experimental conclusion: The siphon tube 5 is triggered only at 5 mL, with an error less than 2%, effectively controlling the liquid volume.

[0049] A filter membrane 15 is provided in the filtration chamber 102. The filter membrane 15 is located below the partition plate 4 and is detachably connected to the inner wall of the preparation cylinder 1 by a buckle. The main function of the filter membrane 15 is to intercept solid particles and impurities in the mixed liquid, allowing the clear filtrate to pass through, thereby ensuring the accuracy and sensitivity of subsequent spectral analysis.

[0050] The filtering chamber 102 is a conical structure with the cone tip facing downwards, and a spiral groove 16 is provided on the side wall of the filtering chamber 102. The spiral groove 16 is opened on the inner side wall of the preparation cylinder 1. An outlet 6 is opened at the bottom of the filtering chamber 102. When the filtrate flows downward along the side wall of the conical filtering chamber 102, it will be guided by the spiral groove 16 and slide along the path of the spiral groove 16. During this process, the filtrate continuously changes its flow direction in the spiral groove 16, achieving the effect of mixing and shaking the filtered sample to be measured. Finally, it flows out from the outlet 6 and is collected by the operator.

[0051] Experiment 3: Evaluate the mixing uniformity and the performance of the filtering component.

[0052] Experimental steps: 1. Use a fluorescent tracer to simulate heavy metal samples and stir at 600 rpm for 45 min.

[0053] 2. Take samples at different positions in the mixing chamber and detect the standard deviation of the fluorescence intensity.

[0054] 3. Add solid particles (50 mg / L) to the mixed solution, and detect the residual amount of the filtrate after filtration.

[0055] Experimental data: Table 3: Experimental conclusion: The mixing uniformity of this device is improved by 83% (the standard deviation drops from 18.6 to 3.2), and the residual particles in the filtrate are reduced to 0.8 mg / L, and the turbidity is close to the pure water level (1.2 NTU).

[0056] Example 2: As shown in the appendix Figure 2 The difference from Example 1 is that the dosing amount of the sample to be measured is 0.10 - 0.12 g, and the dosing amount of the deep eutectic solvent is 1.42 - 1.50 g. Since the excessive use of the deep eutectic solvent will cause the viscosity of the mixed liquid to decrease, while too little dosing of the deep eutectic solvent will result in too high viscosity, which will hinder the movement of the dissolved substances and affect the conductivity, mass transfer phenomenon and heat transfer rate of the deep eutectic solvent. Therefore, designing to limit the dosing amounts of the deep eutectic solvent and the sample to be measured can improve the efficiency of extraction pretreatment, thereby improving the accuracy of subsequent spectral determination.

[0057] The inner side wall of the mixing chamber 101 is designed as a vertical arc structure. During the mixing process, the design of the vertical arc structure reduces the contact area between the inner side wall of the mixing chamber 101 and the sample to be measured, and the contact surface is smoother. The sample to be measured flows along the arc wall surface under the action of the stirring blade 12. Compared with a right-angled or flat structure, this design can reduce the wall sticking and accumulation phenomena, which helps to ensure the mixing quality of the sample to be measured and the deep eutectic solvent, so as to further ensure the concentration of the mixed liquid, and thus ensure the accuracy and scientificity of subsequent spectral analysis.

[0058] Example 3: As shown in the attached Figure 4 figure, the difference from Example 2 is that during the process of heating, stirring and mixing, due to the increase in temperature, the solvent may volatilize, resulting in a change in the sample concentration. If too much solvent volatilizes, it may cause the sample to concentrate, resulting in an enhanced signal during spectral measurement, thus affecting the accuracy of the measurement results. For this reason, it is designed that the surface of the solvent tank 2 and the sample tank 3 can be detachably connected with a tank cover 17, and sealing rings are sleeved on the edges of the tank cover 17. Using this design can prevent the volatilization of the solvent, thereby reducing the impact of the heating and stirring process on subsequent spectral measurement.

[0059] Pressure sensors 7 fixedly connected to the preparation cylinder 1 by screws are provided on both the solvent tank 2 and the sample tank 3. Electric control valves 8 are provided at the communication parts between the solvent tank 2 and the sample tank 3 and the mixing chamber 101. A number of electric control valves 8 and pressure sensors 7 are all connected to the control system in signal. The mass of the sample to be measured and the eutectic solvent placed in the solvent tank 2 and the sample tank 3 is monitored by the pressure sensor 7, and the mass information is transmitted to the control system for monitoring, effectively avoiding the excess or deficiency of the solvent or the sample. Only when the mass threshold is reached, the electric control valve 8 is opened to realize the control of the dosing amount.

[0060] Experiment 4: Test the control accuracy of the pressure sensor 7 and the electric control valve 8 for the dosing amount of the solvent and the sample Experimental steps: 1. Put the eutectic solvent (1.42 - 1.50 g) and the sample (0.10 - 0.12 g) into the solvent tank 2 and the sample tank 3 respectively for 10 times.

[0061] 2. Record the actual dosing mass through the pressure sensor 7 and compare it with the set value.

[0062] Experimental data: Collect the deviation between the actual dosing mass of the solvent and the sample and the preset value.

[0063] Table 4: Dosing accuracy of the solvent and the sample (n = 10) Conclusion: The dosing error of the pressure sensor 7 and the electric control valve 8 is less than 1%, which is significantly better than manual operation.

[0064] Example 4: The difference from Example 3 is that the control system includes a pressure acquisition and analysis module, a temperature acquisition and analysis module, and a drive module.

[0065] The pressure acquisition and analysis module collects pressure data through pressure sensors 7 located on the solvent tank 2 and the sample tank 3 respectively, converts the pressure data into mass data, and determines the masses placed in the solvent tank 2 and the sample tank 3 respectively. When the mass data of the eutectic solvent placed in the solvent tank 2 is 1.42 - 1.50 g, a signal for driving the corresponding electromagnetic valve 8 is sent to the driving module. When the mass data of the sample tank 3 is 0.10 - 0.12 g, a signal for driving the corresponding electromagnetic valve 8 is sent to the driving module.

[0066] The temperature acquisition and analysis module collects the temperature data in the mixing chamber 101 through the temperature sensor 14 and determines the temperature data. When the temperature in the mixing chamber 101 collected is lower than 68 °C, a signal for starting the electric heating plate 13 is sent to the driving module. When the temperature in the mixing chamber 101 collected is higher than 70 °C, a driving signal for stopping the electric heating plate 13 is sent to the driving module.

[0067] The driving module receives the driving signals transmitted by each module, and transmits signals to several electromagnetic valves 8 and the electric heating plate 13 according to the driving signals. Then, when both the electromagnetic valves 8 on both sides are opened, a signal is transmitted to the servo motor 10 to make the servo motor 10 rotate at a rotation speed of 600 rpm, and the rotation time is recorded. When the rotation time reaches 45 min, a stop signal is sent to the servo motor 10.

[0068] Obviously, the above embodiments are only examples given for clear illustration and are not limitations on the implementation manners. For those of ordinary skill in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to list all the implementation manners here. The obvious changes or modifications derived therefrom still fall within the protection scope of the present invention.

Claims

1. An auxiliary device for spectral determination of heavy metal elements, comprising a preparation cylinder body (1), wherein solvent tanks (2) and sample tanks (3) are respectively arranged on both sides of the top of the preparation cylinder body (1), and a partition plate (4) is fixedly connected in the preparation cylinder body (1), and is characterized in that, The partition plate (4) divides the interior of the preparation cylinder body (1) from top to bottom into a mixing chamber (101) and a filtering chamber (102). The solvent tank (2) and the sample tank (3) are both communicated with the mixing chamber (101). A driving assembly for providing rotational drive is provided at the top of the preparation cylinder body (1), and the driving assembly is signal-connected to a control system for intelligently regulating the preparation environment; The bottom of the driving assembly is fixedly connected with a stirring assembly for converting rotation into a stirring action. A temperature control assembly for regulating the stirring and mixing temperature is also provided in the mixing chamber (101). The temperature control assembly is signal-connected to the control system. Siphon tubes (5) are symmetrically and fixedly connected to the side wall of the mixing chamber (101). One end of each siphon tube (5) extends to the bottom surface of the mixing chamber (101), and the other end of each siphon tube (5) penetrates through the side wall of the preparation cylinder body (1) and extends into the filtering chamber (102); A filtering assembly for filtering the stirred sample is provided in the filtering chamber (102), and a liquid outlet (6) is opened at the bottom of the filtering chamber (102).

2. The auxiliary device for spectrometric determination of heavy metal elements according to claim 1, wherein, Pressure sensors (7) are provided on both the solvent tank (2) and the sample tank (3). Electric control valves (8) are provided at the communication positions between the solvent tank (2) and the sample tank (3) and the mixing chamber (101). A plurality of electric control valves (8) and pressure sensors (7) are all signal-connected to the control system.

3. The auxiliary device for heavy metal element spectral determination according to claim 2, wherein, The inner side wall of the mixing chamber (101) is designed as a vertical arc structure.

4. The auxiliary device for determining the spectrum of heavy metal elements according to claim 3, characterized in that, The driving assembly includes a driving box body (9) fixedly connected to the top surface of the preparation cylinder body (1). A servo motor (10) is fixedly connected to the inner top wall of the driving box body (9). The output shaft of the servo motor (10) penetrates through the bottom wall of the driving box body (9) and the top wall of the preparation cylinder body (1) and extends into the mixing chamber (101). The stirring assembly includes a rotating cylinder (11) coaxially and fixedly connected to the output shaft of the servo motor (10). A plurality of stirring blades (12) integrally formed with the rotating cylinder (11) are fixedly connected to the side wall of the rotating cylinder (11) along its circumference.

5. The auxiliary device for spectral determination of heavy metal elements according to claim 4, characterized in that, The temperature control assembly includes a plurality of electric heating plates (13) located in the mixing chamber (101). The electric heating plates (13) are all fixedly connected to the inner side wall of the preparation cylinder body (1). The electric heating plates (13) are all signal-connected to the control system. A temperature sensor (14) fixedly connected to the inner top wall of the preparation cylinder body (1) is also provided in the mixing chamber (101). The temperature sensor (14) is signal-connected to the control system.

6. The auxiliary device for determining the spectrum of heavy metal elements according to claim 5, wherein, The filtering assembly includes a filter membrane (15). The filter membrane (15) is located below the partition plate (4) and is detachably connected to the inner wall of the preparation cylinder body (1) by a buckle.

7. The auxiliary device for spectrometric determination of heavy metal elements according to claim 6, characterized in that, The filtering chamber (102) is a conical structure with a pointed bottom, and a spiral groove (16) is provided on the side wall of the filtering chamber (102). The spiral groove (16) is opened on the inner side wall of the preparation cylinder body (1).

8. The auxiliary device for spectral determination of heavy metal elements according to claim 7, characterized in that, The solvent tank (2) is used for putting a eutectic solvent, and the eutectic solvent is a mixed solvent obtained by heating and stirring maleic acid and choline chloride in a molar ratio of 1:1 - 1:2; Lid (17) can be detachably connected to the surfaces of the solvent tank (2) and the sample tank (3), and sealing rings are sleeved on the edges of the lid (17).

9. The auxiliary device for spectral determination of heavy metal elements according to claim 8, wherein The control system includes a pressure acquisition and analysis module, a temperature acquisition and analysis module, and a driving module; The pressure acquisition and analysis module is used to acquire pressure data through pressure sensors (7) respectively located on the solvent tank (2) and the sample tank (3), convert the pressure data into mass data, and respectively determine the masses placed in the solvent tank (2) and the sample tank (3). When the mass data of the eutectic solvent placed in the solvent tank (2) is 1.42 - 1.50 g, a signal for driving the corresponding electromagnetic valve (8) is sent to the driving module. When the mass data of the sample tank (3) is 0.10 - 0.12 g, a signal for driving the corresponding electromagnetic valve (8) is sent to the driving module; The temperature acquisition and analysis module is used to acquire the temperature data inside the mixing chamber (101) through the temperature sensor (14) and determine the temperature data. When the temperature inside the mixing chamber (101) collected is lower than 68 °C, a signal for starting the heating plate (13) is sent to the driving module. When the temperature inside the mixing chamber (101) collected is higher than 70 °C, a driving signal for stopping the heating plate (13) is sent to the driving module; The driving module is used to receive the driving signals transmitted by each module, and transmit signals to several electromagnetic valves (8) and the heating plate (13) according to the driving signals. Then, when both electromagnetic valves (8) on both sides are opened, a signal is transmitted to the servo motor (10) to make the servo motor (10) rotate at a rotation speed of 600 rpm, and the rotation time is recorded. When the rotation time reaches 45 min, a stop signal is sent to the servo motor (10).

10. The auxiliary device for spectrometric determination of heavy metal elements according to claim 9, characterized in that, The folding inflection point of the siphon tube (5) is located at the volume height of 5 mL in the mixing chamber (101).

Images