An elemental measurement device

Abstract

The utility model discloses an element determination equipment, and the equipment includes pipette device, pure water room, waste liquid room, a plurality of analysis chambers and a plurality of solution chambers, and the progressive connection's sampling device, high temperature hydrolytic device, condenser, liquid collecting bottle, the sampling device is used to deliver sample to high temperature hydrolytic device, high temperature hydrolytic device is used to carry out high temperature hydrolysis to sample, the condenser is used to carry out condensation to the gas produced after sample high temperature hydrolysis and sends into liquid collecting bottle, the solution chamber is used to store the solution used in different types experiment, the pipette device includes the interconnection's multiport valve and quantitative pump subassembly, and the multiport valve is communicated with liquid collecting bottle, pure water room, waste liquid room, each analysis chamber and each solution chamber respectively. The utility model has the advantages of high testing efficiency, high testing accuracy and high testing continuity.

Description

Technical Field

[0001] This utility model relates to the field of element content determination technology, and in particular to an element determination device. Background Technology

[0002] Fluorine and chlorine in coal exist primarily in inorganic forms. Fluorine often combines with elements such as aluminum and calcium, while chlorine mainly exists as chlorides. Emissions of fluorine and chlorine pollute the atmosphere, water bodies, and soil. Chlorine corrodes boilers and pipes, shortening equipment lifespan. Excessive intake of fluorine and chlorine can lead to diseases such as dental fluorosis and skeletal fluorosis. Therefore, accurate determination of the fluorine and chlorine content in coal is of great importance for environmental protection and human health.

[0003] Currently, there are many methods for detecting fluorine and chlorine in coal, such as the national standards GB / T 4633-2014 "Determination of Fluorine in Coal" and GB / T 3558-2014 "Determination of Chlorine in Coal". The national standard GB / T 4633-2014 uses the high-temperature combustion hydrolysis + standard addition method (or standard curve method) to determine the total fluorine content in coal. This method requires manual sample preparation for high-temperature hydrolysis, manual pH adjustment, and volume determination, making the pretreatment and analysis steps relatively cumbersome. Furthermore, only one fluorine value can be measured per sample. The national standard GB / T 3558-2014, "Determination of Chlorine in Coal", adopts the high-temperature combustion hydrolysis + potentiometric titration method and the Aldrin fusion + hydrogen sulfate titration method. The high-temperature combustion hydrolysis + potentiometric titration method requires manual sample pushing for high-temperature combustion, manual pH adjustment, and volume adjustment, making the pretreatment and analysis steps relatively cumbersome. The Aldrin fusion + hydrogen sulfate titration method has even more complex pretreatment, and both methods can only measure one chlorine value per sample. Utility Model Content

[0004] The technical problem to be solved by this utility model is to overcome the shortcomings of the existing technology and provide an element determination device with high testing efficiency, high testing accuracy and high testing continuity.

[0005] To solve the above-mentioned technical problems, the present invention adopts the following technical solution: An elemental analysis device includes a pipetting device, a pure water chamber, a waste liquid chamber, multiple analytical chambers, and multiple solution chambers, as well as a sample injection device, a high-temperature hydrolysis device, a condenser, and a collection bottle connected in sequence. The sample injection device is used to deliver the sample to the high-temperature hydrolysis device, which performs high-temperature hydrolysis on the sample. The condenser is used to condense the gas generated after the sample is hydrolyzed at high temperature and send it to the collection bottle. The solution chambers are used to store solutions used in different types of experiments. The pipetting device includes a multi-way valve and a metering pump assembly connected to each other. The multi-way valve is connected to the collection bottle, the pure water chamber, the waste liquid chamber, each analytical chamber, and each solution chamber.

[0006] As a further improvement to the above technical solution: The sample introduction device includes a sealing tube, a sample release box, and a sample delivery mechanism. The sample release box is connected to the sealing tube. The sample delivery mechanism includes a sample delivery rod, a magnetic guide module, and a drive mechanism. The sample delivery rod is located inside the sealing tube and is equipped with a magnetic guide block. The drive mechanism is used to drive the magnetic guide module to reciprocate along the outer wall of the sealing tube so as to drive the sample delivery rod with the magnetic guide block to move synchronously.

[0007] The high-temperature hydrolysis device includes a high-temperature furnace, and a quartz tube and a steam generating tube disposed inside the high-temperature furnace. The quartz tube includes an inner quartz tube and an outer quartz tube sleeved outside the inner quartz tube. One end of the inner quartz tube is connected to a condenser and the other end is connected to a sample box. The outer quartz tube is provided with a first steam hole communicating with the steam generating tube, and the inner quartz tube is provided with a second steam hole communicating with the outer quartz tube.

[0008] The high-temperature hydrolysis device also includes a steam pump, which is used to supply water to the steam generating pipe in a metered manner.

[0009] The solution chamber includes a pH indicator solution chamber and a sodium hydroxide solution chamber. The collection bottle is equipped with a color sensor for detecting the color of the collected liquid in the collection bottle. The color sensor is connected to a metering pump assembly and is used to control the metering pump assembly to pump the pH indicator solution in the pH indicator solution chamber into the collection bottle and to pump the sodium hydroxide solution in the sodium hydroxide solution chamber into the collection bottle to achieve pH adjustment of the collected liquid in the collection bottle.

[0010] The collection bottle is equipped with a liquid level sensor for detecting the liquid level in the collection bottle. The liquid level sensor is connected to a metering pump assembly and is used to control the metering pump assembly to pump pure water from the pure water chamber into the collection bottle to achieve a constant volume of the collected liquid in the collection bottle.

[0011] The liquid collecting bottle is also equipped with a liquid collecting tube, one end of which is connected to the condenser and the other end extends to the bottom of the liquid collecting bottle.

[0012] The analytical chamber includes a fluorine analysis chamber and a chlorine analysis chamber.

[0013] As a further improvement to the above technical solution: The analysis chamber includes a fluorine analysis chamber and a chlorine analysis chamber; in step S5, the test solution in the fluorine analysis chamber is used to determine the fluorine value of the sample by the fluoride ion selective electrode method; the test solution in the chlorine analysis chamber is used to determine the chlorine value of the sample by the silver nitrate titration method or the ion electrode method.

[0014] Compared with the prior art, the advantages of this utility model are: 1. The element determination equipment of this utility model separates the sample solution in the collection bottle through a pipette device, which can test multiple elements with one sample, resulting in high testing efficiency. The pH adjustment, volume fixation and other processes are all quantitatively operated by a quantitative pump assembly, resulting in high testing accuracy. When the sample solution of the previous sample is separated to the analysis chamber for analysis, the next sample can simultaneously undergo high-temperature hydrolysis, pH adjustment and other processes to form a new sample solution that enters the collection bottle. After the element determination of the previous sample is completed, the analysis chamber is cleaned, and the next sample can be directly measured, realizing continuous sample determination, high testing efficiency and high testing continuity.

[0015] 2. The element determination device of this utility model uses a drive mechanism to push the sample by magnetic attraction, which makes the sealing tube more reliable and prevents air from interfering with the high-temperature hydrolysis of the sample.

[0016] 3. In the element determination device of this utility model, the water in the steam generating tube is heated into steam by a high-temperature furnace. The steam enters the quartz tube through the first steam hole to supply steam to the quartz tube. Compared with the existing technical solution of setting up a separate steam pipe and heater, the energy utilization rate is high and the cost is low. In addition, after the steam enters the outer quartz tube, it can be heated again by the high-temperature furnace to prevent the steam from condensing before entering the inner quartz tube, which would cause water accumulation and lead to explosive combustion of coal samples. The high-temperature hydrolysis effect is better.

[0017] 4. The element determination equipment of this utility model can adjust the steam flow rate by controlling the water supply from the steam pump to the steam generating tube. Compared with the existing technical solution of adjusting the steam flow rate by adjusting the heating power of the electric furnace, the steam flow rate control is more precise and the analysis accuracy is higher.

[0018] 5. The element determination device of this utility model identifies the color of the solution through a color sensor and controls whether the metering pump assembly pumps sodium hydroxide solution according to the color change of the solution. This enables the metering pump assembly to accurately add sodium hydroxide solution to the collection bottle, making pH adjustment more precise and avoiding the release of chloride ions by traditional pH adjustment technology, which would interfere with the determination of chloride content in the sample. Attached Figure Description

[0019] Figure 1 This is a front sectional view of the element determination device of this utility model.

[0020] Figure 2 This is a rear view of the element determination device of this utility model.

[0021] Figure 3 This is a schematic diagram of the sample introduction device and the high-temperature hydrolysis device in the element determination equipment of this utility model.

[0022] Figure 4 This is a schematic diagram of the liquid collecting bottle in the element determination device of this utility model.

[0023] Figure 5 This is a schematic diagram of the pipetting device in the element determination equipment of this utility model.

[0024] Figure 6 This is a schematic diagram of the analysis chamber in the elemental determination equipment of this utility model.

[0025] The labels in the diagram represent: 1. Sample injection device; 11. Sealing tube; 12. Sample box; 13. Sample delivery mechanism; 131. Sample delivery rod; 132. Magnetic guide module; 133. Drive mechanism; 2. High-temperature hydrolysis device; 21. Quartz tube; 211. Inner quartz tube; 2111. Second water vapor hole; 212. Outer quartz tube; 2121. First water vapor hole; 22. Water vapor generating tube; 23. High-temperature furnace; 3. Condenser; 4. Collection bottle; 41. Color sensor; 42. Liquid level sensor; 43. Collection tube; 5. Pipette; 51. Multi-way valve; 52. Quantitative pump assembly; 6. Analysis chamber; 61. Fluorine analysis chamber; 62. Chlorine analysis chamber; 7. Solution chamber. Detailed Implementation

[0026] The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0027] In the description of this utility model, it should be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this utility model and simplifying the description, and do not 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 utility model.

[0028] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of this utility model, "a plurality of" means two or more, unless otherwise explicitly specified.

[0029] In this utility model, unless otherwise explicitly specified and limited, the terms "assembly," "connection," "joining," and "fixing" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; 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; they can refer to the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model according to the specific circumstances.

[0030] Example 1: like Figures 1 to 6 As shown, the element determination device of this embodiment includes a pipetting device 5, a pure water chamber, a waste liquid chamber, multiple analysis chambers 6 and multiple solution chambers 7, and a sample injection device 1, a high-temperature hydrolysis device 2, a condenser 3, and a collection bottle 4 connected in sequence. The sample injection device 1 is used to transport the sample to the high-temperature hydrolysis device 2, which is used to perform high-temperature hydrolysis on the sample. The condenser 3 is used to condense the gas generated after the sample is hydrolyzed at high temperature and send it to the collection bottle 4. The solution chambers 7 are used to store solutions used in different types of experiments. The pipetting device 5 includes a multi-way valve 51 and a quantitative pump assembly 52 connected to each other. The multi-way valve 51 is connected to the collection bottle 4, the pure water chamber, the waste liquid chamber, each analysis chamber 6 and each solution chamber 7 respectively.

[0031] In this embodiment of the elemental determination equipment, during operation, the sample introduction device 1 delivers the sample to the high-temperature hydrolysis device 2, where the sample undergoes high-temperature hydrolysis. The gas generated after hydrolysis is condensed by the condenser 3 and enters the collection bottle 4 to form a collected liquid. The metering pump assembly 52 draws pH indicator from the solution chamber 7 and adds it to the collection bottle 4, and also draws sodium hydroxide solution from the solution chamber 7 and adds it to the collection bottle 4 to adjust the pH of the collected liquid. The metering pump assembly 52 draws pure water from the pure water chamber and adds it to the collection bottle 4 to bring the collected liquid to a constant volume and stir it to form a sample solution. The metering pump assembly 52 then dispenses the sample solution from the collection bottle 4 into each analysis chamber 6, and draws reagent solution from the solution chamber 7... The solution is added to each analysis chamber 6. Pure water is drawn from the pure water chamber and added to each analysis chamber 6 to make up the volume and stir to form the test solution. At the same time, the metering pump assembly 52 draws pure water from the solution chamber 7 to clean the collection bottle 4. The metering pump assembly 52 draws the cleaning waste liquid from the collection bottle 4 to the waste liquid chamber. The above steps are performed, and the next sample forms a sample solution in the collection bottle 4. The test solutions in each analysis chamber 6 are analyzed to obtain the content of each element. The metering pump assembly 52 draws the test waste liquid from the analysis chamber 6 to the waste liquid chamber, draws pure water from the solution chamber 7 to clean the analysis chamber 6, and then draws the cleaning waste liquid from the analysis chamber 6 to the waste liquid chamber. The above steps are repeated to test multiple samples.

[0032] The element determination device in this embodiment separates the sample solution in the collection bottle 4 using the pipette 5, enabling the testing of multiple elements from a single sample, resulting in high testing efficiency. pH adjustment, volume determination, and other processes are all quantitatively operated by the quantitative pump assembly 52, ensuring high testing accuracy. While the sample solution from the previous sample is being separated and analyzed in the analysis chamber 6, the next sample can simultaneously undergo high-temperature hydrolysis, pH adjustment, and other processes to form a new sample solution that enters the collection bottle 4. After the element determination of the previous sample is completed, the analysis chamber 6 is cleaned, allowing direct measurement of the next sample, thus achieving continuous sample determination with high testing efficiency and continuity.

[0033] Furthermore, in this embodiment, the sample introduction device 1 includes a sealing tube 11, a sample placement box 12, and a sample delivery mechanism 13. The sample placement box 12 is connected to the sealing tube 11. The sample delivery mechanism 13 includes a sample delivery rod 131, a magnetic guide module 132, and a drive mechanism 133. The sample delivery rod 131 is disposed inside the sealing tube 11 and is provided with a magnetic guide block. The drive mechanism 133 is used to drive the magnetic guide module 132 to reciprocate along the outer wall of the sealing tube 11 to drive the sample delivery rod 131 with the magnetic guide block to move synchronously. The drive mechanism 133 drives the sample delivery rod 131 to push the sample by magnetic attraction, making the sealing tube 11 more reliable and preventing air interference with the high-temperature hydrolysis of the sample.

[0034] Preferably, in this embodiment, the driving mechanism 133 includes a drive motor and a transmission belt (not shown in the figure). The drive motor drives the transmission belt to move, thereby causing the magnetic guide module 132, the sample feeding rod 131, and the transmission belt to reciprocate synchronously. Of course, in other embodiments, the reciprocating motion of the sample feeding rod 131 can also be achieved by using a slide rail and a slider.

[0035] Furthermore, in this embodiment, the high-temperature hydrolysis device 2 includes a high-temperature furnace 23, and a quartz tube 21 and a steam generating tube 22 disposed in the high-temperature furnace 23. The quartz tube 21 includes an inner quartz tube 211 and an outer quartz tube 212 sleeved outside the inner quartz tube 211. One end of the inner quartz tube 211 is connected to the condenser 3 and the other end is connected to the sample box 12. The outer quartz tube 212 is provided with a first steam hole 2121 communicating with the steam generating tube 22, and the inner quartz tube 211 is provided with a second steam hole 2111 communicating with the outer quartz tube 212. Water in the steam generating tube 22 is heated into steam by the high-temperature furnace 23. The steam enters the quartz tube 21 through the first steam hole 2121 to supply steam to the quartz tube 21. Compared with the existing technical solution of setting up a separate steam pipe and heater, the energy utilization rate is high and the cost is low. In addition, after the steam enters the outer quartz tube 212, it can be heated again by the high-temperature furnace 23 to prevent the steam from condensing before entering the inner quartz tube 211, which would cause water accumulation and lead to the explosive combustion of the coal sample. The high-temperature hydrolysis effect is better.

[0036] Furthermore, in this embodiment, the high-temperature hydrolysis device 2 also includes a steam pump (not shown in the figure), which is used to quantitatively supply water to the steam generating tube 22. By controlling the amount of water supplied by the steam pump to the steam generating tube 22, the steam flow rate can be adjusted. Compared with the existing technical solution of adjusting the steam flow rate by adjusting the heating power of the electric furnace, the steam flow rate control is more precise and the analysis accuracy is higher.

[0037] Furthermore, in this embodiment, the solution chamber 7 includes a pH indicator solution chamber and a sodium hydroxide solution chamber. The collection bottle 4 is equipped with a color sensor 41 for detecting the color of the collected liquid in the collection bottle 4. The color sensor 41 is connected to the metering pump assembly 52 and is used to control the metering pump assembly 52 to pump the pH indicator solution (e.g., bromocresol green indicator) in the pH indicator solution chamber into the collection bottle 4 and to pump the sodium hydroxide solution in the sodium hydroxide solution chamber into the collection bottle 4 to achieve pH adjustment of the collected liquid in the collection bottle 4. Existing methods typically use pH electrodes to adjust the pH of the collection solution. These electrodes employ a double salt bridge, where potassium chloride solution in the first salt bridge slowly seeps into the potassium nitrate solution in the second. If the potassium nitrate solution in the second salt bridge is not replaced over a long period, the chloride ion concentration in the potassium nitrate solution increases, eventually seeping into the sample collection solution and interfering with the determination of chloride content in the sample. This embodiment uses a color sensor 41 to identify the solution color and controls the metering pump assembly 52 to pump in sodium hydroxide solution based on the color change. This allows the metering pump assembly 52 to precisely add sodium hydroxide solution to the collection bottle 4, resulting in more accurate pH adjustment and avoiding the release of chloride ions that interfere with the determination of chloride content in the sample, a problem common in traditional pH adjustment techniques.

[0038] Furthermore, in this embodiment, the collection bottle 4 is equipped with a liquid level sensor 42 for detecting the liquid level in the collection bottle 4. The liquid level sensor 42 is connected to the metering pump assembly 52 and is used to control the metering pump assembly 52 to pump pure water from the pure water chamber into the collection bottle 4 to achieve constant volume of the collected liquid in the collection bottle 4. By detecting the liquid level in the collection bottle 4 through the liquid level sensor 42, the constant volume of the collected liquid in the collection bottle 4 is made more accurate.

[0039] Furthermore, in this embodiment, the liquid collecting bottle 4 is also provided with a liquid collecting tube 43. One end of the liquid collecting tube 43 is connected to the condenser 3, and the other end extends to the bottom of the liquid collecting bottle 4. The gas generated after high-temperature hydrolysis is condensed by the condenser 3 and flows into the bottom of the liquid collecting bottle 4 under the action of gravity, avoiding liquid splashing, loss, and errors in the measurement results.

[0040] Furthermore, in this embodiment, the analysis chamber 6 includes a fluorine analysis chamber 61 and a chlorine analysis chamber 62. The fluorine analysis chamber 61 is equipped with a fluorine ion selective electrode and a fluorine reference electrode, and the chlorine analysis chamber 62 is equipped with a silver electrode and a chlorine reference electrode, which can detect the fluorine or chlorine content in the sample.

[0041] Preferably, in this embodiment, the solution chamber 7 further includes a sulfuric acid solution chamber, a saturated potassium nitrate solution chamber, a sodium chloride solution chamber, a silver nitrate solution chamber, a buffer solution chamber, and a sodium fluoride solution chamber; the metering pump assembly 52 includes multiple plunger pumps, which can pump each solution separately to prevent cross-contamination between reagents.

[0042] Preferably, in this embodiment, both the bottom of the collection bottle 4 and the analysis chamber 6 are equipped with magnetic stirrers to facilitate uniform mixing of the liquids in the collection bottle 4 and the analysis chamber 6.

[0043] Preferably, this embodiment also includes a robotic arm, which can grip or place samples, resulting in a higher degree of automation.

[0044] Preferably, in this embodiment, a circulating cooling device is also included, which is used to provide cooling water to the high-temperature hydrolysis device 2 and the condenser 3.

[0045] Example 2: The element determination method of this embodiment includes the following steps: Step S1: The sample introduction device 1 delivers the sample to the high-temperature hydrolysis device 2, which hydrolyzes the sample at high temperature. The gas generated after high-temperature hydrolysis is condensed by the condenser 3 and enters the collection bottle 4 to form a collection liquid. Specifically, 0.5g of sample is weighed into a porcelain boat, 0.5g of quartz sand is added, and the quartz sand and sample are mixed with a paperclip. Then, an appropriate amount of quartz sand is spread on top, the porcelain boat is placed on the sample stage, and the robotic arm picks up the porcelain boat and places it into the sample box 12. Oxygen and water vapor are introduced into the quartz tube 21. Under the push of the sample delivery rod 131, the front end of the porcelain boat stays at 300℃, 600℃ and 800℃ for 5 minutes each, and finally stays in the constant temperature zone of 1100℃ for 15 minutes. The constant temperature can be adjusted within the range of 0℃-1200℃. Of course, in other embodiments, appropriate residence time and temperature can be selected according to the actual situation. Step S2: The metering pump assembly 52 draws pH indicator from solution chamber 7 and adds it to collection bottle 4, and draws sodium hydroxide solution from solution chamber 7 and adds it to collection bottle 4 to adjust the pH of the collected liquid in collection bottle 4; specifically, the metering pump assembly 52 draws 0.1-0.5 mL of bromocresol green indicator and adds it to collection bottle 4, the collected liquid in collection bottle 4 turns yellow, the metering pump assembly 52 slowly adds sodium hydroxide solution to collection bottle 4, and when the color sensor 41 detects that the collected liquid turns blue, the metering pump assembly 52 stops adding sodium hydroxide solution, and the pH adjustment is completed; Step S3: The metering pump assembly 52 draws pure water from the pure water chamber and adds it to the collection bottle 4. The collected liquid in the collection bottle 4 is then diluted to a fixed volume and stirred to form a sample solution. Specifically, the metering pump assembly 52 slowly adds pure water to the collection bottle 4, and after dilution and stirring, 125 mL of sample solution is formed. Step S4: The metering pump assembly 52 extracts the sample solution from the collection bottle 4 and distributes it into each analysis chamber 6. It also extracts the reagent solution from the solution chamber 7 and adds it into each analysis chamber 6. Finally, it extracts pure water from the pure water chamber and adds it to each analysis chamber 6 to make up the volume and stir, thus forming the test solution. Specifically, the metering pump assembly 52 distributes the sample solution into the fluoride analysis chamber 61 and the chlorine analysis chamber 62, with 45 mL dispensed into the fluoride analysis chamber 61 and 60 mL dispensed into the chlorine analysis chamber 62. The metering pump assembly 52 adds 10 mL of buffer solution to the fluoride analysis chamber 61 and makes up the volume to 100 mL. The metering pump assembly 52 adds 1 mL of sulfuric acid, 3 mL of saturated potassium nitrate, and 5 mL of sodium chloride to the chlorine analysis chamber 62 and makes up the volume to 100 mL. The metering pump assembly 52 draws pure water from the solution chamber 7 to clean the collection bottle 4. The metering pump assembly 52 draws the cleaning waste liquid from the collection bottle 4 to the waste liquid chamber and executes steps S1 to S3. The next sample forms a sample liquid in the collection bottle 4. Specifically, after the separation is completed, the collection bottle is cleaned, the robotic arm picks up the sample that has been hydrolyzed at high temperature and puts it into the sample stage, and then picks up a new sample and puts it into the sample box 21 to start the high temperature hydrolysis of the next sample. Step S5: Analyze the test solutions in each analysis chamber 6 to obtain the content of each element; specifically, the fluoride value in the sample is determined by the fluoride ion selective electrode method in the test solution in the fluoride analysis chamber 61; the chlorine value in the sample is determined by the silver nitrate titration method or the ion electrode method in the test solution in the chlorine analysis chamber 62. Step S6: The metering pump assembly 52 draws the test waste liquid from the analysis chamber 6 to the waste liquid chamber, draws pure water from the solution chamber 7 to clean the analysis chamber 6, and then draws the cleaning waste liquid from the analysis chamber 6 to the waste liquid chamber. Step S7: Repeat steps S4 to S6 to test multiple samples.

[0046] Preferably, in this embodiment, before step S1, it is also necessary to calibrate the fluorine standard curve and test the fluorine-chlorine blank to make the measurement results more accurate.

[0047] The element determination method in this embodiment uses a quantitative pump assembly 52 to separate the sample solution in the collection bottle 4, enabling the testing of multiple elements from a single sample, resulting in high testing efficiency. pH adjustment, volume determination, and other processes are all quantitatively operated by the quantitative pump assembly 52, ensuring high testing accuracy. While the sample solution from the previous sample is being separated and analyzed in the analysis chamber 6, the next sample can simultaneously undergo high-temperature hydrolysis, pH adjustment, and other processes to form a new sample solution that enters the collection bottle 4. After the element determination of the previous sample is completed, the analysis chamber 6 is cleaned, allowing direct measurement of the next sample, thus achieving continuous sample determination with high testing efficiency and continuity.

[0048] Preferably, in this embodiment, the metering pump assembly 52 dispenses the sample solution into the fluoride analysis chamber 61 and the chlorine analysis chamber 62, with less sample solution dispensed into the fluoride analysis chamber 61 than into the chlorine analysis chamber 62. Since the detection limit for chlorine content using titration is lower than that for fluoride, transferring more sample solution to the chlorine analysis chamber 62 ensures measurement accuracy. Preferably, in this embodiment, after the quantitative pump assembly 52 dispenses the sample solution in the collection bottle 4 into the fluoride analysis chamber 61 and the chlorine analysis chamber 62, a portion of the sample solution remains in the collection bottle 4, which allows for precise control of the volume of the sample solution added to the fluoride analysis chamber 61 and the chlorine analysis chamber 62.

[0049] Preferably, in this embodiment, when determining the fluoride value in a sample using the fluoride ion selective electrode method, a standard curve or a standard addition method can be used. The specific process of the standard addition method is as follows: 1) The lower-level machine obtains the fluoride calibration formula, sodium fluoride standard solution concentration, and fluoride volume adjustment volume from the upper-level machine. These two parameters and the formula are stored in the lower-level machine. If the formula is changed, the lower-level machine will inform the upper-level machine of the formula, such as y = 4.11033 - 0.01676X, where y represents lgC and X represents the potential; 2) When the lower-level machine reads the E1 potential, it calculates lgC1 according to the above formula, calculates the C1 concentration based on the inverse function, and then calculates the target E2 = E1 + 30. Substitute E2 into the formula to calculate C2, add standard solution Vs = (C2-C1)*Vf / C standard sodium fluoride. If the potential difference does not reach 20mV after adding sodium fluoride, add another 0.04mL until the potential difference is between 20-40mV and then stop adding. 3) When the volume of Vs is greater than 0.02mL, retain two decimal places and add sodium fluoride by 4-5 rounding. If it is less than 0.02, add 0.02mL. If it is greater than 0.02, retain two decimal places and add sodium fluoride by 4-5 rounding.

[0050] Existing testing methods require operators to select different concentrations of fluoride standard solution based on the initial potential of the test solution and add 1 mL. Incorrect standard solution concentration selection can lead to potential changes exceeding 20-40 mV, affecting the accuracy of the test results. Furthermore, existing methods involve slowly adding the standard solution based on its initial potential, resulting in long testing times and inaccurate low-concentration tests due to excessive volume of fluoride standard solution added. The method in this embodiment allows for a single titration based on the initial potential of the solution, offering high efficiency and accuracy. It requires only one concentration of standard solution and has a high detection limit. Moreover, the fluoride calibration formula is based on the slope of the fluoride electrode, allowing for timely updates to the electrode calibration formula and ensuring the accuracy of the standard solution addition. The potential change when adding the standard solution to different concentrations of fluoride test solution is within the range of 30 ± 2 mV, eliminating errors caused by large potential fluctuations at different concentrations.

[0051] The above description is merely a preferred embodiment of the present utility model and is not intended to limit the present utility model in any way. Although the present utility model has been disclosed above with reference to preferred embodiments, it is not intended to limit the present utility model. Any person skilled in the art can make many possible variations and modifications to the technical solution of the present utility model using the methods and techniques disclosed above, or modify it into equivalent embodiments with equivalent changes, without departing from the spirit and technical solution of the present utility model. Therefore, any simple modifications, equivalent substitutions, equivalent changes and modifications made to the above embodiments based on the technical essence of the present utility model without departing from the content of the technical solution of the present utility model shall still fall within the protection scope of the technical solution of the present utility model.

Claims

1. An element determination device, characterized in that: The device includes a pipetting device (5), a pure water chamber, a waste liquid chamber, multiple analysis chambers (6) and multiple solution chambers (7), and a sample injection device (1), a high-temperature hydrolysis device (2), a condenser (3) and a collection bottle (4) connected in sequence. The sample injection device (1) is used to transport the sample to the high-temperature hydrolysis device (2), the high-temperature hydrolysis device (2) is used to perform high-temperature hydrolysis on the sample, the condenser (3) is used to condense the gas generated after the sample is hydrolyzed at high temperature and send it to the collection bottle (4), the solution chamber (7) is used to store solutions used in different types of experiments, and the pipetting device (5) includes a multi-way valve (51) and a metering pump assembly (52) connected to each other. The multi-way valve (51) is connected to the collection bottle (4), the pure water chamber, the waste liquid chamber, each analysis chamber (6) and each solution chamber (7) respectively.

2. The element determination device according to claim 1, characterized in that: The sample feeding device (1) includes a sealing tube (11), a sample placement box (12), and a sample delivery mechanism (13). The sample placement box (12) is connected to the sealing tube (11). The sample delivery mechanism (13) includes a sample delivery rod (131), a magnetic guide module (132), and a drive mechanism (133). The sample delivery rod (131) is located inside the sealing tube (11). The sample delivery rod (131) is provided with a magnetic guide block. The drive mechanism (133) is used to drive the magnetic guide module (132) to reciprocate along the outer wall of the sealing tube (11) so as to drive the sample delivery rod (131) with the magnetic guide block to move synchronously.

3. The element determination device according to claim 2, characterized in that: The high-temperature hydrolysis device (2) includes a high-temperature furnace (23), and a quartz tube (21) and a steam generating tube (22) disposed in the high-temperature furnace (23). The quartz tube (21) includes an inner quartz tube (211) and an outer quartz tube (212) sleeved outside the inner quartz tube (211). One end of the inner quartz tube (211) is connected to the condenser (3) and the other end is connected to the sample box (12). The outer quartz tube (212) is provided with a first steam hole (2121) communicating with the steam generating tube (22), and the inner quartz tube (211) is provided with a second steam hole (2111) communicating with the outer quartz tube (212).

4. The element determination device according to claim 3, characterized in that: The high-temperature hydrolysis device (2) also includes a steam pump, which is used to supply water to the steam generating pipe (22) in a metered manner.

5. The element determination device according to claim 1, characterized in that: The solution chamber (7) includes a pH indicator solution chamber and a sodium hydroxide solution chamber. The collection bottle (4) is equipped with a color sensor (41) for detecting the color of the collected liquid in the collection bottle (4). The color sensor (41) is connected to the metering pump assembly (52) and is used to control the metering pump assembly (52) to pump the pH indicator solution in the pH indicator solution chamber into the collection bottle (4) and to pump the sodium hydroxide solution in the sodium hydroxide solution chamber into the collection bottle (4) to achieve pH adjustment of the collected liquid in the collection bottle (4).

6. The element determination device according to claim 1, characterized in that: The collection bottle (4) is equipped with a liquid level sensor (42) for detecting the liquid level in the collection bottle (4). The liquid level sensor (42) is connected to the metering pump assembly (52) and is used to control the metering pump assembly (52) to pump pure water from the pure water chamber into the collection bottle (4) to achieve constant volume of the collected liquid in the collection bottle (4).

7. The element determination device according to claim 1, characterized in that: The liquid collecting bottle (4) is also provided with a liquid collecting tube (43), one end of which is connected to the condenser (3), and the other end extends to the bottom of the liquid collecting bottle (4).

8. The element determination apparatus according to any one of claims 1 to 7, characterized in that: The analysis chamber (6) includes a fluorine analysis chamber (61) and a chlorine analysis chamber (62).

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