A device for measuring fluorine in grain

By designing a fluoride detection device for grains that includes a sample boat, a weighing box, and a quartz tube, and employing grinding and high-temperature combustion hydrolysis methods, the problems of expensive instruments and complex operation in existing technologies have been solved, achieving low-cost, rapid, and accurate fluoride detection.

CN224553257UActive Publication Date: 2026-07-24CHINA UNIV OF MINING & TECH (BEIJING)
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Patent Information

Application Number
CN202520928317.5
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-05-13
Publication Date
2026-07-24
Estimated Expiration
2035-05-13

AI Technical Summary

Technical Problem

Existing methods for determining fluoride in grain samples use expensive and complex instruments, making them difficult to popularize, and the test results are prone to error.

Method used

A device for measuring fluoride in grains was designed, comprising a sample boat, a first weighing box, a grinding box, a second weighing box, and a quartz tube. Through grinding, weighing, and high-temperature combustion hydrolysis, combined with the supply of water vapor and oxygen, a simple and rapid detection method is achieved.

Benefits of technology

It enables low-cost, simple, and rapid testing, improves the accuracy of test results, and reduces errors caused by grinding losses.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model discloses a device is measured in grain fluorine, including sample boat and the first weighing box, grinding box, second weighing box, quartz tube that communicate in proper order, be provided with first weighing platform in the first weighing box, be provided with grinding device in grinding box, be provided with second weighing platform in second weighing box, quartz tube is communicated with water vapor supply device, oxygen supply device and high temperature combustion furnace respectively, and the export of quartz tube is downward and the export communication has absorption bottle. The instrument used is low in price, and the integrated operation is simple, quick, and the grain sample can be further crushed after the grinding of the grinding device in the grinding box, the high temperature combustion hydrolysis efficiency is improved, and the accuracy of the detection result is improved further, and the grain sample is weighed in the first weighing box and the second weighing box before and after the grinding and crushing respectively, and the error caused by the grinding loss can be eliminated when calculating the result, and the accuracy of the detection result is improved further.
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Description

Technical Field

[0001] This utility model relates to the field of experimental device technology, specifically to a device for measuring fluoride in grains. Background Technology

[0002] Fluorine is a widely distributed element in nature. It possesses the strongest electronegativity, a small atomic radius, and low polarizability, allowing it to form the strongest single bond with carbon. Fluoropolymers are already used in chemical processing, the medical industry, electrical equipment, and communication equipment. The introduction of fluorine can enhance biological activity and metabolic stability; therefore, fluorine plays a crucial role in modern drug development. Fluorine-containing compounds account for approximately 25% of clinical small molecule drugs, and 18F-labeled radiopharmaceuticals are widely used in medical imaging. Fluorine is also an essential trace element for the human body. Appropriate amounts of fluorine are beneficial, but excessive amounts can negatively impact health, causing conditions such as dental fluorosis and skeletal fluorosis.

[0003] In recent years, with the rapid development of agriculture and industry, fluoride pollution has become a significant factor in environmental pollution, and various forms of fluoride pollution have attracted serious attention. Existing methods for determining fluoride in grain samples mainly employ proton-induced gamma-ray emission spectrometry (PIGE) and mass spectrometry. These methods utilize direct analytical instruments that are rapid, sensitive, and advanced; however, these instruments are expensive and complex to operate, making them difficult to popularize. Therefore, we propose a device for determining fluoride in grains. Utility Model Content

[0004] The technical problem to be solved by this utility model is to overcome the existing defects and provide a device for measuring fluoride in grains. The instrument used is inexpensive, the integrated operation is simple and fast, and the high-temperature combustion hydrolysis time is short, resulting in fewer interfering ions in the sample solution, which can improve the accuracy of the detection results and effectively solve the problems in the background technology.

[0005] To achieve the above objectives, this utility model provides the following technical solution: an apparatus for measuring fluoride in grain, comprising a sample boat and a first weighing box, a grinding box, a second weighing box, and a quartz tube connected in sequence. The first weighing box is provided with a first weighing platform, the grinding box is provided with a grinding device, the second weighing box is provided with a second weighing platform, the quartz tube is connected to a steam supply device, an oxygen supply device, and a high-temperature combustion furnace, the outlet of the quartz tube faces downward and is connected to an absorption bottle, and a condenser tube is provided on the outside of the outlet of the quartz tube.

[0006] As a preferred technical solution of this utility model, the upper surface of the first weighing box is provided with a placement opening, and a sealing cover is provided at the placement opening.

[0007] As a preferred technical solution of this utility model, the side surface of the first weighing box is provided with an opening, a sealing plug is provided inside the opening, the side surface of the sealing plug is provided with a through hole, and a sample feeding rod for pushing the sample boat to move inside the first weighing box, the grinding box, the second weighing box and the quartz tube is provided inside the through hole.

[0008] As a preferred technical solution of this utility model, the end of the injection rod is provided with a hook for pulling the sample boat along the direction of the quartz tube, the second weighing box, the grinding box, and the first weighing box.

[0009] As a preferred technical solution of this utility model, the grinding device includes a first push rod installed on the lower surface of the top plate of the grinding box, a first motor is provided inside the movable end of the first push rod, the output shaft of the first motor passes through the lower surface of the movable end of the first push rod and is connected to the grinding block, and the shape of the grinding block matches the sample boat.

[0010] As a preferred embodiment of this utility model, a second push rod is installed on the inner surface of the second weighing box, and a second motor is provided on the movable end side surface of the second push rod. The output shaft of the second motor passes through the cavity opened inside the movable end of the second push rod and is connected to the driving bevel gear. A driven bevel gear that meshes with the driving bevel gear is rotatably arranged in the cavity of the movable end of the second push rod. The center of the driven bevel gear is fixedly connected to the rotating shaft. The rotating shaft passes through the side surface of the movable end of the second push rod and is connected to the rotating brush. The rotating brush can enter the grinding box to clean the surface of the grinding block under the drive of the second push rod.

[0011] As a preferred embodiment of this utility model, the steam supply device includes a temperature-regulating electric heater, on which a distillation flask is placed. The top outlet of the distillation flask is connected to an explosion-proof ball through a conduit, and the explosion-proof ball is connected to a quartz tube through a conduit.

[0012] As a preferred embodiment of this utility model, the oxygen supply device includes an oxygen cylinder, which is connected to a quartz tube via a gas delivery pipe.

[0013] As a preferred embodiment of this utility model, a thermocouple is installed inside the high-temperature combustion furnace, and the thermocouple is connected to a temperature controller installed outside the high-temperature combustion furnace.

[0014] As a preferred embodiment of this utility model, a spiral tube is provided inside the condenser tube, the spiral tube is sleeved on the outside of the vertical part at the outlet of the quartz tube, a water inlet pipe is provided at the top of the spiral tube, a water return pipe is provided at the top of the spiral tube, and both the water inlet pipe and the water return pipe are connected to an external condensate water equipment.

[0015] Compared with the prior art, the beneficial effects of this utility model are: the instrument used is inexpensive, the integrated operation is simple and fast, the grain sample can be further crushed after being ground by the grinding device in the grinding box, which improves the high-temperature combustion hydrolysis efficiency and thus improves the accuracy of the test results. Moreover, the grain sample is weighed in the first weighing box and the second weighing box before and after grinding, respectively. When calculating the results, the error caused by grinding loss can be eliminated, which further improves the accuracy of the test results. Attached Figure Description

[0016] Figure 1 This is a schematic diagram of the structure of this utility model.

[0017] In the diagram: 1 First weighing box, 11 Sealing cover, 12 First weighing platform, 13 Sealing plug, 14 Sample inlet rod, 15 Hook, 2 Grinding box, 21 First push rod, 22 Grinding block, 3 Second weighing box, 31 Second weighing platform, 32 Second push rod, 33 Second motor, 34 Rotating brush, 4 Quartz tube, 5 Steam supply device, 51 Temperature regulating heater, 52 Distillation flask, 53 Explosion-proof ball, 54 Water outlet pipe, 6 Oxygen supply device, 61 Oxygen cylinder, 62 Gas delivery pipe, 7 High-temperature combustion furnace, 71 Temperature controller, 72 Thermocouple, 8 Condenser, 81 Spiral tube, 82 Water inlet pipe, 83 Water return pipe, 9 Absorption bottle. Detailed Implementation

[0018] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0019] Please see Figure 1 This utility model provides a technical solution: an apparatus for measuring fluoride in grain, comprising a sample boat and a first weighing box 1, a grinding box 2, a second weighing box 3, and a quartz tube 4 connected in sequence. The first weighing box 1 is provided with a first weighing platform 12 for weighing the sample before grinding. The grinding box 2 is provided with a grinding device for grinding and pulverizing the grain sample in the sample boat, improving hydrolysis efficiency, and thus improving the accuracy of the detection results.

[0020] The second weighing box 3 is equipped with a second weighing platform 31, which is used to weigh the ground and pulverized grain sample. When calculating the results, the error caused by grinding loss can be eliminated, which further improves the accuracy of the test results.

[0021] The quartz tube 4 is connected to the steam supply device 5, the oxygen supply device 6, and the high-temperature combustion furnace 7. The steam supply device 5 includes a temperature-regulating electric heater 51, on which a distillation flask 52 is placed. The distillation flask 52 is filled with deionized water and its bottom is placed in the groove of the temperature-regulating electric heater. The temperature-regulating electric heater 51 heats the distillation flask 52. The top outlet of the distillation flask 52 is connected to the explosion-proof ball 53 through a quartz tube. The explosion-proof ball 53 is connected to the quartz tube 4 through a tube. The deionized water vapor in the explosion-proof ball 53 enters the quartz tube 4, thereby hydrolyzing the burning grain sample.

[0022] The oxygen supply device 6 includes an oxygen cylinder 61, which is connected to the quartz tube 4 via a gas supply pipe 62 to supply oxygen to the quartz tube 4, thereby providing combustion support for the grain sample.

[0023] A thermocouple 72 is installed inside the high-temperature combustion furnace 7. The thermocouple 72 is connected to a temperature controller 71 located outside the high-temperature combustion furnace 7. A commonly used temperature controller, such as the YY-F660 six-channel temperature controller, is selected. The temperature controller 71 is used to adjust the temperature of the thermocouple 72, which is used to heat the grain samples and quartz sand inside the sample boat. The high-temperature combustion furnace 7 has through holes corresponding to the thermocouple 72, allowing the thermocouple 72 to move up and down under external action or an external pushing device, such as an electric push rod, to facilitate its insertion into the sample boat.

[0024] The outlet section of the quartz tube 4 is vertical with the outlet facing downwards, and the outlet is connected to an absorption bottle 9, which is used to collect the liquid after hydrolysis and condensation.

[0025] A condenser tube 8 is installed on the outside of the outlet of the quartz tube 4, and a spiral tube 81 is installed on the inside of the condenser tube 8. The spiral tube 81 is sleeved on the outside of the vertical part of the outlet of the quartz tube 4. A water inlet pipe 82 and a water return pipe 83 are installed at the top of the spiral tube 81. Both the water inlet pipe 82 and the water return pipe 83 are connected to external condensation equipment (including a cold water tank, a circulating pump, and a refrigerator such as a semiconductor refrigeration chip). The cold water in the spiral tube 81 cools the outlet of the quartz tube 4, causing the hydrolyzed gas sample to condense into a liquid, which is convenient for collection and detection.

[0026] A distillation flask containing deionized water is heated by a temperature-regulating heater at its bottom, causing water vapor to enter a blast-proof bulb. From the top of the blast-proof bulb, the vapor travels through a rubber tube into the lower right part of a quartz tube, thus hydrolyzing the grain sample at high temperature. The hydrolyzed gas sample enters the vertical section of the quartz tube through the left side. Under the cooling effect of circulating water in the condenser, the gas sample condenses into a liquid, which then flows into absorption bottle 9. The liquid in absorption bottle 9 can then be analyzed using existing, commonly used methods. This device uses inexpensive, integrated, simple, and fast-acting instruments. It features short high-temperature combustion hydrolysis time, produces a sample solution with few interfering ions, and offers high detection accuracy.

[0027] Before receiving the condensate flowing from the outlet of quartz tube 4, add 0.2 mol / L sodium hydroxide solution to absorption bottle 9. After combustion and hydrolysis are complete, remove the absorption tube, add 1 to 2 drops of 0.5% phenolphthalein indicator to the absorption tube, neutralize with 2 mol / L nitric acid until the red color disappears, then add the appropriate volume of ionic strength adjuster, dilute to the mark with deionized water, and shake well before testing.

[0028] Preferably, a drain pipe 54 is also provided on the lower side of the quartz tube 4, and a valve is provided on the drain pipe 54. The drain pipe 54 is used to drain the liquid in the quartz tube after the experiment.

[0029] In a preferred embodiment, the upper surface of the first weighing box 1 has a placement opening, and a sealing cover 11 is provided at the placement opening. Opening the sealing cover 11 allows the grain sample to be placed into the sample boat. Closing the sealing cover 11 seals the first weighing box 1, preventing gases generated after hydrolysis from escaping and affecting the detection results of fluoride in the grain.

[0030] In a preferred embodiment, the side surface of the first weighing box 1 has an opening, and a sealing plug 13 is provided inside the opening. The side surface of the sealing plug 13 has a through hole, and a sample feeding rod 14 is provided inside the through hole for moving the sample boat within the first weighing box 1, the grinding box 2, the second weighing box 3, and the quartz tube 4. By pushing the sample feeding rod 14, the sample boat can be weighed once in the first weighing box 1, ground and crushed in the grinding box 2, weighed twice in the second weighing box 3, and hydrolyzed at high temperature in the quartz tube 4.

[0031] A sliding seal is provided between the through hole of the sealing plug 13 and the injection rod 14.

[0032] In a further preferred embodiment, the end of the injection rod 14 is provided with a hook 15 for pulling the sample boat along the direction of the quartz tube 4, the second weighing box 3, the grinding box 2, and the first weighing box 1. The injection rod 14 can also rotate at the through hole of the sealing plug 13. When the hook 15 is rotated to the horizontal position or to the upper side of the sample boat, the entire injection rod 14 is on the upper side of the sample boat; when the hook 15 is rotated to the lower side, it can contact the sample boat, facilitating pushing or pulling the sample boat.

[0033] In a preferred embodiment, a first push rod 21 is installed on the lower surface of the top plate of the grinding box 2. A first motor is installed inside the movable end of the first push rod 21. The output shaft of the first motor passes through the lower surface of the movable end of the first push rod 21 and is connected to the grinding block 22. The grinding block 22 matches the shape of the sample boat. The first push rod 21 is used to drive the grinding block 22 to move up and down, enter the sample boat to grind the grain sample and quartz sand, and then leave the sample boat so that it can enter the second weighing box 3. The first motor drives the grinding block 22 to rotate, grinding and pulverizing the grain sample and quartz sand.

[0034] Both the grinding block 22 and the sample boat are frustum-shaped. The opening on the upper side of the sample boat is larger than its bottom surface area, which makes it convenient for the grinding block 22 to enter the sample boat to grind and crush grain samples and quartz sand.

[0035] In a preferred embodiment, a second push rod 32 is installed on the inner surface of the second weighing box 3. The first push rod 21, the second push rod 32, etc., can be electric push rods, hydraulic cylinders, or pneumatic cylinders commonly used in the prior art. A second motor 33 is provided on the movable end side surface of the second push rod 32. The output shaft of the second motor 33 passes through a cavity opened on the inner side of the movable end of the second push rod 32 and is connected to the driving bevel gear. A driven bevel gear is rotatably arranged in the cavity of the movable end of the second push rod 32, meshing with the driving bevel gear. The center of the driven bevel gear is fixedly connected to a rotating shaft. The rotating shaft passes through the side surface of the movable end of the second push rod 32 and is connected to a rotating brush 34. The rotating brush 34 can enter the inner side of the grinding box 2 under the drive of the second push rod 32. When the grinding block 22 is finished grinding and moves to the upper side, the rotating brush 34 extends to its lower side and rotates under the drive of the second motor 33 to clean the surface of the grinding block 22. The cleaned sample powder falls into the sample boat, which can reduce sample loss and improve the accuracy of the test results.

[0036] The first push rod 21, the second push rod 32, the first motor, the second motor 33, the thermocouple 72, the temperature controller 71, the temperature-regulating heater 51, etc. used in this application are all commonly used electronic components in the prior art. Their specific structures, working principles, control methods, circuit connections, power supplies, etc. are all known technologies and will not be described in detail here.

[0037] The parts not disclosed in this utility model are all prior art, and their specific structures, materials, and working principles will not be described in detail. Although embodiments of this utility model have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principles and spirit of this utility model, the scope of which is defined by the appended claims and their equivalents.

Claims

1. An apparatus for measuring fluoride in grain, characterized in that: The sample boat includes a first weighing box (1), a grinding box (2), a second weighing box (3), and a quartz tube (4) connected in sequence. The first weighing box (1) is equipped with a first weighing platform (12), the grinding box (2) is equipped with a grinding device, the second weighing box (3) is equipped with a second weighing platform (31), the quartz tube (4) is connected to a steam supply device (5), an oxygen supply device (6), and a high-temperature combustion furnace (7), respectively. The outlet of the quartz tube (4) faces downward and is connected to an absorption bottle (9). A condenser (8) is provided on the outside of the outlet of the quartz tube (4).

2. The device for determining fluoride in grain according to claim 1, characterized in that: The first weighing box (1) has a placement opening on its upper surface, and a sealing cover plate (11) is provided at the placement opening.

3. The apparatus for determining fluoride in grain according to claim 1, characterized in that: The first weighing box (1) has an opening on its side surface, and a sealing plug (13) is provided inside the opening. The sealing plug (13) has a through hole on its side surface, and a sample feeding rod (14) is provided inside the through hole for pushing the sample boat to move inside the first weighing box (1), the grinding box (2), the second weighing box (3) and the quartz tube (4).

4. The apparatus for determining fluoride in grain according to claim 3, characterized in that: The end of the sample feed rod (14) is provided with a hook (15) for pulling the sample boat along the direction of the quartz tube (4), the second weighing box (3), the grinding box (2), and the first weighing box (1).

5. The apparatus for determining fluoride in grain according to claim 1, characterized in that: The grinding device includes a first push rod (21) mounted on the lower surface of the top plate of the grinding box (2). A first motor is installed inside the movable end of the first push rod (21). The output shaft of the first motor passes through the lower surface of the movable end of the first push rod (21) and is connected to the grinding block (22). The grinding block (22) matches the shape of the sample boat.

6. The apparatus for determining fluoride in grain according to claim 5, characterized in that: The inner surface of the second weighing box (3) is equipped with a second push rod (32), and the movable end side surface of the second push rod (32) is provided with a second motor (33). The output shaft of the second motor (33) passes through the cavity opened inside the movable end of the second push rod (32) and is connected to the driving bevel gear. The cavity at the movable end of the second push rod (32) is rotatably provided with a driven bevel gear that meshes with the driving bevel gear. The center of the driven bevel gear is fixedly connected to the rotating shaft. The rotating shaft passes through the side surface of the movable end of the second push rod (32) and is connected to the rotating brush (34). The rotating brush (34) can enter the grinding box (2) to clean the surface of the grinding block (22) under the drive of the second push rod (32).

7. The apparatus for determining fluoride in grain according to claim 1, characterized in that: The steam supply device (5) includes a temperature-regulating electric heater (51), on which a distillation flask (52) is placed. The top outlet of the distillation flask (52) is connected to an explosion-proof ball (53) through a conduit. The explosion-proof ball (53) is connected to a quartz tube (4) through a conduit.

8. The apparatus for determining fluoride in grain according to claim 1, characterized in that: The oxygen supply device includes an oxygen cylinder (61), which is connected to a quartz tube (4) via an air supply pipe (62).

9. The apparatus for determining fluoride in grain according to claim 1, characterized in that: The high-temperature combustion furnace (7) is equipped with a thermocouple (72), which is connected to a temperature controller (71) located on the outside of the high-temperature combustion furnace (7).

10. The apparatus for determining fluoride in grain according to claim 1, characterized in that: A spiral tube (81) is provided inside the condenser tube (8). The spiral tube (81) is sleeved on the outside of the vertical part at the outlet of the quartz tube (4). A water inlet pipe (82) is provided at the top of the spiral tube (81), and a water return pipe (83) is provided at the top of the spiral tube (81). Both the water inlet pipe (82) and the water return pipe (83) are connected to the external condenser equipment.