Constant-temperature lifting water bath equipment for measuring fluorine content of fluorite and measuring method

Abstract

The invention relates to the technical field of fluorite fluorine content determination, in particular to constant-temperature lifting water bath equipment for fluorite fluorine content determination and a determination method.The constant-temperature lifting water bath equipment comprises an oil bath pan, a distillation beaker is arranged above the oil bath pan, one end of the distillation beaker is connected with a steam generation bottle through a hose, and the steam generation bottle is installed in a temperature-adjusting electric heater; the other end of the distillation beaker is connected with a condensation pipe through a hose, the condensation pipe is obliquely arranged above the oil bath pan, and a plastic beaker is placed at the bottom end of the condensation pipe; the oil bath pot has the beneficial effects that the insertion plate which can be slidably connected is arranged on the top surface of the oil bath pot, the traction plate and the extension plate are arranged on the insertion plate, and the distillation beaker is clamped and hung above the oil bath pot by utilizing the extension plate. When the oil bath pan is used, the distillation beaker can be stably clamped only through simple operation (loosening the hand-twisted screw rod, drawing and pulling the extension plate and the like), an additional bracket does not need to be specially configured, the functionality of the oil bath pan is expanded, meanwhile, the tedious process of taking and storing the bracket is avoided, and the convenience and the efficiency of experimental operation are improved.

Description

Technical Field

[0001] This invention relates to the field of fluorite fluorine content determination technology, specifically to a constant temperature and temperature-controlled water bath device and method for determining fluorite fluorine content. Background Technology

[0002] The determination of fluorite fluorine content requires specific equipment to perform a series of operations, including distillation and condensation, to accurately determine the fluorine content. Traditional equipment has some shortcomings:

[0003] The distillation beaker is inconvenient to hold: There is no convenient device specifically designed for the stable holding of the distillation beaker above the oil bath. Usually, an additional support is required, which not only increases the complexity of the equipment, but also makes it cumbersome to take out and store the support, thus affecting the efficiency of the experimental operation.

[0004] Inconvenient reagent storage and use: Reagents such as sulfuric acid or perchloric acid are required in the determination process, but the lack of suitable storage devices makes it inconvenient to store and use the reagents, which may affect the smooth progress of the experiment.

[0005] Condenser pipe support and storage issues: Condenser pipes need to be installed at an angle, but there is a lack of effective support structures. Furthermore, the support structures cannot be easily hidden and stored when not in use, which takes up space and affects the overall aesthetics and practicality of the equipment. Summary of the Invention

[0006] The purpose of this invention is to provide a constant temperature and humidity water bath device and method for determining the fluorine content of fluorite, so as to solve the problems mentioned in the background art.

[0007] To achieve the above objectives, the present invention provides the following technical solution: a constant temperature lifting water bath device for determining the fluorine content of fluorite, comprising an oil bath, a distillation beaker disposed above the oil bath, one end of the distillation beaker being connected to a steam generator via a hose, the steam generator being installed in a temperature-regulating electric heater, the other end of the distillation beaker being connected to a condenser via a hose, the condenser being inclinedly disposed above the oil bath, and a plastic beaker being placed at the bottom of the condenser.

[0008] The top surface of the oil bath is slidably connected to an insert plate, and the surface of the insert plate is rotatably connected to two traction plates. One end of the traction plate is movably inserted with a condenser tube, and the two condenser tubes clamp the top of the distillation beaker. After the extension plate retracts into the traction plate, it pushes the traction plate into the insert plate. After the insert plate is pushed down, it is inserted into the oil bath for storage. The surface of the insert plate is embedded with a sampling tube that contains sulfuric acid or perchloric acid.

[0009] The top surface of the oil bath is slidably connected to a support plate, and a limit block is fixed at the top of the support plate. The limit block supports the condenser tube below. After the condenser tube is pulled off the limit block, the limit block is pushed down and inserted into the oil bath.

[0010] Preferably, the top surface of the oil bath pot is provided with a reserved groove 1, the bottom surface of the reserved groove 1 is fixed with a limiting rod, the top surface of the insert plate is provided with a reserved groove 3 for the limiting rod to pass through, the reserved groove 3 is an inverted "T" shaped round hole, the limiting rod is a "T" shaped round rod, and a hand-tightening screw 2 is screwed to the surface of the insert plate, the hand-tightening screw 2 clamps the limiting rod and brakes the insert plate.

[0011] Preferably, the surface of the insert plate is provided with mounting grooves that correspond one-to-one with the traction plate. The two parallel sidewalls of the mounting groove are fixed with a limiting shaft at the bottom. The limiting shaft passes through a through hole on the surface of the traction plate. The two parallel sidewalls of the mounting groove are fixed with rubber clamps at the top. After the traction plate is pushed into the mounting groove, the rubber clamps are clamped between the traction plate and the mounting groove and produce elastic deformation.

[0012] Preferably, the end of the traction plate away from the insert plate has a notch, and the surface of the notch has a slot for inserting the extension plate. One side of the traction plate has a side groove, and a hand-tightening screw is screwed onto the surface of the side groove. The hand-tightening screw clamps the extension plate, and the extension plate has a "T" shaped plate structure.

[0013] Preferably, an arc-shaped groove is provided on one side of the extension plate, and a silicone gasket is fixed on the surface of the groove, with the silicone gasket sandwiched between the extension plate and the distillation beaker.

[0014] Preferably, the surface of the insert plate has two U-shaped storage slots, in which the sampling tube is inserted. Elastic clips are fixed on the two parallel sidewalls of the storage slots, and the elastic clips hold the sampling tube in the storage slots.

[0015] Preferably, the top surface of the oil bath pot is provided with a reserved groove 2, the bottom surface of the reserved groove 2 is provided with a telescopic groove, the support plate is inserted into the telescopic groove, a hand-tightening screw 4 is screwed to one side of the oil bath pot, one end of the hand-tightening screw 4 extends into the telescopic groove to clamp the support plate, the top of the limiting block is provided with a slope groove, and the condenser tube extends into the slope groove.

[0016] Preferably, the limiting block has side grooves on both sides, and a hand-tightening screw is screwed onto the surface of the side groove. One end of the hand-tightening screw extends into the groove, and a rubber block is fixed to one end of the hand-tightening screw. The hand-tightening screw squeezes the rubber block to clamp the condenser tube.

[0017] A method for determining fluorite fluoride content using a constant temperature and humidity water bath device, the method comprising the following steps:

[0018] Weigh 0.2g of the drying reagent into a distillation flask, accurate to ±0.0001g. Place a 500ml plastic beaker under the condenser to collect the distilled solution.

[0019] Add 30 ml of sulfuric acid or 10 ml of perchloric acid to the distillation beaker through the dosing line; add 3 / 5 water and several boiling chips to the steam generator and heat; heat the distillation beaker in an oil bath until the solution temperature reaches 150°C (when using sulfuric acid) or 135°C (when using perchloric acid); distill for 150 min, then disconnect the distillation beaker from the steam generator, stop distillation, and wash the condenser; pour the distillate into a 500 ml volumetric flask, dilute the solution to the mark, and mix well;

[0020] Transfer 100 ml of distillate to a beaker, add 3.5 ml of alizarin sulfonate solution, add sodium hydroxide solution until a pink color appears, add hydrochloric acid solution dropwise until the solution turns yellow, add another 1.5 ml of alizarin sulfonate solution, add 3 ml of buffer solution, and finally add 2 ml of methylene blue solution. At this point, the solution turns green. Titrate with thorium nitrate solution until a blue color appears as the endpoint.

[0021] Preferably, the method further includes: calculating the analytical results to obtain the mass fraction (%) of fluorine according to the formula:

[0022] W(F)%=C Th（NO3)4 * (V3 - V2) * 18.998 * 10 -3 *100 / m1

[0023] In the formula:

[0024] C Th（NO3)4 —The actual concentration of the thorium nitrate standard titration solution, in moles per liter;

[0025] V3—The volume of thorium nitrate standard solution consumed during the titration of the sample solution, in milliliters;

[0026] V2 — The volume of thorium nitrate standard solution consumed during the titration of the blank test solution, in milliliters;

[0027] m1 — Mass of sample transferred, in grams;

[0028] 18.998 — Molar mass of fluorine, in grams per mole.

[0029] Compared with the prior art, the beneficial effects of the present invention are:

[0030] This invention proposes a constant-temperature lifting water bath device and method for determining the fluorine content of fluorite. A slidable insert plate is installed on the top surface of the oil bath, with a traction plate and an extension plate on the insert plate. The extension plate clamps and suspends the distillation beaker above the oil bath. In use, the distillation beaker can be stably clamped by simple operations (loosening the screw, pulling the extension plate, etc.), eliminating the need for additional supports and expanding the functionality of the oil bath. This also avoids the cumbersome process of removing and storing supports, improving the convenience and efficiency of experimental operations. A sampling tube is embedded in the surface of the insert plate, and a storage groove and elastic clamp are provided for storing sampling tubes containing sulfuric acid or perchloric acid. In use, the sampling tube is pushed into the storage groove and held in place by the elastic clamp; when reagents are needed, the sampling tube is simply pulled out of the storage groove, and the reagent is injected into the distillation beaker using a syringe. This design makes reagent storage and retrieval more convenient and safer, facilitating the smooth progress of experiments.

[0031] A sliding support plate is connected to the top of the oil bath, with a fixed limiting block at the top of the support plate to support the condenser tubes. In use, the support plate and limiting block are raised by loosening the hand-tightening screw, pushing the condenser tubes into the groove of the limiting block. The condenser tubes are then gently clamped using the hand-tightening screw and rubber block to prevent breakage. When not in use, the limiting block is pushed down, causing the support plate to insert into the telescopic groove in the oil bath for concealed storage. This design satisfies the requirement for inclined condenser tubes while also providing convenient storage of the support structure, saving space and improving the overall practicality and aesthetics of the equipment. Attached Figure Description

[0032] Figure 1 This is a schematic diagram of the structure of the present invention;

[0033] Figure 2 for Figure 1 Sectional view of the structure at point AA;

[0034] Figure 3 for Figure 2 Enlarged schematic diagram of the structure at point C;

[0035] Figure 4 for Figure 1 Structural cross-section view at point BB;

[0036] Figure 5 This is a schematic diagram of the oil bath structure of the present invention;

[0037] Figure 6 This is a schematic diagram of the traction plate structure of the present invention;

[0038] Figure 7 for Figure 6 Sectional view of the structure at point DD;

[0039] Figure 8This is a schematic diagram of the connection structure between the tray and the limiting block of the present invention;

[0040] Figure 9 This is a schematic diagram of the insert structure of the present invention.

[0041] In the diagram: 1. Oil bath pot, 101. Reserved slot 1, 1011. Limiting rod, 102. Reserved slot 2, 1021. Telescopic slot, 2. Temperature-regulating electric heater, 201. Steam generator bottle, 3. Distillation beaker, 4. Condenser, 5. Plastic beaker, 6. Insert plate, 601. Reserved slot 3, 602. Installation slot, 6021. Limiting shaft, 6022. Rubber clamp, 603. Traction plate, 603. Notched slot, 6031. Slot, 6032. Side slot, 6033. Hand-tightening screw 1, 6034. Extension plate, 604. Clip slot, 6041. Silicone gasket, 6042. Hand-tightening screw 2, 605. Storage slot, 606. Elastic clamp, 6061. Sampling tube, 607. Perforation, 608. Support plate, 701. Limiting block, 7011. Slope groove, 7012. Hand-tightening screw 3, 7013. Hand-tightening screw 4, 7014. Detailed Implementation

[0042] To make the objectives, technical solutions, and advantages of the present invention clear and complete, the embodiments of the present invention will be further described in detail below with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are only some, not all, embodiments of the present invention, and are merely illustrative of the embodiments of the present invention. They are not intended to limit the embodiments of the present invention. All other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0043] Example 1, please refer to Figures 1 to 9 The present invention provides a technical solution: a constant temperature lifting water bath device for determining the fluorine content of fluorite, including an oil bath 1, a distillation beaker 3 above the oil bath 1, one end of the distillation beaker 3 being connected to a steam generator 201 via a hose, the steam generator 201 being installed in a temperature-regulating electric heater 2, the other end of the distillation beaker 3 being connected to a condenser 4 via a hose, the condenser 4 being inclinedly positioned above the oil bath 1, and a plastic beaker 5 being placed at the bottom of the condenser 4.

[0044] To achieve the goal of using an extension plate 604 to clamp and suspend the distillation beaker 3 above the oil bath 1, the following technical features are proposed:

[0045] The top surface of the oil bath 1 is slidably connected to a plug plate 6. The specific installation method adopts the following structure: a pre-reserved groove 101 is opened on the top surface of the oil bath 1; a limit rod 1011 is fixed to the bottom surface of the pre-reserved groove 101; a pre-reserved groove 601 is opened on the top surface of the plug plate 6 for the limit rod 1011 to pass through; the pre-reserved groove 601 is an inverted "T"-shaped circular hole; the limit rod 1011 is a "T"-shaped circular rod; a hand-tightening screw 605 is screwed onto the surface of the plug plate 6; the hand-tightening screw 605 clamps the limit rod 1011. 11 brakes are applied to the insert plate 6; two traction plates 603 are rotatably connected to the surface of the insert plate 6. When the traction plates 603 are housed in the insert plate 6, the following structure is used: the surface of the insert plate 6 has mounting grooves 602 corresponding to the traction plates 603 one-to-one; the two parallel sidewalls of the mounting grooves 602 are fixed with a limiting shaft 6021 at the bottom; the limiting shaft 6021 passes through a through hole 608 on the surface of the traction plates 603; and rubber clamps 60 are fixed at the top of the two parallel sidewalls of the mounting grooves 602. 22. After the traction plate 603 is pushed into the mounting groove 602, the rubber clamp 6022 clamps between the traction plate 603 and the mounting groove 602, causing elastic deformation; a condenser tube 4 is movably inserted into one end of the traction plate 603, and the two condenser tubes 4 clamp the top of the distillation beaker 3; after the extension plate 604 retracts into the traction plate 603, it pushes the traction plate 603 into the insert plate 6, and the insert plate 6 is pushed down and inserted into the oil bath 1 for storage; a notch 6031 is opened at the end of the traction plate 603 away from the insert plate 6, and the surface of the notch 6031... The extension plate 604 is provided with a slot 6032 for insertion. A side groove 6033 is provided on one side of the traction plate 603. A hand screw 6034 is screwed onto the surface of the side groove 6033. The hand screw 6034 clamps the extension plate 604. The extension plate 604 has a "T" shaped plate structure. An arc-shaped buckle groove 6041 is provided on one side of the extension plate 604. A silicone gasket 6042 is fixed on the surface of the buckle groove 6041. The silicone gasket 6042 is clamped between the extension plate 604 and the distillation beaker 3.

[0046] The usage and storage procedures for the power strip 6 are as follows:

[0047] When using insert plate 6, first loosen the second hand screw 605 to release it from clamping the limiting rod 1011, and lift insert plate 6 until the top plate of the limiting rod 1011 overlaps the bottom surface of the reserved slot 601. Then, tighten the second hand screw 605 to clamp the limiting rod 1011. At this point, insert plate 6 is lifted and limited, and will not fall. Then, loosen the first hand screw 6034 to release it from clamping the extension plate 604, and pull the extension plate 604 towards the notch 6031. Move the outer side, then tighten the hand screw 6034 to clamp the condenser tube 4. When both sets of extension plates 604 are extended and braked by the corresponding hand screws 6034, push the top neck of the distillation beaker 3 into the slot 6041 between the two extension plates 604. At this time, the silicone gasket 6042 is clamped between the neck and the slot 6041, preventing the distillation beaker 3 from falling. Under the weight of the distillation beaker 3, the traction plate 603 is in a flat position. When the insert plate 6 is not needed, push the extension plate 604 into the traction plate 603, push the traction plate 603 back into the mounting slot 602, and then push the insert plate 6 down into the reserved slot 101 for storage. In this way, there is no need to specially configure a bracket for clamping the distillation beaker 3, which expands the functionality of the oil bath 1 and avoids the cumbersome process of taking out and storing the bracket.

[0048] The following technical features are proposed for the storage of sulfuric acid or perchloric acid that is required for use:

[0049] The surface of the insert plate 6 is fitted with a sampling tube 607 that contains sulfuric acid or perchloric acid. The surface of the insert plate 6 has two U-shaped storage slots 606. The sampling tube 607 is inserted into the storage slot 606, and elastic clips 6061 are fixed on the two parallel side walls of the storage slot 606. The elastic clips 6061 hold the sampling tube 607 in the storage slot 606.

[0050] The specific procedures for storing and using sulfuric acid or perchloric acid are as follows:

[0051] Prepare two sampling tubes 607 with threaded sealing caps. Put sulfuric acid and perchloric acid into the two sampling tubes 607 respectively. Then push the sampling tubes 607 into the corresponding receiving grooves 606 and clamp them in place by the corresponding elastic clips 6061. When using sulfuric acid or perchloric acid, pull the sampling tubes 607 out of the receiving grooves 606 and use a syringe to draw up the sulfuric acid or perchloric acid. Then inject the sulfuric acid or perchloric acid into the distillation beaker 3.

[0052] To achieve inclined support for the condenser tube 4 and to conceal the support structure, the following technical features are proposed:

[0053] A support plate 7 is slidably connected to the top surface of the oil bath 1. A limiting block 701 is fixed to the top of the support plate 7, and the limiting block 701 supports the condenser tube 4 below. After the condenser tube 4 is pulled away from the limiting block 701, the limiting block 701 is pushed down and inserted into the oil bath 1. This is achieved through the following structure: a reserved groove 102 is opened on the top surface of the oil bath 1, and a telescopic groove 1021 is opened on the bottom surface of the reserved groove 102. The support plate 7 is inserted into the telescopic groove 1021. A hand-tightening screw 7014 is screwed to one side of the oil bath 1. One end of the hand-tightening screw 7014 extends into the telescopic groove 1021 to clamp the support plate 7. The top of the limiting block 701 is provided with a slope groove 7011, and the condenser tube 4 extends into the slope groove 7011. Side grooves 7012 are provided on both sides of the limiting block 701. The surface of the side groove 7012 is screwed with a hand-tightening screw 7013. One end of the hand-tightening screw 7013 extends into the slope groove 7011, and a rubber block is fixed to one end of the hand-tightening screw 7013. The hand-tightening screw 7013 squeezes the rubber block to clamp the condenser tube 4.

[0054] When using the limiting block 701, first loosen the hand screw 7014 to stop clamping the support plate 7, pull the limiting block 701 upward to move the support plate 7 upward, then tighten the hand screw 7014 to clamp the support plate 7, push the condenser tube 4 into the groove 7011, and then tighten the hand screw 7013 to gently clamp the condenser tube 4. Since the end of the hand screw 7013 is equipped with a rubber pad, it will not cause the condenser tube 4 to break during clamping.

[0055] Example 2, based on Example 1, proposes a measurement method, including the following steps:

[0056] Weigh 0.2g of the drying reagent into a distillation flask, accurate to ±0.0001g. Place a 500ml plastic beaker 5 below the condenser 4 to collect the distilled solution.

[0057] Add 30 ml of sulfuric acid (1.84 g / ml) or 10 ml of perchloric acid (1.60 g / ml) to distillation beaker 3 through the dosing pipe; add 3 / 5 water and several boiling stones to steam generator flask 201 and heat; heat distillation beaker 3 using oil bath 1 until the solution temperature reaches 150℃ (when using sulfuric acid) or 135℃ (when using perchloric acid); distill for 150 min, then disconnect distillation beaker 3 from steam generator flask 201, stop distillation, and wash condenser 4; pour the distillate into a 500 ml volumetric flask, dilute the solution to the mark, and mix well;

[0058] Transfer 100 ml of distillate to a beaker, add 3.5 ml of alizarin sulfonate solution, then add sodium hydroxide solution (20 g / L) until a pink color appears. Add hydrochloric acid solution (0.06 mol / L) dropwise until the solution turns yellow. Add another 1.5 ml of alizarin sulfonate solution and 3 ml of buffer solution. Finally, add 2 ml of methylene blue solution. At this point, the solution will be green. Titrate with thorium nitrate solution until a blue color appears as the endpoint.

[0059] The mass fraction (%) of fluorine was calculated using the formula:

[0060] W(F)%=C Th（NO3)4 * (V3 - V2) * 18.998 * 10 -3 *100 / m1

[0061] In the formula:

[0062] C Th（NO3)4 —The actual concentration of the thorium nitrate standard titration solution, in moles per liter;

[0063] V3—The volume of thorium nitrate standard solution consumed during the titration of the sample solution, in milliliters;

[0064] V2 — The volume of thorium nitrate standard solution consumed during the titration of the blank test solution, in milliliters;

[0065] m1 — Mass of sample transferred, in grams;

[0066] 18.998 — Molar mass of fluorine, in grams per mole.

[0067] Example 3, based on Example 2, proposes a method for using a constant temperature and humidity water bath device for determining the fluorine content of fluorite.

[0068] 1. Equipment preparation and installation

[0069] 1) Installation of the insert plate and related components: Loosen the second hand screw 605 so that it no longer clamps the limiting rod 1011. Lift the insert plate 6 until the top plate of the limiting rod 1011 overlaps the bottom surface of the reserved slot 601. Tighten the second hand screw 605 to clamp the limiting rod 1011. At this time, the insert plate 6 is lifted and limited, and will not fall. Extension plate adjustment: Loosen the first hand screw 6034 so that it no longer clamps the extension plate 604. Pull the extension plate 604 outward to the outside of the notch 6031 to the appropriate position. Tighten the first hand screw 6034 back to clamp the extension plate 604. At this time, both sets of extension plates 604 are extended and braked by the corresponding first hand screw 6034. Distillation beaker installation: Push the top neck of distillation beaker 3 into the locking groove 6041 between the two extension plates 604. At this time, the silicone gasket 6042 is clamped between the neck and the locking groove 6041 to prevent distillation beaker 3 from falling. Under the action of its own weight, the traction plate 603 is in a horizontal position.

[0070] 2) Sampling tube preparation: Prepare two sampling tubes 607 with threaded sealing caps. Fill the two sampling tubes 607 with sulfuric acid and perchloric acid respectively. Push the sampling tubes 607 into the corresponding receiving slots 606. The elastic clips 6061 on the two parallel sidewalls of the receiving slots 606 clamp and limit the sampling tubes 607.

[0071] 3) Installation of the support plate and limiting block: Lifting the support plate and limiting block: Loosen the hand screw 7014 so that it no longer clamps the support plate 7. Pull the limiting block 701 upward, moving the support plate 7 upward. Tighten the hand screw 7014 back to clamp the support plate 7. Condenser tube placement: Push the condenser tube 4 into the groove 7011 at the top of the limiting block 701. Tighten the hand screw 7013 so that the rubber block at its end gently clamps the condenser tube 4, avoiding any breakage due to clamping.

[0072] 4) Connection of other components: Connect one end of the distillation beaker 3 to the steam generator 201 via a hose. The steam generator 201 is installed in the temperature-controlled heater 2. Connect the other end of the distillation beaker 3 to the condenser 4 via a hose. The condenser 4 is tilted above the oil bath 1, and the plastic beaker 5 is placed at the bottom of the condenser 4.

[0073] 3. Measurement Procedure

[0074] Reagent Weighing and Placement: Weigh 0.2g of the dried reagent into a distillation flask, accurate to ±0.0001g. Place a 500ml plastic beaker 5 below the condenser 4 to collect the distilled solution.

[0075] Reagent addition: Extract sampling tube 607 containing sulfuric acid (1.84 g / ml) or perchloric acid (1.60 g / ml) from storage tank 606. Aspirate the sulfuric acid or perchloric acid from sampling tube 607 using a syringe, and inject 30 ml of sulfuric acid or 10 ml of perchloric acid into distillation beaker 3.

[0076] Steam generator preparation: Add 3 / 5 water and several boiling stones to steam generator 201 and heat.

[0077] 4. Distillation operation

[0078] Heat distillation beaker 3 using oil bath 1 until the solution temperature reaches 150℃ (when using sulfuric acid) or 135℃ (when using perchloric acid). After distilling for 150 minutes, disconnect distillation beaker 3 from steam generator flask 201 to stop distillation. Wash condenser 4.

[0079] 5. Solution treatment and titration

[0080] Solution dilution: Pour the distillate into a 500ml volumetric flask, dilute to the mark, and mix well. Titration preparation: Transfer 100ml of the distillate to a beaker. Reagent addition: Add 3.5ml of alizarin sulfonate solution. Add sodium hydroxide solution (20g / L) until a pink color appears. Add hydrochloric acid solution (0.06mol / L) dropwise until the solution turns yellow. Add another 1.5ml of alizarin sulfonate solution. Add 3ml of buffer solution. Finally, add 2ml of methylene blue solution; the solution will now turn green. Endpoint determination: Titrate with thorium nitrate solution until a blue color appears as the endpoint.

[0081] 6. Calculation of Analysis Results

[0082] The mass fraction (%) of fluorine is calculated using the formula: W(F)% = C Th（NO3)4 * (V3 - V2) * 18.998 * 10 -3 *100 / m1.

[0083] 7. Equipment storage

[0084] Storage of insert plate and related components: Push the extension plate 604 into the traction plate 603. Push the traction plate 603 back into the mounting slot 602. Push the insert plate 6 down into the reserved slot 101 for storage. Loosen the hand screw 7014 to release the tray 7. Push down the limit block 701 to insert the tray 7 into the telescopic slot 1021 in the reserved slot 102 on the top surface of the oil bath 1. Storage of sampling tube: Push the used sampling tube 607 into the corresponding storage slot 606, where it is held and limited by the elastic clip 6061.

[0085] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A constant temperature lifting water bath device for determining the fluorine content of fluorite, comprising an oil bath (1), a distillation beaker (3) above the oil bath (1), one end of the distillation beaker (3) being connected to a steam generator bottle (201) via a hose, the steam generator bottle (201) being installed in a temperature-regulating electric heater (2), the other end of the distillation beaker (3) being connected to a condenser (4) via a hose, the condenser (4) being inclined above the oil bath (1), and a plastic beaker (5) being placed at the bottom of the condenser (4); Its features are: The top surface of the oil bath (1) is slidably connected to a plate (6), and the surface of the plate (6) is rotatably connected to two traction plates (603). One end of the traction plate (603) is movably inserted with a condenser (4), and the two condenser (4) clamp the top of the distillation beaker (3). After the extension plate (604) retracts into the traction plate (603), the traction plate (603) is pushed into the plate (6), and the plate (6) is pushed down and inserted into the oil bath (1) for storage. The surface of the plate (6) is embedded with a sampling tube (607) that contains sulfuric acid or perchloric acid. A support plate (7) is slidably connected to the top surface of the oil bath (1). A limit block (701) is fixed at the top of the support plate (7). The limit block (701) is supported below the condenser (4). After the condenser (4) is pulled off the limit block (701), the limit block (701) is pushed down and inserted into the oil bath (1).

2. The constant temperature lifting water bath device for determining the fluorine content of fluorite according to claim 1, characterized in that: The top surface of the oil bath pot (1) is provided with a reserved groove 1 (101), and a limit rod (1011) is fixed on the bottom surface of the reserved groove 1 (101). The top surface of the insert plate (6) is provided with a reserved groove 3 (601) for the limit rod (1011) to pass through. The reserved groove 3 (601) is an inverted "T" shaped round hole. The limit rod (1011) is a "T" shaped round rod. The surface of the insert plate (6) is screwed with a hand screw 2 (605). The hand screw 2 (605) clamps the limit rod (1011) and brakes the insert plate (6).

3. The constant temperature lifting water bath device for determining the fluorine content of fluorite according to claim 2, characterized in that: The surface of the insert plate (6) is provided with mounting grooves (602) that correspond one-to-one with the traction plate (603). The two parallel sidewalls of the mounting groove (602) are fixed with a limiting shaft (6021) at the bottom. The limiting shaft (6021) passes through the through hole (608) on the surface of the traction plate (603). The two parallel sidewalls of the mounting groove (602) are fixed with rubber clamps (6022) at the top. After the traction plate (603) is pushed into the mounting groove (602), the rubber clamps (6022) are clamped between the traction plate (603) and the mounting groove (602) and undergo elastic deformation.

4. The constant temperature lifting water bath device for determining the fluorine content of fluorite according to claim 1, characterized in that: The traction plate (603) has a notch (6031) at one end away from the insert plate (6). The surface of the notch (6031) has a slot (6032) for inserting the extension plate (604). The traction plate (603) has a side groove (6033) on one side. A hand screw (6034) is screwed onto the surface of the side groove (6033). The hand screw (6034) clamps the extension plate (604). The extension plate (604) has a "T" shaped plate structure.

5. The constant temperature lifting water bath device for determining the fluorine content of fluorite according to claim 4, characterized in that: An arc-shaped groove (6041) is provided on one side of the extension plate (604), and a silicone gasket (6042) is fixed on the surface of the groove (6041). The silicone gasket (6042) is clamped between the extension plate (604) and the distillation beaker (3).

6. The constant temperature lifting water bath device for determining the fluorine content of fluorite according to claim 1, characterized in that: The surface of the insert plate (6) has two U-shaped storage slots (606). The sampling tube (607) is inserted into the storage slot (606), and elastic clips (6061) are fixed on the two parallel side walls of the storage slot (606). The elastic clips (6061) hold the sampling tube (607) in the storage slot (606).

7. The constant temperature lifting water bath device for determining the fluorine content of fluorite according to claim 1, characterized in that: The top surface of the oil bath (1) is provided with a reserved groove 2 (102), and the bottom surface of the reserved groove 2 (102) is provided with a telescopic groove (1021). The support plate (7) is inserted into the telescopic groove (1021). A hand-tightening screw 4 (7014) is screwed to one side of the oil bath (1). One end of the hand-tightening screw 4 (7014) extends into the telescopic groove (1021) to hold the support plate (7). The top of the limiting block (701) is provided with a slope groove (7011), and the condenser pipe (4) extends into the slope groove (7011).

8. The constant temperature lifting water bath device for determining the fluorine content of fluorite according to claim 7, characterized in that: The limiting block (701) has side grooves (7012) on both sides. A hand-tightening screw (7013) is screwed onto the surface of the side groove (7012). One end of the hand-tightening screw (7013) extends into the slope groove (7011), and a rubber block is fixed to one end of the hand-tightening screw (7013). The hand-tightening screw (7013) squeezes the rubber block to clamp the condenser tube (4).

9. A determination method, using the constant temperature and pressure water bath equipment for determining the fluorite fluorine content according to any one of claims 1-8, characterized in that: The method includes the following steps: Weigh 0.2g of the drying reagent into a distillation flask, accurate to ±0.0001g. Place a 500ml plastic beaker (5) below the condenser (4) to collect the distilled solution. Add 30 ml of sulfuric acid or 10 ml of perchloric acid to the distillation beaker (3) through the dosing pipe; add 3 / 5 water and several boiling stones to the steam generator (201) and heat; heat the distillation beaker (3) using an oil bath (1) until the solution temperature reaches 150℃ (when using sulfuric acid) or 135℃ (when using perchloric acid); distill for 150 min, disconnect the distillation beaker (3) and the steam generator (201), stop the distillation, and wash the condenser (4); pour the distillate into a 500 ml volumetric flask, dilute the solution to the mark, and mix well; Transfer 100 ml of distillate to a beaker, add 3.5 ml of alizarin sulfonate solution, add sodium hydroxide solution until a pink color appears, add hydrochloric acid solution dropwise until the solution turns yellow, add another 1.5 ml of alizarin sulfonate solution, add 3 ml of buffer solution, and finally add 2 ml of methylene blue solution. At this point, the solution turns green. Titrate with thorium nitrate solution until a blue color appears as the endpoint.

10. The determination method according to claim 9, characterized in that: The method further includes: calculating the analytical results and obtaining the mass fraction (%) of fluorine according to the formula: W(F)%=C Th（NO3)4 *(V3-V2)*18.998*10 -3 *100 / m1 In the formula: C Th（NO3)4 —The actual concentration of the thorium nitrate standard titration solution, in moles per liter; V3—The volume of thorium nitrate standard solution consumed during the titration of the sample solution, in milliliters; V2 — The volume of thorium nitrate standard solution consumed during the titration of the blank test solution, in milliliters; m1 — Mass of sample transferred, in grams; 18.998 — Molar mass of fluorine, in grams per mole.

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