Method for detecting tin content in rutile
The detection of the tin content in rutile by alkali melting method and inductively coupled plasma emission spectrometry solves the problem of lack of detection methods in the prior art, and achieves rapid and efficient tin content determination and personnel safety protection.
Patent Information
- Application Number
- CN202510501813.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-21
- Publication Date
- 2025-07-15
AI Technical Summary
The prior art lacks an effective detection method for tin content in rutile, which affects the impurity removal process of sponge titanium production.
The alkali melting method was used to use a nickel crucible container combined with inductively coupled plasma emission spectrometry. The samples were melted at high temperature and leaching with mixed solution of sulfate hydrochloric acid to prepare a standard solution and the content of tin element was detected.
The pre-test treatment time is shortened, the content of tin in rutile is quickly and efficiently determined, and reliable technical support is provided for the production of high-quality titanium sponge, and the prevention of scalding by automated equipment.
Smart Images
Figure CN120314286A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of tin element detection, and specifically to a method for detecting the tin content in rutile. Background Art
[0002] The production of titanium sponge is a process of reducing and purifying titanium from raw materials. Effective impurity removal is the key to ensuring its quality. As one of the important raw materials for producing titanium sponge, accurately judging its impurity components and content is crucial. Research shows that the impurity tin element in titanium sponge mainly comes from rutile. Therefore, determining the tin content in rutile can provide a reliable reference basis for the impurity removal process of titanium sponge.
[0003] However, there is no analysis method for tin in the chemical analysis methods for high-titanium slag and rutile YS / T 514-2009. Other relevant standards for detecting the tin content in rutile do not mention it either.
[0004] Therefore, in view of this, research and improvement are carried out on the existing structure and deficiencies, and a method for detecting the tin content in rutile is proposed. Summary of the Invention
[0005] Aiming at the deficiencies of the prior art, the present invention provides a method for detecting the tin content in rutile, and solves the problems raised in the above background art.
[0006] To achieve the above purposes, the present invention is realized through the following technical solutions: A method for detecting the tin content in rutile, the method for detecting the tin content in rutile includes the following steps: S1: Mix the sample rutile with sodium peroxide and sodium hydroxide, place them in a nickel crucible, and melt them at high temperature in a muffle furnace; S2: Leach the melted sample with a mixed solution of sulfuric acid and hydrochloric acid and make it constant volume to obtain a sample solution to be measured; S3: Use an inductively coupled plasma emission spectrometer to detect the content of tin element.
[0007] Further, in the step S1, 0.1 g is weighed from the sample rutile and placed in a nickel crucible, and then 0.7 - 1.0 g of sodium peroxide and 0.3 - 0.5 g of sodium hydroxide are added and mixed evenly.
[0008] Further, in the step S2, the melted sample cooled to room temperature together with the nickel crucible is put into a beaker, 20 - 40 mL of water is added and heated; then 2 - 3 mL of sulfuric acid with a concentration of 50% and 45 - 55 mL of hydrochloric acid with a concentration of 50% are added, and the crucible is taken out after heating until the inner wall of the nickel crucible is clean; continue to heat the solution until it is clarified, cool it to room temperature and transfer it to a 200 mL volumetric flask for constant volume and mixing to obtain a sample solution to be measured.
[0009] Furthermore, in step S3, an inductively coupled plasma optical emission spectrometer is used to detect the content of tin element. Standard solutions with different concentrations are prepared according to the tin element content in rutile to draw a curve. The prepared tin concentrations are 0.00 mg / L, 0.1 mg / L, 0.5 mg / L, and 1 mg / L. The operating conditions of the inductively coupled plasma optical emission spectrometer are: RF power 1150 W, pump speed 50 r / min, auxiliary gas flow rate 0.5 L / min, and the wavelength of tin is 189.989 nm.
[0010] Furthermore, a muffle furnace is applied in the detection method of the tin content in rutile. The muffle furnace includes a furnace body. One side of the furnace body is hinged with a furnace door, and a heating chamber is opened inside the furnace body.
[0011] Furthermore, an automatic feeding and discharging component is arranged inside the heating chamber. The automatic feeding and discharging component includes a lifting guide rail, a spring telescopic rod, and a sliding rod. A spring telescopic rod is fixed on the outer side of the lifting guide rail, and a sliding rod is fixed at the end of the spring telescopic rod.
[0012] Furthermore, the sliding rod is slidably connected inside the lifting guide rail, and an elastic structure is formed between the sliding rod and the lifting guide rail through the spring telescopic rod.
[0013] Furthermore, the automatic feeding and discharging component further includes a tray. A tray is fixed in the middle of the sliding rod, and the surface of the tray is used to carry a nickel crucible.
[0014] Furthermore, the automatic feeding and discharging component further includes a vertical traction rod, a traction rope, and a steering wheel. A vertical traction rod is fixed at the end of the sliding rod, and a traction rope is connected to the bottom of the vertical traction rod. One end of the traction rope away from the vertical traction rod is connected to the inner side surface of the furnace door. A steering wheel is rotatably connected to the bottom inner wall of the heating chamber, and a traction rope is wound around the surface of the steering wheel.
[0015] Furthermore, a thermal sensor is embedded inside the tray. A camera is connected to the outer side surface of the furnace body through a damping rotating shaft, and a prompting sounder is arranged on the top of the furnace body.
[0016] The present invention provides a detection method for the tin content in rutile, having the following beneficial effects: 1. For the detection method of the tin content in rutile, by using a nickel crucible as a container for melting with an alkali flux, the pre-treatment time before detection can be shortened, and combined with the inductively coupled plasma optical emission spectrometry, the tin content in rutile can be quickly and efficiently determined, providing reliable technical support for the production of high-quality sponge titanium.
[0017] 2. Detection method for tin content in rutile. When the furnace door is opened, the rotational force is converted into a tensile force through a traction rope. Thus, when the furnace door is opened, the traction rope pulls the sliding rod, causing the nickel crucible carried by the sliding rod to extend outward together with the sliding rod, so that the nickel crucible automatically moves outside the heating chamber to facilitate the natural cooling of the nickel crucible at room temperature. At the same time, the nickel crucible is placed under the monitoring of a camera, and the temperature of the nickel crucible is monitored in real time by a thermal sensor inside the tray, and a warning sound gives an alarm and a prompt to the person approaching the nickel crucible in a high-temperature state by hand in time to prevent scalding of the person. BRIEF DESCRIPTION OF THE DRAWINGS
[0018] Figure 1 It is a schematic flow chart of a detection method for tin content in rutile according to the present invention; Figure 2 It is a schematic preparation flow chart of a test sample solution for a detection method for tin content in rutile according to the present invention; Figure 3 It is a schematic structural diagram after the tray slides out for a detection method for tin content in rutile according to the present invention; Figure 4 It is a schematic structural diagram when the tray is inside the heating chamber for a detection method for tin content in rutile according to the present invention; Figure 5 It is a schematic bottom structure diagram of the elevation guide rail for a detection method for tin content in rutile according to the present invention; Figure 6 It is a schematic bottom structure diagram of the sliding rod for a detection method for tin content in rutile according to the present invention.
[0019] In the figure: 1, furnace body; 2, furnace door; 3, heating chamber; 4, automatic feeding and discharging assembly; 401, elevation guide rail; 402, spring telescopic rod; 403, sliding rod; 404, tray; 405, vertical traction rod; 406, traction rope; 407, steering wheel; 5, camera; 6, warning sound. DETAILED DESCRIPTION OF THE EMBODIMENTS
[0020] The following further describes in detail the embodiments of the present invention in conjunction with the drawings and embodiments. The following embodiments are used to illustrate the present invention, but cannot be used to limit the scope of the present invention.
[0021] As Figures 1 - 2 shown, the present invention provides a technical solution: a detection method for tin content in rutile. The detection method for tin content in rutile includes the following steps: S1: Mix the sample rutile with sodium peroxide and sodium hydroxide, and place them in a nickel crucible, and melt them at a high temperature in a muffle furnace; Specifically, weigh 0.1 g from the sample rutile and place it in a nickel crucible, and then add 0.7 - 1.0 g of sodium peroxide and 0.3 - 0.5 g of sodium hydroxide and mix well; S2: The melted sample is leached with a mixed solution of sulfuric acid and hydrochloric acid and made up to a fixed volume to obtain a sample solution to be measured. Specifically, the melted sample cooled to room temperature together with the nickel crucible is placed in a beaker, 20 - 40 mL of water is added and heated. Subsequently, 2 - 3 mL of sulfuric acid with a concentration of 50% and 45 - 55 mL of hydrochloric acid with a concentration of 50% are added, and the crucible is taken out after heating until the inner wall of the nickel crucible is clean. The solution is continuously heated until it is clarified, cooled to room temperature and then transferred to a 200 mL volumetric flask to make up to the mark and mixed evenly to obtain the sample solution to be measured. S3: The content of tin element is detected by an inductively coupled plasma emission spectrometer. Specifically, the content of tin element is detected by an inductively coupled plasma emission spectrometer. Standard solutions with different concentrations are prepared according to the tin element content in rutile to draw a curve. The prepared tin concentrations are 0.00 mg / L, 0.1 mg / L, 0.5 mg / L, 1 mg / L, and the working conditions of the inductively coupled plasma emission spectrometer are: RF power 1150 W, pump speed 50 r / min, auxiliary gas flow rate 0.5 L / min, and the wavelength used for tin is 189.989 nm.
[0022] Based on the above description, the present invention uses a nickel crucible as a container through alkali flux melting, which can shorten the pretreatment time before detection, and combines inductively coupled plasma emission spectrometry to quickly and efficiently determine the content of tin in rutile, providing reliable technical support for the production of high-quality sponge titanium.
[0023] Such as Figures 3 - 6As shown in the figure, a muffle furnace is used in the detection method of tin content in rutile. The muffle furnace includes a furnace body 1. One side of the furnace body 1 is hinged with a furnace door 2. And a heating chamber 3 is provided inside the furnace body 1. An automatic feeding and discharging component 4 is arranged inside the heating chamber 3. The automatic feeding and discharging component 4 includes a lifting guide rail 401, a spring telescopic rod 402 and a sliding rod 403. The spring telescopic rod 402 is fixed on the outer side of the lifting guide rail 401. And a sliding rod 403 is fixed at the end of the spring telescopic rod 402. The sliding rod 403 is slidably connected inside the lifting guide rail 401. And an elastic structure is formed between the sliding rod 403 and the lifting guide rail 401 through the spring telescopic rod 402. The automatic feeding and discharging component 4 further includes a tray 404. The middle of the sliding rod 403 is fixed with the tray 404. And the surface of the tray 404 is used for carrying a nickel crucible. The automatic feeding and discharging component 4 further includes a vertical traction rod 405, a traction rope 406 and a steering wheel 407. The end of the sliding rod 403 is fixed with the vertical traction rod 405. And a traction rope 406 is connected to the bottom of the vertical traction rod 405. And one end of the traction rope 406 away from the vertical traction rod 405 is connected to the inner side surface of the furnace door 2. A steering wheel 407 is rotatably connected to the bottom inner wall of the heating chamber 3. And the traction rope 406 is wound around the surface of the steering wheel 407. A thermal sensor is embedded inside the tray 404. The outer side surface of the furnace body 1 is connected with a camera 5 through a damping rotating shaft. And a prompting sounder 6 is arranged on the top of the furnace body 1; The specific operation is as follows. After the nickel crucible is loaded with the mixed solution, it is placed on the surface of the tray 404 and sent into the heating chamber 3. Then the furnace door 2 is closed and heated according to the preset temperature. When taking out the nickel crucible, first open the furnace door 2. At this time, the traction rope 406 is pulled outwards by the rotating force of the furnace door 2. The traction rope 406 applies a pulling force to the sliding rod 403 through the steering wheel 407. The sliding rod 403 slides outwards along the inside of the lifting guide rail 401. Thus, while opening the furnace door 2, the rotating force is converted into a pulling force by the traction rope 406, so that the tray 404 drives the nickel crucible to extend out together with the sliding rod 403, making the nickel crucible automatically move outside the heating chamber 3 to facilitate the natural cooling of the nickel crucible in a room temperature environment. Among them, the traction rope 406 is a high-temperature resistant steel wire rope. And the furnace door 2 has a self-locking structure and enters the self-locking state after it is opened and rotated by 90 degrees; While the sliding rod 403 slides outwards along the inside of the lifting guide rail 401, the spring telescopic rod 402 is forced to extend. At this time, the spring inside the spring telescopic rod 402 enters the compression energy storage state. When the nickel crucible is manually removed and the furnace door 2 is closed, the traction rope 406 becomes slack and loses the pulling force provided to the sliding rod 403. At the same time, the spring telescopic rod 402 releases the stored energy and automatically contracts. Thus, the sliding rod 403 automatically slides back and resets along the inside of the lifting guide rail 401 so that the furnace door 2 can be closed. Among them, the shell of the spring telescopic rod 402 is made of high-temperature resistant and heat-insulating high-temperature ceramic fiber; Moreover, when the tray 404 carries the nickel crucible and moves outside the heating chamber 3 for natural cooling, the camera 5 captures the real-time images of the tray 404 and its surrounding area, and the temperature of the nickel crucible is monitored in real time through the thermal sensor inside the tray 404. If a person approaches the nickel crucible by hand and the temperature of the nickel crucible has not cooled down to a temperature at which it can be picked up by hand, the warning sound 6 will issue an alarm and a prompt, thereby preventing the person from picking up the nickel crucible at a high temperature by hand and causing burns. If the temperature of the nickel crucible has cooled to the preset temperature, the warning sound 6 will issue a voice prompt to prompt the person to pick it up in time. Among them, if the preset temperature is higher than the temperature required for picking up by hand and a person approaches the nickel crucible by hand, the warning sound 6 will also issue an alarm; Based on the above description, when the furnace door 2 is opened, the rotational force of the present invention is converted into a pulling force by the traction rope 406. Thus, when the furnace door 2 is opened, the traction rope 406 pulls the sliding rod 403 so that it carries the nickel crucible and extends outward together with the sliding rod 403, enabling the nickel crucible to automatically move outside the heating chamber 3 to facilitate the natural cooling of the nickel crucible in a room temperature environment. At the same time, the nickel crucible is placed under the monitoring of the camera 5, and the temperature of the nickel crucible is monitored in real time through the thermal sensor inside the tray 404, and the warning sound 6 issues an alarm and a prompt to the person who approaches the nickel crucible at a high temperature by hand in time to prevent the person from being scalded.
[0024] In summary, for the detection method of tin content in rutile, when in use, first weigh 0.1 g from the sample rutile and place it in a nickel crucible, then add 0.7 - 1.0 g of sodium peroxide and 0.3 - 0.5 g of sodium hydroxide and mix evenly, and then place the nickel crucible in a muffle furnace for high-temperature melting; Put the molten sample cooled to room temperature together with the nickel crucible into a beaker, add 20 - 40 mL of water and heat it; then add 2 - 3 mL of sulfuric acid with a concentration of 50% and 45 - 55 mL of hydrochloric acid with a concentration of 50%, heat until the inner wall of the nickel crucible is clean and then take out the crucible; continue to heat the solution until it is clarified, cool it to room temperature and then transfer it to a 200 mL volumetric flask for volume fixing, mix evenly to obtain the sample solution to be measured; Use an inductively coupled plasma emission spectrometer to detect the content of tin element, draw a curve according to the standard solutions with different concentrations prepared according to the tin element content in rutile. The prepared tin concentrations are 0.00 mg / L, 0.1 mg / L, 0.5 mg / L, 1 mg / L, and the working conditions of the inductively coupled plasma emission spectrometer are: RF power 1150 W, pump speed 50 r / min, auxiliary gas flow rate 0.5 L / min, and the wavelength adopted for tin is 189.989 nm; Among them, when taking out the nickel crucible from the muffle furnace, first open the furnace door 2. At this time, use the rotational force of the furnace door 2 to pull the traction rope 406 outward. The traction rope 406 applies a pulling force to the sliding rod 403 through the steering wheel 407. The sliding rod 403 slides outward along the inside of the elevation guide rail 401. Thus, while opening the furnace door 2, use the traction rope 406 to convert the rotational force into a pulling force, so that the tray 404 carries the nickel crucible and extends outward together with the sliding rod 403, making the nickel crucible automatically move outside the heating chamber 3 to facilitate the natural cooling of the nickel crucible at room temperature. Among them, the traction rope 406 is a high-temperature resistant steel wire rope, and the furnace door 2 has a self-locking structure and enters the self-locking state after it is opened and rotated by 90 degrees; While the sliding rod 403 slides and extends along the inside of the elevation guide rail 401, the spring telescopic rod 402 is forced to extend. At this time, the spring inside the spring telescopic rod 402 enters the compressed energy storage state. When the nickel crucible is manually removed and the furnace door 2 is closed, the traction rope 406 becomes slack and loses the pulling force provided to the sliding rod 403. At the same time, the spring telescopic rod 402 releases the stored energy and automatically contracts. Thus, the sliding rod 403 automatically slides back and resets along the inside of the elevation guide rail 401 so that the furnace door 2 can be closed; Moreover, when the tray 404 carries the nickel crucible and moves outside the heating chamber 3 for natural cooling, the camera 5 captures the real-time images of the tray 404 and its surrounding area, and the thermal sensor inside the tray 404 monitors the temperature of the nickel crucible in real time. If there is a situation where someone approaches the nickel crucible by hand and the temperature of the nickel crucible has not cooled down to a temperature at which it can be picked up by hand, the warning sound 6 issues an alarm and a prompt. Thus, it prevents people from picking up the nickel crucible in a high-temperature state by hand and causing burns. If the temperature of the nickel crucible has cooled to the preset temperature, the warning sound 6 issues a voice prompt to prompt the person to pick it up in time. Among them, if the preset temperature is higher than the temperature required for picking up by hand and there is a situation where someone approaches the nickel crucible by hand, the warning sound 6 also issues an alarm.
[0025] The embodiments of the present invention are given for purposes of illustration and description, and are not exhaustive or limit the present invention to the disclosed form. Many modifications and variations are obvious to those of ordinary skill in the art. The embodiments are selected and described to better illustrate the principles and practical applications of the present invention, and to enable those of ordinary skill in the art to understand the present invention and thus design various embodiments with various modifications suitable for specific purposes.
Claims
1. A method for detecting the tin content in rutile, characterized in that: The method for detecting the tin content in rutile includes the following steps: S1: Mix the sample rutile with sodium peroxide and sodium hydroxide, then place them in a nickel crucible and melt them at high temperature in a muffle furnace; S2: Leach the melted sample with a mixed solution of sulfuric acid and hydrochloric acid and make up the volume to obtain a sample solution to be measured; S3: Detect the content of tin element by using an inductively coupled plasma emission spectrometer.
2. The detection method of tin content in rutile according to claim 1, wherein: In step S1, weigh 0.1 g from the sample rutile and place it in a nickel crucible, then add 0.7 - 1.0 g of sodium peroxide and 0.3 - 0.5 g of sodium hydroxide and mix well.
3. The detection method of tin content in rutile according to claim 1, characterized in that: In step S2, put the melted sample cooled to room temperature together with the nickel crucible into a beaker, add 20 - 40 mL of water and heat it; then add 2 - 3 mL of sulfuric acid with a concentration of 50% and 45 - 55 mL of hydrochloric acid with a concentration of 50%, heat until the inner wall of the nickel crucible is clean and then take out the crucible; continue to heat the solution until it is clear, cool it to room temperature and transfer it to a 200 mL volumetric flask to make up the volume, mix well to obtain a sample solution to be measured.
4. The detection method of tin content in rutile according to claim 1, characterized in that: In step S3, detect the content of tin element by using an inductively coupled plasma emission spectrometer, draw a curve according to the standard solutions with different concentrations configured for the tin content in rutile, and the configured tin concentrations are 0.00 mg / L, 0.1 mg / L, 0.5 mg / L, 1 mg / L, and the working conditions of the inductively coupled plasma emission spectrometer are: RF power 1150 W, pump speed 50 r / min, auxiliary gas flow rate 0.5 L / min, and the wavelength adopted for tin is 189.989 nm.
5. The detection method of tin content in rutile according to claim 1, characterized in that: The method for detecting the tin content in rutile uses a muffle furnace, and the muffle furnace includes a furnace body (1), one side of the furnace body (1) is hinged with a furnace door (2), and a heating chamber (3) is opened inside the furnace body (1).
6. The detection method of tin content in rutile according to claim 5, characterized in that: An automatic feeding and discharging assembly (4) is arranged inside the heating chamber (3), and the automatic feeding and discharging assembly (4) includes a lifting guide rail (401), a spring telescopic rod (402) and a sliding rod (403). A spring telescopic rod (402) is fixed on the outer side of the lifting guide rail (401), and a sliding rod (403) is fixed at the end of the spring telescopic rod (402).
7. The detection method of tin content in rutile according to claim 6, characterized in that: The sliding rod (403) is slidably connected to the inside of the lifting guide rail (401), and an elastic structure is formed between the sliding rod (403) and the lifting guide rail (401) through the spring telescopic rod (402).
8. The detection method of tin content in rutile according to claim 6, characterized in that: The automatic feeding and discharging assembly (4) further includes a tray (404), a tray (404) is fixed in the middle of the sliding rod (403), and the surface of the tray (404) is used to carry the nickel crucible.
9. The detection method of tin content in rutile according to claim 6, characterized in that: The automatic feeding and discharging assembly (4) further includes a vertical traction rod (405), a traction rope (406) and a steering wheel (407). A vertical traction rod (405) is fixed at the end of the sliding rod (403), and a traction rope (406) is connected to the bottom of the vertical traction rod (405). One end of the traction rope (406) far from the vertical traction rod (405) is connected to the inner side surface of the furnace door (2). A steering wheel (407) is rotatably connected to the bottom inner wall of the heating chamber (3), and the traction rope (406) is wound around the surface of the steering wheel (407).
10. The detection method of tin content in rutile according to claim 8, wherein: A thermal sensor is embedded inside the tray (404), a camera (5) is connected to the outer side surface of the furnace body (1) through a damping rotating shaft, and a prompting sound device (6) is arranged at the top of the furnace body (1).