A heat digestion treatment device for elemental speciation
By using heat transfer oil as the heat transfer medium in the thermal digestion treatment device, and by improving the heating temperature and uniformity through circulation pipes and liquid circulation devices, the problem of low temperature in hot water digestion method is solved, and efficient element form and valence state transformation is achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- CHINA UNIV OF GEOSCIENCES (WUHAN)
- Filing Date
- 2025-07-08
- Publication Date
- 2026-06-23
Smart Images

Figure CN224399098U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of analytical testing technology, and in particular to a thermal digestion treatment device for elemental valence state transformation. Background Technology
[0002] Currently, the most commonly used technique in the field of elemental speciation analysis is high-performance liquid chromatography-atomic fluorescence spectrometry (HPLC-HG-AFS). Due to the limitations of the HG-AFS testing principle, all analytes need to be converted into an elemental valence state that can chemically react with sodium borohydride / potassium borohydride to produce hydrides before entering the AFS detector. Therefore, an online digestion-reduction system needs to be installed at the instrument connection port. The purpose of this system is to oxidize and reduce high-valence elements or large organic molecules that cannot react to produce hydrides in the online manner using digestion and reducing agents to convert them into suitable low-valence elements and small organic molecules before introducing them into the AFS stage for hydride generation, separation, and detection.
[0003] Existing digestion methods mainly fall into three categories: microwave digestion, hot water digestion, and ultraviolet (UV) lamp digestion. Microwave digestion and hot water digestion are thermal digestion methods. Hot water digestion is more commonly used due to its convenience. It utilizes a constant-temperature water bath to accelerate the online digestion or reduction reaction of the sample solution. However, since the boiling point of water is 100℃, the maximum temperature of the water bath is also 100℃. This relatively low temperature leads to practical problems such as increased reaction time and chromatographic broadening. Utility Model Content
[0004] This invention provides a thermal digestion treatment device for elemental valence state transformation, which solves the problems of low digestion heating temperature and long reaction time in the prior art.
[0005] This utility model provides a thermal digestion treatment device for elemental valence state transformation, including a shell, a digestion tank, a buffer tank, a reaction pipeline, a circulation pipeline, a liquid circulation device, and a heating device. The digestion tank and the buffer tank are each provided with an oil-containing cavity. The digestion tank and the buffer tank are installed inside the shell. The heating device is installed inside the oil-containing cavity. The reaction pipeline is located inside the digestion tank. At least two circulation pipelines are provided, one end of which is connected to the oil-containing cavity of the digestion tank, and the other end of which is connected to the oil-containing cavity of the buffer tank. The liquid circulation device is connected to any one of the circulation pipelines to drive the liquid to circulate between the digestion tank and the buffer tank.
[0006] Furthermore, the reaction pipeline includes a pipeline support and a spiral reaction tube disposed within the pipeline support, wherein the spiral reaction tube has a reaction liquid inlet and a reaction liquid outlet extending out of the pipeline support at both ends.
[0007] Furthermore, the top of the shell is provided with an installation port, which is positioned opposite to the digestion tank. A movable cover plate is installed on the installation port, and the movable cover plate is provided with an upper cover hole for the reaction liquid inlet and the reaction liquid outlet to extend out.
[0008] Furthermore, the pipeline support is fixedly connected inside the digestion tank, and the sidewall of the pipeline support has a hollow structure.
[0009] Furthermore, the liquid circulation device includes a circulation pump.
[0010] Furthermore, the liquid circulation device includes a liquid delivery wheel and a motor that drives the liquid delivery wheel to rotate, the liquid delivery wheel being rotatably connected inside the circulation pipe.
[0011] Furthermore, a liquid addition pipe is provided at the top of the digestion tank and / or the buffer tank, and a liquid outlet pipe is provided at the bottom of the digestion tank and / or the buffer tank. The liquid addition pipe and the liquid outlet pipe are respectively connected to the oil-containing cavity, and control valves are respectively connected to the liquid addition pipe and the liquid outlet pipe.
[0012] Furthermore, the digestion tank and the buffer tank are fixedly connected to the outer wall of the digestion tank and the buffer tank by a plurality of fixed support legs located at the bottom of the digestion tank and the buffer tank.
[0013] Furthermore, the circulation pipeline is configured as a flexible hose, and a handle is fixedly connected to the outer wall of the digestion tank.
[0014] Furthermore, it also includes a controller and a temperature sensor, the temperature sensor being disposed within the digestion tank, and the liquid circulation device, the temperature sensor, and the heating device being connected to the controller respectively.
[0015] The beneficial effects of this utility model's thermal digestion treatment device for elemental valence state transitions are as follows: By setting up an oil-containing chamber to hold heat-conducting oil and using the heat-conducting oil as a heat transfer medium to heat the reaction pipeline, the heating temperature is increased, resulting in strong digestion capacity, fast digestion speed, high peak separation, and solving the problem of spectral line broadening. Furthermore, it is radiation-free and environmentally friendly. On the other hand, by setting up a buffer tank and connecting it to the digestion tank through a circulation pipe, a liquid circulation device drives the heat-conducting oil to circulate between the buffer tank and the digestion tank, thereby making the temperature rise of the heat-conducting oil more stable during heating. Attached Figure Description
[0016] Figure 1 This is a schematic diagram of the overall structure of an embodiment of this utility model.
[0017] Figure 2 This is a schematic diagram of the internal structure of an embodiment of this utility model.
[0018] Figure 3This is a schematic diagram of the pipe support structure according to an embodiment of the present invention.
[0019] Figure label:
[0020] 1. Housing; 11. Mounting port; 12. Movable cover plate; 121. Cover hole; 13. Liquid outlet hole; 14. Support leg fixing hole; 2. Digestion tank; 21. Oil chamber; 22. Liquid filling pipe; 23. Handle; 3. Buffer tank; 31. Liquid outlet pipe; 32. Control valve; 4. Reaction pipeline; 41. Pipeline support; 42. Spiral reaction tube; 421. Reaction liquid inlet; 422. Reaction liquid outlet; 5. Circulation pipeline; 6. Liquid circulation device; 61. Liquid delivery wheel; 62. Motor; 63. Rotating belt; 7. Heating device; 8. Fixed support leg; 9. Controller; 91. Temperature sensor; 92. CNC box; 93. Electrical wire. Detailed Implementation
[0021] To make the objectives, technical solutions, and advantages of this utility model clearer, the technical solutions of this utility model will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this utility model, not all embodiments. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this utility model.
[0022] The terms "first" and "second" in the specification and claims of this utility model may explicitly or implicitly include one or more of the features. In the description of this utility model, unless otherwise stated, "multiple" means two or more. Furthermore, in the specification and claims, "and / or" indicates at least one of the connected objects, and the character " / " generally indicates that the preceding and following objects are in an "or" relationship.
[0023] In the description of this utility model, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the accompanying drawings, and are only for the convenience of describing this utility model and simplifying the description, and are not intended to indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this utility model.
[0024] The following is combined with Figures 1-3This invention describes a thermal digestion treatment device for elemental valence state transformation.
[0025] The thermal digestion treatment device for elemental valence state transformation provided by this utility model includes a shell 1, a digestion tank 2, a buffer tank 3, a reaction pipeline 4, a circulation pipeline 5, a liquid circulation device 6, and a heating device 7. An oil-containing cavity 21 is provided inside the digestion tank 2 and the buffer tank 3. The digestion tank 2 and the buffer tank 3 are installed inside the shell 1. The heating device 7 is installed inside the oil-containing cavity 21. The reaction pipeline 4 is located inside the digestion tank 2. At least two circulation pipelines 5 are provided. One end of the circulation pipeline 5 is connected to the oil-containing cavity 21 of the digestion tank 2, and the other end of the circulation pipeline 5 is connected to the oil-containing cavity 21 of the buffer tank 3. The liquid circulation device 6 is connected to any one of the circulation pipelines 5 to drive the liquid to circulate between the digestion tank 2 and the buffer tank 3.
[0026] Specifically, such as Figure 1 As shown, digestion tank 2 and buffer tank 3 are disposed within shell 1, and two circulation pipes 5 are provided. One end of each circulation pipe 5 is connected to the oil-containing chamber 21 of digestion tank 2, and the other end is connected to the oil-containing chamber 21 of buffer tank 3. Heat transfer oil is placed in the oil-containing chamber 21, and the heat transfer oil is driven to circulate between buffer tank 3 and digestion tank 2 by the liquid circulation device 6 on the circulation pipes 5. A heating device 7 is installed in the oil-containing chamber 21 of digestion tank 2, or alternatively, in the oil-containing chamber 21 of buffer tank 3, or simultaneously in the oil-containing chambers 21 of both digestion tank 2 and buffer tank 3.
[0027] Specifically, heat transfer oils with high flash points and low viscosity are preferred, with a flash point above 250℃, such as methyl silicone oil, phenyl silicone oil, olive oil, and cottonseed oil. Their advantages include high melting and boiling points, high digestion temperatures, uniform heating, long service life, non-toxicity, ozone resistance, light resistance, aging resistance, and high insulation. This solves the practical difficulty of achieving hot water digestion temperatures below 100℃, significantly improving digestion efficiency and speed.
[0028] When using the thermal digestion device, the reaction liquid sample is placed in the reaction pipeline 4, which extends into the heat transfer oil. The heating device 7 heats the heat transfer oil. The liquid circulation device 6 is activated, driving the heat transfer oil to flow within the circulation pipe 5, thus circulating the heat transfer oil between the digestion tank 2 and the buffer tank 3, resulting in a more uniform and stable temperature rise of the heat transfer oil. The high-temperature heat transfer oil heats the reaction pipeline 4, thereby providing energy for the digestion reaction of the reaction liquid sample within the reaction pipeline 4.
[0029] In an optional embodiment, the sidewalls of the digestion tank 2 and the buffer tank 3 are made of high-temperature resistant, acid and alkali resistant polytetrafluoroethylene or stainless steel, with a thickness greater than 3 mm. The digestion tank 2 and the buffer tank 3 can be cylindrical or cuboid in shape. The shell 1 is made of stainless steel or polymer material and is cuboid or cylindrical.
[0030] In an optional embodiment, an electric heating tube is used as the heating device 7. The electric heating tube is embedded and fixed in the digestion tank 2 and close to the inner wall edge of the digestion tank 2, without contacting the reaction pipeline 4. When energized, it heats the heat transfer liquid.
[0031] Furthermore, the reaction pipeline 4 includes a pipeline support 41 and a spiral reaction tube 42 disposed within the pipeline support 41. The spiral reaction tube 42 has a reaction liquid inlet 421 and a reaction liquid outlet 422 extending out of the pipeline support 41 at both ends.
[0032] Specifically, such as Figure 2 As shown, the pipeline support 41 is installed inside the oil-containing cavity 21 of the digestion tank 2. The spiral reaction tube 42 is placed inside the pipeline support 41, which positions the spiral reaction tube 42 to ensure it is completely submerged in the digestion tank 2. The reaction solution sample undergoes a chemical reaction inside the spiral reaction tube 42. The reaction solution sample is placed inside the spiral reaction tube 42, which extends into the heat transfer oil, increasing the contact area and improving the heating effect on the reaction solution sample. The reaction solution inlet 421 is connected to other sample pretreatment equipment; the reaction solution outlet 422 is connected to the downstream detection equipment.
[0033] In an optional embodiment, the pipe support 41 and the spiral reaction tube 42 are made of a high-temperature resistant and acid / alkali resistant polymer material, such as polytetrafluoroethylene or quartz. The reaction liquid inlet 421 and the reaction liquid outlet 422 are interchangeable, with an inner diameter of 0.1-2.0 mm. The spiral reaction tube 42 has an inner diameter of 0.1-2.0 mm, a length of 50-2000 cm, and an outer diameter of 10-50 mm. The required length and diameter of the spiral reaction tube 42 can be selected according to the properties of the reaction solution and the testing requirements.
[0034] Furthermore, the top of the shell 1 is provided with an installation port 11, which is positioned opposite to the digestion tank 2. A movable cover plate 12 is installed on the installation port 11, and the movable cover plate 12 is provided with an upper cover hole 121 for the reaction liquid inlet 421 and the reaction liquid outlet 422 to extend out.
[0035] Specifically, such as Figure 2As shown, a movable cover plate 12 is installed on the mounting port 11. The movable cover plate 12 is movably connected to the mounting port 11 and is used for inspection and maintenance of the internal structure. The movable cover plate 12 has a top cover hole 121 in the middle, with a diameter of 10-50 mm, allowing the reaction liquid inlet 421 and reaction liquid outlet 422 to pass through. In an optional embodiment, the movable cover plate 12 is made of a transparent material, such as glass or transparent plastic, allowing observation of the reaction in the spiral reaction tube 42 through the movable cover plate 12.
[0036] Furthermore, the pipeline support 41 is fixedly connected inside the digestion tank 2, and the side wall of the pipeline support 41 has a hollow structure.
[0037] Specifically, such as Figure 2 , Figure 3 As shown, the pipe support 41 is set as a hollow structure support, which can be fixed in the digestion tank 2, and a section of its upper end is reserved outside the digestion tank 2. The heat transfer oil contacts the spiral reaction tube 42 through the hollow part.
[0038] Furthermore, in an optional embodiment, the liquid circulation device 6 is configured as a circulation pump, which drives the heat transfer oil to circulate within the digestion tank 2 and the buffer tank 3.
[0039] In another alternative embodiment, the liquid circulation device 6 includes a liquid delivery wheel 61 and a motor 62 that drives the liquid delivery wheel 61 to rotate. The liquid delivery wheel 61 is rotatably connected to the circulation pipe 5.
[0040] Specifically, such as Figure 2 As shown, the infusion wheel 61 is rotatably connected to the circulation pipe 5. The motor 62 is linked to the infusion wheel 61 through the rotating belt 63. The motor 62 drives the infusion wheel 61 to rotate through the belt drive, thereby realizing the circulation of heat transfer oil in the digestion tank 2 and the buffer tank 3.
[0041] Furthermore, a liquid addition pipe 22 is provided at the top of the digestion tank 2 and / or the buffer tank 3, and a liquid outlet pipe 31 is provided at the bottom of the digestion tank 2 and / or the buffer tank 3. The liquid addition pipe 22 and the liquid outlet pipe 31 are respectively connected to the oil holding chamber 21, and control valves 32 are respectively connected to the liquid addition pipe 22 and the liquid outlet pipe 31.
[0042] Specifically, in one alternative embodiment, such as Figure 2 As shown, the liquid addition pipe 22 is connected to the top of the digestion tank 2, and the liquid outlet pipe 31 is connected to the bottom of the buffer tank 3. An outlet port 13 is provided at the bottom of the shell 1, through which the oil supply outlet pipe 31 extends. The outlet port 13 is concentric and coaxial with the outlet pipe 31, allowing the outlet pipe 31 to pass through. Heat transfer oil is added to the oil chamber 21 through the liquid addition pipe 22 and discharged through the outlet pipe 31. The opening and closing of the liquid addition port and outlet port are controlled by the control valve 32. This design allows for easy replacement of the heating medium, recyclability of the device, and low overall cost.
[0043] Furthermore, the outer walls of the digestion tank 2 and the buffer tank 3 are fixedly connected with multiple fixed support legs 8 located at the bottom of the digestion tank 2 and the buffer tank 3.
[0044] Specifically, such as Figure 2 As shown, multiple fixed support legs 8 are evenly distributed on the bottom surfaces of the digestion tank 2 and the buffer tank 3. In an optional embodiment, each fixed support leg 8 is threaded and fixedly connected to the bottom of the housing 1 by high-temperature resistant and corrosion-resistant screws. The bottom of the housing 1 is provided with support leg fixing holes 14 for screw installation, and the support leg fixing holes 14 are correspondingly provided with the fixed support legs 8. The screws enable the digestion tank 2 and the buffer tank 3 to be detachably fixed within the housing 1, while the support legs prevent the digestion tank 2 and the buffer tank 3 from contacting the housing 1, reducing heat loss. The side wall of the housing 1 is provided with a heat insulation layer, which further reduces heat loss and prevents personnel from being burned by contact with the housing 1.
[0045] Furthermore, the circulation pipe 5 is configured as a flexible hose, and a handle 23 is fixedly connected to the outer wall of the digestion tank 2.
[0046] Specifically, such as Figure 2 As shown, two handles 23 are provided, located on the top of the left and right sides of the digestion tank 2, respectively. The handles 23 allow for manual movement of the digestion tank 2. The circulation pipe 5 can be a high-temperature resistant metal flexible hose, such as a stainless steel flexible hose, with both ends detachably connected to the digestion tank 2 and the buffer tank 3, respectively.
[0047] Furthermore, it also includes a controller 9 and a temperature sensor 91. The temperature sensor 91 is installed in the digestion tank 2. The liquid circulation device 6, the temperature sensor 91, and the heating device 7 are respectively connected to the controller 9.
[0048] Specifically, such as Figure 2 As shown, the liquid circulation device 6 and the heating device 7 are controlled by the controller 9, and the temperature sensor 91 transmits the temperature signal of the heat transfer oil in the digestion tank 2 to the controller 9. In an optional embodiment, the controller 9 consists of a CNC box 92 and electrical wires 93. One end of the CNC box 92 is connected to a power source, and the temperature sensor 91 and the heating device 7 are connected via the electrical wires 93. A temperature setting device and a temperature display screen can be installed inside the CNC box 92. An electric heating rod or an electric heating tube can be selected as the heating device 7. Through CNC technology, the online digestion temperature and heating time can be precisely and continuously adjusted, providing the optimal online digestion temperature for different elemental forms and ensuring the stability of the digestion reaction effect.
[0049] Where there is no conflict, the above embodiments and features described herein can be combined with each other.
[0050] The above description is only a preferred embodiment of the present utility model and is not intended to limit the present utility model. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present utility model should be included within the protection scope of the present utility model.
Claims
1. A thermal digestion treatment device for elemental valence state transformation, characterized in that: The device includes a shell, a digestion tank, a buffer tank, a reaction pipeline, a circulation pipeline, a liquid circulation device, and a heating device. The digestion tank and the buffer tank each have an oil-containing cavity. The digestion tank and the buffer tank are installed inside the shell. The heating device is installed inside the oil-containing cavity. The reaction pipeline is located inside the digestion tank. At least two circulation pipelines are provided, one end of which is connected to the oil-containing cavity of the digestion tank, and the other end of which is connected to the oil-containing cavity of the buffer tank. The liquid circulation device is connected to either of the circulation pipelines to drive the liquid to circulate between the digestion tank and the buffer tank.
2. The thermal digestion treatment device for elemental valence state transformation according to claim 1, characterized in that: The reaction pipeline includes a pipeline support and a spiral reaction tube disposed within the pipeline support. The spiral reaction tube has a reaction liquid inlet and a reaction liquid outlet extending out of the pipeline support at both ends.
3. The thermal digestion treatment device for elemental valence state transformation according to claim 2, characterized in that: The top of the shell has an installation port located above the digestion tank. A movable cover plate is installed on the installation port, and the movable cover plate has an upper cover hole for the reaction liquid inlet and the reaction liquid outlet to extend out.
4. The thermal digestion treatment device for elemental valence state transformation according to claim 2, characterized in that: The pipeline support is fixedly connected inside the digestion tank, and the side wall of the pipeline support has a hollow structure.
5. The thermal digestion treatment device for elemental valence state transformation according to claim 1, characterized in that: The liquid circulation device includes a circulation pump.
6. The thermal digestion treatment apparatus for elemental valence state transformation according to claim 1, characterized in that: The liquid circulation device includes a liquid delivery wheel and a motor that drives the liquid delivery wheel to rotate. The liquid delivery wheel is rotatably connected to the circulation pipe.
7. The thermal digestion treatment apparatus for elemental valence state transformation according to claim 1, characterized in that: A liquid addition pipe is provided at the top of the digestion tank and / or the buffer tank, and a liquid outlet pipe is provided at the bottom of the digestion tank and / or the buffer tank. The liquid addition pipe and the liquid outlet pipe are respectively connected to the oil-containing cavity, and control valves are respectively connected to the liquid addition pipe and the liquid outlet pipe.
8. The thermal digestion treatment apparatus for elemental valence state transformation according to claim 1, characterized in that: The digestion tank and the buffer tank are fixedly connected to the outer wall by a plurality of fixed support legs located at the bottom of the digestion tank and the buffer tank.
9. The thermal digestion treatment apparatus for elemental valence state transformation according to claim 1, characterized in that: The circulation pipeline is configured as a flexible hose, and a handle is fixedly connected to the outer wall of the digestion tank.
10. The thermal digestion treatment apparatus for elemental valence state transformation according to any one of claims 1-9, characterized in that: It also includes a controller and a temperature sensor, the temperature sensor being disposed within the digestion tank, and the liquid circulation device, the temperature sensor, and the heating device being connected to the controller.